CN110790512A - Method for stripping quartz plate by wet etching - Google Patents
Method for stripping quartz plate by wet etching Download PDFInfo
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- CN110790512A CN110790512A CN201910967785.2A CN201910967785A CN110790512A CN 110790512 A CN110790512 A CN 110790512A CN 201910967785 A CN201910967785 A CN 201910967785A CN 110790512 A CN110790512 A CN 110790512A
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- quartz plate
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling compositions
- C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
- C09K13/08—Etching, surface-brightening or pickling compositions containing an inorganic acid containing a fluorine compound
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- Organic Chemistry (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a method for stripping a quartz wafer by wet etching, which comprises the following steps: soaking the quartz plate in the cleaning agent for 30min, and performing ultrasonic treatment for 15min to remove metal and organic impurities; washing the quartz plate with deionized water at 12mol‑1Soaking in L HCl for 12 h; washing the quartz plate with deionized water again, wrapping the quartz plate with tinfoil, and roasting the wrapped quartz plate in a muffle furnace at 550 ℃ for 12 hours to remove residues and impurities; etching the surface of the quartz plate by using hydrofluoric acid, and controlling different acid concentrations and etching duration time to enable the quartz plate to generate different etching effects so as to realize quantitative control of the thickness of the quartz plate; after etching, washing the modified quartz plate by deionized water until the pH value of the water after cleaning reaches 6.5-7.5; and drying the cleaned quartz plate in an oven or a vacuum drying oven at 50 ℃ for 12 h. The invention can prepare the quartz plates with different thicknesses and different roughness, and meets the requirement of materialsThe processing requirement of quartz wafers in the field effectively improves the uniformity and controllability of the wet etching process.
Description
Technical Field
The invention belongs to the technical field of environmental materials and chemistry, and particularly relates to a method for stripping a quartz plate by wet etching.
Background
Quartz glass is a glass with a single component of silicon dioxide, has superior performances of high temperature resistance, low expansion coefficient, radiation irradiation resistance, thermal shock resistance, chemical stability, wide spectrum transmission range, electrical insulation and the like, is an ideal structural material, and is widely applied to various fields. However, quartz glass, which is a typical brittle and hard material, has a disadvantage of poor workability. Therefore, an effective processing method of quartz glass is an important issue concerning its application.
The existing quartz glass processing methods comprise ultrasonic processing, mechanical processing, laser processing, dry etching, wet etching and the like. The traditional processing methods such as ultrasound, machinery, laser and the like have higher efficiency, but the processing form is single, the processing quality and precision are limited, the processing error is large, the bottleneck in precision and size is difficult to break through, and the processing requirement of a complex microstructure cannot be met. The dry etching and the wet etching are used for processing the high-precision quartz body. The dry etching mainly comprises plasma etching and reactive ion etching, the size of the dry etching is well controlled, and a high-aspect-ratio structure with a smooth surface can be obtained; but the processing time is long, the speed is low (about tens of nanometers per minute), the equipment is expensive, the processing cost is high, and the industrial popularization is not facilitated. Wet etching is anisotropic etching which uses a chemical reaction between an etching solution and an etched material to realize etching, and has the advantages of simple equipment, easy operation, low cost, relatively high speed (the etching speed per minute can reach several micrometers), and relatively low processing cost.
Generally, hydrofluoric acid is used as a corrosive agent for quartz wet etching to process quartz glass components, and chemical etching, chemical polishing and the like are mainly performed. Research shows that the corrosion result of the quartz plate in hydrofluoric acid can be influenced by many factors such as the concentration and the fluidity of liquid. The existing wet etching technology is difficult to control, has low efficiency and large manual investment, and is difficult to realize batch industrial production. Therefore, the method for stripping the quartz plate by wet etching, which is easy to control, high in efficiency and simple to operate, is used for controlling the etching thickness and the etching uniformity of the quartz plate.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provides a method for stripping a quartz plate by wet etching aiming at the technical situation that the effect of hydrofluoric acid on the quartz plate is not ideal, and the method is used for processing the quartz plate in the field of environmental materials.
