Startseite Research progress in preparation technology of micro and nano titanium alloy powder
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Research progress in preparation technology of micro and nano titanium alloy powder

  • Yan Jisen EMAIL logo , Wang Minghui , Zhang Tingan , Xie Fang , Zhang Xi , Zhao Ke , Liu Gang und Cheng Chu EMAIL logo
Veröffentlicht/Copyright: 30. April 2024
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Nanotechnology Reviews
Aus der Zeitschrift Nanotechnology Reviews Band 13 Heft 1

Abstract

Titanium alloys have excellent properties and are widely used in aerospace, medicine, chemical industry, and other fields. With the rapid development of the powder metallurgy and 3D printing industries, the demand for ultra-fine titanium alloy powders has increased significantly. It should be noted that the particle size of titanium alloy powders determines the application process. However, the high melting point of titanium and titanium alloys and the limitation of many factors, such as the prepared powders being easily contaminated by secondary pollution, make the preparation cost higher, which restricts their promotion and application. In this study, the research progress of micro and nano titanium alloy powder preparation process is described, and the existing problems of various processes are analyzed and discussed, and it is proposed that the direct reduction in TiO2 to obtain micro and nano titanium alloy powder is the key research direction in the future. In particular, the preparation of micro and nano titanium alloy powder by “calciothermic self-propagation process” has great industrial potential.

Keywords: titanium; atomization; electrolysis; reduction; self-propagation

1 Introduction

Titanium and titanium alloys have outstanding advantages such as high specific strength, corrosion resistance, non-magnetic, low damping, and good biocompatibility. They also have the characteristics of superconductivity, shape memory, and hydrogen storage. They are known as “all-around metals” [1,2,3]. Titanium is also listed as a strategic metal by countries worldwide. Titanium and titanium alloys are widely used in aerospace, marine engineering, medical industry, nuclear industry, chemical industry, energy, and other fields [4,5,6]. In 1791, the English priest Gregor realized that there was an unknown metal in the ilmenite. It was not until 1910, more than 100 years later, that the American chemist Hunter obtained 99.9% pure titanium by the metal Na reduction process. This is because titanium has a strong affinity with oxygen.

The particle size of titanium alloy powders is critical for the manufacturing process, such as 15–53 μm powder for selective laser melting, 15–45 μm powder for thermal spraying, 45–105 μm powder for e-beam printing, and 0–150 μm powder for powder metallurgy. At present, the atomization process and hydro-dehydration (HDH) process are the main production process for the commercial preparation of micro and nano titanium alloy powder. The atomization process mainly includes the inert gas atomization process, ultrasonic atomization (UA) process, centrifugal atomization (CA) process, and plasma atomization (PA) process. The titanium and titanium alloy powder produced by the atomization process has the advantages of good sphericity, narrow particle size distribution, and fewer satellite spheres. However, because the atomization process uses high-purity titanium as the raw material, the product price is high. Because titanium element easily reacts with oxygen, nitrogen, hydrogen, carbon, and other elements to cause pollution, secondary pollution is often caused in the production process of titanium and titanium alloy powder. When the atomization process is used to prepare powders, the process of melting titanium and titanium alloys is moving toward a crucible-free direction. The atomization process can regulate the particle size of the product by controlling the gas flow rate and electrode speed. HDH process has low requirements for products and lacks refining links in the process, so the product quality is low and cannot meet the requirements of the high-end industry. The HDH process can control the particle size of the product by ball milling titanium hydride powder. The mechanical alloy process is less used because of its long ball milling time and ease to pollute the products. At present, it is in the experimental stage. The preparation of titanium and titanium alloy powders by electrolysis has great application prospects. In particular, the university of science and technology Beijing (USTB) process is the closest process to commercialization, but the problem of electrolyte recycling still needs to be solved. Titanium and titanium alloy powders are directly prepared by using metal oxides such as TiO2 as raw materials, which avoids the chlorination process, and has a better environmental protection effect. In the process of metal thermal reduction, the particle size of the product can be controlled based on the particle size grade of the raw material, making it easier to produce products with micro and nano particle sizes. Compared to other processes, it has the characteristic of high flexibility.

In this study, the main preparation process of micro and nano titanium alloy powders is systematically described, and the advantages and disadvantages of each process are deeply analyzed. The future development trend of titanium and titanium alloys has prospected. It may play an enlightening role for relevant researchers.

2 Atomization process

The atomization process is a powder-making technology that disperses the molten titanium alloy melt under the action of external force and then rapidly solidifies to obtain a powder [7,8]. Atomization technology can increase the solid solubility of alloying elements, reduce the segregation of components in the titanium alloy, and eliminate harmful phases. High-quality titanium alloy powders are mostly produced by CA, UA, PA, etc. The alloy powders produced by this process have a narrow particle size distribution, high sphericity, and other advantages, but the production cost is higher [9,10].

With the help of high-speed airflow to break the metal stream, it can be dispersed only by overcoming the bonding force between the liquid metal atoms. The atomization method can produce titanium alloy powders with a uniform particle size distribution. The mean particle size of ungraded atomized TC4 titanium alloy powder is typically 50–60 μm. Generally, a water-cooled copper crucible is used to convert the syndicates, and then a high-speed inert gas stream is sprayed through a nozzle at the bottom of the crucible. The high-speed air stream sprays the metal solution into a spray shape, and the alloy droplets are quickly condensed to obtain a powder [11]. Due to the strong activity of titanium, there is almost no crucible that can avoid the contamination of titanium so far. At present, the inert gas atomization process is developing in the crucible-free direction. And in 1988, a device with an annual output of 11 t was built. In 1990, Leybold AG of Germany applied for a patent for making atomized titanium and titanium alloy using inert gas without crucible melting [12]. Japan’s Sumitomo Sitix company adopted a similar process and put it into production in 1994. Using the same process, China Bangzhen titanium industry company has developed a device with an annual output of 150 t titanium alloy powder and put it into use [13] (Figure 1).

Figure 1 Product morphology by inert gas atomization: (a) Ti powder; (b) Hollow Ti powder; and (c) TiAl3 powder [14,15].
Figure 1

Product morphology by inert gas atomization: (a) Ti powder; (b) Hollow Ti powder; and (c) TiAl3 powder [14,15].

At present, the inert gas atomization process has some disadvantages, such as low melting efficiency, large energy loss, low fine powder yield, high cost, large equipment investment, hollow ball, and so on. German researchers invented the vortex centrifugal cavity centrifugal-UA technology, which reduced the particle size of the atomized titanium powder and improved the yield of fine titanium powder [16]. Scholars from Shaanxi Normal University improved the atomization technology and obtained Ti6Al4V alloy powder with a spherical ratio of about 94%, with an average particle size of about 100 μm [17]. The CA process is a process of dispersing molten titanium alloy under the action of centrifugal force, forming spherical particles under the action of surface tension, and obtaining metal powder after rapid cooling. The product has a smooth surface, good fluidity, and narrow particle size distribution, but the yield of fine powder is low. The titanium alloy powder prepared by the PA process has uniform particle size distribution, high sphericity, good fluidity, no satellite spheres, and hollow spheres, but the cost is high, especially the high cost of the wire titanium alloy used [7,8] (Figure 2).

Figure 2 Morphology of Ti6Al4V alloy powder produced by CA [18].
Figure 2

Morphology of Ti6Al4V alloy powder produced by CA [18].

