CN110977629B - Sapphire window sheet and polishing process thereof - Google Patents
Sapphire window sheet and polishing process thereof Download PDFInfo
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- CN110977629B CN110977629B CN201911342333.1A CN201911342333A CN110977629B CN 110977629 B CN110977629 B CN 110977629B CN 201911342333 A CN201911342333 A CN 201911342333A CN 110977629 B CN110977629 B CN 110977629B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
- B24B1/04—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes subjecting the grinding or polishing tools, the abrading or polishing medium or work to vibration, e.g. grinding with ultrasonic frequency
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B49/00—Measuring or gauging equipment for controlling the feed movement of the grinding tool or work; Arrangements of indicating or measuring equipment, e.g. for indicating the start of the grinding operation
- B24B49/006—Measuring or gauging equipment for controlling the feed movement of the grinding tool or work; Arrangements of indicating or measuring equipment, e.g. for indicating the start of the grinding operation taking regard of the speed
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B49/00—Measuring or gauging equipment for controlling the feed movement of the grinding tool or work; Arrangements of indicating or measuring equipment, e.g. for indicating the start of the grinding operation
- B24B49/16—Measuring or gauging equipment for controlling the feed movement of the grinding tool or work; Arrangements of indicating or measuring equipment, e.g. for indicating the start of the grinding operation taking regard of the load
- B24B49/165—Measuring or gauging equipment for controlling the feed movement of the grinding tool or work; Arrangements of indicating or measuring equipment, e.g. for indicating the start of the grinding operation taking regard of the load for grinding tyres
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
- C30B33/10—Etching in solutions or melts
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
A sapphire window sheet polishing process belongs to the technical field of sapphire window sheet manufacturing. The sapphire window sheet polishing process comprises the following steps: soaking treatment: firstly, soaking a sapphire sheet subjected to fine grinding treatment in high-temperature high-concentration concentrated phosphoric acid, taking out the sapphire sheet and soaking the sapphire sheet in hydrofluoric acid; ultrasonic polishing: and (3) putting the sapphire sheet subjected to soaking treatment into a double-sided polishing machine, and polishing by adopting an alumina polishing solution with large particle size and high pH value under the assistance of ultrasound to obtain the sapphire window sheet. The method provided by the invention can improve the polishing rate and ensure the precision requirement of the surface roughness of the sapphire window sheet.
Description
Technical Field
The invention relates to the technology in the polishing field, in particular to a sapphire window sheet and a polishing process thereof.
Background
The sapphire window sheet has the main component of alumina, has excellent mechanical property, thermal property, electrical property and dielectric property, is chemical corrosion resistant, and has the advantages of high temperature resistance, good heat conduction, high hardness, infrared transmission and good chemical stability. Therefore, the optical glass is commonly used for replacing other optical materials to manufacture optical elements and infrared-transmitting optical window sheets, and is widely applied to the aspects of infrared and far infrared military equipment, such as instruments such as night vision infrared and far infrared sighting lenses, night vision cameras and the like, satellites, instruments and meters of space technology, windows of high-power lasers, various optical prisms, optical windows, UV and IR windows and lenses, observation ports of low-temperature experiments, and the like, and is fully applied to the aspects of high-precision instruments and meters for aviation and aviation in seagoing and aviation.
At present, the processing quality of the surface of the sapphire substrate sheet or the window sheet plays an important role in the epitaxial growth quality and performance of materials. At present, the sapphire sheets produced industrially in China generally have the defects of coarse grinding (consistence), fine grinding (flattening) and polishing (mirror surface), and because the sapphire belongs to a hard and brittle material, the defects of low efficiency, deep and shallow scratches, pits, fogging and the like on the surface are easy to occur in the polishing process.
In the prior art, silicon oxide-based (80-120 nm) or aluminum oxide-based (about 300 nm) polishing solution is directly adopted after fine grinding, the polishing efficiency is low by 5-6 mu m/h, the scratch rate is 5%, and the surface roughness Ra is about 0.3 nm.
