Method for attaching a vacuum panel lining

By combining ultra-fine composite grinding, non-woven fabric internal and external adhesive bonding, and high-pressure steam bonding with vacuum technology, the problem of secondary pollution of equipment and pipeline inner walls during the preparation of wet electronic chemicals has been solved, enabling the production of high-purity chemicals and reducing the content of metal ions and particulate matter.

CN118977503BActive Publication Date: 2026-06-05BEIJING UNIV OF CHEM TECH

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
BEIJING UNIV OF CHEM TECH
Filing Date
2024-09-28
Publication Date
2026-06-05

AI Technical Summary

Technical Problem

In existing technologies, wet electronic chemicals are easily contaminated by the inner walls of equipment and pipelines during the preparation process, leading to secondary contamination by metal ions and solid particles, which affects product purity and chip electrical performance.

Method used

The inner wall of the workpiece is treated using ultra-fine composite grinding technology, combined with non-woven fabric bonding inside and out and high-pressure steam bonding. Then, a vacuuming operation is performed, and a special board lining material and ultra-pure nitrogen are used for sealing to ensure a tight connection between the inner wall and the lining.

Benefits of technology

It effectively blocks the penetration of metal ions and particulate matter, improves the purity of chemicals, reduces the impurity content to below 5ppt, meets G5 grade requirements, extends the service life of the lining plate, and reduces costs.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a kind of vacuum plate lining attaching method, specifically comprising the following steps: (1) the workpiece to be treated is superfine composite polishing and polishing;(2) the wall surface of the workpiece to be treated is coated with glue, and the non-woven fabric is connected;(3) the surface of the non-woven fabric is coated with glue, and the plate lining material is connected;(4) pure nitrogen is introduced, and high-pressure steam is introduced;(5) vacuum operation is carried out between the inner wall of the workpiece to be treated and the plate lining material, and it is obtained immediately.The high-strength attaching vacuum plate lining technology used in the application is a special technology with characteristics such as corrosion resistance, wear resistance, high temperature resistance, chemical corrosion resistance, etc.It can efficiently block the penetration of metal ions and particulate matter in the inner wall of equipment and pipeline during the production process of wet electronic chemicals, greatly improves the purity of chemical products, meets the production requirements of G5 grade wet electronic chemicals, creatively reduces the content of various metal ion impurities to below 5ppt, significantly improves economic benefits, and speeds up the production process of high-purity high-end chemical production.
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Description

Technical Field

[0001] This invention relates to the field of chemical equipment manufacturing technology, and more specifically to a method for attaching a vacuum plate liner. Background Technology

[0002] Wet electronic chemicals are widely used in the microfabrication processes of electronic components such as chips, display panels, solar cells, and LEDs, including cleaning, photolithography, development, etching, and doping. In chip manufacturing, wet electronic chemicals can effectively remove residual contaminants from wafer surfaces and reduce the content of metal impurities, thus ensuring the quality of downstream products.

[0003] Distillation and absorption technologies are commonly used and crucial techniques for chemical purification, and are also indispensable in the preparation of wet electronic chemicals. During the preparation of wet electronic chemicals, materials are easily contaminated through contact with tower equipment, tank equipment, pump equipment, pipelines, etc., thus affecting the purity of the wet electronic chemicals.

[0004] To ensure a high yield rate for chips, wet electronic chemicals have extremely high requirements for metal ions and particulate matter content, at the ppt level. This is equivalent to exceeding the limit by 200 times if a single drop of ink is added to a standard swimming pool. Trace amounts of metal impurities can severely affect the electrical performance of chips and reduce their reliability. Throughout the entire production process, metal ions and particulate matter seeping from all equipment and pipes in contact with the materials inevitably cause secondary contamination of the wet electronic chemicals.

[0005] Therefore, how to avoid secondary pollution from wet electronic chemicals is a problem that urgently needs to be solved by those skilled in the art. Summary of the Invention

[0006] In view of this, the purpose of the present invention is to provide a method for attaching a vacuum plate liner to overcome the shortcomings of the prior art.

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

[0008] A method for attaching a vacuum plate liner, characterized by comprising the following steps:

[0009] (1) Perform ultra-fine composite grinding and polishing on the workpiece (steel or container) to be processed;

[0010] (2) Apply glue to the wall surface of the workpiece to be processed and connect the non-woven fabric;

[0011] (3) Apply glue to the surface of the non-woven fabric and connect the board lining material;

[0012] (4) When ultra-fine composite grinding and polishing, applying glue, connecting non-woven fabric and connecting board lining material, ultra-pure nitrogen is continuously introduced, and high-pressure steam is continuously introduced when connecting non-woven fabric and connecting board lining material.