The purpose of the invention is realized by the following technical scheme.
The method for stripping the quartz wafer by wet etching comprises the following steps:
the first step is as follows: soaking the quartz plate in the cleaning agent for 30min, and performing ultrasonic treatment for 15min to remove metal and organic impurities;
the second step is that: washing the quartz plate with deionized water at 12mol-1Soaking in L HCl for 12 h;
the third step: washing the quartz plate with deionized water again, wrapping the quartz plate with tinfoil, and roasting the wrapped quartz plate in a muffle furnace at 550 ℃ for 12 hours to remove residues and impurities;
the fourth step: etching the surface of the quartz plate by using hydrofluoric acid, and controlling different acid concentrations and etching duration time to enable the quartz plate to generate different etching effects so as to realize quantitative control of the thickness of the quartz plate;
the fifth step: after etching, washing the modified quartz plate by deionized water until the pH value of the water after cleaning reaches 6.5-7.5;
and a sixth step: and drying the cleaned quartz plate in an oven or a vacuum drying oven at 50 ℃ for 12 h.
The quartz plates in the first step have a smooth surface prior to impurity removal.
In the fourth step, the volume percentage of the hydrofluoric acid solution is 2-36%.
And in the fourth step, selecting the etching duration time to be 0-12h according to the required etching thickness of the quartz plate.
And in the fourth step, the hydrofluoric acid corrosion stripping process is carried out at room temperature.
And in the fourth step, quartz plate samples with different thicknesses and different surface uniformity are prepared by combining hydrofluoric acid with different concentrations and duration at different moments.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
(1) the invention obtains the glass slides with different thicknesses by controlling the concentration of the corrosive agent and the etching time, thereby realizing the quantitative control of the thickness of the glass slides.
(2) Compared with the traditional wet etching, the method enhances the fluidity of the etching solution by continuously stirring the stirring equipment in the reactor, and the quartz plate obtained by corrosion stripping is uniformly etched. As the concentration of the corrosive agent is increased and the etching time is prolonged, the surface roughness of the quartz plate is not greatly changed, but the uniformity is obviously increased, and the product quality is improved.
(3) The method uses hydrofluoric acid as the corrosive agent, accelerates the dissolving process, shortens the dissolving time, reduces the time cost, has easily controlled process requirement conditions, is simple and convenient to operate, and is easy for industrial production.
Drawings
FIG. 1 is an AFM image of a quartz wafer after wet etch stripping of example 1;
FIG. 2 is an AFM image of a quartz wafer after wet etch stripping of example 2;
FIG. 3 is an AFM image of a quartz wafer after wet etch stripping of example 3.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
The method for stripping the quartz wafer by wet etching comprises the following steps:
the first step is as follows: soaking the quartz plate in the cleaning agent for 30min, and performing ultrasonic treatment for 15min to remove metal and organic impurities. Wherein the quartz plate has a smooth surface prior to impurity removal. 2% Extran can be used as cleaning agentTMA laboratory cleaning agent.
The second step is that: washing the quartz plate with deionized water at 12mol-1Soaking in L HCl for 12 hr.
The third step: and washing the quartz plate with deionized water again, wrapping the quartz plate with the tin foil, and roasting the wrapped quartz plate in a muffle furnace at 550 ℃ for 12 hours to remove residues and impurities.
The fourth step: and etching the surface of the quartz plate by using hydrofluoric acid, and controlling different acid concentrations and etching duration time to enable the quartz plate to generate different etching effects, thereby realizing quantitative control of the thickness of the quartz plate. The hydrofluoric acid etching stripping process is performed at room temperature. Wherein, through the combination of hydrofluoric acid with different concentrations and duration at different moments, quartz plate samples with different thicknesses and different surface uniformity can be prepared.