The present invention has been made to solve the above-mentioned problems occurring in the prior art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the sapphire window sheet and the polishing process thereof, which can improve the polishing rate and ensure the precision requirement of the surface roughness of the sapphire window sheet.
The invention relates to a sapphire window sheet polishing process, which comprises the following steps:
soaking treatment: firstly, soaking a sapphire sheet subjected to fine grinding treatment in high-temperature high-concentration concentrated phosphoric acid, taking out the sapphire sheet and then soaking the sapphire sheet in hydrofluoric acid;
ultrasonic polishing: and (3) putting the sapphire sheet subjected to soaking treatment into a double-sided polishing machine, and polishing by adopting polishing solution under the assistance of ultrasound to obtain the sapphire window sheet.
The concentration of the concentrated phosphoric acid is 83-98 percent, and the temperature is 100-200 ℃.
In the soaking treatment step, the sapphire sheet is soaked in concentrated phosphoric acid for 20-40min and in hydrofluoric acid for 10-20 min. Preferably, the soaking time in concentrated phosphoric acid is 30min, and the soaking time in hydrofluoric acid is 10-15 min.
The polishing solution is alumina polishing solution, pH value is 13-14, and the particle diameter D50 of alumina particles is 0.8-2.0 μm, preferably 0.8-1.2 μm; by adopting the alumina-based polishing solution with large particle size, the pH value of the polishing solution is increased, the balance of chemical mechanical polishing can be achieved, and the polishing efficiency is improved more effectively.
In the ultrasonic polishing step, the polishing pressure is 450-.
In the polishing step, a suba800 grooved polishing pad is adopted, and the main component is polyurethane doped with various mixtures.
The invention relates to a sapphire window sheet which is manufactured by adopting the polishing process.
Technical effects
Compared with the prior art, the invention has the following technical effects:
1) the polishing rate can reach 8-10 μm/h, the overall yield is more than 96%, 50 x 50 μm2The surface roughness Ra of the sapphire window sheet with the size is 0.2-0.3 nm;
2) before polishing, the sapphire wafer is subjected to long-time high-temperature soaking treatment by concentrated phosphoric acid to complete surface corrosion, and then a damaged layer caused by concentrated phosphoric acid corrosion is repaired by soaking with hydrofluoric acid to release stress; the subsequent ultrasonic polishing treatment is facilitated, and the problem that the corrosion of the polishing solution cannot reach the global condition in the direct polishing is avoided;
3) the ultrasonic-assisted polishing is adopted, so that the problem that polishing solution particles are agglomerated and mechanical stirring is difficult to disperse is solved, and the problem that scratches appear on the surface of sapphire due to the agglomeration of the particles in the polishing process is avoided.
Drawings
FIG. 1 is a flow chart of an embodiment of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific embodiments.
Example 1
As shown in fig. 1, the present embodiment includes the following steps:
s1, cleaning the 2-inch sapphire sheets after the fine grinding treatment, and dividing the sapphire sheets into 144 pieces in each group according to the thickness, wherein the thickness error of the same group is within 2 mu m;
s2, measuring the thicknesses of all sapphire sheet center points, and recording serial numbers and thickness data;
s3, soaking the sapphire sheets prepared in the S1 and S2 in concentrated phosphoric acid with the temperature of 100 ℃ and the concentration of 95% for 30min, then soaking in hydrofluoric acid for 15min, taking out the sapphire sheets after soaking, cleaning, and sequentially placing in a 18B double-side polishing machine;
s4, adhering a suba800 grooved polishing pad on the upper disc and the lower disc of the double-sided polishing machine, circularly polishing for 8 times by using an alumina polishing solution with the particle size D50 of 0.8 mu m and the weight ratio of alumina particles to water of 1:10 according to the polishing pressure of 450kg, the lower disc rotation speed of 40rpm and the flow of 5L/min, controlling the pH value of the polishing solution to be 13, polishing for 60min to obtain a sapphire window sheet, and taking out and cleaning after polishing; in the polishing process, 20-120kHz ultrasonic auxiliary polishing is adopted;
and S5, measuring the quality of the finished product, wherein the center point thickness of the sapphire window slice is measured clockwise by using a measuring meter from the starting slice, and the defect surface of the sapphire window slice is inspected by using a microscope, and the result is shown in the table 1.
