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Oxygen plasma assisted room temperature bonding for manufacturing SU-8 polymer micro/nanoscale nozzle

  • Ran Guo , Xuan Li EMAIL logo , Weilong Niu EMAIL logo and Jianbo Feng
Published/Copyright: September 1, 2023
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Nanotechnology Reviews
From the journal Nanotechnology Reviews Volume 12 Issue 1

Abstract

Electrohydrodynamic-jet (E-jet) printing is an on-demand additive manufacturing method that allows various functional materials to be directly deposited on the target substrate. Many theoretical and experimental results indicate that E-jet has scale effect, and reducing the inner diameter of the nozzle can effectively improve printing resolution. Herein, a method for fabricating SU-8 polymer micro/nanoscale nozzle by oxygen plasma assisted room temperature bonding was proposed. It can prevent channel deformation and blockage caused by excessive bonding temperature. The surface modification parameters of silicon nano-mold were optimized, the influence of hot embossing parameters on the replication precision of nano patterns was investigated, the effect of UV lithography parameters on the micro and nanochannel was analyzed, the relationship between the oxygen plasma treatment parameters on the contact angle of SU-8 was revealed, the influence of bonding pressure on the morphology of the nanochannel was discussed, and the bonding principle at room temperature was deeply analyzed. This method can fabricate SU-8 polymer micro/nanoscale nozzle with low cost and high precision, and provide a new idea for the realization of room temperature bonding to manufacture SU-8 polymer nozzle.

Keywords: room temperature bonding; polymer; oxygen plasma treatment

1 Introduction

The development of nanomanufacturing technology is critical for the advancement of micro nanotechnology and nanoscience. According to the white paper “Nanoscience and Technology: Present Situation and Expectations for 2019,” the worldwide economic effect of nanotechnology would approach US$125 billion per year by 2024. Electrohydrodynamic-jet (E-jet) printing is a method that uses solution ink to directly print micro/nano images by using an electric field force to drive solution ink through the nozzle to form an incredibly thin jet. This method does not require pricey experimental apparatus, clean rooms, or extremely clean vacuum settings. It can directly print different functional materials onto the target substrate and is made with on-demand additions, enabling low-cost direct printing of high-resolution micro/nano graphics. It may be used to make field-effect transistors [1,2,3], organic light-emitting diodes [4,5,6], flexible electronic devices [7,8,9], and biochemical printing [10,11,12].

Many theoretical analysis and practical results in recent years have revealed that the inner diameter of the nozzle is the most important element influencing printing resolution. The scale effect of electrohydraulic power jet printing can produce droplets considerably smaller than the inner diameter of the nozzle. Reducing the inner diameter of nozzle can significantly increase printing resolution [13,14,15]. At present, many different methods of nozzle manufacturing have been reported. Louwerse et al. [16] prepared a metal nozzle of 1 μm by femtosecond laser method. However, this method requires expensive experimental equipment and therefore cannot be widely used [17,18,19]. Twente University reported that silicon nano-nozzle with a width of 4 μm and a depth of 200 nm can be manufactured by using low-pressure chemical vapor deposition, photolithography, and wet etching methods [20]. However, this method has a complex manufacturing process and low productivity. The Belder research group at the University of Leipzig in Germany prepared a glass nozzle with an inner diameter of 10 μm and used computer numerical control milling to create a cone, pulled the heated pin and sharpened the nozzle using wet etching [21]. Lee et al. [22] manufactured a glass nozzle with an inner diameter of 7 μm using a Sutter drawing machine and heating stretching method. A novel micro injection device was constructed by fusing glass micro-nozzle with microvalve based on polydimethylsiloxane (PDMS). At present, quartz glass nozzles are mainly used to generate electrohydrodynamic fluid jets, while the smallest quartz glass nozzle has an inner diameter of 300 nm and was produced by World Precision Instruments in the United States. The quartz glass nozzle was obtained by heating and stretching, and it was difficult to control the inner diameter of the nozzle during the stretching process, making it difficult to produce repeatable nozzles.

The technology, which employs UV lithography as the main process method to graphically prepare polymer nozzles on polymer materials, offers the advantages of simple process, low cost, and flexible and controllable pattern size. Therefore, polymer nozzle devices were considered as potential low-cost, high-throughput E-jet nozzle devices. However, due to the diffraction effect that occurs during the exposure process, the nozzle channel was only at the micron level. Many researchers make polymer nano-nozzles using a combination of thermal imprinting and ultraviolet lithography. Sun et al. [23] created silicon nano-molds through inclined evaporation method, copied the nano patterns on the silicon nano-molds onto the polymer material using hot embossing method to obtain nozzle nano-channels, and finally obtained a sealed polymer nozzle device using thermal bonding process. However, due to the large size of the silicon nano-mold, only a SU-8 polymer nozzle with a width of 380 nm was obtained. The Yin research group of Jilin University cleverly utilized the nano cracks formed by thermal and volume shrinkage caused by stress release during the development of SU-8 photoresist to prepare SU-8 polymer nozzle with a width of 250 nm [24]. This method is simple in process, but difficult to control in size and low in repeatability.

Here we propose a method for obtaining SU-8 polymer micro/nanoscale nozzle through room temperature bonding. By preparing silicon nano molds to obtain nanostructures, the nanostructures were replicated into polymer materials using a hot embossing process. Finally, oxygen plasma assisted room temperature bonding was used to seal the micro and nano channels of the nozzle. The effect of oxygen plasma treatment parameters on the surface contact angle of SU-8 photoresist was investigated, and also, the influence of UV lithography process parameters on the morphology of micro and nano channels was investigated. It can prevent channel deformation and blockage caused by excessive bonding temperature. This method has the advantage of low cost and high repeatability. The manufacturing of micro/nanoscale nozzle devices will greatly promote the research on the transport characteristics of E-jet fluid in nanoscale channels, and further develop applications based on E-jet.

2 Experiments

2.1 Fabrication of concave silicon nano-mold

The concave silicon nano-mold was fabricated by the side-etch lift-off method. The fabrication process was simple and the specific process has been described in detail in previous paper [25], so it is briefly explained here. The technological process is shown in Figure 1.