Preparing hydrofluoric acid solution with required concentration, wherein the volume percentage of the hydrofluoric acid solution is 2-36%; putting a quartz plate to be corroded into the net and clamping the quartz plate by a clamp arranged at the tail end of the bracket; placing a bracket and the quartz plate to be corroded fixed at the tail end of the bracket in a reaction vessel; adding 3/4 parts of etching solution to the reaction vessel; the stirring device is turned on and stirring is continued until the corresponding etching time. And selecting the etching duration time to be 0-12h according to the required etching thickness of the quartz plate. The stirring device is a magnetic stirrer (mechanical stirring can also be used) to maintain uniform etching conditions, and the stirring speed is 100 r/min.
The fifth step: after etching, the modified quartz plate was rinsed thoroughly with deionized water until the pH of the rinsed water reached 6.5-7.5.
And a sixth step: and drying the cleaned quartz plate in an oven or a vacuum drying oven at 50 ℃ for 12 h.
The quartz wafer stripped by wet etching is used for industrial application or scientific research and has important significance for improving the quality of quartz glass components and expanding the application field.
Example 1:
a method for stripping a quartz plate by wet etching under low concentration and short etching time comprises the following specific steps:
1. pretreatment of the quartz wafer: the quartz plate is selected to have the size of 10mm by 10mm and the thickness of 1.60 mm. The quartz plate was coated with 2% ExtranTMSoaking in a laboratory cleaning agent for 30min, and performing ultrasonic treatment for 15min to remove metal and organic impurities.
2. Acid washing of quartz plates: thoroughly washing the quartz plate with deionized water at 12mol-1Soaking in L HCl for 12 hr.
3. Removing quartz piece residues: and washing the quartz plate with deionized water again, wrapping the quartz plate with the tin foil, and roasting the wrapped quartz plate in a muffle furnace at 550 ℃ for 12 hours to remove residues and impurities.
4. And (3) hydrofluoric acid corrosion stripping: the hydrofluoric acid etching stripping process is performed at room temperature. Preparing a hydrofluoric acid solution with the volume percentage of 2%; putting a quartz plate to be corroded into the net and clamping the quartz plate by a clamp arranged at the tail end of the bracket; placing a bracket and the quartz plate to be corroded fixed at the tail end of the bracket in a reaction vessel; adding 3/4 parts of etching solution to the reaction vessel; starting the stirring device, and continuously stirring until the etching time of the quartz plate reaches 20 min. The stirring device is a magnetic stirrer, and the stirring speed is 100 r/min. Wherein, the magnetic stirrer model is: IKA Color liquid.
5. Washing: after etching, the modified quartz plate was rinsed thoroughly with deionized water. Until the pH of the rinse water reaches 6.5-7.5.
6. Drying: the cleaned quartz pieces were dried in an oven at 50 ℃ for 12 h.
The two-dimensional AFM image of the quartz plate after wet etching and stripping is shown in FIG. 1, the root mean square roughness of the quartz plate after wet etching and stripping is 0.0104 μm, the dissolution effect of hydrofluoric acid on the quartz plate is not obvious due to low concentration of hydrofluoric acid and short etching time, and the thickness of the modified quartz plate is about 1.60 mm.
Example 2:
a method for stripping a quartz plate by wet etching under low concentration and short etching time comprises the following specific steps:
1. pretreatment of the quartz wafer: the quartz plate is selected to have the size of 10mm by 10mm and the thickness of 1.60 mm. The quartz plate was coated with 2% ExtranTMSoaking in a laboratory cleaning agent for 30min, and performing ultrasonic treatment for 15min to remove metal and organic impurities.
2. Acid washing of quartz plates: thoroughly washing the quartz plate with deionized water at 12mol-1Soaking in L HCl for 12 hr.
3. Removing quartz piece residues: and washing the quartz plate with deionized water again, wrapping the quartz plate with the tin foil, and roasting the wrapped quartz plate in a muffle furnace at 550 ℃ for 12 hours to remove residues and impurities.