[0013] (5) Perform a vacuuming operation between the inner wall of the workpiece to be processed and the plate lining material to obtain the final product.

[0014] Furthermore, in step (1) above, the ultra-fine composite grinding and polishing includes at least one of ultrasonic grinding, magnetic grinding, chemical grinding and mechanical grinding.

[0015] Furthermore, the above-mentioned ultrasonic grinding specifically involves placing the workpiece to be processed in an ultrasonic environment, with an ultrasonic wavelength λ of 0.02 to 2 cm.

[0016] The further beneficial effect of the above method is that it uses ultrasonic waves to remove loose burrs and particles from the surface of the workpiece.

[0017] Furthermore, the above-mentioned magnetic abrasive grinding specifically involves filling the workpiece with high-performance abrasive and polishing materials such as silicon nitride grinding media balls, silicon carbide, diamond, and resin. The workpiece is then accompanied by a fluid flow, rotating at a certain speed while simultaneously vibrating axially. A strong DC magnetic field is applied in a plane perpendicular to the axis of the workpiece and the electric field lines.

[0018] The further beneficial effect of the above-mentioned method is that the "abrasive brush" composed of magnetic abrasives rapidly impacts the surface of the workpiece to be treated, removing particulate matter and crystals.

[0019] Furthermore, the aforementioned chemical grinding specifically involves placing the workpiece to be treated in an electrolyte environment and passing an electric current through it for electrochemical treatment.

[0020] The further beneficial effect of the above method is that the anode of the current and voltage is connected to the burr crystallization part of the workpiece to be treated, the cathode is connected to the conductive tool with abrasive particles, and the electrolyte is driven by the pump to flow through the cathode and anode to the burr crystallization part of the workpiece to be treated and reach the return tank. This can precisely remove burrs, smooth the surface of the workpiece to be treated, and control the surface roughness Ra of the workpiece to be treated to be 0.2 to 2 μm.

[0021] Furthermore, in steps (2) and (3) above, the adhesive is at least one of the following film-forming adhesives: acrylic acid, modified copolymer emulsion of acrylic acid and vinyl acetate, and hot melt adhesive web.

[0022] The further beneficial effect of the above method is that the non-woven fabric is coated with adhesive on both the inner and outer sides, and different types of adhesive are selected according to the wall material and lining material of the workpiece to be treated, so as to strongly adhere to the wall and lining.

[0023] Furthermore, in step (2) above, the nonwoven fabric is at least one of polypropylene, polyester, natural fiber and chemical fiber.

[0024] Furthermore, in step (3) above, the plate lining material is an alloy containing at least one of chromium, manganese and molybdenum, and is treated by a quenching process, with a surface roughness Ra of less than 10 μm.

[0025] The further beneficial effects of the above-mentioned method are that the lining material selected in this invention has a smooth lining surface in contact with chemicals, and the lining material after quenching is wear-resistant, corrosion-resistant, and does not release pollutants harmful to the material. The side in contact with the non-woven fabric adheres strongly to the non-woven fabric, which can effectively prevent metal ions and particles from penetrating into the material from the wall of the workpiece to be treated.

[0026] Furthermore, in step (4) above, the gauge pressure of the high-pressure steam is 10 to 200 kPa.

[0027] The further beneficial effects of the above-mentioned approach are that ultra-pure nitrogen gas is introduced into the ultra-fine composite grinding and polishing process, the non-woven fabric and inner / outer adhesive application process, and the lining installation process, thus avoiding the introduction of secondary pollution. High-pressure steam is continuously introduced during the installation of the non-woven fabric and lining, accelerating the adhesion of the non-woven fabric and lining to the adhesive. Simultaneously, the high-pressure steam ensures the flatness, smoothness, and integrity of the non-woven fabric and lining installation, keeping the maximum height Rz of the installation contour below 5μm.

[0028] Furthermore, in step (5) above, a vacuum is drawn until the absolute pressure of the gap is 30 to 98 kPa.

