CN113072306A - Preparation method of electronic grade mixed acid etching solution - Google Patents
Preparation method of electronic grade mixed acid etching solution Download PDFInfo
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- CN113072306A CN113072306A CN202110376327.9A CN202110376327A CN113072306A CN 113072306 A CN113072306 A CN 113072306A CN 202110376327 A CN202110376327 A CN 202110376327A CN 113072306 A CN113072306 A CN 113072306A
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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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Abstract
The invention discloses a preparation method of an electronic grade mixed acid etching solution, which comprises the following specific steps of adding electronic grade hydrofluoric acid into a mixed acid preparation tank, and simultaneously opening a stirrer; then, adding electronic grade concentrated nitric acid into the mixed acid preparation tank, and uniformly stirring to prepare mixed acid; and selectively adding inorganic acid and organic acid, and mixing and stirring uniformly. The weight ratio of each component is as follows: the electronic grade hydrofluoric acid comprises electronic grade concentrated nitric acid, inorganic acid and organic acid, and the ratio of the inorganic acid to the organic acid is 1: 1-4.5: 0-5.0: 0-1.5. In order to inhibit unstable chemical reaction of single hydrofluoric acid and silicon dioxide, improve etching efficiency and etching quality, a mixed acid etching solution composed of multiple components is prepared by adding an inorganic acid or an organic acid into the hydrofluoric acid, so that the chemical etching process of a liquid crystal panel/glass substrate and a solar cell panel (sheet) is further improved, the whole etching process is stable, effective and controllable, the generation of poor salient points on the glass surface and the further diffusion of pits and scratches in the whole etching process can be effectively inhibited, and the high-quality product rate of products is greatly improved.
Description
Technical Field
The invention relates to a preparation method of an electronic grade mixed acid etching solution, which is applied to etching thinning of a liquid crystal panel and a glass substrate, cleaning and texturing of a solar cell panel (sheet) and the like, and belongs to the technical field of electronic chemical application.
Background
At the beginning of thinning the liquid crystal panel and the glass substrate, pure water is added by single hydrofluoric acid to dilute the liquid crystal panel and the glass substrate and then react with the glass, the thinning requirements such as the thinning thickness is increased continuously and the diversification of glass materials are improved, and the chemical etching requirements of the liquid crystal panel and the glass substrate cannot be met only by the original single hydrofluoric acid in the practical operation of the industry. The main problems are reflected in the following aspects:
1. hydrofluoric acid is greatly affected by temperature changes, which causes unstable changes in etching efficiency and makes it difficult to control the etching process.
2. Is easy to react with SiO2The reaction generates insoluble substances such as white silicate crystals and the like, and the substances are suspended in the etching solution and adhered and etched in the pipeline of the equipment, thereby seriously influencing the operation of the etching equipment and the recycling of the etching solution.
3. The surface quality of the etched product is seriously affected by the poor salient points and the like generated on the surface and the edge caused by the adhesion of the insoluble impurities to the surface of the etched product.
4. The defects such as pits and scratches on the surface of an etched product are easily amplified.
5. The etching process has unstable speed, and the utilization rate of hydrofluoric acid is not high, so that the cost for treating the neutralized waste acid in the later period is increased. And hydrofluoric acid is easy to volatilize at high temperature, thereby increasing potential safety hazard.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of an electronic grade mixed acid etching solution.
The technical scheme provided by the invention is as follows: a preparation method of an electronic grade mixed acid etching solution is characterized by comprising the following specific steps:
(1) cleaning a mixed acid preparation tank with a polytetrafluoroethylene coating as an inner lining by using pure water; conveying the electronic-grade hydrofluoric acid to a hydrofluoric acid metering tank, and metering for later use; conveying the electronic-grade concentrated nitric acid to a nitric acid metering tank, and metering for later use; conveying the inorganic acid to an inorganic acid metering tank, and metering for later use; conveying the organic acid to an organic acid metering tank, and metering for later use; the inorganic acid is at least one of concentrated sulfuric acid or phosphoric acid, and the organic acid is one of acetic acid, peroxyacetic acid, formic acid and propionic acid; the mass ratio of each component is as follows: electronic grade hydrofluoric acid, electronic grade concentrated nitric acid, inorganic acid and organic acid, wherein the ratio of the inorganic acid to the organic acid is 1: 1-4.5: 0-5.0: 0-1.5;
(2) firstly, pumping electronic-grade hydrofluoric acid into a mixed acid preparation tank by using a corrosion-resistant pump, and simultaneously opening a stirrer;
(3) then pumping electronic grade concentrated nitric acid into the mixed acid preparation tank by using another corrosion-resistant pump, and uniformly stirring to prepare mixed acid;
(4) on the basis of the mixed acid, the inorganic acid and the organic acid are selectively added, the mixture is uniformly mixed and stirred, the sample is sampled and tested, and the qualified mixed acid is put into a mixed acid storage tank for sale.