4. And (3) hydrofluoric acid corrosion stripping: the hydrofluoric acid etching stripping process is performed at room temperature. Preparing 8 percent hydrofluoric acid solution by volume percentage; putting a quartz plate to be corroded into the net and clamping the quartz plate by a clamp arranged at the tail end of the bracket; placing a bracket and the quartz plate to be corroded fixed at the tail end of the bracket in a reaction vessel; adding 3/4 parts of etching solution to the reaction vessel; starting the stirring device, and continuously stirring until the etching time of the quartz plate reaches 30 min. The stirring device is a magnetic stirrer, and the stirring speed is 100 r/min. Wherein, the magnetic stirrer model is: IKA Color liquid.
5. Washing: after etching, the modified quartz plate was rinsed thoroughly with deionized water. Until the pH of the rinse water reaches 6.5-7.5.
6. Drying: the cleaned quartz pieces were dried in an oven at 50 ℃ for 12 h.
The two-dimensional AFM image of the quartz plate after wet etch stripping is shown in FIG. 2.
It can be seen that the root mean square roughness of the quartz plate after 30min etching with the 8% hydrofluoric acid solution was 0.0092 μm, and the roughness of the quartz plate was not changed much as compared with example 1, but the rough surface was more uniform, and the uniformity of etching was significantly changed. Meanwhile, hydrofluoric acid has an obvious dissolving effect on the quartz plate, the thickness of the modified quartz plate is about 1.05mm, and the thickness of the quartz plate is reduced by about 0.55mm, so that the quantitative control of the thickness of the quartz plate is realized.
Example 3:
a method for stripping a quartz plate by wet etching under high concentration and long etching time comprises the following specific steps:
1. pretreatment of the quartz wafer: the quartz plate size is 18mm by 18mm, and the thickness is 1.60 mm. The quartz plate was coated with 2% ExtranTMSoaking in a laboratory cleaning agent for 30min, and performing ultrasonic treatment for 15min to remove metal and organic impurities.
2. Acid washing of quartz plates: thoroughly washing the quartz plate with deionized water at 12mol-1Soaking in L HCl for 12 hr.
3. Removing quartz piece residues: and washing the quartz plate with deionized water again, wrapping the quartz plate with the tin foil, and roasting the wrapped quartz plate in a muffle furnace at 550 ℃ for 12 hours to remove residues and impurities.
4. And (3) hydrofluoric acid corrosion stripping: the hydrofluoric acid etching stripping process is performed at room temperature. Preparing 36 volume percent hydrofluoric acid solution; putting a quartz plate to be corroded into the net and clamping the quartz plate by a clamp arranged at the tail end of the bracket; placing a bracket and the quartz plate to be corroded fixed at the tail end of the bracket in a reaction vessel; adding 3/4 parts of etching solution to the reaction vessel; starting the stirring device, and continuously stirring until the etching time of the quartz plate reaches 12 h. The stirring device is a magnetic stirrer, and the stirring speed is 100 r/min. Wherein, the magnetic stirrer model is: IKA Color liquid.
5. Washing: after etching, the modified quartz plates were rinsed thoroughly with deionized water until the pH of the rinse water reached 6.5-7.5.
6. Drying: the cleaned quartz pieces were dried in an oven at 50 ℃ for 12 h.
The two-dimensional AFM image of the quartz plate after wet etch stripping is shown in FIG. 3.
As can be seen, the root mean square roughness of the quartz plate was 0.0096 μm after the etching time of the 36% hydrofluoric acid solution was 12 hours. The roughness of the modified quartz plate is not changed greatly by controlling different acid concentrations and different etching duration, but the rough surface becomes more uniform along with the increase of the acid concentration and the increase of the etching duration, and the uniformity of corrosion is changed obviously. Meanwhile, hydrofluoric acid has an obvious dissolving effect on the quartz plate, the thickness of the quartz plate is about 0.50mm after modification, and the thickness of the quartz plate is reduced by about 1.10mm along with the increase of the acid concentration and the increase of the etching duration, so that the quantitative control of the thickness of the quartz plate is realized.