[0029] The further beneficial effect of adopting the above-mentioned method is that it enables vacuuming of the gaps in the nonwoven fabric connection, making the connection between the liner and the inner wall of the workpiece to be treated tighter, preventing the liner from falling off, reducing the impurity content and mass transfer driving force, and preventing the penetration of metal ions and particulate matter.

[0030] As can be seen from the above technical solution, compared with the prior art, the beneficial effects of the present invention are as follows:

[0031] 1. This invention utilizes ultra-fine composite grinding technology, employing ultrasonic, magnetic, chemical, and mechanical methods to grind the inner wall of the workpiece, efficiently removing burrs and crystals from the inner wall. This reduces the release of metal ions and particulate matter at the source. Furthermore, this ultra-fine composite grinding and polishing technology is more efficient than single grinding techniques, ensuring the smoothness and flatness of the inner wall while removing burrs or crystals, preventing the introduction of secondary burrs or crystals. A specially formulated non-woven fabric is used for internal and external adhesive bonding, strongly adhering the lining. A special lining material is developed, with a smooth, precise, wear-resistant, and corrosion-resistant surface, preventing the penetration of impurities such as metal ions and solid particles. A new high-pressure steam drum-type installation process is proposed to ensure the lining's blocking effect. A vacuum operation is performed between the equipment's inner wall and the lining to prevent the penetration of metal ions and lining detachment from the equipment and pipe walls. The internal and external adhesive bonding method of the non-woven fabric, combined with the vacuum technology in the gaps of the non-woven fabric, provides dual protection for the connection between the inner wall and the lining, greatly extending the life of the lining and saving costs. An ultra-pure nitrogen sealing film prevents secondary contamination during transportation.

[0032] 2. This invention achieves effective prevention of metal ions and particulate matter penetration from the surface of the workpiece by using ultra-fine grinding of the workpiece wall, strong adhesion of non-woven fabric inside and outside, development of special board lining materials, high-pressure steam drum pressing and installation, vacuuming operation between the inner wall of the equipment and the lining, and ultra-pure nitrogen sealing film, thereby greatly improving the purity of chemicals.

[0033] 3. The high-strength vacuum lining technology used in this invention is a special technology with special properties such as corrosion resistance, wear resistance, high temperature resistance, and chemical corrosion resistance. In the production process of wet electronic chemicals, it can effectively block the penetration of metal ions and particulate matter into the inner wall of equipment and pipelines, greatly improving the purity of chemical products and meeting the production requirements of G5 grade wet electronic chemicals. It creatively reduces the content of various metal ion impurities to below 5ppt, significantly improving economic benefits and accelerating the production process of high-purity and high-end chemicals. Attached Figure Description

[0034] Figure 1 A schematic diagram of ultra-fine composite grinding and polishing;

[0035] Figure 2 This is a schematic diagram of the method for attaching a vacuum plate liner. Detailed Implementation

[0036] The technical solutions in the embodiments of the present invention will be clearly and completely described below. 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 skilled in the art without creative effort are within the scope of protection of the present invention.

[0037] Example 1

[0038] Vacuum plate liner application method, such as Figure 1 and Figure 2 As shown, the specific steps include:

[0039] (1) Perform ultra-fine composite grinding and polishing on the workpiece to be processed;

[0040] Ultrasonic grinding and magnetic grinding are used. External reinforcing magnetic poles and ultrasonic sources are placed in a plane perpendicular to the axis and electric field lines of the workpiece to be treated. The ultrasonic wavelength λ is controlled to 2cm to remove loose burrs and particles from the wall surface. Silicon nitride grinding media balls are filled into the workpiece to be treated. They flow over the wall surface along the axial direction and cut the magnetic field lines in an axial and rotational manner. The magnetic abrasive in the high-performance grinding and polishing material is stirred to grind the wall surface and remove burrs and crystals.

[0041] (2) Apply acrylic adhesive to the wall surface of the workpiece to be treated and connect it with polypropylene non-woven fabric;

[0042] (3) Coat the surface of the polypropylene nonwoven fabric with acrylic adhesive and connect the chromium manganese alloy plate lining material.

[0043] (4) When ultra-fine composite grinding and polishing, applying acrylic glue, connecting polypropylene non-woven fabric and connecting chromium manganese alloy plate lining material, ultra-pure nitrogen gas is continuously introduced, and when connecting polypropylene non-woven fabric and connecting chromium manganese alloy plate lining material, high-pressure steam with a gauge pressure of 10 kPa is continuously introduced.