Further, the mass concentration of the electronic grade hydrofluoric acid is 48.5% -49.5%, and the mass concentration of the electronic grade concentrated nitric acid is 68.5% -70.5%.
Further, the mass ratio of the phosphoric acid to the electronic grade hydrofluoric acid is 0-4.0: 1.
Further, the mass ratio of the concentrated sulfuric acid to the electronic-grade hydrofluoric acid is 0-1.0: 1.
Further, the concentrated sulfuric acid, the phosphoric acid, the acetic acid, the peroxyacetic acid, the formic acid and the propionic acid are all of the grade higher than the analytical purity of the chemical reagent.
The invention has the beneficial effects that: the invention overcomes the adverse effect caused by using a single-component hydrofluoric acid etching solution, in order to inhibit the unstable chemical reaction of single hydrofluoric acid and silicon dioxide, improve the etching efficiency and improve the etching quality, a mixed acid etching solution consisting of a plurality of components is prepared by adding inorganic acid or organic acid into the hydrofluoric acid, and reasonable, proper and effective mixture ratio among the components is researched and explored through a large number of experiments, the components are mutually matched, the advantages and the disadvantages are promoted and compensated, the respective advantages and characteristics are fully exerted, the chemical etching process of a liquid crystal panel/glass substrate and a solar panel (sheet) is further improved, the whole etching process is stable, effective and controllable, the generation of poor salient points on the glass surface in the whole etching process and the further diffusion of concave points and scratches can be effectively inhibited, thereby greatly improving the high-grade product rate of the product.
Detailed Description
The following detailed description of the embodiments of the invention:
example 1: electronic grade mixed acid (HF, HNO)3 、H2SO4 、HAC) The preparation method of the etching solution comprises the following steps: the mixed acid preparation tank lined with the polytetrafluoroethylene coating was washed with pure water. Conveying electronic-grade hydrofluoric acid with the mass concentration of 48.5% to a hydrofluoric acid metering tank, and metering 315kg for later use; conveying the electronic grade concentrated nitric acid with the mass concentration of 69% to a nitric acid metering tank, and metering 373kg for later use; conveying concentrated sulfuric acid with the grade higher than analytical purity to a sulfuric acid metering tank, and metering 215kg for later use; the acetic acid of grade above analytical grade was sent to an acetic acid metering tank and 370kg was metered for use. Putting the metered acetic acid into a mixed acid preparation tank, and simultaneously opening a stirrer; pumping the measured electronic grade hydrofluoric acid into the mixed acid preparation tank by using a corrosion-resistant pump; then pumping the measured electronic grade concentrated nitric acid into the mixed acid preparation tank by using another corrosion-resistant pump, and uniformly stirring; finally, adding the metered concentrated sulfuric acid, and uniformly stirring. Sampling and testing, and putting the qualified mixed acid into a mixed acid storage tank for sale.
Example 2: electronic grade mixed acid (HF, HNO)3 、H3PO4) The preparation method of the etching solution comprises the following steps: the mixed acid preparation tank lined with the polytetrafluoroethylene coating was washed with pure water. Conveying the electronic-grade hydrofluoric acid with the mass concentration of 49.5% to a hydrofluoric acid metering tank, and metering 100kg for later use; conveying the electronic grade concentrated nitric acid with the mass concentration of 70% to a nitric acid metering tank, and metering 450kg for later use; the phosphoric acid with the grade higher than the analytical purity is conveyed to a phosphoric acid metering tank, and 200kg of phosphoric acid is metered for standby. Pumping the metered electronic grade hydrofluoric acid into a mixed acid preparation tank by using a corrosion-resistant pump, and simultaneously opening a stirrer; then pumping the measured electronic grade concentrated nitric acid into the mixed acid preparation tank by using another corrosion-resistant pump, and uniformly stirring;then adding the metered phosphoric acid and stirring uniformly. Sampling and testing, and putting the qualified mixed acid into a mixed acid storage tank for sale.
Example 3: electronic grade mixed acid (HF, HNO)3 、H2SO4、H3PO4) The preparation method of the etching solution comprises the following steps: the mixed acid preparation tank lined with the polytetrafluoroethylene coating was washed with pure water. Conveying the electronic-grade hydrofluoric acid with the mass concentration of 49% to a hydrofluoric acid metering tank, and metering 199kg for later use; conveying the electronic grade concentrated nitric acid with the mass concentration of 70.5% to a nitric acid metering tank, and metering 236kg for later use; conveying concentrated sulfuric acid with the grade higher than analytical purity to a sulfuric acid metering tank, and metering 147kg for later use; the phosphoric acid of grade above the analytical grade was fed to a phosphoric acid metering tank and 721kg was metered for use. Pumping the metered electronic grade hydrofluoric acid into a mixed acid preparation tank by using a corrosion-resistant pump, and simultaneously opening a stirrer; then pumping the measured electronic grade concentrated nitric acid into the mixed acid preparation tank by using another corrosion-resistant pump, and uniformly stirring; then adding metered concentrated sulfuric acid and phosphoric acid, and uniformly stirring. Sampling and testing, and putting the qualified mixed acid into a mixed acid storage tank for sale.