Figure 1 Fabrication process of concave silicon nano-mold: (a) UV-photolithography, (b) wet etching, (c) Cu vertical deposition, (d) lift-off, (e) DRIE, and (f) silica and Cu removal.
Figure 1

Fabrication process of concave silicon nano-mold: (a) UV-photolithography, (b) wet etching, (c) Cu vertical deposition, (d) lift-off, (e) DRIE, and (f) silica and Cu removal.

A layer of AZ5214E photoresist (Clariant AZ5214E) was spin-coated on a silicon wafer with a silica layer, and micro photoresist mesas were obtained by UV exposure (Figure 1a). The silicon wafer was then placed in buffered hydrofluoric acid under 60°C water bath to wet etch the silica (Figure 1b). A thin film deposition system (ZZS400, costar group, China) was used for vertical evaporation to deposit a layer of Cu with a thickness of about 100 nm as a Cu mask during Deep reactive ion-etching (DRIE) (Figure 1c). After depositing the Cu mask, the silicon wafer was placed in acetone and the photoresist was lift-off to obtain nanochannels (Figure 1d). DRIE was performed to transfer the nanochannels to the silicon wafer (Figure 1e). The silica layer and Cu layer were removed to obtain concave silicon nano-mold (Figure 1f). Figure 2 is the SEM image of concave silicon nano-mold with a width of 188 ± 1 nm and a depth of 120 ± 5 nm.

Figure 2 SEM images of concave silicon nano-mold.
Figure 2

SEM images of concave silicon nano-mold.

2.2 Fabrication of convex PDMS nano-mold

PDMS has the advantages of optical transparency, easy processing, low cost, and easy demolding. Therefore, PDMS was selected to manufacture convex PDMS nano-mold. Figure 3 shows the fabrication process of the convex PDMS nano-mold.

Figure 3 Fabrication process of convex PDMS nano-mold: (a) pouring PDMS on the hydrophobically treated concave silicon nano-mold and (b) removing the cured PDMS from the concave silicon nano-mold to obtain a (c) convex PDMS nano-mold.
Figure 3

Fabrication process of convex PDMS nano-mold: (a) pouring PDMS on the hydrophobically treated concave silicon nano-mold and (b) removing the cured PDMS from the concave silicon nano-mold to obtain a (c) convex PDMS nano-mold.

First, PDMS and curing agent were mixed at a volume ratio of 5:1, stirred for 5 min, and then placed in a vacuum to remove internal bubbles. Then, the PDMS was poured onto the concave silicon nano-mold, which had been hydrophobized, and then placed in a vacuum with a vacuum condition of 10 Pa for 1 h to ensure that the PDMS was filled into the nanochannels (Figure 3a). After vacuuming, the concave silicon nano-mold covered with PDMS was placed in an oven at 60°C for 4 h. After cooling to room temperature, the PDMS was separated from concave silicon nano-mold (Figure 3b) to obtain convex PDMS nano-mold (Figure 3c). Figure 4 shows the SEM image of the convex PDMS nano-mold, in which the size of the nano-ridge was 187 ± 6 nm wide and 104 ± 6 nm high.

Figure 4 SEM image of the convex PDMS nano-mold.
Figure 4

SEM image of the convex PDMS nano-mold.

2.3 Fabrication of SU-8 polymer micro/nanoscale nozzle

SU-8 photoresist has excellent thermal and chemical stability, solvent resistance, and mechanical properties, so SU-8 was selected to manufacture polymer micro/nanoscale nozzle. Figure 5 shows the fabrication process of SU-8 polymer micro/nanoscale nozzle by hot embossing and UV exposure.

Figure 5 Fabrication process of SU-8 nozzle. (a) Spin-coating the first layer of SU-8 photoresist on silica substrate, (b) UV exposure and development to obtain a base of nozzle, (c) spin-coating the second layer of SU-8 on the first layer of SU-8, (d) thermal imprinting, (e) UV exposure, (f) removing convex PDMS nano-mold and developing, (g) spin-coating SU-8 on the PDMS, (h) bonding under room temperature, (i) removing PDMS substrate and UV exposure, (j) developing, and (k) wet etching silica.
Figure 5

Fabrication process of SU-8 nozzle. (a) Spin-coating the first layer of SU-8 photoresist on silica substrate, (b) UV exposure and development to obtain a base of nozzle, (c) spin-coating the second layer of SU-8 on the first layer of SU-8, (d) thermal imprinting, (e) UV exposure, (f) removing convex PDMS nano-mold and developing, (g) spin-coating SU-8 on the PDMS, (h) bonding under room temperature, (i) removing PDMS substrate and UV exposure, (j) developing, and (k) wet etching silica.

The silicon wafer was put into an oxidation furnace with a temperature of 1,080°C for dry oxidation, and the oxidation time was about 40 min to obtain a silica layer with a thickness of about 100 nm. As shown in Figure 5a, the first layer of SU-8 (MicroChem, SU-8 2015) with a thickness of about 10 μm was spin-coated on the silica layer at 5,000 rpm, where the spin-coating time was 30 s. The silicon wafer spin-coated with SU-8 was placed on a horizontal hot plate at 85°C for 30 min to remove the solvent in the SU-8, so that the photoresist layer was cured and the exposure performance was fixed. In order to improve the adhesion between the silica layer and SU-8, it is necessary to perform oxygen plasma treatment on the silica layer before spin-coating SU-8, where the pressure was 60 Pa, and the oxygen plasma treatment power was 40 W, and the time was 1 min. The UV lithography was performed on SU-8, where the exposure intensity was 1 mW/cm2, the exposure time was 4 min, and the SU-8 substrate layer was obtained after developing for 90 s (Figure 5b). A second layer of SU-8 with a thickness of about 8 μm was spin-coated on the SU-8 substrate layer at a speed of 7,000 rpm for 30 s and pre-baked at 85°C for 30 min (Figure 5c). Then, the convex PDMS nano-mold was imprinted in the second layer of SU-8 with a pressure of 0.2 MPa under a temperature of 85°C for 20 min to obtain nanochannels (Figure 5d). After cooling, the UV light was passed through the mask and convex PDMS nano-mold to expose the second layer of SU-8, where the exposure intensity was 1 mW/cm2 and the exposure time was 4 min (Figure 5e). Post baking in an oven at 85°C for 2 min, the convex PDMS nano-mold was removed, and the unexposed SU-8 was dissolved in SU-8 developer for 90 s to obtain SU-8 microchannel (Figure 5f).