3 HDH process

The HDH process is to break the titanium alloy after hydrogen absorption by using the hydrogen embrittlement characteristics of titanium and then dehydrogenating it under vacuum to obtain titanium alloy powder. The advantages of this process are that the process is simple, the cost is low, and the requirements for raw materials are low, but the quality of the produced products is low, which cannot meet the requirements of high-end industries. For example, C.R.F. Azevedo et al. successfully prepared Ti6Al4V powder by this process, but the oxygen content increased from 1,484 to 5,200 ppm, the nitrogen content increased from 90 to 280 ppm, and the hydrogen content increased from 84 to 270 ppm [19].

HDH process is mainly based on the following reactions:

(1) 2 x Ti ( s ) + H 2 ( g ) = 2 x TiH X ( s ) + Q .

The reaction is reversible. When the temperature reaches 350°C, the reaction begins to proceed violently and absorbs a large amount of hydrogen [20]. When hydrogen atoms enter the titanium lattice, The TiH2 phase is formed, which reduces the impact toughness of titanium and makes it easy to mechanically break. Generally, the impact toughness of pure α-Ti is about 180 J/cm2. When w(H) = 0.015%, the impact toughness is reduced to 30 J/cm2. After the hydrogen absorption reaction, the mass of hydrogen absorption accounts for 3.8 ± 0.3% of the total mass [21]. The dehydrogenation reaction of titanium hydride is carried out in a high vacuum environment. The titanium hydride is heated, and reaction (1) proceeds to the left at this time, and titanium powder is obtained after the reaction is completed. Studies have shown that the decomposition starting temperature of titanium hydride is 510°C, and the decomposition process is divided into multiple stages [22,23]. To avoid the sintering of titanium powder in the dehydrogenation process, the temperature should not be too high.

Given the irregular particle size, low tap density, and poor fluidity of titanium powder produced by the HDH process, many scholars have carried out research on the spheronization process. For example, after the PCS system is used to shape the HDH titanium powder, an approximately spherical titanium powder can be obtained, which significantly improves the fluidity [24]. Some scholars use double grinding discs to shape titanium hydride powder and then dehydrogenate it, and finally obtain nearly spherical titanium powder, the fluidity of this powder can reach 26 s/50 g [25] (Figure 3).

Figure 3 (a) TiH2 powder and (b) Ti powder (HDH) [26,27].
Figure 3

(a) TiH2 powder and (b) Ti powder (HDH) [26,27].

4 Mechanical process

The mechanical preparation of titanium alloy powder is to grind the titanium powder together with other alloying element powders in a vacuum high-energy ball mill [28,29]. Through the long-term impact, collision, and extrusion between the powder particles and the grinding ball, the process of welding–fracture–welding between the powder particles continuously occurs during the grinding process, resulting in the diffusion between the powder atoms, and finally, the alloy powder is obtained. When titanium powder and aluminum–vanadium alloy powder are used as raw materials to prepare TiAlV alloy powder, the particle size of the powder gradually becomes finer with the extension of the ball-milling time, and the shape of the powder tends to be spherical. When the ball milling time reaches 60 h, the welding and mechanical crushing reach the equilibrium state. At this time, the powder particle size will tend to be stable [30]. Using titanium powder and other alloying element powders after 12 h of high-energy ball milling, ultra-fine size Ti35Nb2.5Sn5HA composite powder can be obtained, in which the α-Ti phase is completely transformed into the β-Ti phase [31].

5 Granulation-sintering-deoxygenation (GSD) process

The GSD process is a new process for preparing spherical titanium and titanium alloy powder proposed in 2016 [32,33,34]. The low-oxygen spherical titanium is prepared through three steps granulation, sintering, and deoxidation. This process uses waste titanium as raw material, and the process flow is shown in Figure 4. After deoxidation at 750°C for 12 h, the oxygen content in the raw material decreased to 0.10 wt%. The core of the process is the use of “low-temperature molten salt technology” to deoxidize spherical titanium powder [35]. This eutectic salt composed of CaCl2 (melting point 772°C) and KCl (melting point 770°C) has a melting point of 690°C. When the deoxidation reaction is performed at a temperature of 750°C, the salt is in a molten state, but the calcium and alloy powder is in a solid state, so sintering between powder particles can be avoided. Another reason for using the low-temperature deoxidation process is that the equilibrium oxygen content in metallic titanium will decrease as the temperature decreases, so the low-temperature deoxidation process can make the oxygen content in the titanium alloy lower. However, the surface of the spherical titanium alloy particles obtained by this process is not as smooth as the powder prepared by the atomization process. This is because the titanium particles do not undergo a molten state during the preparation process (condensation after melting can produce a very smooth surface).

Figure 4 Flow chart of the GSD process [32].
Figure 4

Flow chart of the GSD process [32].

The advantage of this process is that the source of raw materials is wide, and waste titanium can be used (after ball milling it is pulverized), and the final product has good fluidity. However, the entire process flow is long, the utilization rate of metallic calcium is low, and the eutectic molten salt used is difficult to recycle, which will have an impact on the environment.

6 Electrolytic process

6.1 Fray Farthing and Chen (FFC) process

Fray et al. proposed the idea of preparing metallic titanium powder by molten salt electrolysis (FFC) [36,37,38]. This process first proposed the use of electrolytic TiO2 to produce metallic titanium powder. Once this process was proposed, it attracted great attention from scholars around the world. The process uses sintered TiO2 as the cathode, graphite as the anode, and CaCl2 molten salt as the electrolyte. Electrolysis is carried out at a temperature of 850–950°C and a voltage of 3.0–3.2 V, and finally, metal titanium powder with a size of about 12 μm can be obtained. During the reaction, TiO2 ionizes oxygen ions at the cathode, and these oxygen ions are oxidized to oxygen at the anode or combined with graphite to generate CO2 gas [39,40]. The specific reaction of the two electrodes is as follows:

(2) Cathode : Ti O 2 + 4 e − = Ti + 2 O 2 − ,

(3) Anode : 2 O 2 − − 4 e − = O 2 , 2 O 2 − − 4 e − + C = C O 2 .

However, the FFC process uses a block of TiO2 as the cathode. TiO2 itself does not have electrical conductivity and conducts electricity only when electrons are obtained. Therefore, there are problems with uneven current and low electrolysis efficiency. The first use of a non-conductive material as a cathode for electrolysis is the biggest contribution of the FFC process. And there is no chlorination process in the whole generation process, which reduces the production cost, can realize continuous production, and the produced titanium powder is relatively pure.

Scholars used the FFC process to successfully prepare TiV, TiFe [41,42], TiZrNb [43], TiTaNb [44], and TiTaSn [45] alloy powders. Scholars have conducted a lot of investigations into the impurity of CaTiO3 in the FFC process. Recent studies have shown that using TiO as an electrode material instead of TiO2 (Ti3O5, Ti2O3) can avoid this problem [46,47,48]. However, in the past 20 years, technical problems such as low electrolytic current efficiency have not been solved, and the FFC process is still at the stage of experimental research (Figure 5).

Figure 5 Reaction principle of the FFC process.
Figure 5

Reaction principle of the FFC process.

6.2 OS process

To overcome the problems of the FFC process, Japanese scholars Ono et al. proposed the OS process in 2002 based on previous work [49,50]. The “OS” process uses graphite as the anode, stainless steel crucible as the cathode, and a mixture of CaCl2 and CaO as the electrolyte. Ca and TiO2 are added to the cathode crucible from the outside of the electrolytic reaction cell [51]. The electrolysis temperature during the deoxidation of this process is 877–917°C, and the electrolysis voltage is 2.8–3.2 V. The specific reaction of the two electrodes is as follows:

(4) Cathode : C a 2 + + 2 e − = Ca , Ti O 2 + 2 Ca = Ti + 2 O 2 − + 2 Ca 2 + ,

(5) Anode : 2 O 2 − − 4 e − + C = C O 2 .

