Glass micropore inner surface polishing device and method

By using a plasma cyclic scouring method with hydrogen and HCl gases, the complexity and residue problems of glass micropore polishing in the prior art have been solved, achieving a high-efficiency and low-cost micropore inner wall polishing effect.

CN121888976APending Publication Date: 2026-04-17SHENZHEN UNIV
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
SHENZHEN UNIV
Filing Date
2026-01-14
Publication Date
2026-04-17

AI Technical Summary

Technical Problem

Existing glass micropore polishing technology suffers from problems such as complex processes, high costs, difficulty in handling blind holes and micropores, and easy retention of contaminants.

Method used

A plasma cyclic scouring process is performed using a mixture of hydrogen and HCl gases. Hydrogen ions react with the silicon-oxygen bonds in the glass to generate hydroxyl groups and hydrides, while chloride ions remove metal ions, thus polishing the inner walls of the glass micropores.

Benefits of technology

It achieves efficient and residue-free polishing of the inner walls of glass micropores, significantly reducing surface roughness. It is suitable for polishing various complex shapes and large numbers of micropores, reducing costs and simplifying the process.

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Abstract

The invention discloses a glass micropore inner surface polishing device and method, and aims to solve the problem of efficient polishing of glass micropores with special structures. The device core comprises a vacuum heat treatment furnace and a radio frequency oscillation device, the vacuum heat treatment furnace is communicated with a gas inlet pipe, a gas suction pipe, a gas outlet pipe and a circulation pipeline with a circulation gas pump, the radio frequency oscillation device is installed at a circulation gas inlet in the tail end of the circulation pipeline, and gas combinations can be flexibly selected according to TGV plate materials. According to the method, mixed gas of hydrogen and HCl gas is subjected to radio frequency treatment and then is circularly polished, and a plurality of TGV plates, adaptive blind holes, special-shaped holes and other special holes and array micropores can be treated at the same time. The mixed gas after radio frequency treatment is used as a polishing medium, and the method has the advantages of being simple in process, free of hole pattern constraint, free of residual pollution and the like, and is suitable for polishing the inner surfaces of various special glass micropores.
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Description

Technical Field

[0001] This invention relates to the field of glass substrate manufacturing technology, and more specifically to a glass micropore inner surface polishing apparatus and method. Background Technology

[0002] With the rapid development of industries such as 5G, smart cars, and medical devices, electronic products are constantly evolving towards greater portability and convenience, placing higher demands on the manufacturing, integration, and packaging of sensors. Against this backdrop, through-glass via (TGV) technology has emerged. TGV technology is a vertical electrical interconnection technology using glass substrates. Glass substrates possess superior electrical performance and lower parasitic capacitance compared to ordinary silicon and SOI substrates, facilitating the expansion of high-frequency signal transmission. Furthermore, the excellent optical properties of glass make it more suitable for optical applications such as micro-opto-electro-mechanical systems (MOEMS). By adjusting the glass composition and optimizing surface treatment, the coefficient of thermal expansion (CTE) and mechanical strength of the substrate can be altered, thereby improving metal adhesion, stress control, and reliability. TGV technology supports a wide range of wafer thicknesses and large sizes, as well as panels. Moreover, glass-based processes are simpler, eliminating the need to deposit an insulating layer on the inner wall of the TGV, making the manufacturing cost of glass-encapsulated substrates significantly lower than that of silicon substrates.

[0003] Currently, TGV (Through Glass Vias) typically employs laser technology for drilling, resulting in microvias with relatively rough inner walls. The roughness of the inner wall of TGV vias significantly impacts their performance. Firstly, roughness affects the electrical properties of the via. Studies show that lower inner wall roughness leads to lower resistance and less resistance uncertainty in the via's lead connection structure. This is because lower roughness allows for smoother charge transport paths, reducing charge scattering and obstruction during transport, thus lowering resistance. Secondly, inner wall roughness also affects the mechanical properties of the via. Excessive roughness leads to more microscopic defects and stress concentration points on the via wall surface, reducing the mechanical strength and reliability of the via. Furthermore, inner wall roughness affects the filling quality of the via. During electroplating, a rougher wall can cause uneven distribution of the filler material, resulting in voids or gaps, affecting the conductivity and reliability of the via. Therefore, during the manufacturing of glass vias, the roughness of the inner wall should be strictly controlled to ensure good electrical and mechanical properties.