A layer of SU-8 was spin-coated on the PDMS substrate at 5,000 rpm for 30 s to make a SU-8 cover layer (10 µm thick), which was then placed on a horizontal hot plate at 85°C for 30 min (Figure 5g). To improve the bonding strength, the second layer of SU-8 with micro-nano channels and SU-8 cover layer were treated with oxygen plasma by Emitech K1050X. The optimized exposed and unexposed SU-8 oxygen plasma treatment parameters were 10 W for 15 s. After the oxygen plasma treatment, the SU-8 cover layer and the second layer of SU-8 with micro-nano channels were bonded together at a room temperature (Figure 5h).

After bonding, the PDMS substrate was removed, and the SU-8 cover layer was exposed to UV light (Figure 5i). After baking on a horizontal hot plate at 85°C for 2 min, the unexposed SU-8 was dissolved in the SU-8 developer, and the reservoir was fabricated (Figure 5j). The silica layer under the SU-8 nozzle was etched by buffer hydrofluoric acid and the SU-8 nozzle was released (Figure 5k).

3 Results and discussion

3.1 Surface modification of concave silicon nano-mold

The convex PDMS nano-mold was fabricated by casting PDMS on concave silicon nano-mold (Figure 3). In order to achieve non-destructive demolding and improve the anti-adhesion properties of silicon nano-mold, it was necessary to perform dimethyldichlorosilane surface treatment on the concave silicon nano-molds before pouring PDMS. The specific treatment steps were: (1) Ultrasonic cleaning. First, the concave silicon nano-mold was ultrasonically cleaned in acetone solution for 5 min, then ultrasonically cleaned in 95% ethanol solution for 5 min, and finally placed in deionized water for ultrasonic cleaning for 5 min. (2) Hot concentrated sulfuric acid cleaning. The concave silicon nano-mold was placed in boiling concentrated sulfuric acid for 10 min, soaked for 30 min, and then placed in a mixed solution of hydrogen peroxide and concentrated sulfuric acid (H2O2:H2SO4 = 1:1) for 15 min, and finally rinsed with deionized water. (3) No. 1 solution cleaning. The concave silicon nano-mold was placed in the boiling solution of No. 1 (H2O:H2O2:NH4OH = 5:2:1) for 5 min, and then rinsed with deionized water. (4) No. 2 solution cleaning. The concave silicon nano-mold was placed in the boiling solution of No. 2 (H2O:H2O2:HCl = 8:2:1) for 5 min, and then rinsed with deionized water. The cleaned concave silicon nano-mold was placed in an oven at 100°C for 30 min to remove surface moisture. (5) Oxygen plasma treatment. The concave silicon nano-mold was treated by a plasma etcher/Asher, where the oxygen plasma treatment power was 40 W and the treatment time was 1 min. (6) The concave silicon nano-mold was immerse in dimethyldichlorosilane for 15 s to graft the methyl group onto the surface of the silicon nano-mold. (7) The methylated concave silicon nano-mold was washed with toluene and anhydrous ethanol for 15 s, respectively, and dried to complete the hydrophobic treatment of the concave silicon nano-mold. The flowchart is shown in Figure 6.

Figure 6 Flow chart of surface modification of silicon nano-mold.
Figure 6

Flow chart of surface modification of silicon nano-mold.

The contact angles of the unsurfaced and surface-treated concave silicon nano-molds were measured using a drop shape analyzer (DSA100, Kruss, Germany), as shown in Figure 7. After the concave silicon nano-mold was cleaned, a large number of –OH groups were generated on the surface, and the measured contact angle was 37.4°, which was hydrophilic. After treatment with dimethyldichlorosilane, the –OH group on the surface of the concave silicon nano-mold was replaced by –CH3 group, and the measured contact angle was 115.9°, which changed from hydrophilic to hydrophobic properties, providing a guarantee for nondestructive demolding of concave silicon nano-mold.

Figure 7 Contact angles of silicon nano-mold. (a) Untreated with dimethyldichlorosilane and (b) treated with dimethyldichlorosilane.
Figure 7

Contact angles of silicon nano-mold. (a) Untreated with dimethyldichlorosilane and (b) treated with dimethyldichlorosilane.

3.2 Analysis of the embossing temperature and embossing time

The imprinting quality of the nanochannel was evaluated by the replication precision of the SU-8 nanochannel, as shown in Figure 8. The replication precision of SU-8 nanochannels is defined as follows:

(1) R = ∑ i = 1 n s i S i / n × 100 % ,

where R is the replication precision, S i is the area between two adjacent nano-ridges, and s i is the area filled with SU-8 photoresist between two adjacent nano-ridges.

Figure 8 Schematic diagram of replication precision of SU-8.
Figure 8

Schematic diagram of replication precision of SU-8.

During the hot embossing process, the hot embossing pressure was unchanged, and three samples were imprinted under each hot embossing parameter, and the average value and standard deviation of their replication precision were calculated.