Since the decomposition voltage of CaO is 1.66 V, which is lower than the electrolysis voltage and the decomposition voltage of calcium chloride, when the electrolysis starts, CaO is first electrolyzed to produce Ca to promote the reduction of TiO2 [52]. In this way, the current instability problem caused by direct electrolysis of TiO2 is avoided, and the electrolysis efficiency is improved. However, since TiO2 directly contacts the reducing agent, it is easy to enrich the impurities in Ti. Due to the small density of Ca, it is easy to float on the surface of molten salt and cause waste. In 2017, Ono et al. used 2 t of molten salt for experiments and achieved good results [53]. Some scholars have studied the electrochemical decomposition process of CaTiO3, and by optimizing the experimental conditions, titanium powder with an oxygen content of less than 0.42 wt% can be obtained [54,55,56] (Figure 6).

Figure 6 Reaction principle diagram of the OS process.
Figure 6

Reaction principle diagram of the OS process.

6.3 Electronically mediated reaction/Molten salt electrolysis (EMR/MSE) process

To overcome the problem of reducing agent impurities in the OS process that easily pollute the product Ti powder, Park et al. proposed the EMR/MSE process in 2004 [57]. This process follows the idea of using metal Ca as a reducing agent in the OS process but uses a separator to separate the reduction tank and the electrolytic tank. The biggest feature of this process is that TiO2 does not directly contact the reducing agent, and only uses molten CaCl2 to transfer electrons for reduction [58,59]. In the electrolysis process, the TiO2 powder is directly placed in the stainless steel mesh cage and immersed in the CaCl2 melt, and electron exchange occurs with the liquid calcium–nickel alloy. In the reduction tank, an electron exchange occurs between Ca2+ and the graphite anode to synthesize a calcium–nickel alloy. This process effectively controls the accumulation of impurities in the product, realizes that the reduction process of metallic titanium and the preparation process of the calcium–nickel alloy is carried out independently, and the energy utilization efficiency is improved [60,61]. The following reactions exist in the electrolysis process:

The reactions in the reduction tank (EMR) are

(6) Cathode : Ti O 2 + 4 e − = Ti + 2 O 2 − ,

(7) Anode : Ca − 2 e − = C a 2 + .

The reactions in the electrolytic tank (MSE) are

(8) Cathode : 2 O 2 − − 4 e − + C = C O 2 ,

(9) Anode : C a 2 + + 2 e − = Ca .

The titanium powder produced by the EMR/MSE process has high purity, but the equipment used is more complicated (Figure 7).

Figure 7 Reaction principle of EMR/MS process.
Figure 7

Reaction principle of EMR/MS process.

6.4 USTB process

Zhu et al. proposed the USTB process [62,63], that is, TiO2 is first mixed with carbon in the temperature range of 600–1,600°C for reduction and sintering to obtain a Ti–C–O composite material with good conductivity and use as an anode. The electrolysis temperature of this process is 400–1,000°C. During the electrolysis process, the carbon in the anode combines with oxygen and escapes in the form of CO and CO2. At the same time, the titanium in the anode enters the molten salt in the form of low-valent titanium ions. The titanium ions are reduced at the cathode to obtain pure titanium powder [64,65,66,67]. The process overcomes the technical problems of low electrolytic current density and low current efficiency commonly existing in electrolytic processes such as the FFC process and OS process. The current efficiency in the laboratory is generally maintained at about 90%, and the purity of metal titanium is more than 99.90%. It is great progress in the electrolytic titanium production process and has a good application prospect. The following reactions exist in the electrolysis process (Figure 8):

(10) Cathode : T i n + + n e − = Ti ,

(11) Anode : x O 2 − − 2 x e − + C = C O x , 2 O 2 − − 4 e − = O 2 .

Figure 8 Reaction principle of the USTB process.
Figure 8

Reaction principle of the USTB process.

7 Thermal reduction process

In addition to the electrolytic process for preparing metallic titanium, thermal reduction is another promising process for preparing metallic titanium. That is, titanium or titanium alloy powder is prepared by reducing titanium oxide or titanium chloride with alkali metal sodium or alkaline earth metal magnesium, calcium, etc. In particular, the preparation of titanium metal by direct reduction of titanium oxide using a reducing agent is the most promising low-cost clean process.

7.1 Mg thermal reduction process

The Kroll process is the classic process for producing titanium in the world. Although it has been around for nearly 90 years, no alternative process has been found so far. It first adds carbon to the raw material (titanium concentrate, high-titanium slag) and then chlorinates it to obtain titanium tetrachloride. After removing impurities, titanium tetrachloride is reduced with excess magnesium in the range of 800–950°C, and after vacuum distillation and purification, sponge-like metallic titanium is obtained [68,69,70]. The by-product MgCl2 can obtain Mg and Cl2 after electrolysis, which realizes the recycling of Mg and Cl2. The process uses purified TiCl4 as raw material and the Mg, MgCl2, and Ti in the final product are easy to separate and purify, so the product purity is high. However, this process has problems such as a long production cycle, discontinuous production, large energy consumption, serious pollution, and corroded equipment [71].

Given the current problems of the Kroll process, scholars have made improvements in different aspects. One is to improve the traditional operating process. Improve the MgCl2 electrolysis equipment, appropriately reduce the cell voltage and improve the current efficiency. The integrated reduction-distillation operation saves operating time and electricity [72,73]. The other is to improve the process. Aiming at the disadvantages of large investment and high energy consumption in the MgCl2 electrolysis process, a new process was proposed to obtain MgO and Cl2 by direct oxidation and pyrolysis of the by-product MgCl2 [74,75]. The TiRO process uses TiCl4 as raw material and Mg powder is used as a reducing agent for the reduction in a fluidized bed. Finally, Mg and MgCl2 are removed to obtain pure titanium powder. This process can produce titanium powder with an oxygen content of less than 0.25 wt%, but the particle size distribution range of titanium powder is wide [76,77] (Figure 9).

Figure 9 The morphology of titanium powder produced by the TiRO process [76].
Figure 9

The morphology of titanium powder produced by the TiRO process [76].

7.2 Na thermal reduction process

The Na thermal reduction process to prepare titanium sponge was proposed by Hunter et al. in 1910. It is similar to the Kroller process. First, TiCl4 is prepared, and then TiCl4 is reduced by metallic sodium to obtain sponge titanium. The by-product NaCl is electrolyzed to obtain Na and Cl2 for recycling. However, the price of Na is relatively high and it is not easy to store, and the product Ti has the disadvantages of poor casting performance and high chlorine content. Now it is seldom used [78].

The Armstrong process is an improvement of the Hunter process. Taking advantage of the low melting point of Na, TiCl4 vapor is sprayed into molten Na. Excess Na has the effect of cooling the reduction product and carrying the product into the separation process. After the product is crushed and sorted, commercial first-class titanium powder can be obtained. Changing the raw materials into TiCl4, VCl4, and AlCl3, we can obtain TiAlV alloy powder with an oxygen content as low as 0.2%. However, there are problems such as short equipment life, low separation efficiency, and serious Na loss [79,80]. This process is relatively simpler than the Hunter process, can be produced continuously, and has a lower reaction temperature. The product obtained is a high-purity powder without further purification. The product is suitable for rapid processing techniques such as powder metallurgy and injection molding. However, the life of production equipment is short, and the separation efficiency between products and by-products is low (Figure 10).