While the present invention has been described in terms of its functions and operations with reference to the accompanying drawings, it is to be understood that the invention is not limited to the precise functions and operations described above, and that the above-described embodiments are illustrative rather than restrictive, and that various changes and modifications may be effected therein by one skilled in the art without departing from the scope or spirit of the invention as defined by the appended claims.
Claims (6)
1. A method for stripping a quartz wafer by wet etching is characterized by comprising the following steps:
the first step is as follows: soaking the quartz plate in the cleaning agent for 30min, and performing ultrasonic treatment for 15min to remove metal and organic impurities;
the second step is that: washing the quartz plate with deionized water at 12mol-1Soaking in L HCl for 12 h;
the third step: washing the quartz plate with deionized water again, wrapping the quartz plate with tinfoil, and roasting the wrapped quartz plate in a muffle furnace at 550 ℃ for 12 hours to remove residues and impurities;
the fourth step: etching the surface of the quartz plate by using hydrofluoric acid, and controlling different acid concentrations and etching duration time to enable the quartz plate to generate different etching effects so as to realize quantitative control of the thickness of the quartz plate;
the fifth step: after etching, washing the modified quartz plate by deionized water until the pH value of the water after cleaning reaches 6.5-7.5;
and a sixth step: and drying the cleaned quartz plate in an oven or a vacuum drying oven at 50 ℃ for 12 h.
2. The method of wet etching quartz plate for removal according to claim 1, wherein the quartz plate has a smooth surface before impurities are removed in the first step.
3. The method for wet etching release of quartz wafers according to claim 1, wherein the hydrofluoric acid solution in the fourth step is 2-36% by volume.
4. The method for wet etching and stripping the quartz plate as claimed in claim 1, wherein the etching duration time in the fourth step is selected to be 0-12h according to the etching thickness required by the quartz plate.
5. The method for wet etching stripping quartz plate according to claim 1, wherein said hydrofluoric acid etching stripping process in the fourth step is performed at room temperature.
6. The method for wet etching stripping of quartz wafers according to claim 1, characterized in that in the fourth step, quartz wafer samples of different thickness and different surface homogeneity are prepared by a combination of different concentrations of hydrofluoric acid and different time durations.
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| CN201910967785.2A CN110790512A (en) | 2019-10-12 | 2019-10-12 | Method for stripping quartz plate by wet etching |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005064587A (en) * | 2003-08-13 | 2005-03-10 | Seiko Epson Corp | Etching composition for wet etching of quartz, surface processing method of quartz plate, and quartz plate obtained from processing method |
| CN101219429A (en) * | 2007-01-10 | 2008-07-16 | 北京北方微电子基地设备工艺研究中心有限责任公司 | Method for cleaning quartz parts surface in polycrystal etching cavity |
| CN106087066A (en) * | 2016-06-15 | 2016-11-09 | 廊坊中电熊猫晶体科技有限公司 | A kind of method improving quartz crystal slice surface roughness |
| KR20190027636A (en) * | 2017-09-07 | 2019-03-15 | 주식회사 원익큐엔씨 | Quartz surface treatment method for quartz surface coating |
| 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 |
-
2019
- 2019-10-12 CN CN201910967785.2A patent/CN110790512A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005064587A (en) * | 2003-08-13 | 2005-03-10 | Seiko Epson Corp | Etching composition for wet etching of quartz, surface processing method of quartz plate, and quartz plate obtained from processing method |
| CN101219429A (en) * | 2007-01-10 | 2008-07-16 | 北京北方微电子基地设备工艺研究中心有限责任公司 | Method for cleaning quartz parts surface in polycrystal etching cavity |
| CN106087066A (en) * | 2016-06-15 | 2016-11-09 | 廊坊中电熊猫晶体科技有限公司 | A kind of method improving quartz crystal slice surface roughness |
| KR20190027636A (en) * | 2017-09-07 | 2019-03-15 | 주식회사 원익큐엔씨 | Quartz surface treatment method for quartz surface coating |
| 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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