SU-8 photoresist has excellent thermal and chemical stability with a glass transition temperature (T g) of about 55°C and a viscous flow temperature of about 80°C [26]. During the hot embossing process, the unexposed SU-8 photoresist was a photosensitive thermoplastic material. When the temperature was lower than T g, the SU-8 photoresist was in a glass state, and its mechanical properties are similar to those of glass. At this time, the molecular chain and its segments of the SU-8 photoresist are in a “frozen” state. The SU-8 photoresist has little deformation after being stressed. When the temperature rises to the glass transition region, the segments of the SU-8 photoresist molecules are “thawed” and the deformation increases. As the temperature continues to rise, the SU-8 photoresist will enter a rubbery/high elastic state. At this time, the movement of the molecular segments of the SU-8 photoresist is no longer bound and can be greatly deformed by a small force. With the further increase in the temperature, when the viscous flow temperature (T f) is exceeded, the SU-8 photoresist enters a viscous flow state, and the motion of the SU-8 photoresist segment becomes more intense. The whole molecular chain moves, and the deformation rapidly increases, resulting in irreversible deformation. Therefore, in this study, hot embossing experiments were performed on SU-8 photoresist at temperatures of 65°C (rubber state), 75°C (viscous flow transition zone), and 85°C (viscous flow state), respectively, and the nanochannels of SU-8 were characterized by SEM under different hot embossing time. Figure 9 shows the SEM images of the cross-section of the SU-8 nanochannels imprinted at different hot embossing temperatures for 3, 6, and 9 min. As can be seen in Figure 9a–f, at low temperatures (65 and 75°C) only slight deformation occurs due to the higher viscosity of SU-8. With the increase in hot embossing temperature (85°C), the viscosity of SU-8 became smaller, the fluidity was good, the deformation was large, and the filling speed was fast, as shown in Figure 9g–h. With the extension of the hot embossing time, the replication precision became higher and higher, and when the time reached 9 min, the filling was basically completed (Figure 9i). It can be seen that the filling speed of SU-8 at high temperature was faster and the replication precision was higher than that at low temperature. This is because SU-8 photoresist has poor plastic deformation at low temperature and cannot completely fill the mold. However, the higher the temperature, the lower the stress relaxation strength, the better the plastic deformation, the better the filling rate, and the higher the replication accuracy of SU-8 photoresist. Therefore, 85°C was selected as the optimal hot embossing temperature.

Figure 9 SEM images of nanochannel at different hot embossing temperature and hot embossing time.
Figure 9

SEM images of nanochannel at different hot embossing temperature and hot embossing time.

The longer the embossing time, the higher the replication precision and the better the nano-pattern morphology. However, if the embossing time was too long, the internal stress of the photoresist will increase, so it was necessary to study the influence of the hot embossing time on the replication precision. As shown in Figure 10, when the hot embossing temperature was 85°C, with the extension of the hot embossing time, the replication precision becomes higher and higher. When the embossing time was 20 min, the replication precision remains basically unchanged. Therefore, 20 min was chosen as the optimal hot embossing time. Under this condition, the nano-pattern replication precision can reach 98.5%.

Figure 10 The influence of hot embossing time on the replication precision at a temperature of 85°C.
Figure 10

The influence of hot embossing time on the replication precision at a temperature of 85°C.

3.3 Influence of the UV exposure parameters on the topography of micro channel

After hot embossing, the nanochannels are cured by UV exposure, and the microchannels are fabricated at the same time (Figure 5e). During the exposure process, the exposure intensity of the photoresist was not completely the same everywhere, owing to the influence of the absorption rate and Fresnel diffraction of SU-8 photoresist. The intensity distribution formula for Fresnel straight edge diffraction is as follows [27]:

(2) I i ( x , z ) = I o 2 { [ φ ( u 2 ) − φ ( u 1 ) ] 2 + [ ψ ( u 2 ) − ψ ( u 1 ) ] 2 } ,

where I 0 is the incident light intensity, φ(u) and ψ(u) are the Fresnel diffraction integrals, and the expressions are as follows [28]:

(3) φ ( u ) = ∫ o u cos π 2 v 2 d v ,

(4) ψ ( u ) = ∫ o u sin π 2 v 2 d v ,

where u is the Fresnel number, and the expression is [28]

(5) u 1 = x 1 2 λ ( g + z ) ,

(6) u 2 = x 2 2 λ ( g + z ) ,

where x 1 and x 2 are the distances from any point on the photoresist to the rightmost and leftmost boundaries of the mask, respectively, where λ is the wavelength of the light source (the wavelength of near ultraviolet light used in this work is 365 nm), g is the exposure gap (the exposure gap used in this simulation is 50 μm), and z is the depth of the photoresist. After UV irradiation, part of the energy will be absorbed by the active photosensitive compound in the SU-8 photoresist. As the depth increases, the light intensity decays exponentially, as shown in formula (7) [29].

(7) U ( z ) = I 0 e − ε z ,

where ε is the absorption coefficient of light. Therefore, the actual expression for light intensity distribution is as follows [30]:

(8) I i ( x , z ) = e ( − ε z ) I o 2 { [ φ ( u 2 ) − φ ( u 1 ) ] 2 + [ ψ ( u 2 ) − ψ ( u 1 ) ] 2 } ,

where the optical absorption coefficient of SU-8 photoresist is 79.32 cm−1 [30].

According to formula (8), the light intensity distribution of SU-8 photoresist at different depths was simulated by computer simulation, as shown in Figure 11. It can be seen from the figure that as the depth of the photoresist increases, the light intensity continues to decay. Therefore, it is necessary to optimize the exposure dose so that all the active photosensitive compounds in the photoresist have just absorbed photons and “lost” the activity of absorbing photons within the thickness range of SU-8 photoresist. Here the effect of exposure time on the morphology of micro and nano channels was studied by changing the exposure time to change the exposure dose.

Figure 11 Light intensity distribution of SU-8 photoresist at different depths.
Figure 11

Light intensity distribution of SU-8 photoresist at different depths.

Figure 12 shows the microscope images of SU-8 polymer micro/nanoscale nozzle at different exposure times (exposure intensity: 1 mW/cm2). As shown in Figure 12a, when the exposure time was 3 min, the SU-8 at the bottom was corroded. This is because the exposure time was too short, the exposure dose was insufficient, and the strong acid generated was not enough to make the SU-8 photoresist completely cross-linked during post-baking. When the exposure time was extended to 7 min, the SU-8 at the microchannel was cross-linked and the microchannel was blocked (Figure 12c). This is because there was a layer of PDMS between the SU-8 and the mask, which belongs to non-contact exposure. In this case, the longer the exposure time was, the more exposure dose the SU-8 in the microchannel obtained under the diffracted light, resulting in cross-linking of the SU-8 in the microchannel, which cannot be removed during development, thus causing blockage. Therefore, 5 min was chosen as the optimal exposure time (Figure 12b).

Figure 12 The microscope images of micro and nanochannels under different exposure times. (a) 3 min, (b) 5 min, (c) 7 min (exposure intensity: 1 mW/cm2).
Figure 12

The microscope images of micro and nanochannels under different exposure times. (a) 3 min, (b) 5 min, (c) 7 min (exposure intensity: 1 mW/cm2).

