阅读说明：本技术 一种湿法腐蚀剥离石英片的方法 (Method for stripping quartz plate by wet etching ) 是由 崔丽敏 赵鹏 赵伟高 田一梅 于 2019-10-12 设计创作，主要内容包括：本发明公开了一种湿法腐蚀剥离石英片的方法：将石英片在清洗剂中浸泡30min,超声处理15min,去除金属和有机杂质；用去离子水清洗石英片,在12mol<Sup>-1</Sup>L HCL中浸泡12h；再次用去离子水洗涤石英片,锡纸包裹后在马弗炉中550℃下焙烧12h,去除残留物和杂质；使用氢氟酸蚀刻石英片表面,控制不同的酸浓度和蚀刻持续时间,使石英片产生不同的刻蚀效果,实现石英片厚度的量化控制；蚀刻后,用去离子水冲洗改性石英片,直至清洗后水的pH达到6.5-7.5；将清洗后的石英片在烘箱或真空干燥箱中50℃下干燥12h。本发明可以制备出不同厚度和不同粗糙度的石英片,满足了材料领域石英片的加工需求,有效提高了湿法腐蚀工艺的均一性、可控性。(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 ‑1 Soaking 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.)

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.

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 agent^TMA 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.