Figure 10 The morphology of Ti powder produced by the Armstrong process [80].
Figure 10

The morphology of Ti powder produced by the Armstrong process [80].

7.3 Ca thermal reduction process

Toru et al. proposed the preform reduction process (PRP) to prepare titanium powder. In the PRP process, TiO2, CaCl2, CaO, and the binder are thoroughly mixed with a stirrer and then pressed into a block (preformed), and then calcined at a temperature of 800°C for 1–3 h to remove the binder and moisture. Ca was used to reduce the calcined block at a temperature of 800–1,000°C for 6 h, wash, and dry to obtain titanium powder with a purity of 99%. The advantage of this process is that it reduces the contact area between the material and the container after performing, and reduces the chance of contamination of the material. However, it is necessary to place a certain amount of titanium sponge to purify the gas in the container. Compared with electrochemistry, the amount of molten salt used in this process is greatly reduced [81].

In the PRP process, the reactor needs to be welded and sealed before each experiment. After the experiment, the reactor needs to be destroyed to obtain the sample. The reactor structure is complicated and the process flow is long. Relevant scholars from Kunming University of Science and Technology designed a simpler reduction process based on the PRP process, eliminating the need for sintering and adding sponge titanium, and greatly shortening the reaction time. The particle size of the powder obtained ranges from 10 to 18 micron. The shape is irregular and does not contain any other metallic impurities [82,83,84,85]. However, during the experiment, it is necessary to add CaCl2 twice the mass of titanium dioxide as an additive. In theory, 3.34 g of calcium chloride is required for every 1 g of Ti produced. At present, there is still a lack of process for large-scale treatment of metal chlorides. In addition, there are problems such as the low utilization rate of calcium vapor and a large amount of calcium vapor condensing in the upper part of the reactor (Figures 11 and 12).

Figure 11 Schematic diagram of the principle of the PRP process.
Figure 11

Schematic diagram of the principle of the PRP process.

Figure 12 The morphology of Ti powder produced by the PRP process [81].
Figure 12

The morphology of Ti powder produced by the PRP process [81].

7.4 Hydrogen-assisted magnesiothermic reduction (HAMR) process

The preparation of Ti powder by the HAMR process involves the main steps: reduction of TiO2 and deoxidation of Ti–O solid solution [86,87,88]. Between these two steps, a heat treatment process is performed to control the specific surface area and particle size of the powder. The process flow is shown in Figure 13. TiO2, MgCl2, and Mg are mixed in a certain mass ratio and then put into a tube furnace for heating. The heating temperature is between 720 and 900°C and flowing pure H2 gas is introduced. The holding time is 3–12 h to obtain Ti–H–O solid solution. The obtained Ti–H–O solid solution powder is continuously heated to 750–1,000°C in the H2 atmosphere and kept for 5–240 min, and its specific surface area is reduced. The heat-treated Ti–H–O solid solution powder is continuously added to the mixture of MgCl2 and Mg, and heated to 650–750°C while H2 is continuously flowing for reduction to obtain titanium hydride powder. After the titanium hydride powder is dehydrogenated, titanium powder with an oxygen content of 1,000–2,000 ppm is obtained. The reaction by-product MgO and the remaining reducing agent Mg and MgCl2 molten salt need to be leached with clear water and dilute hydrochloric acid solution after each step of the operation.

Figure 13 Process flow of HAMR process [86].
Figure 13

Process flow of HAMR process [86].

The principle of preparing Ti powder by the HAMR process is to use the property of Ti–O solid solution to absorb hydrogen, form Ti–H–O solid solution in a hydrogen atmosphere, and then reduce the Ti–H–O solid solution to obtain Ti powder. Thermodynamic calculations show that the oxygen potential in Ti–H–O solid solution is lower than that in the Ti–O solid solution, which increases the thermodynamic driving force for the combination of magnesium and oxygen atoms in the Ti–H–O solid solution. In other words, hydrogen atoms destroy the stability of the Ti–O solid solution, making it easier to react with Mg [89,90,91].

7.5 Multi-stage deep reduction (MDR) process

It is difficult to use metal Mg alone to reduce the oxygen content in Ti to the application requirements. In order to obtain products with oxygen content meeting the standard, it is often necessary to use more metallic Ca as a reducing agent to further deoxidize.

Dou et al. [92,93,94] proposed a MDR process based on the thermodynamic characteristics of the gradual reduction of high-valent metal oxides, which used metal oxides (TiO2, V2O5) as raw materials. First, a self-propagating primary reduction reaction is carried out, and the obtained product is acid-leached to remove the MgO by-product to obtain the primary reduction product. Then, the primary reduction product is added to Ca for a deep reduction reaction, and finally, the deep reduction product is acid leached to remove the CaO by-product, washed and dried to obtain titanium and titanium alloy powder (Figure 14). Since the raw material (TiO2) used has a particle size of 200–500 nm, the product can have a particle size of less than 500 nm, but the high temperatures of the reaction process cause the products to sinter together. This process has the characteristics of low cost and clean production. This process successfully prepared titanium powder and Ti6Al4V alloy powder with an oxygen content of less than 0.3%. The 200 t/a titanium powder production line built by this process was put into production in December 2019 [95], laying a good foundation for the industrialization of low-cost and clean preparation of titanium and titanium alloy powder. Figure 15 is a microscopic picture of the product obtained by this process [96,97,98]. The team has recently attempted to combine self-spreading high temperature synthesis with electrodeposition for the preparation of low-oxygen titanium powders. The electrooxidation process replaced the calorimetric deep deoxidation process and reduced the oxygen content of the titanium powder to 0.121 wt% [99,100].

Figure 14 Flow chart of the MDR process [96].
Figure 14

Flow chart of the MDR process [96].

Figure 15 Product of the MDR process: (a) Ti and (b) Ti6Al4V [97,98].
Figure 15

Product of the MDR process: (a) Ti and (b) Ti6Al4V [97,98].

This process avoids the trouble caused by using TiCl4 as an intermediate product and does not have the difficulty that the molten salt cannot be recycled in the electrolysis process and the traditional thermal reduction process. Compared with traditional metal thermal reduction, the utilization rate of the reducing agent is improved, and the production cost is reduced. This process has great commercial value.

7.6 Two-stage aluminothermic reduction (TSAR) process

Zhao et al. first studied the process of preparing titanium by molten salt electrolysis. The results show that the current efficiency is low and the impurity content in the product is high [101,102,103]. In order to find a simple and effective method to make titanium, they also studied the process of thermit reduction of Na2TiF6 to make Ti/TiAl powder. A novel two-stage process, based on aluminothermic reduction of Na2TiF6, (TSAR) has been proposed to prepare Ti/Ti-Al powders by them [104,105,106].

First, Na2TiF6, NaF, and Al powder are uniformly mixed, then pressed into a block and finally put into the reactor for the thermite reduction reaction. After the reduction reaction is completed, distillation is performed to separate the product and cryolite. The metal product obtained by the reduction is loose agglomerates and easy to grind into powder. After grinding the reduction product to a fine powder with a particle size of less than 74 μm, Ti powder (O: 0.35 wt%), Ti3Al (O: 0.22 wt%), TiAl (O: 0.24 wt%), and TiAl3 (O: 0.4 wt%) can be obtained. The reactions involved are shown in formulas (12)–(15). The main components of the distillation product are Na3AlF6, Na5Al3F14, and a small amount of Na3TiF6, titanium-containing compounds, in which the titanium content is about 3–10%. The Ti-containing cryolite is subjected to secondary aluminothermic reduction, and finally, white titanium-free cryolite and Al-Ti alloy can be obtained. If the raw material is changed, Ti6Al4V alloy powder can be obtained by adding Al–V alloy powder [107].