[0004] Micropores manufactured using TGV technology typically have small diameters and large depth-to-diameter ratios, making it difficult to perform grinding and polishing on the inner walls of these micropores using traditional processing methods. Currently, there are few polishing techniques available for the inner walls of TGV pores. Two common techniques are chemical polishing, which involves ultrasonic treatment using a mixture of various acids. Specific steps include ultrasonication with a 10% HNO3 solution, ultrasonic cleaning with deionized water, ultrasonication with a mixture of dilute HNO3 and HF, ultrasonic cleaning with deionized water, ultrasonication with a mixture of dilute HNO3, HF, and dilute H2SO4, ultrasonic cleaning with deionized water, ultrasonication with a mixture of HF, dilute H2SO4, and NH4Cl, ultrasonic cleaning with deionized water, ultrasonication with ethanol, and finally drying. Chemical polishing can achieve nanoscale surface roughness. Another type is magnetic micro-abrasive jet technology. Its principle is to use magnetic micro-abrasive focusing technology under dynamic magnetic field to concentrate magnetic micro-abrasive at the jet center to polish the inner wall of micropores. By simulating the polishing process under different parameters through the coupling of finite element method and discrete element method, the flow field distribution, erosion rate and wall shear force are analyzed. Magnetic micro-abrasive jet technology can achieve uniform polishing of the inner wall of complex-shaped micropores, remove burrs and other defects, and improve the quality of the inner wall. The surface roughness after processing is significantly reduced, and there is a better rounding effect at the orifice.

[0005] Existing polishing technologies for glass micropores all have certain shortcomings. Chemical polishing is complex, requiring strict control of the concentration and processing time of the chemical solution, and it also presents the problem of chemical waste disposal. Furthermore, for blind holes with small diameters, liquid chemical etchants are difficult to penetrate into the hole for polishing due to factors such as wettability and air pressure, and residual etchant is difficult to clean after polishing. Magnetic micro-abrasive jet technology and magnetorheological polishing not only require precise control of magnetic field strength and jet parameters, resulting in high equipment costs, but also have poor polishing effects on blind holes or micropores. In addition, magnetic abrasives tend to remain on the inner wall of the micropores during polishing, forming residual contaminants. Summary of the Invention

[0006] In view of this, the present invention provides a hydrogen-based mixed gas circulation polishing method, which involves mixing a certain proportion of HCl gas into hydrogen gas, and then using radio frequency oscillation to ionize the mixed gas to form H2O. + Cl - And at high temperature, the glass micropores are subjected to plasma cyclic scouring; through hydrogen ions (H + The ions react with the silicon-oxygen bonds (Si-O-Si) in the glass to generate hydroxyl groups (Si-OH) and hydrides (H-Si), thus achieving a removal effect. Simultaneously, the introduced chloride ions (Cl...) - This process removes metal ions and other impurities from the glass. Through repeated erosion of the micropore inner walls, the effect of polishing the micropore inner walls is ultimately achieved.

[0007] To achieve the above objectives, the present invention adopts the following technical solution:

[0008] First, the present invention provides a glass microporous inner surface polishing device, comprising:

[0009] A vacuum heat treatment furnace, wherein the vacuum heat treatment furnace is connected to an inlet pipe, an exhaust pipe, an outlet pipe, a circulation pipeline and a radio frequency oscillation device;

[0010] The air intake pipe is connected to multiple air supply pipes;

[0011] The exhaust pipe is connected to an exhaust gas treatment device.

[0012] Both ends of the circulation pipeline are connected to the vacuum heat treatment furnace, and a circulation air pump is installed on the circulation pipeline.

[0013] The radio frequency oscillation device is installed on the circulation pipeline at the end where the circulating gas enters the vacuum heat treatment furnace.

[0014] Preferably, there are two or more gas supply pipes, and the multiple gas supply pipes can be connected to different gases respectively.

[0015] The present invention also provides a method for polishing the inner surface of glass micropores, which is carried out using the apparatus described in the above technical solution, and includes the following steps:

[0016] (1) Place the TGV plate perpendicular to the airflow direction in the vacuum heat treatment furnace, and then evacuate the heat treatment furnace to a vacuum through the evacuation pipe;

[0017] (2) Hydrogen and HCl gas are fed into the inlet pipe through the gas supply pipe and mixed, and then injected into the vacuum heat treatment furnace through the inlet pipe.