[0044] (5) Perform a vacuuming operation between the inner wall of the workpiece to be processed and the plate lining material, and vacuum until the absolute pressure of the gap is 30 kPa.

[0045] Example 2

[0046] Vacuum plate liner application method, such as Figure 1 and Figure 2 As shown, the specific steps include:

[0047] (1) Perform ultra-fine composite grinding and polishing on the workpiece to be processed;

[0048] Chemical grinding and magnetic grinding are used. The anode of the external voltage is connected to the inner wall of the workpiece to be treated with burrs and crystals, and the cathode of the external voltage is connected to silicon carbide. The silicon carbide flows through the wall along the axis of the workpiece and electrolyzes to remove the burrs and crystals on the inner wall, so as to achieve the leveling of the wall surface of the workpiece to be treated.

[0049] (2) Apply acrylic adhesive to the wall surface of the workpiece to be treated and connect it with polypropylene non-woven fabric;

[0050] (3) Coat the surface of the polypropylene nonwoven fabric with acrylic adhesive and connect the chromium manganese alloy plate lining material.

[0051] (4) When ultra-fine composite grinding and polishing, applying acrylic glue, connecting polypropylene non-woven fabric and connecting chromium manganese alloy plate lining material, ultra-pure nitrogen gas is continuously introduced, and when connecting polypropylene non-woven fabric and connecting chromium manganese alloy plate lining material, high-pressure steam with a gauge pressure of 200 kPa is continuously introduced.

[0052] (5) Perform a vacuuming operation between the inner wall of the workpiece to be processed and the plate lining material, and vacuum until the absolute pressure of the gap is 98 kPa.

[0053] Performance testing

[0054] Vacuum lining plates were attached to the inner walls of all equipment and pipelines in contact with materials during the entire process of electronic-grade hydrofluoric acid production, respectively, according to the methods of Example 1 and Example 2. The particle content and metal ion content in the electronic-grade hydrofluoric acid product were then tested.

[0055] The particle content was detected using scanning electron microscopy-X-ray energy-dispersive spectroscopy (SEM-EDX), which included the following steps:

[0056] I. Preliminary Preparations

[0057] 1. Check whether the connections of the power supply, cooling water, vacuum pump and other equipment are normal, and ensure that the voltage is stable and meets the equipment requirements.

[0058] 2. Place the prepared sample on the sample stage, ensuring good contact between the sample and the stage surface. If necessary, use conductive tape or clamps to secure it. Place the sample stage containing the sample into the sample chamber of the scanning electron microscope and close the sample chamber door.

[0059] II. Vacuuming and Equipment Start-up

[0060] 1. Use a vacuum pump to evacuate the air from the sample chamber to achieve the required vacuum level (usually less than 10). -3 Pa).

[0061] 2. Start the scanning electron microscope (SEM) and open the relevant software interface. Set the SEM parameters such as accelerating voltage, magnification, and scanning speed on the software interface.

[0062] III. Focusing and Calibration

[0063] 1. Focus the sample by adjusting the objective lens and lens to make the image clear.

[0064] 2. Perform necessary calibration operations, such as adjusting the scanning speed and scanning mode of the electron beam, to ensure the accuracy and stability of the image.

[0065] IV. EDS Analysis

[0066] 1. Select test type: Select the EDS test type on the software interface. Commonly used tests include point scan (Point & ID), line scan, and area scan (Mapping).

[0067] 2. Scan Image: Scan the sample to obtain an image, depending on the selected test type.

[0068] 3. EDS Test: For point scan tests, select the point to be tested or the rectangular area to be tested, and the software will automatically perform spectral analysis. For area scan tests, first scan the image, then select to acquire distribution map data and start the test.

[0069] 4. Identify the particle types in the sample using Auto ID or manual selection. Switch to the Calculate Components interface, edit the columns, and check the desired component percentages (e.g., At%) to calculate the relative content of particles.

[0070] The metal ion content was detected using inductively coupled plasma mass spectrometry (ICP-MS), which specifically included the following steps:

[0071] I. Sample Pretreatment

[0072] 1. Sample digestion: The sample is completely dissolved using methods such as acid digestion, microwave digestion, and hot plate digestion, while avoiding the loss or contamination of the analyte.

[0073] 2. Volume Adjustment and Dilution: The digested sample solution needs to be adjusted to an appropriate volume and diluted as necessary according to the concentration of the element to be measured to ensure that the measurement results are within the linear range of ICP-MS.