3.4 Optimization of parameters for the O2 plasma treatment

Oxygen plasma treatment can effectively reduce the contact angle of the SU-8 surface, increase the surface energy, and improve the bonding strength. Therefore, the influence of oxygen plasma treatment parameters on the contact angle of SU-8 was studied. Figure 13 shows the curve of contact angle vs time for exposed SU-8 and unexposed SU-8 at different oxygen plasma treatment powers. It can be seen that under different oxygen plasma treatment powers, with the extension of time, the contact angle of both the exposed SU-8 and unexposed SU-8 decreases rapidly at the beginning, then decreases slowly, and finally remains unchanged after reaching the minimum value. In order to obtain the smallest contact angle and avoid the etching of SU-8 nanochannels, 10 W and 15 s were selected as the optimal oxygen plasma treatment parameters for exposed SU-8 and unexposed SU-8.

Figure 13 Influence of oxygen plasma treatment parameters on the contact angle of (a) exposed SU-8 photoresist and (b) unexposed SU-8 photoresist.
Figure 13

Influence of oxygen plasma treatment parameters on the contact angle of (a) exposed SU-8 photoresist and (b) unexposed SU-8 photoresist.

3.5 Effect of bonding pressure on the morphology of nanochannels

After the oxygen plasma treatment, the SU-8 nozzle and SU-8 cover layer were bonded together at room temperature, and the bonding time was 5 min. In the bonding process, the bonding pressure was the important factor affecting the bonding strength. The interface gap between the SU-8 nozzle and the SU-8 cover layer can be reduced by applying pressure, and the groups generated by oxygen plasma treatment on the two interfaces can be close to each other and attract each other to generate adsorption force. With the gradual reduction in the interface distance, it finally reached a stable state. If the bonding pressure and bonding strength were insufficient, cracking and leakage will occur. Therefore, the influence of bonding pressure on bonding strength was studied.

The nanochannels were bonded under the bonding pressures of 0.06, 0.12, 0.18, and 0.24 MPa, respectively, and the cross-sectional SEM images of the nanochannels are shown in Figure 14. When the bonding pressure was less than 0.06 MPa, the SU-8 cover layer cannot be bonded with the SU-8 nozzle due to the small bonding pressure. When the bonding pressure was greater than 0.06 MPa, the nanochannels were well sealed, as shown in Figure 14a–d. Under 0.06 MPa bonding pressure, the size of the nanochannel was 95 ± 2 nm deep and 184 ± 3 nm wide. Under the bonding pressure of 0.12 MPa, the size of nanochannel was 96 ± 3 nm deep and 188 ± 2 nm wide. Under the bonding pressure of 0.18 MPa, the size of nanochannel was 98 ± 2 nm deep and 187 ± 1 nm wide. At 0.24 MPa bonding pressure, the size of nanochannel was 97 ± 3 nm deep and 189 ± 2 nm wide. It can be seen that if the bonding pressure was too small (<0.06 MPa), the interface of the two layers cannot be closely attached, resulting in the failure of the bonding. When the bonding pressure was greater than 0.06 MPa, the nanochannels were successfully bonded, and the bonding pressure had little effect on the morphology of nanochannel. In order to verify the reliability of the process parameters, the bonding strength of the SU-8 nozzle was tested. The SU-8 nozzle was tested by the method of compressed gas introduction. The equipment shown in Figure 14e was designed and built to test the bonding strength. The air compressor was used as the gas source and the pressure regulator was used to regulate the gas pressure. Connect the air inlet of the SU-8 nozzle with the gas conduit, input gas into the SU-8 nozzle through the gas conduit, and observe the gas pressure inside the SU-8 nozzle in real time through the barometer. The outlet of the SU-8 nozzle was blocked by epoxy resin glue, put the SU-8 nozzle into a container filled with water, introduce gas, gradually increase the gas pressure, and observe whether there are air bubbles in the water. Under the pressure of 0.7 MPa for 30 min, no bubbles were formed in the water, indicating that the SU-8 nozzle did not crack or leak under this parameter. Therefore, the bonding strength of the SU-8 polymer micro/nanoscale nozzle was at least 0.7 MPa. The bonding strength can meet the requirements of SU-8 nozzle EHD printing.

Figure 14 SEM image of nanotubes under different bonding pressures at room temperature. (a) 0.06 MPa, (b) 0.12 MPa, (c) 0.18 MPa, (d) 0.24 MPa, and (e) test setup for testing bonding strength.
Figure 14

SEM image of nanotubes under different bonding pressures at room temperature. (a) 0.06 MPa, (b) 0.12 MPa, (c) 0.18 MPa, (d) 0.24 MPa, and (e) test setup for testing bonding strength.

3.6 Analysis of bonding principle at room temperature

The bonding process of SU-8 was essentially the bonding of two interfaces, which transfers mechanical force and work through the interface. Figure 15 shows the schematic diagram of oxygen plasma assisted room temperature bonding. After the oxygen plasma treatment, the T g of the SU-8 surface was reduced [31], which was also one of the factors that promote the bonding of SU-8 at room temperature. At the same time, after the oxygen plasma treatment, polar functional groups (–OH, –COOH, and –CO) are generated on the surface of the SU-8. When the two SU-8 layers were close to each other, the polar groups at the interface will be close to each other as the distance between the interfaces decreases. When the distance was less than 1 nm, these groups will have dipole interactions and attract each other to generate adsorption force. Under the action of the adsorption force, the distance between the two interfaces will be further reduced to a steady state [32,33]. On the microscopic scale, the roughness of the SU-8 surface will also cause the materials to penetrate into each other at the unevenness of the interface, resulting in mechanical occlusion [34]. When the two layers of interface were tightly combined, the molecules at the interface diffuse under the action of Brownian motion and chain segment creep, penetrate each other, and the interface gradually disappears, finally a firm bonding surface was formed [35]. In addition, since the substrate of SU-8 nozzle was silicon wafer, the surface of the silicon wafer has high flatness, so that the contact surface of the bonding surface was larger, which was helpful for bonding. Using the same process scheme, the SU-8 nozzle was fabricated on the glass substrates, and it cannot be bonded at room temperature. This is because the flatness of the glass is much lower than that of the silicon wafer. The low surface flatness makes the distance between the two layers of interface too large, which is not enough to attract each other to produce adsorption force and cannot form a strong bonding surface. Therefore, the surface flatness is an important factor affecting the room temperature bonding [36,37].