(12) 12 N a 2 Ti F 6 + 16 Al = 12 Ti + 3 N a 3 Al F 6 + 3 N a 5 A l 3 F 14 + 4 Al F 3 ,

(13) 12 N a 2 Ti F 6 + 20 Al = 4 Ti 3 Al + 3 N a 3 Al F 6 + 3 N a 5 A l 3 F 14 + 4 Al F 3 ,

(14) 12 N a 2 Ti F 6 + 28 Al = 12 TiAl + 3 N a 3 Al F 6 + 3 N a 5 A l 3 F 14 + 4 Al F 3 ,

(15) 12 N a 2 Ti F 6 + 52 Al = 12 Ti Al 3 + 4 N a 3 Al F 6 + 3 N a 5 A l 3 F 14 + 4 Al F 3 .

The process is environmentally friendly and energy-saving, but the oxygen content in the final product is too high to be directly used Figure 16.

Figure 16 The morphology of (a) Ti and, (b) Ti6Al4V powder produced by TSAR process [103].
Figure 16

The morphology of (a) Ti and, (b) Ti6Al4V powder produced by TSAR process [103].

7.7 Calciothermic self-propagation (CSP) process

Dou et al. [108] proposed a new process of preparing Ti6Al4V powder using the CSP process. His team successfully prepared nearly spherical Ti6Al4V alloy powders with low-oxygen, which used Ca as a reducing agent and TiO2, V2O5, and Al as raw materials. This process has significant characteristics of simplicity, energy conservation, and efficiency. It is a breakthrough in the metal thermal reduction method. It breaks through the rule that additives must be used to prevent the generation of CaTiO3 in the traditional calcium thermal reduction process. During the reaction, TiO2 is reduced in liquid calcium. The argon pressure inside the reactor increases the boiling point of Ca above the melting point of Ti, and the metal titanium generated in liquid calcium spontaneously contracts into spheres. Based on the density difference, the CaO generated by the reaction spontaneously separates from the temporarily unreacted TiO2, weakening the kinetic conditions for the generation of CaTiO3 and avoiding its formation. The author adjusts the grain size and specific surface area of TiO2 through the roasting process, to optimize the reaction kinetics conditions. These methods effectively shorten the migration path of O2– within the TiO2 lattice, thereby maintaining the oxygen content in the product at 0.187 wt% when the reaction reaches equilibrium. The median particle size of the product is 15.28 μm [109]. In the 120 kg amplification experiment, the reaction process only ended in a few minutes. The excessively fast cooling rate enables the metal Ti droplets to maintain their original morphology of nearly spherical shape (Figure 17).

Figure 17 (a)–(c) SEM morphology analysis of the product, (d) TEM morphology of the product, and (e) TEM-EDS analysis of the product [109].
Figure 17

(a)–(c) SEM morphology analysis of the product, (d) TEM morphology of the product, and (e) TEM-EDS analysis of the product [109].

8 Comparison between various processes

Table 1 compares the advantages and disadvantages of the various process for preparing titanium and titanium alloy powder mentioned in the article. The atomization process, HDH process, and mechanical alloy process all use titanium and titanium alloy as raw materials, and still cannot get rid of the production link of TiCl4. The GSD process is the secondary processing and utilization of waste titanium materials, which has significant environmental protection significance. The electrolysis or thermal reduction process using TiO2 as a raw material avoids the problems of high energy consumption and high pollution caused by the process of preparing TiCl4 and will be the research focus of future scientific researchers.

Table 1

Comparison between various processes

Raw material Advantage Disadvantage
Atomization process Titanium and titanium alloys The particle size of the product is uniform High cost
HDH process Titanium and titanium alloys Low cost The product quality is low and the particle size is uneven
Mechanical process Titanium and titanium alloys Low cost Low product quality and long production cycle
GSD process Waste titanium Low cost Long cycle and difficult molten salt circulation
FFC process TiO2 Friendly environment and high-product quality Low electrolytic efficiency
OS process TiO2 Electrolytic current stability High Ca loss rate, difficulty in handling molten salt
EMR/MSE process TiO2 High product quality Complex equipment
USTB process TiO2 The current efficiency is high, and the intermediate amplification experiment is successful
MAHR process TiO2 The particle size of the product is uniform and easy to control Long production cycle
Kroll process TiCl4 Stable product quality High energy consumption, long production cycle
Hunter process TiCl4 The reducing agent Na has a lower melting point Energy-intensive, expensive sodiumreductant
PRP process TiO2 Produces with low oxygen content, high titanium slag can be used instead of TiO2 Ca utilization rate is low, and CaCl2 molten salt is difficult to recycle
MDR process TiO2 The quality of the product is high, and the 100 kg scale amplification experiment has been successful Irregular product morphology
STAR process Na2TiF6 Environmentally friendly and energy-saving High oxygen content
CSP process TiO2 The short production cycle, relatively regular product morphology, and low cost

It is proposed to evaluate different processes based on three indicators: product morphology, production cost, product quality, practical application potential, production efficiency, and semi-industrial scale experiment. The six indicators collectively determine whether this process has broad application prospects. Product quality is fundamental to the process. The morphology of the product determines its application field. The production cost means whether there will be new processes to replace it in the future. Production efficiency determines whether it can meet market demand. Semi-industrial scale experiments are the necessary path for technology to shift toward industrial production. From the comparison results in Figure 18, it can be seen that the CSP process has excellent prospects.

Figure 18 Comparison of the production among different processes.
Figure 18

Comparison of the production among different processes.

9 Conclusion and outlook

At present, the preparation process of high-quality micro and nano titanium alloy powder still uses the atomization process, but the problems of the atomization process are still not to be underestimated, such as the high production cost and the environmental pollution caused by the production process of sponge titanium. In addition, the atomization method has a low yield of fine particles and it is difficult to produce nanoscale titanium alloy powders. In order to expand the application range of titanium and titanium alloys, it is urgent to develop a low-cost micro and nano titanium alloy powder production process. TiO2 particle size can easily reach the nanoscale, how to use nanoscale TiO2 to produce low oxygen ultrafine titanium alloy powder is the focus of research. Therefore, the direct reduction of TiO2 as a raw material to produce micro and nano titanium alloy powder is the focus of future research, such as electrolysis, thermal reduction, and so on. Although the electrolysis process has been proposed at the beginning of this century, the problems of the large consumption of molten salt, the difficulty of recycling the molten salt, and the difficulty of separating the product from the molten salt still cannot be solved well, which limits the further development of the electrolysis process. The metal thermal reduction process, which uses metal with stronger oxygen-binding force to directly reduce TiO2 and adds other metal oxides as alloying elements, is the most promising type of process for commercial application. In the process of metal thermal reduction, the particle size of raw materials can be smoothly “inherited” to produce products, which is a very promising process for producing micro and nano scale titanium alloy powders. However, the metal thermal reduction process requires an acidic solution to separate the by-products, and the effective treatment of the waste liquid caused by the production process will make the metal thermal reduction process more prospective commercially.