Example 2
The embodiment comprises the following steps:
s1, cleaning the 2-inch sapphire sheets after the fine grinding treatment, and dividing the sapphire sheets into 144 pieces in each group according to the thickness, wherein the thickness error of the same group is within 2 mu m;
s2, measuring the thicknesses of all sapphire sheet center points, and recording serial numbers and thickness data;
s3, soaking the sapphire sheets prepared in the S1 and S2 in concentrated phosphoric acid with the temperature of 150 ℃ and the concentration of 88% for 30min, then soaking in hydrofluoric acid for 15min, taking out the sapphire sheets after soaking, cleaning, and sequentially placing in a 18B double-side polishing machine;
s4, adhering a suba800 grooved polishing pad on the upper disc and the lower disc of the double-sided polishing machine, circularly polishing for 8 times by using an alumina polishing solution with the particle diameter D50 of 1 mu m and the weight ratio of alumina particles to water of 1:10 according to the polishing pressure of 500kg, the lower disc rotation speed of 40rpm and the flow of 5L/min, controlling the pH value of the polishing solution to be 13.5, polishing for 60min to obtain a sapphire window sheet, and taking out and cleaning after polishing; in the polishing process, 20-120kHz ultrasonic auxiliary polishing is adopted;
and S5, measuring the quality of the finished product, wherein the center point thickness of the sapphire window slice is measured clockwise by using a measuring meter from the starting slice, and the defect surface of the sapphire window slice is inspected by using a microscope, and the result is shown in the table 1.
Example 3
The embodiment comprises the following steps:
s1, cleaning the 2-inch sapphire sheets after the fine grinding treatment, and dividing the sapphire sheets into 144 pieces in each group according to the thickness, wherein the thickness error of the same group is within 2 mu m;
s2, selecting a sapphire wafer as an initial wafer, and measuring the thickness of a central point of the sapphire wafer; measuring the thickness of the center points of other sapphire sheets in the same group clockwise, and recording to obtain the thickness data of the center points of all the sapphire sheets; repeating the operation, and measuring the thickness of the center point of each remaining group of sapphire sheets;
s3, soaking the sapphire sheets prepared in the S1 and S2 in 93% concentrated phosphoric acid at the temperature of 150 ℃ for 30min, then soaking the sapphire sheets in hydrofluoric acid for 15min, taking out the sapphire sheets after soaking, cleaning the sapphire sheets, and sequentially placing the sapphire sheets in a 18B double-side polishing machine;
s4, adhering a suba800 grooved polishing pad on the upper disc and the lower disc of the double-sided polishing machine, circularly polishing for 8 times by using an alumina polishing solution with the particle diameter D50 of 1.2 mu m and the weight ratio of alumina particles to water of 1:10 according to the polishing pressure of 500kg, the rotation speed of the lower disc of 45rpm and the flow of 8L/min, controlling the pH value of the polishing solution to be 13.5, polishing for 60min to obtain a sapphire window sheet, and taking out and cleaning after polishing; in the polishing process, 20-120kHz ultrasonic auxiliary polishing is adopted;
and S5, measuring the quality of the finished product, wherein the center point thickness of the sapphire window slice is measured clockwise by using a measuring meter from the starting slice, and the defect surface of the sapphire window slice is inspected by using a microscope, and the result is shown in the table 1.