Figure 15 Schematic diagram of oxygen plasma assisted room temperature bonding.
Figure 15

Schematic diagram of oxygen plasma assisted room temperature bonding.

3.7 Fluorescence test

The bonding quality of SU-8 nozzle was also characterized by fluorescence test method. The fluorescent solution of rhodamine B with a concentration of 20 mg/ml was injected into the SU-8 nozzle bonded at room temperature, and it was illuminated by a mercury lamp. The flow of fluorescent dyes in the micro and nanochannels was observed by means of an inverted fluorescence microscope, as shown in Figure 16. It can be seen that the rhodamine B fluorescent dye fills the entire micro-nano channel without blockage or leakage, which proves that the SU-8 polymer micro/nanoscale nozzle has been completely bonded.

Figure 16 Fluorescence images of the SU-8 polymer micro/nanoscale nozzle.
Figure 16

Fluorescence images of the SU-8 polymer micro/nanoscale nozzle.

4 Conclusion

In this work, a method for fabricating SU-8 polymer micro/nanoscale nozzle by oxygen plasma assisted room temperature bonding was proposed, which solves the problem of blockage or deformation of nanochannels due to high bonding temperature. The relationship between the parameters of hot embossing and the replication precision of nanochannels was analyzed, and the replication accuracy can reach 98.5%. The light intensity will gradually decrease with the increase in the depth of the photoresist during the exposure process. Therefore, the influence of UV exposure time on the morphology of micro and nano channel was studied, and the UV exposure time was optimized to be 5 min. The oxygen plasma treatment parameters and bonding pressure parameters were also optimized, the SU-8 nozzle with 95 ± 2 nm deep and 184 ± 3 nm wide was obtained. The bonding strength was at least 0.7 MPa, which can meet the requirements of SU-8 nozzle EHD printing. The bonding principle at room temperature was analyzed. The results show that the T g on the surface of SU-8 decreases after oxygen plasma treatment. Meanwhile, polar functional groups (–OH, –COOH, and –CO) were generated on the surface of SU-8. The uneven surface of SU-8 photoresist will also cause the materials to penetrate into each other at the interface, resulting in mechanical occlusion. As the interface distance decreases, the groups at the interface also undergo dipole interactions, attracting each other to reach a stable state. When the interface is tightly combined, the molecules at the interface will diffuse under the action of Brownian motion and chain segment creep, and penetrate each other, the interface gradually disappears, finally forming a firm bonding surface. At the same time, the substrate of SU-8 nozzle obtained by oxygen plasma assisted room temperature bonding was silicon wafer, and the surface of the silicon wafer has high flatness, and the lower surface roughness makes the bonding surface larger, which was conducive to bonding.

Acknowledgments

The authors are grateful for the reviewer’s valuable comments that improved the manuscript. This research work was supported by National Natural Science Foundation of China (No. 52205491), Natural Science Foundation of Jiangsu Province (No. BK20210710), and Excellent Postdoctoral Program of Jiangsu Province (No. 2023ZB694).

  1. Funding information: This research work was supported by National Natural Science Foundation of China (No. 52205491), Natural Science Foundation of Jiangsu Province (No. BK20210710), and Excellent Postdoctoral Program of Jiangsu Province (No. 2023ZB694).

  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.

  4. Data availability statement: All data generated or analysed during this study are included in this published article.

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Received: 2023-05-23
Revised: 2023-06-29
Accepted: 2023-08-03
Published Online: 2023-09-01

© 2023 the author(s), published by De Gruyter

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

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https://doi.org/10.1515/ntrev-2023-0113
Keywords for this article
room temperature bonding; polymer; oxygen plasma treatment
Creative Commons
BY 4.0