Aerospace vehicles and transportation are the two main directions for future applications of titanium alloys, and high production costs have always been a huge problem for the titanium industry. Replacing important additive elements in titanium alloys such as V, Mo, and Nb and other high-priced elements with low-priced additive elements is an option. However, it does not solve the problem fundamentally. Due to the high melting point of titanium, and with oxygen, carbon, nitrogen, and other atoms of the affinity of the product contamination, these two characteristics of the product preparation process are very demanding, requiring great vacuum and ambient temperature. The use of titanium sponge as a raw material for the preparation of micro and nano titanium alloy powders increases the production cost and also has the potential threat of secondary pollution. Therefore, the use of titanium oxide direct reduction to produce powders is the main research direction for the preparation of micro and nano titanium alloy powders in short flow in recent years. The use of titanium oxides for the preparation of micro and nano titanium alloy powders is still faced with the problem of incomplete removal of oxygen and contamination of the product with impurity elements. This requires that the reaction process should be fast enough so that the impurity elements do not have time to react with the titanium elements. At the same time, the process and equipment must be simple to reduce the cost of maintenance and production costs. CSP method utilizes the principle of calcium-thermal self-propagating reaction to prepare micro and nano titanium alloy powders, with a rapid reaction process, low energy consumption, low oxygen content in the product, and the product morphology is regular, which has a great potential for commercialization.

  1. Funding information: This work was supported by the Natural Science Foundation of China (Grant No. 52204359); Scientific and Technological Project of Nanyang (23KJGG017); The Basic and Frontier Technology Research Project of Nanyang (23JCQY2013); Henan Natural Science Foundation Project (232300420326); The Key Specialized Research & Development and Promotion Project (Scientific and Technological Project) of Henan Province (232102221022; 232102230049).

  2. Author contributions: All authors have accepted responsibility for the entire content of this manuscript and approved its submission.

  3. Conflict of interest: The authors state no conflict of interest.

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Received: 2023-05-18
Revised: 2024-03-27
Accepted: 2024-03-28
Published Online: 2024-04-30

© 2024 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

Artikel in diesem Heft

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https://doi.org/10.1515/ntrev-2024-0016
Schlagwörter für diesen Artikel
titanium; atomization; electrolysis; reduction; self-propagation
Creative Commons
BY 4.0