[0018] (3) Heat the vacuum heat treatment furnace to the preset temperature and then keep it at that temperature;

[0019] (4) Turn on the circulating gas pump to make the mixed gas of hydrogen and acid gas rushing into the vacuum heat treatment furnace circulate through the micropores on the TGV plate. Turn on the radio frequency oscillation device to ionize the circulating gas at the outlet of the circulating pipeline. After circulating polishing for a certain period of time, turn off the heat preservation and radio frequency oscillation device to allow the TGV plate to be cooled in the furnace. During the cooling process, continue to keep the mixed gas circulating.

[0020] (5) When the temperature drops to room temperature, hydrogen is introduced again to discharge the mixed gas in the vacuum heat treatment furnace through the outlet pipe into the tail gas treatment device to eliminate the residual HCl gas component in the mixed gas.

[0021] (6) After the mixed gas is exhausted, open the furnace and take out the polished TGV plate.

[0022] Preferably, in step (1), the vacuum level is 5×10⁻⁶.-4 Pa-1×10 -3 Pa.

[0023] Preferably, the volume ratio of hydrogen to HCl gas is (8-10):1.

[0024] Preferably, the gas pressure inside the furnace in step (2) is 0.7-1.1 MPa.

[0025] Preferably, the preset temperature in step (3) is 600-1200℃.

[0026] Preferably, in step (4), the frequency of the radio frequency oscillation device is 13.56MHz; the flow rate of the circulating air pump is 0.3-0.5m / s, and the circulation time is 1.5-2h.

[0027] Preferably, the exhaust gas treatment device is a water tank filled with water.

[0028] Preferably, one or more TGV plates can be processed simultaneously. Multiple TGV plates are placed in parallel in a vacuum heat treatment furnace, allowing multiple TGV plates to be processed at the same time. This method is suitable for polishing the inner surfaces of special structures such as tiny blind holes, irregular holes, and slender holes, as well as for polishing the inner surfaces of a large number of arrayed micropores or irregularly arranged micropores.

[0029] As can be seen from the above technical solution, compared with the prior art, the present invention discloses a glass microporous inner surface polishing device and method, which has the following beneficial effects:

[0030] The polishing medium used in this method is a mixed gas. Compared with polishing methods based on liquid polishing media, such as chemical polishing technology and magnetic micro-abrasive jet technology, it has the advantages of simple process, simple control process, no constraint on hole shape, and no residual pollution. It is especially suitable for polishing special glass micropores such as blind holes, irregular holes, and slender holes. Attached Figure Description

[0031] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on the provided drawings without creative effort.

[0032] Figure 1 This is a structural diagram of a glass micropore inner surface polishing device.

[0033] Figure 2 The hexagonal TGV plate of Example 1;

[0034] Figure 3The TGV blind hole plate of Example 2;

[0035] In the diagram: 1-TGV plate; 2-vacuum heat treatment furnace; 3-extraction pipe; 4-hydrogen supply pipe; 5-HCl gas supply pipe; 6-inlet pipe; 7-heater; 8-circulating gas inlet; 9-radio frequency oscillation device; 10-circulating gas pump; 11-circulating pipeline; 12-circulating gas; 13-outlet pipe; 14-residual gas; 15-water tank. Detailed Implementation

[0036] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0037] The glass micropore inner surface polishing device used in the following embodiments is as follows: Figure 1 As shown, it includes:

[0038] Vacuum heat treatment furnace 2, which is connected to an inlet pipe 6, an exhaust pipe 3, an outlet pipe 13, a circulation pipeline 11 and a radio frequency oscillation device 9;

[0039] The air inlet pipe 6 is connected to multiple air supply pipes, namely hydrogen gas supply pipe 4 and HCl gas supply pipe 5.

[0040] The exhaust pipe 13 is connected to an exhaust gas treatment device, namely a water tank 15;

[0041] Both ends of the circulation pipeline 11 are connected to the vacuum heat treatment furnace 2, and a circulation air pump 10 is installed on the circulation pipeline 11.

[0042] The radio frequency oscillation device 9 is installed on the circulation pipeline 11 at one end where the circulating gas enters the vacuum heat treatment furnace 2.

[0043] Example 1

[0044] Polishing of irregularly shaped TGV holes:

[0045] (1) Prepare a 1 mm thick TGV plate with irregularly shaped holes. The material is quartz glass, the irregularly shaped holes are hexagonal in shape, and the pore diameter is 200 μm. The inner wall of the micropores is relatively rough after laser drilling, and the surface roughness Ra is about 1.2 μm. Figure 2 The TGV plate is placed perpendicular to the airflow direction in the vacuum heat treatment furnace 2, and then the vacuum heat treatment furnace 2 is evacuated to a vacuum level of 1×10 through the vacuum pump connected by the evacuation pipe 3. -3 Pa;

[0046] (2) Based on the volume ratio, hydrogen and HCl are supplied to the inlet pipe 6 through the hydrogen supply pipe 4 and the HCl gas supply pipe 5 respectively in a ratio of 10:1 and mixed. The mixture is then injected into the vacuum heat treatment furnace 2 through the inlet pipe 6 to ensure that the residual air in the furnace is completely replaced and the gas pressure reaches 0.7 MPa.