Example 4
The embodiment comprises the following steps:
s1, cleaning the 2-inch sapphire sheets after the fine grinding treatment, and dividing the sapphire sheets into 144 pieces in each group according to the thickness, wherein the thickness error of the same group is within 2 mu m;
s2, measuring the thicknesses of all sapphire sheet center points, and recording serial numbers and thickness data;
s3, soaking the sapphire sheets prepared in the S1 and S2 in concentrated phosphoric acid with the temperature of 200 ℃ and the concentration of 92% for 30min, then soaking in hydrofluoric acid for 15min, taking out the sapphire sheets after soaking, cleaning, and sequentially placing in a 18B double-side polishing machine;
s4, adhering a suba800 grooved polishing pad on the upper disc and the lower disc of the double-sided polishing machine, circularly polishing for 8 times by using an alumina polishing solution with the particle diameter D50 of 1.2 mu m and the weight ratio of alumina particles to water of 1:10 according to the polishing pressure of 500kg, the lower disc rotation speed of 50rpm and the flow rate of 8L/min, controlling the pH value of the polishing solution at 14, polishing for 60min to obtain a sapphire window sheet, and taking out and cleaning after polishing; in the polishing process, 20-120kHz ultrasonic auxiliary polishing is adopted;
and S5, measuring the quality of the finished product, wherein the center point thickness of the sapphire window slice is measured clockwise by using a measuring meter from the starting slice, and the defect surface of the sapphire window slice is inspected by using a microscope, and the result is shown in the table 1.
Example 5
The embodiment comprises the following steps:
s1, cleaning the 2-inch sapphire sheets after the fine grinding treatment, and dividing the sapphire sheets into 144 pieces in each group according to the thickness, wherein the thickness error of the same group is within 2 mu m;
s2, measuring the thicknesses of all sapphire sheet center points, and recording serial numbers and thickness data;
s3, soaking the sapphire sheets prepared in the S1 and S2 in concentrated phosphoric acid with the temperature of 200 ℃ and the concentration of 90% for 30min, then soaking in hydrofluoric acid for 15min, taking out the sapphire sheets after soaking, cleaning, and sequentially placing in a 18B double-side polishing machine;
s4, adhering a suba800 grooved polishing pad on the upper disc and the lower disc of the double-sided polishing machine, circularly polishing for 8 times by using an alumina polishing solution with the particle diameter D50 of 1.2 mu m and the weight ratio of alumina particles to water of 1:10 according to the polishing pressure of 550kg, the lower disc rotation speed of 50rpm and the flow rate of 8L/min, controlling the pH value of the polishing solution to be 13, polishing for 60min to obtain a sapphire window sheet, and taking out and cleaning after polishing; in the polishing process, 20-120kHz ultrasonic auxiliary polishing is adopted;
and S5, measuring the quality of the finished product, wherein the center point thickness of the sapphire window slice is measured clockwise by using a measuring meter from the starting slice, and the defect surface of the sapphire window slice is inspected by using a microscope, and the result is shown in the table 1.
Example 6
The embodiment comprises the following steps:
s1, cleaning the 2-inch sapphire sheets after the fine grinding treatment, and dividing the sapphire sheets into 144 pieces in each group according to the thickness, wherein the thickness error of the same group is within 2 mu m;
s2, measuring the thicknesses of all sapphire sheet center points, and recording serial numbers and thickness data;
s3, soaking the sapphire sheets prepared in the S1 and S2 in concentrated phosphoric acid with the temperature of 200 ℃ and the concentration of 94% for 30min, then soaking in hydrofluoric acid for 15min, taking out the sapphire sheets after soaking, cleaning, and sequentially placing in a 18B double-side polishing machine;
s4, adhering a suba800 grooved polishing pad on the upper disc and the lower disc of the double-sided polishing machine, circularly polishing for 8 times by using an alumina polishing solution with the particle diameter D50 of 1.2 mu m and the weight ratio of alumina particles to water of 1:10 according to the polishing pressure of 550kg, the lower disc rotation speed of 50rpm and the flow rate of 10L/min, controlling the pH value of the polishing solution at 14, polishing for 60min to obtain a sapphire window sheet, and taking out and cleaning after polishing; in the polishing process, 20-120kHz ultrasonic auxiliary polishing is adopted;
and S5, measuring the quality of the finished product, wherein the center point thickness of the sapphire window slice is measured clockwise by using a measuring meter from the starting slice, and the defect surface of the sapphire window slice is inspected by using a microscope, and the result is shown in the table 1.