Articles in the same Issue

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  22. Parametric simulation of hybrid nanofluid flow consisting of cobalt ferrite nanoparticles with second-order slip and variable viscosity over an extending surface
  23. Chitosan-capped silver nanoparticles with potent and selective intrinsic activity against the breast cancer cells
  24. Multi-core/shell SiO2@Al2O3 nanostructures deposited on Ti3AlC2 to enhance high-temperature stability and microwave absorption properties
  25. Solution-processed Bi2S3/BiVO4/TiO2 ternary heterojunction photoanode with enhanced photoelectrochemical performance
  26. Electroporation effect of ZnO nanoarrays under low voltage for water disinfection
  27. NIR-II window absorbing graphene oxide-coated gold nanorods and graphene quantum dot-coupled gold nanorods for photothermal cancer therapy
  28. Nonlinear three-dimensional stability characteristics of geometrically imperfect nanoshells under axial compression and surface residual stress
  29. Investigation of different nanoparticles properties on the thermal conductivity and viscosity of nanofluids by molecular dynamics simulation
  30. Optimized Cu2O-{100} facet for generation of different reactive oxidative species via peroxymonosulfate activation at specific pH values to efficient acetaminophen removal
  31. Brownian and thermal diffusivity impact due to the Maxwell nanofluid (graphene/engine oil) flow with motile microorganisms and Joule heating
  32. Appraising the dielectric properties and the effectiveness of electromagnetic shielding of graphene reinforced silicone rubber nanocomposite
  33. Synthesis of Ag and Cu nanoparticles by plasma discharge in inorganic salt solutions
  34. Low-cost and large-scale preparation of ultrafine TiO2@C hybrids for high-performance degradation of methyl orange and formaldehyde under visible light
  35. Utilization of waste glass with natural pozzolan in the production of self-glazed glass-ceramic materials
  36. Mechanical performance of date palm fiber-reinforced concrete modified with nano-activated carbon
  37. Melting point of dried gold nanoparticles prepared with ultrasonic spray pyrolysis and lyophilisation
  38. Graphene nanofibers: A modern approach towards tailored gypsum composites
  39. Role of localized magnetic field in vortex generation in tri-hybrid nanofluid flow: A numerical approach
  40. Intelligent computing for the double-diffusive peristaltic rheology of magneto couple stress nanomaterials
  41. Bioconvection transport of upper convected Maxwell nanoliquid with gyrotactic microorganism, nonlinear thermal radiation, and chemical reaction
  42. 3D printing of porous Ti6Al4V bone tissue engineering scaffold and surface anodization preparation of nanotubes to enhance its biological property
  43. Bioinspired ferromagnetic CoFe2O4 nanoparticles: Potential pharmaceutical and medical applications
  44. Significance of gyrotactic microorganisms on the MHD tangent hyperbolic nanofluid flow across an elastic slender surface: Numerical analysis
  45. Performance of polycarboxylate superplasticisers in seawater-blended cement: Effect from chemical structure and nano modification
  46. Entropy minimization of GO–Ag/KO cross-hybrid nanofluid over a convectively heated surface
  47. Oxygen plasma assisted room temperature bonding for manufacturing SU-8 polymer micro/nanoscale nozzle
  48. Performance and mechanism of CO2 reduction by DBD-coupled mesoporous SiO2
  49. Polyarylene ether nitrile dielectric films modified by HNTs@PDA hybrids for high-temperature resistant organic electronics field
  50. Exploration of generalized two-phase free convection magnetohydrodynamic flow of dusty tetra-hybrid Casson nanofluid between parallel microplates
  51. Hygrothermal bending analysis of sandwich nanoplates with FG porous core and piezomagnetic faces via nonlocal strain gradient theory
  52. Design and optimization of a TiO2/RGO-supported epoxy multilayer microwave absorber by the modified local best particle swarm optimization algorithm
  53. Mechanical properties and frost resistance of recycled brick aggregate concrete modified by nano-SiO2
  54. Self-template synthesis of hollow flower-like NiCo2O4 nanoparticles as an efficient bifunctional catalyst for oxygen reduction and oxygen evolution in alkaline media
  55. High-performance wearable flexible strain sensors based on an AgNWs/rGO/TPU electrospun nanofiber film for monitoring human activities
  56. High-performance lithium–selenium batteries enabled by nitrogen-doped porous carbon from peanut meal
  57. Investigating effects of Lorentz forces and convective heating on ternary hybrid nanofluid flow over a curved surface using homotopy analysis method
  58. Exploring the potential of biogenic magnesium oxide nanoparticles for cytotoxicity: In vitro and in silico studies on HCT116 and HT29 cells and DPPH radical scavenging
  59. Enhanced visible-light-driven photocatalytic degradation of azo dyes by heteroatom-doped nickel tungstate nanoparticles
  60. A facile method to synthesize nZVI-doped polypyrrole-based carbon nanotube for Ag(i) removal
  61. Improved osseointegration of dental titanium implants by TiO2 nanotube arrays with self-assembled recombinant IGF-1 in type 2 diabetes mellitus rat model
  62. Functionalized SWCNTs@Ag–TiO2 nanocomposites induce ROS-mediated apoptosis and autophagy in liver cancer cells
  63. Triboelectric nanogenerator based on a water droplet spring with a concave spherical surface for harvesting wave energy and detecting pressure
  64. A mathematical approach for modeling the blood flow containing nanoparticles by employing the Buongiorno’s model
  65. Molecular dynamics study on dynamic interlayer friction of graphene and its strain effect
  66. Induction of apoptosis and autophagy via regulation of AKT and JNK mitogen-activated protein kinase pathways in breast cancer cell lines exposed to gold nanoparticles loaded with TNF-α and combined with doxorubicin
  67. Effect of PVA fibers on durability of nano-SiO2-reinforced cement-based composites subjected to wet-thermal and chloride salt-coupled environment
  68. Effect of polyvinyl alcohol fibers on mechanical properties of nano-SiO2-reinforced geopolymer composites under a complex environment
  69. In vitro studies of titanium dioxide nanoparticles modified with glutathione as a potential drug delivery system
  70. Comparative investigations of Ag/H2O nanofluid and Ag-CuO/H2O hybrid nanofluid with Darcy-Forchheimer flow over a curved surface
  71. Study on deformation characteristics of multi-pass continuous drawing of micro copper wire based on crystal plasticity finite element method
  72. Properties of ultra-high-performance self-compacting fiber-reinforced concrete modified with nanomaterials
  73. Prediction of lap shear strength of GNP and TiO2/epoxy nanocomposite adhesives
  74. A novel exploration of how localized magnetic field affects vortex generation of trihybrid nanofluids
  75. Fabrication and physicochemical characterization of copper oxide–pyrrhotite nanocomposites for the cytotoxic effects on HepG2 cells and the mechanism
  76. Thermal radiative flow of cross nanofluid due to a stretched cylinder containing microorganisms
  77. In vitro study of the biphasic calcium phosphate/chitosan hybrid biomaterial scaffold fabricated via solvent casting and evaporation technique for bone regeneration
  78. Insights into the thermal characteristics and dynamics of stagnant blood conveying titanium oxide, alumina, and silver nanoparticles subject to Lorentz force and internal heating over a curved surface
  79. Effects of nano-SiO2 additives on carbon fiber-reinforced fly ash–slag geopolymer composites performance: Workability, mechanical properties, and microstructure
  80. Energy bandgap and thermal characteristics of non-Darcian MHD rotating hybridity nanofluid thin film flow: Nanotechnology application