[0074] 3. Filtration and purification: To avoid damage to the ICP-MS instrument from suspended particles or impurities in the sample, the digested sample solution needs to be filtered and purified through a filter membrane.

[0075] II. Instrument Preparation

[0076] 1. Power-on preheating: Start the ICP-MS instrument and its supporting equipment (such as autosampler, gas supply system, etc.) and preheat it to allow the instrument to reach a stable state.

[0077] 2. Instrument Tuning: Use tuning fluid to tune the ICP-MS instrument, adjusting various parameters (such as RF power, plasma gas flow rate, sampling cone angle, etc.) to ensure the instrument is in optimal working condition. During tuning, pay attention to performance indicators such as sensitivity, resolution, oxide ratio, and double charge ratio.

[0078] III. Sample Determination

[0079] 1. Standard Curve Construction: A standard curve is constructed by using a series of standard solutions of known concentrations. The correlation coefficient of the standard curve should be above 0.99 to ensure the accuracy of the measurement results.

[0080] 2. Sample Determination: The prepared sample solution is introduced into the ICP-MS instrument for determination. Based on the different mass-to-charge ratios of the analytes, the instrument will automatically separate and detect the ion signal intensity of each element.

[0081] The test results are shown in Table 1.

[0082] Table 1. Particle content and metal ion content in Examples 1-2 used for the production of electronic-grade hydrofluoric acid.

[0083]

[0084] As shown in Table 1, the hydrofluoric acid produced by the equipment and pipeline inner walls after the vacuum plate lining is attached using the method of the present invention can reach the electronic grade and the E2 grade, indicating high quality.

[0085] The above experiments demonstrate that the high-strength vacuum lining technology used in this invention is a special technology with characteristics such as corrosion resistance, wear resistance, high temperature resistance, and chemical corrosion resistance. In the production process of wet electronic chemicals, it can effectively block the penetration of metal ions and particulate matter into the inner walls of equipment and pipelines, greatly improving the purity of chemical products. It can meet the production requirements of G5 grade wet electronic chemicals, creatively reducing the content of various metal ion impurities to below 5ppt, significantly improving economic benefits, and accelerating the production process of high-purity and high-end chemicals.

[0086] 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 method for attaching vacuum plate liners used in chemical equipment, characterized in that, Specifically, the following steps are included: (1) Perform ultra-fine composite grinding and polishing on the workpiece to be processed; The workpiece to be processed is steel. The ultra-fine composite grinding and polishing includes at least two of ultrasonic grinding, magnetic grinding, chemical grinding and mechanical grinding; The ultrasonic grinding process specifically involves placing the workpiece to be processed in an ultrasonic environment, where the ultrasonic wavelength λ is 0.02–2 cm. The magnetic abrasive grinding specifically involves: filling the workpiece with high-performance abrasive and polishing material, allowing fluid to flow through the workpiece, rotating at a certain speed while simultaneously vibrating axially, and applying a strong DC magnetic field in a plane perpendicular to the axis of the workpiece and the electric field lines. The chemical grinding process specifically involves placing the workpiece to be treated in an electrolyte environment and passing an electric current through it for electrochemical treatment. (2) Apply glue to the wall surface of the workpiece to be processed and connect the non-woven fabric; The nonwoven fabric is at least one of polypropylene, polyester and natural fibers; (3) Apply glue to the surface of the non-woven fabric and connect the board lining material; In steps (2) and (3), the adhesive is at least one of acrylic acid and modified copolymer emulsion of acrylic acid and vinyl acetate; The plate lining material is an alloy containing at least one of chromium, manganese and molybdenum, and is treated by quenching process, with a surface roughness Ra of less than 10 μm; (4) When ultra-fine composite grinding and polishing, applying glue, connecting non-woven fabric and connecting board lining material, ultra-pure nitrogen is continuously introduced, and high-pressure steam is continuously introduced when connecting non-woven fabric and connecting board lining material. (5) Perform a vacuuming operation between the inner wall of the workpiece to be processed and the plate lining material to obtain the final product.

2. The method for attaching a vacuum plate liner to chemical equipment according to claim 1, characterized in that, In step (4), the gauge pressure of the high-pressure steam is 10 to 200 kPa.

3. The method for attaching a vacuum plate liner to chemical equipment according to claim 1, characterized in that, In step (5), the vacuum is drawn until the absolute pressure of the gap is 30-98 kPa.