TABLE 1 comparison table of sapphire window sheet process and performance
It is to be emphasized that: the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and all simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (4)
1. A sapphire window sheet polishing process is characterized by comprising the following steps:
soaking treatment: firstly, soaking a sapphire sheet subjected to fine grinding treatment in high-temperature high-concentration concentrated phosphoric acid, taking out the sapphire sheet and soaking the sapphire sheet in hydrofluoric acid;
ultrasonic polishing: putting the sapphire sheet subjected to soaking treatment into a double-sided polishing machine, and polishing by adopting polishing solution under the assistance of ultrasound to obtain a sapphire window sheet;
in the soaking treatment step, the concentration of concentrated phosphoric acid is 83-98%, the temperature is 100-200 ℃, the soaking time of the sapphire sheet in the concentrated phosphoric acid is 20-40min, and the soaking time in hydrofluoric acid is 10-20 min;
in the ultrasonic polishing step, the polishing solution is alumina polishing solution, the pH value is 13-14, and the particle size D50 of alumina particles is 0.8-2.0 μm.
2. The sapphire window wafer polishing process of claim 1, wherein in the soaking treatment step, the sapphire wafer is soaked in concentrated phosphoric acid for 30min and in hydrofluoric acid for 10-15 min.
3. The sapphire window wafer polishing process of claim 1, wherein in the ultrasonic polishing step, the polishing pressure is 450kg and 550kg, the lower disc rotation speed is 40-50rpm, and the flow rate is 5-10L/min.
4. A sapphire window plate produced by the polishing process of any one of claims 1 to 3.
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| CN105058174A (en) * | 2015-08-04 | 2015-11-18 | 常州市好利莱光电科技有限公司 | Machining method for sapphire watch window |
| CN106206279A (en) * | 2016-07-28 | 2016-12-07 | 常州亿晶光电科技有限公司 | A kind of chemically polishing method of sapphire filament wafer |
| CN106271900A (en) * | 2016-08-31 | 2017-01-04 | 天通银厦新材料有限公司 | A kind of sapphire glossing |
| JP2017185560A (en) * | 2016-04-01 | 2017-10-12 | 富士紡ホールディングス株式会社 | Polishing pad and production method and polishing method of polishing pad |
| CN110316970A (en) * | 2019-05-31 | 2019-10-11 | 中国建筑材料科学研究总院有限公司 | The preparation method of ultra-thin quartz glass piece |
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2019
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101716745A (en) * | 2009-11-09 | 2010-06-02 | 清华大学 | Device and method for polishing sapphire substrate material by ultrasound assisted chemical machinery |
| CN104842225A (en) * | 2015-04-22 | 2015-08-19 | 苏州爱彼光电材料有限公司 | Wet processing method for large-dimension sapphire substrate surface |
| CN105058174A (en) * | 2015-08-04 | 2015-11-18 | 常州市好利莱光电科技有限公司 | Machining method for sapphire watch window |
| JP2017185560A (en) * | 2016-04-01 | 2017-10-12 | 富士紡ホールディングス株式会社 | Polishing pad and production method and polishing method of polishing pad |
| CN106206279A (en) * | 2016-07-28 | 2016-12-07 | 常州亿晶光电科技有限公司 | A kind of chemically polishing method of sapphire filament wafer |
| CN106271900A (en) * | 2016-08-31 | 2017-01-04 | 天通银厦新材料有限公司 | A kind of sapphire glossing |
| CN110316970A (en) * | 2019-05-31 | 2019-10-11 | 中国建筑材料科学研究总院有限公司 | The preparation method of ultra-thin quartz glass piece |
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Effective date of registration: 20220629 Address after: 215000 first and second floors on the east side of Building 8, No. 432 Fengyang Road, Yangchenghu Town, Xiangcheng District, Suzhou City, Jiangsu Province Patentee after: Suzhou routao New Material Co.,Ltd. Address before: 215000 No. 488 Songshan Road, high tech Zone, Suzhou City, Jiangsu Province Patentee before: Suzhou Nanodispersions Ltd. |