Artikel in diesem Heft

  1. Research Articles
  2. Tension buckling and postbuckling of nanocomposite laminated plates with in-plane negative Poisson’s ratio
  3. Polyvinylpyrrolidone-stabilised gold nanoparticle coatings inhibit blood protein adsorption
  4. Energy and mass transmission through hybrid nanofluid flow passing over a spinning sphere with magnetic effect and heat source/sink
  5. Surface treatment with nano-silica and magnesium potassium phosphate cement co-action for enhancing recycled aggregate concrete
  6. Numerical investigation of thermal radiation with entropy generation effects in hybrid nanofluid flow over a shrinking/stretching sheet
  7. Enhancing the performance of thermal energy storage by adding nano-particles with paraffin phase change materials
  8. Using nano-CaCO3 and ceramic tile waste to design low-carbon ultra high performance concrete
  9. Numerical analysis of thermophoretic particle deposition in a magneto-Marangoni convective dusty tangent hyperbolic nanofluid flow – Thermal and magnetic features
  10. Dual numerical solutions of Casson SA–hybrid nanofluid toward a stagnation point flow over stretching/shrinking cylinder
  11. Single flake homo p–n diode of MoTe2 enabled by oxygen plasma doping
  12. Electrostatic self-assembly effect of Fe3O4 nanoparticles on performance of carbon nanotubes in cement-based materials
  13. Multi-scale alignment to buried atom-scale devices using Kelvin probe force microscopy
  14. Antibacterial, mechanical, and dielectric properties of hydroxyapatite cordierite/zirconia porous nanocomposites for use in bone tissue engineering applications
  15. Time-dependent Darcy–Forchheimer flow of Casson hybrid nanofluid comprising the CNTs through a Riga plate with nonlinear thermal radiation and viscous dissipation
  16. Durability prediction of geopolymer mortar reinforced with nanoparticles and PVA fiber using particle swarm optimized BP neural network
  17. Utilization of zein nano-based system for promoting antibiofilm and anti-virulence activities of curcumin against Pseudomonas aeruginosa
  18. Antibacterial effect of novel dental resin composites containing rod-like zinc oxide
  19. An extended model to assess Jeffery–Hamel blood flow through arteries with iron-oxide (Fe2O3) nanoparticles and melting effects: Entropy optimization analysis
  20. Comparative study of copper nanoparticles over radially stretching sheet with water and silicone oil
  21. Cementitious composites modified by nanocarbon fillers with cooperation effect possessing excellent self-sensing properties
  22. Confinement size effect on dielectric properties, antimicrobial activity, and recycling of TiO2 quantum dots via photodegradation processes of Congo red dye and real industrial textile wastewater
  23. Biogenic silver nanoparticles of Moringa oleifera leaf extract: Characterization and photocatalytic application
  24. Novel integrated structure and function of Mg–Gd neutron shielding materials
  25. Impact of multiple slips on thermally radiative peristaltic transport of Sisko nanofluid with double diffusion convection, viscous dissipation, and induced magnetic field
  26. Magnetized water-based hybrid nanofluid flow over an exponentially stretching sheet with thermal convective and mass flux conditions: HAM solution
  27. A numerical investigation of the two-dimensional magnetohydrodynamic water-based hybrid nanofluid flow composed of Fe3O4 and Au nanoparticles over a heated surface
  28. Development and modeling of an ultra-robust TPU-MWCNT foam with high flexibility and compressibility
  29. Effects of nanofillers on the physical, mechanical, and tribological behavior of carbon/kenaf fiber–reinforced phenolic composites
  30. Polymer nanocomposite for protecting photovoltaic cells from solar ultraviolet in space
  31. Study on the mechanical properties and microstructure of recycled concrete reinforced with basalt fibers and nano-silica in early low-temperature environments
  32. Synergistic effect of carbon nanotubes and polyvinyl alcohol on the mechanical performance and microstructure of cement mortar
  33. CFD analysis of paraffin-based hybrid (Co–Au) and trihybrid (Co–Au–ZrO2) nanofluid flow through a porous medium
  34. Forced convective tangent hyperbolic nanofluid flow subject to heat source/sink and Lorentz force over a permeable wedge: Numerical exploration
  35. Physiochemical and electrical activities of nano copper oxides synthesised via hydrothermal method utilising natural reduction agents for solar cell application
  36. A homotopic analysis of the blood-based bioconvection Carreau–Yasuda hybrid nanofluid flow over a stretching sheet with convective conditions
  37. In situ synthesis of reduced graphene oxide/SnIn4S8 nanocomposites with enhanced photocatalytic performance for pollutant degradation
  38. A coarse-grained Poisson–Nernst–Planck model for polyelectrolyte-modified nanofluidic diodes
  39. A numerical investigation of the magnetized water-based hybrid nanofluid flow over an extending sheet with a convective condition: Active and passive controls of nanoparticles
  40. The LyP-1 cyclic peptide modified mesoporous polydopamine nanospheres for targeted delivery of triptolide regulate the macrophage repolarization in atherosclerosis
  41. Synergistic effect of hydroxyapatite-magnetite nanocomposites in magnetic hyperthermia for bone cancer treatment
  42. The significance of quadratic thermal radiative scrutinization of a nanofluid flow across a microchannel with thermophoretic particle deposition effects
  43. Ferromagnetic effect on Casson nanofluid flow and transport phenomena across a bi-directional Riga sensor device: Darcy–Forchheimer model
  44. Performance of carbon nanomaterials incorporated with concrete exposed to high temperature
  45. Multicriteria-based optimization of roller compacted concrete pavement containing crumb rubber and nano-silica
  46. Revisiting hydrotalcite synthesis: Efficient combined mechanochemical/coprecipitation synthesis to design advanced tunable basic catalysts
  47. Exploration of irreversibility process and thermal energy of a tetra hybrid radiative binary nanofluid focusing on solar implementations
  48. Effect of graphene oxide on the properties of ternary limestone clay cement paste
  49. Improved mechanical properties of graphene-modified basalt fibre–epoxy composites
  50. Sodium titanate nanostructured modified by green synthesis of iron oxide for highly efficient photodegradation of dye contaminants
  51. Green synthesis of Vitis vinifera extract-appended magnesium oxide NPs for biomedical applications
  52. Differential study on the thermal–physical properties of metal and its oxide nanoparticle-formed nanofluids: Molecular dynamics simulation investigation of argon-based nanofluids
  53. Heat convection and irreversibility of magneto-micropolar hybrid nanofluids within a porous hexagonal-shaped enclosure having heated obstacle
  54. Numerical simulation and optimization of biological nanocomposite system for enhanced oil recovery
  55. Laser ablation and chemical vapor deposition to prepare a nanostructured PPy layer on the Ti surface
  56. Cilostazol niosomes-loaded transdermal gels: An in vitro and in vivo anti-aggregant and skin permeation activity investigations towards preparing an efficient nanoscale formulation
  57. Linear and nonlinear optical studies on successfully mixed vanadium oxide and zinc oxide nanoparticles synthesized by sol–gel technique
  58. Analytical investigation of convective phenomena with nonlinearity characteristics in nanostratified liquid film above an inclined extended sheet
  59. Optimization method for low-velocity impact identification in nanocomposite using genetic algorithm
  60. Analyzing the 3D-MHD flow of a sodium alginate-based nanofluid flow containing alumina nanoparticles over a bi-directional extending sheet using variable porous medium and slip conditions
  61. A comprehensive study of laser irradiated hydrothermally synthesized 2D layered heterostructure V2O5(1−x)MoS2(x) (X = 1–5%) nanocomposites for photocatalytic application
  62. Computational analysis of water-based silver, copper, and alumina hybrid nanoparticles over a stretchable sheet embedded in a porous medium with thermophoretic particle deposition effects
  63. A deep dive into AI integration and advanced nanobiosensor technologies for enhanced bacterial infection monitoring
  64. Effects of normal strain on pyramidal I and II 〈c + a〉 screw dislocation mobility and structure in single-crystal magnesium
  65. Computational study of cross-flow in entropy-optimized nanofluids
  66. Significance of nanoparticle aggregation for thermal transport over magnetized sensor surface
  67. A green and facile synthesis route of nanosize cupric oxide at room temperature
  68. Effect of annealing time on bending performance and microstructure of C19400 alloy strip
  69. Chitosan-based Mupirocin and Alkanna tinctoria extract nanoparticles for the management of burn wound: In vitro and in vivo characterization
  70. Electrospinning of MNZ/PLGA/SF nanofibers for periodontitis
  71. Photocatalytic degradation of methylene blue by Nd-doped titanium dioxide thin films
  72. Shell-core-structured electrospinning film with sequential anti-inflammatory and pro-neurogenic effects for peripheral nerve repairment
  73. Flow and heat transfer insights into a chemically reactive micropolar Williamson ternary hybrid nanofluid with cross-diffusion theory
  74. One-pot fabrication of open-spherical shapes based on the decoration of copper sulfide/poly-O-amino benzenethiol on copper oxide as a promising photocathode for hydrogen generation from the natural source of Red Sea water
  75. A penta-hybrid approach for modeling the nanofluid flow in a spatially dependent magnetic field
  76. Advancing sustainable agriculture: Metal-doped urea–hydroxyapatite hybrid nanofertilizer for agro-industry
  77. Utilizing Ziziphus spina-christi for eco-friendly synthesis of silver nanoparticles: Antimicrobial activity and promising application in wound healing
  78. Plant-mediated synthesis, characterization, and evaluation of a copper oxide/silicon dioxide nanocomposite by an antimicrobial study
  79. Effects of PVA fibers and nano-SiO2 on rheological properties of geopolymer mortar
  80. Investigating silver and alumina nanoparticles’ impact on fluid behavior over porous stretching surface
  81. Potential pharmaceutical applications and molecular docking study for green fabricated ZnO nanoparticles mediated Raphanus sativus: In vitro and in vivo study
  82. Effect of temperature and nanoparticle size on the interfacial layer thickness of TiO2–water nanofluids using molecular dynamics
  83. Characteristics of induced magnetic field on the time-dependent MHD nanofluid flow through parallel plates
  84. Flexural and vibration behaviours of novel covered CFRP composite joints with an MWCNT-modified adhesive