[0047] (3) Heat the vacuum heat treatment furnace 2 to 1200℃ and then keep it at that temperature;

[0048] (4) Turn on the circulating gas pump 10 to make the mixed gas of hydrogen and HCl that enters the vacuum heat treatment furnace 2 circulate back and forth through the micropores on the TGV plate. The gas flow rate is 0.5m / s. Turn on the radio frequency oscillation device and set the frequency to 13.56MHz to ionize the circulating gas at the outlet of the circulation pipeline. After 2 hours of circulating polishing, turn off the heat preservation to allow the TGV plate to be cooled in the furnace. During the cooling process, the mixed gas continues to circulate.

[0049] During the circulation process, the mixed plasma continuously undergoes chemical reactions with the inner surface of the micropores, producing hydrogen ions (H+). + It reacts with the silicon-oxygen bonds (Si-O-Si) in the glass to form hydroxyl groups (Si-OH) and hydrides (H-Si), while chloride ions (Cl-O-Si) are released. - To remove doped metal ions from the glass and gradually remove micro-protrusions on the inner surface, a polishing effect is achieved.

[0050] (5) When the temperature drops to room temperature, hydrogen is introduced again to discharge the mixed gas in the vacuum heat treatment furnace 2 through the outlet pipe 13 into the tail gas treatment device (water tank 15) to eliminate the residual HCl gas component in the mixed gas.

[0051] (6) After the mixed gas is exhausted, open the furnace and take out the polished TGV plate.

[0052] Polishing effect inspection:

[0053] Surface roughness inspection: The through hole was cut along the axial direction, and the roughness of the inner surface of the polished hexagonal quartz TGV hole was inspected using an atomic force microscope (AFM). The results showed that the inner wall was smooth and flat after polishing, and the surface roughness Ra was reduced to 0.04 μm, which was about 126% lower than before polishing, meeting the requirements of high-precision polishing.

[0054] Example 2

[0055] TGV blind hole polishing:

[0056] (1) A TGV board with a thickness of 1 mm, a blind hole diameter of 80 μm, and a depth of 0.5 mm was selected. The material was borosilicate glass. After laser drilling, the surface roughness Ra of the inner wall of the blind hole was about 1.5 μm, and there was obvious unevenness at the bottom of the blind hole, such as Figure 3 The TGV plate is placed perpendicular to the airflow direction in the vacuum heat treatment furnace 2, with the opening of the blind hole facing the outlet of the circulating gas pipe. Then, the vacuum heat treatment furnace 2 is evacuated to a vacuum level of 5×10⁻⁶ through the vacuum pump connected to the evacuation pipe 3. -4 Pa;

[0057] (2) Based on the volume ratio, hydrogen and HCl are supplied to the inlet pipe 6 in a ratio of 8:1 through hydrogen supply pipe 4 and HCl gas supply pipe 5 respectively, and mixed. The mixture is then injected into the vacuum heat treatment furnace 2 through the inlet pipe 6 to ensure that the residual air in the furnace is completely replaced and the gas pressure reaches 1.1 MPa.

[0058] (3) Heat the vacuum heat treatment furnace 2 to 600°C and then keep it at that temperature;

[0059] (4) Turn on the circulating gas pump 10 to make the mixed gas of hydrogen and HCl that enters the vacuum heat treatment furnace 2 circulate back and forth through the micropores on the TGV plate. The gas flow rate is 0.3m / s. Turn on the radio frequency oscillation device and set the frequency to 13.56MHz to ionize the circulating gas at the outlet of the circulation pipeline. After circulating and polishing for 1.5h, turn off the heat preservation to allow the TGV plate to be cooled in the furnace. During the cooling process, the mixed gas continues to circulate.

[0060] During the circulation process, the mixed plasma continuously undergoes chemical reactions with the inner surface of the micropores, producing hydrogen ions (H+). + It reacts with the silicon-oxygen bonds (Si-O-Si) in the glass to form hydroxyl groups (Si-OH) and hydrides (H-Si), while chloride ions (Cl-O-Si) are released. - To remove doped metal ions from the glass and gradually remove micro-protrusions on the inner surface, a polishing effect is achieved.