  81. Green synthesis and characterization of ginger-extract-based oxali-palladium nanoparticles for colorectal cancer: Downregulation of REG4 and apoptosis induction
  82. Abnormal evolution of resistivity and microstructure of annealed Ag nanoparticles/Ag–Mo films
  83. Preparation of water-based dextran-coated Fe3O4 magnetic fluid for magnetic hyperthermia
  84. Statistical investigations and morphological aspects of cross-rheological material suspended in transportation of alumina, silica, titanium, and ethylene glycol via the Galerkin algorithm
  85. Effect of CNT film interleaves on the flexural properties and strength after impact of CFRP composites
  86. Self-assembled nanoscale entities: Preparative process optimization, payload release, and enhanced bioavailability of thymoquinone natural product
  87. Structure–mechanical property relationships of 3D-printed porous polydimethylsiloxane films
  88. Nonlinear thermal radiation and the slip effect on a 3D bioconvection flow of the Casson nanofluid in a rotating frame via a homotopy analysis mechanism
  89. Residual mechanical properties of concrete incorporated with nano supplementary cementitious materials exposed to elevated temperature
  90. Time-independent three-dimensional flow of a water-based hybrid nanofluid past a Riga plate with slips and convective conditions: A homotopic solution
  91. Lightweight and high-strength polyarylene ether nitrile-based composites for efficient electromagnetic interference shielding
  92. Review Articles
  93. Recycling waste sources into nanocomposites of graphene materials: Overview from an energy-focused perspective
  94. Hybrid nanofiller reinforcement in thermoset and biothermoset applications: A review
  95. Current state-of-the-art review of nanotechnology-based therapeutics for viral pandemics: Special attention to COVID-19
  96. Solid lipid nanoparticles for targeted natural and synthetic drugs delivery in high-incidence cancers, and other diseases: Roles of preparation methods, lipid composition, transitional stability, and release profiles in nanocarriers’ development
  97. Critical review on experimental and theoretical studies of elastic properties of wurtzite-structured ZnO nanowires
  98. Polyurea micro-/nano-capsule applications in construction industry: A review
  99. A comprehensive review and clinical guide to molecular and serological diagnostic tests and future development: In vitro diagnostic testing for COVID-19
  100. Recent advances in electrocatalytic oxidation of 5-hydroxymethylfurfural to 2,5-furandicarboxylic acid: Mechanism, catalyst, coupling system
  101. Research progress and prospect of silica-based polymer nanofluids in enhanced oil recovery
  102. Review of the pharmacokinetics of nanodrugs
  103. Engineered nanoflowers, nanotrees, nanostars, nanodendrites, and nanoleaves for biomedical applications
  104. Research progress of biopolymers combined with stem cells in the repair of intrauterine adhesions
  105. Progress in FEM modeling on mechanical and electromechanical properties of carbon nanotube cement-based composites
  106. Antifouling induced by surface wettability of poly(dimethyl siloxane) and its nanocomposites
  107. TiO2 aerogel composite high-efficiency photocatalysts for environmental treatment and hydrogen energy production
  108. Structural properties of alumina surfaces and their roles in the synthesis of environmentally persistent free radicals (EPFRs)
  109. Nanoparticles for the potential treatment of Alzheimer’s disease: A physiopathological approach
  110. Current status of synthesis and consolidation strategies for thermo-resistant nanoalloys and their general applications
  111. Recent research progress on the stimuli-responsive smart membrane: A review
  112. Dispersion of carbon nanotubes in aqueous cementitious materials: A review
  113. Applications of DNA tetrahedron nanostructure in cancer diagnosis and anticancer drugs delivery
  114. Magnetic nanoparticles in 3D-printed scaffolds for biomedical applications
  115. An overview of the synthesis of silicon carbide–boron carbide composite powders
  116. Organolead halide perovskites: Synthetic routes, structural features, and their potential in the development of photovoltaic
  117. Recent advancements in nanotechnology application on wood and bamboo materials: A review
  118. Application of aptamer-functionalized nanomaterials in molecular imaging of tumors
  119. Recent progress on corrosion mechanisms of graphene-reinforced metal matrix composites
  120. Research progress on preparation, modification, and application of phenolic aerogel
  121. Application of nanomaterials in early diagnosis of cancer
  122. Plant mediated-green synthesis of zinc oxide nanoparticles: An insight into biomedical applications
  123. Recent developments in terahertz quantum cascade lasers for practical applications
  124. Recent progress in dielectric/metal/dielectric electrodes for foldable light-emitting devices
  125. Nanocoatings for ballistic applications: A review
  126. A mini-review on MoS2 membrane for water desalination: Recent development and challenges
  127. Recent updates in nanotechnological advances for wound healing: A narrative review
  128. Recent advances in DNA nanomaterials for cancer diagnosis and treatment
  129. Electrochemical micro- and nanobiosensors for in vivo reactive oxygen/nitrogen species measurement in the brain
  130. Advances in organic–inorganic nanocomposites for cancer imaging and therapy
  131. Advancements in aluminum matrix composites reinforced with carbides and graphene: A comprehensive review
  132. Modification effects of nanosilica on asphalt binders: A review
  133. Decellularized extracellular matrix as a promising biomaterial for musculoskeletal tissue regeneration
  134. Review of the sol–gel method in preparing nano TiO2 for advanced oxidation process
  135. Micro/nano manufacturing aircraft surface with anti-icing and deicing performances: An overview
  136. Cell type-targeting nanoparticles in treating central nervous system diseases: Challenges and hopes
  137. An overview of hydrogen production from Al-based materials
  138. A review of application, modification, and prospect of melamine foam
  139. A review of the performance of fibre-reinforced composite laminates with carbon nanotubes
  140. Research on AFM tip-related nanofabrication of two-dimensional materials
  141. Advances in phase change building materials: An overview
  142. Development of graphene and graphene quantum dots toward biomedical engineering applications: A review
  143. Nanoremediation approaches for the mitigation of heavy metal contamination in vegetables: An overview
  144. Photodynamic therapy empowered by nanotechnology for oral and dental science: Progress and perspectives
  145. Biosynthesis of metal nanoparticles: Bioreduction and biomineralization
  146. Current diagnostic and therapeutic approaches for severe acute respiratory syndrome coronavirus-2 (SARS-COV-2) and the role of nanomaterial-based theragnosis in combating the pandemic
  147. Application of two-dimensional black phosphorus material in wound healing
  148. Special Issue on Advanced Nanomaterials and Composites for Energy Conversion and Storage - Part I
  149. Helical fluorinated carbon nanotubes/iron(iii) fluoride hybrid with multilevel transportation channels and rich active sites for lithium/fluorinated carbon primary battery
  150. The progress of cathode materials in aqueous zinc-ion batteries
  151. Special Issue on Advanced Nanomaterials for Carbon Capture, Environment and Utilization for Energy Sustainability - Part I
  152. Effect of polypropylene fiber and nano-silica on the compressive strength and frost resistance of recycled brick aggregate concrete
  153. Mechanochemical design of nanomaterials for catalytic applications with a benign-by-design focus
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