  85. Experimental research on mechanically and thermally activation of nano-kaolin to improve the properties of ultra-high-performance fiber-reinforced concrete
  86. Analysis of variable fluid properties for three-dimensional flow of ternary hybrid nanofluid on a stretching sheet with MHD effects
  87. Biodegradability of corn starch films containing nanocellulose fiber and thymol
  88. Toxicity assessment of copper oxide nanoparticles: In vivo study
  89. Some measures to enhance the energy output performances of triboelectric nanogenerators
  90. Reinforcement of graphene nanoplatelets on water uptake and thermomechanical behaviour of epoxy adhesive subjected to water ageing conditions
  91. Optimization of preparation parameters and testing verification of carbon nanotube suspensions used in concrete
  92. Max-phase Ti3SiC2 and diverse nanoparticle reinforcements for enhancement of the mechanical, dynamic, and microstructural properties of AA5083 aluminum alloy via FSP
  93. Advancing drug delivery: Neural network perspectives on nanoparticle-mediated treatments for cancerous tissues
  94. PEG-PLGA core–shell nanoparticles for the controlled delivery of picoplatin–hydroxypropyl β-cyclodextrin inclusion complex in triple-negative breast cancer: In vitro and in vivo study
  95. Conduction transportation from graphene to an insulative polymer medium: A novel approach for the conductivity of nanocomposites
  96. Review Articles
  97. Developments of terahertz metasurface biosensors: A literature review
  98. Overview of amorphous carbon memristor device, modeling, and applications for neuromorphic computing
  99. Advances in the synthesis of gold nanoclusters (AuNCs) of proteins extracted from nature
  100. A review of ternary polymer nanocomposites containing clay and calcium carbonate and their biomedical applications
  101. Recent advancements in polyoxometalate-functionalized fiber materials: A review
  102. Special contribution of atomic force microscopy in cell death research
  103. A comprehensive review of oral chitosan drug delivery systems: Applications for oral insulin delivery
  104. Cellular senescence and nanoparticle-based therapies: Current developments and perspectives
  105. Cyclodextrins-block copolymer drug delivery systems: From design and development to preclinical studies
  106. Micelle-based nanoparticles with stimuli-responsive properties for drug delivery
  107. Critical assessment of the thermal stability and degradation of chemically functionalized nanocellulose-based polymer nanocomposites
  108. Research progress in preparation technology of micro and nano titanium alloy powder
  109. Nanoformulations for lysozyme-based additives in animal feed: An alternative to fight antibiotic resistance spread
  110. Incorporation of organic photochromic molecules in mesoporous silica materials: Synthesis and applications
  111. A review on modeling of graphene and associated nanostructures reinforced concrete
  112. A review on strengthening mechanisms of carbon quantum dots-reinforced Cu-matrix nanocomposites
  113. Review on nanocellulose composites and CNFs assembled microfiber toward automotive applications
  114. Nanomaterial coating for layered lithium rich transition metal oxide cathode for lithium-ion battery
  115. Application of AgNPs in biomedicine: An overview and current trends
  116. Nanobiotechnology and microbial influence on cold adaptation in plants
  117. Hepatotoxicity of nanomaterials: From mechanism to therapeutic strategy
  118. Applications of micro-nanobubble and its influence on concrete properties: An in-depth review
  119. A comprehensive systematic literature review of ML in nanotechnology for sustainable development
  120. Exploiting the nanotechnological approaches for traditional Chinese medicine in childhood rhinitis: A review of future perspectives
  121. Twisto-photonics in two-dimensional materials: A comprehensive review
  122. Current advances of anticancer drugs based on solubilization technology
  123. Recent process of using nanoparticles in the T cell-based immunometabolic therapy
  124. Future prospects of gold nanoclusters in hydrogen storage systems and sustainable environmental treatment applications
  125. Preparation, types, and applications of one- and two-dimensional nanochannels and their transport properties for water and ions
  126. Microstructural, mechanical, and corrosion characteristics of Mg–Gd–x systems: A review of recent advancements
  127. Functionalized nanostructures and targeted delivery systems with a focus on plant-derived natural agents for COVID-19 therapy: A review and outlook
  128. Mapping evolution and trends of cell membrane-coated nanoparticles: A bibliometric analysis and scoping review
  129. Nanoparticles and their application in the diagnosis of hepatocellular carcinoma
  130. In situ growth of carbon nanotubes on fly ash substrates
  131. Structural performance of boards through nanoparticle reinforcement: An advance review
  132. Reinforcing mechanisms review of the graphene oxide on cement composites
  133. Seed regeneration aided by nanomaterials in a climate change scenario: A comprehensive review
  134. Surface-engineered quantum dot nanocomposites for neurodegenerative disorder remediation and avenue for neuroimaging
  135. Graphitic carbon nitride hybrid thin films for energy conversion: A mini-review on defect activation with different materials
  136. Nanoparticles and the treatment of hepatocellular carcinoma
  137. Special Issue on Advanced Nanomaterials and Composites for Energy Conversion and Storage - Part II
  138. Highly safe lithium vanadium oxide anode for fast-charging dendrite-free lithium-ion batteries
  139. Recent progress in nanomaterials of battery energy storage: A patent landscape analysis, technology updates, and future prospects
  140. Special Issue on Advanced Nanomaterials for Carbon Capture, Environment and Utilization for Energy Sustainability - Part II
  141. Calcium-, magnesium-, and yttrium-doped lithium nickel phosphate nanomaterials as high-performance catalysts for electrochemical water oxidation reaction
  142. Low alkaline vegetation concrete with silica fume and nano-fly ash composites to improve the planting properties and soil ecology
  143. Mesoporous silica-grafted deep eutectic solvent-based mixed matrix membranes for wastewater treatment: Synthesis and emerging pollutant removal performance
  144. Electrochemically prepared ultrathin two-dimensional graphitic nanosheets as cathodes for advanced Zn-based energy storage devices
  145. Enhanced catalytic degradation of amoxicillin by phyto-mediated synthesised ZnO NPs and ZnO-rGO hybrid nanocomposite: Assessment of antioxidant activity, adsorption, and thermodynamic analysis
  146. Incorporating GO in PI matrix to advance nanocomposite coating: An enhancing strategy to prevent corrosion
  147. Synthesis, characterization, thermal stability, and application of microporous hyper cross-linked polyphosphazenes with naphthylamine group for CO2 uptake
  148. Engineering in ceramic albite morphology by the addition of additives: Carbon nanotubes and graphene oxide for energy applications
  149. Nanoscale synergy: Optimizing energy storage with SnO2 quantum dots on ZnO hexagonal prisms for advanced supercapacitors
  150. Aging assessment of silicone rubber materials under corona discharge accompanied by humidity and UV radiation
  151. Tuning structural and electrical properties of Co-precipitated and Cu-incorporated nickel ferrite for energy applications
  152. Sodium alginate-supported AgSr nanoparticles for catalytic degradation of malachite green and methyl orange in aqueous medium
  153. An environmentally greener and reusability approach for bioenergy production using Mallotus philippensis (Kamala) seed oil feedstock via phytonanotechnology
  154. Micro-/nano-alumina trihydrate and -magnesium hydroxide fillers in RTV-SR composites under electrical and environmental stresses
  155. Mechanism exploration of ion-implanted epoxy on surface trap distribution: An approach to augment the vacuum flashover voltages
  156. Nanoscale engineering of semiconductor photocatalysts boosting charge separation for solar-driven H2 production: Recent advances and future perspective
  157. Excellent catalytic performance over reduced graphene-boosted novel nanoparticles for oxidative desulfurization of fuel oil
  158. Special Issue on Advances in Nanotechnology for Agriculture
  159. Deciphering the synergistic potential of mycogenic zinc oxide nanoparticles and bio-slurry formulation on phenology and physiology of Vigna radiata
  160. Nanomaterials: Cross-disciplinary applications in ornamental plants
  161. Special Issue on Catechol Based Nano and Microstructures
  162. Polydopamine films: Versatile but interface-dependent coatings
  163. In vitro anticancer activity of melanin-like nanoparticles for multimodal therapy of glioblastoma
  164. Poly-3,4-dihydroxybenzylidenhydrazine, a different analogue of polydopamine
  165. Chirality and self-assembly of structures derived from optically active 1,2-diaminocyclohexane and catecholamines
  166. Advancing resource sustainability with green photothermal materials: Insights from organic waste-derived and bioderived sources
  167. Bioinspired neuromelanin-like Pt(iv) polymeric nanoparticles for cancer treatment
  168. Special Issue on Implementing Nanotechnology for Smart Healthcare System
  169. Intelligent explainable optical sensing on Internet of nanorobots for disease detection
  170. Special Issue on Green Mono, Bi and Tri Metallic Nanoparticles for Biological and Environmental Applications
  171. Tracking success of interaction of green-synthesized Carbopol nanoemulgel (neomycin-decorated Ag/ZnO nanocomposite) with wound-based MDR bacteria
  172. Green synthesis of copper oxide nanoparticles using genus Inula and evaluation of biological therapeutics and environmental applications
  173. Biogenic fabrication and multifunctional therapeutic applications of silver nanoparticles synthesized from rose petal extract
  174. Metal oxides on the frontlines: Antimicrobial activity in plant-derived biometallic nanoparticles
  175. Controlling pore size during the synthesis of hydroxyapatite nanoparticles using CTAB by the sol–gel hydrothermal method and their biological activities
  176. Special Issue on State-of-Art Advanced Nanotechnology for Healthcare
  177. Applications of nanomedicine-integrated phototherapeutic agents in cancer theranostics: A comprehensive review of the current state of research
  178. Smart bionanomaterials for treatment and diagnosis of inflammatory bowel disease
  179. Beyond conventional therapy: Synthesis of multifunctional nanoparticles for rheumatoid arthritis therapy
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Heruntergeladen am 3.10.2025 von https://www.degruyterbrill.com/document/doi/10.1515/ntrev-2024-0016/html?srsltid=AfmBOoofCUNCZjNUZ1e4jglr6yAlazF4fh9Uaw6TJPPRuY5RMQhkh8L-
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