[0061] (5) When the temperature drops to room temperature, hydrogen is introduced again to discharge the mixed gas in the vacuum heat treatment furnace 2 through the outlet pipe 13 into the tail gas treatment device (water tank 15) to eliminate the residual HCl gas component in the mixed gas.

[0062] (6) After the mixed gas is exhausted, open the furnace and take out the polished TGV plate.

[0063] Surface roughness inspection: The blind hole was cut along the axial direction, and the roughness of the inner surface of the polished borosilicate TGV blind hole was inspected using atomic force microscopy (AFM). The results showed that the inner wall was smooth and flat after polishing, and the surface roughness Ra was reduced to 0.06 μm, which was about 94% lower than before polishing.

[0064] The various embodiments in this specification are described in a progressive manner, with each embodiment focusing on its differences from other embodiments. Similar or identical parts between embodiments can be referred to interchangeably. For the apparatus disclosed in the embodiments, since it corresponds to the method disclosed in the embodiments, the description is relatively simple; relevant parts can be referred to the method section.

[0065] The above description of the disclosed embodiments enables those skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A glass microporous inner surface polishing apparatus, characterized by, include: A vacuum heat treatment furnace, wherein the vacuum heat treatment furnace is connected to an inlet pipe, an exhaust pipe, an outlet pipe, a circulation pipeline and a radio frequency oscillation device; The air intake pipe is connected to multiple air supply pipes; The exhaust pipe is connected to an exhaust gas treatment device. Both ends of the circulation pipeline are connected to the vacuum heat treatment furnace, and a circulation air pump is installed on the circulation pipeline. The radio frequency oscillation device is installed on the circulation pipeline at the end where the circulating gas enters the vacuum heat treatment furnace.

2. The glass microporous inner surface polishing device according to claim 1, characterized in that, There are two or more gas supply pipes.

3. A method for polishing the inner surface of glass micropores, characterized in that, The procedure, performed using the apparatus of claim 1 or 2, includes the following steps: (1) Place the TGV plate perpendicular to the airflow direction in the vacuum heat treatment furnace, and then evacuate the heat treatment furnace to a vacuum through the evacuation pipe; (2) Hydrogen and HCl gas are fed into the inlet pipe through the gas supply pipe and mixed, and then injected into the vacuum heat treatment furnace through the inlet pipe. (3) Heat the vacuum heat treatment furnace to the preset temperature and then keep it at that temperature; (4) Turn on the circulating gas pump to make the mixed gas of hydrogen and acid gas rushing into the vacuum heat treatment furnace circulate through the micropores on the TGV plate. Turn on the radio frequency oscillation device to ionize the circulating gas at the outlet of the circulating pipeline. After circulating polishing for a certain period of time, turn off the heat preservation and radio frequency oscillation device to allow the TGV plate to be cooled in the furnace. During the cooling process, continue to keep the mixed gas circulating. (5) When the temperature drops to room temperature, hydrogen is introduced again to discharge the mixed gas in the vacuum heat treatment furnace through the outlet pipe into the tail gas treatment device to eliminate the residual HCl gas component in the mixed gas. (6) After the mixed gas is exhausted, open the furnace and take out the polished TGV plate.

4. The method for polishing the inner surface of glass micropores according to claim 3, characterized in that, Step (1) was performed to a vacuum degree of 5 x 10 -4 Pa-1 x 10 -3 Pa.

5. The method for polishing the inner surface of glass micropores according to claim 3, characterized in that, The volume ratio of hydrogen to HCl gas is (8-10):

1.

6. The method for polishing the inner surface of glass micropores according to claim 3, characterized in that, In step (2), the gas pressure inside the furnace is 0.7-1.1 MPa.

7. The method for polishing the inner surface of glass micropores according to claim 3, characterized in that, The preset temperature mentioned in step (3) is 600-1200℃.

8. The method for polishing the inner surface of glass micropores according to claim 3, characterized in that, In step (4), the frequency of the radio frequency oscillation device is 13.56MHz; the flow rate of the circulating air pump is 0.3-0.5m / s, and the circulation time is 1.5-2h.

9. The method for polishing the inner surface of glass micropores according to claim 3, characterized in that, The exhaust gas treatment device is a water tank filled with water.

10. The method for polishing the inner surface of glass micropores according to claim 3, characterized in that, One or more TGV plates can be processed simultaneously, and multiple TGV plates are placed in parallel in a vacuum heat treatment furnace.