Example 4: electronic grade mixed acid (HF, HNO)3 、H2SO4 、H3PO4、HCOOH) etching solution, which comprises the following steps: the mixed acid preparation tank lined with the polytetrafluoroethylene coating was washed with pure water. Conveying the electronic-grade hydrofluoric acid with the mass concentration of 49.5% to a hydrofluoric acid metering tank, and metering 260kg for later use; conveying the electronic grade concentrated nitric acid with the mass concentration of 68.5% to a nitric acid metering tank, and metering 260kg for later use; conveying concentrated sulfuric acid with the grade higher than analytical purity to a sulfuric acid metering tank, and metering 260kg for later use; conveying phosphoric acid with grade higher than analytical grade to a phosphoric acid metering tank, and metering 1040kg for later use; the formic acid of grade above the analytical purity is conveyed to a formic acid metering tank, and 390kg of formic acid is metered for standby. Putting the metered formic acid into a mixed acid preparation tank, and simultaneously opening a stirrer; pumping the measured electronic grade hydrofluoric acid into the mixed acid preparation tank by using a corrosion-resistant pump; then the mixture is pumped into a mixed acid preparation tank by another corrosion-resistant pump to obtain the measured electronic grade concentrated nitrateAcid, stirring evenly; finally, adding the metered concentrated sulfuric acid and phosphoric acid, and uniformly stirring. Sampling and testing, and putting the qualified mixed acid into a mixed acid storage tank for sale.
It should be understood that parts of the specification not set forth in detail are well within the prior art. The above examples are only for describing the preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.
Claims (5)
1. A preparation method of an electronic grade mixed acid etching solution is characterized by comprising the following specific steps:
(1) cleaning a mixed acid preparation tank with a polytetrafluoroethylene coating as an inner lining by using pure water; conveying the electronic-grade hydrofluoric acid to a hydrofluoric acid metering tank, and metering for later use; conveying the electronic-grade concentrated nitric acid to a nitric acid metering tank, and metering for later use; conveying the inorganic acid to an inorganic acid metering tank, and metering for later use; conveying the organic acid to an organic acid metering tank, and metering for later use; the inorganic acid is at least one of concentrated sulfuric acid or phosphoric acid, and the organic acid is one of acetic acid, peroxyacetic acid, formic acid and propionic acid; the mass ratio of each component is as follows: electronic grade hydrofluoric acid, electronic grade concentrated nitric acid, inorganic acid and organic acid, wherein the ratio of the inorganic acid to the organic acid is 1: 1-4.5: 0-5.0: 0-1.5;
(2) firstly, pumping electronic-grade hydrofluoric acid into a mixed acid preparation tank by using a corrosion-resistant pump, and simultaneously opening a stirrer;
(3) then pumping electronic grade concentrated nitric acid into the mixed acid preparation tank by using another corrosion-resistant pump, and uniformly stirring to prepare mixed acid;
(4) on the basis of the mixed acid, the inorganic acid and the organic acid are selectively added, the mixture is uniformly mixed and stirred, the sample is sampled and tested, and the qualified mixed acid is put into a mixed acid storage tank for sale.
2. The method for preparing the electronic grade mixed acid etching solution according to claim 1, wherein the mass concentration of the electronic grade hydrofluoric acid is 48.5% -49.5%, and the mass concentration of the electronic grade concentrated nitric acid is 68.5% -70.5%.
3. The method for preparing the electronic grade mixed acid etching solution according to claim 1, wherein the mass ratio of the phosphoric acid to the electronic grade hydrofluoric acid is 0-4.0: 1.
4. The preparation method of the electronic grade mixed acid etching solution according to claim 1, wherein the mass ratio of the concentrated sulfuric acid to the electronic grade hydrofluoric acid is 0-1.0: 1.
5. The method according to claim 1, wherein the concentrated sulfuric acid, phosphoric acid, acetic acid, peroxyacetic acid, formic acid, and propionic acid are all of chemical reagent analytical grade higher than the analytical grade.
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| CN202110376327.9A CN113072306A (en) | 2021-04-08 | 2021-04-08 | Preparation method of electronic grade mixed acid etching solution |
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| CN202110376327.9A CN113072306A (en) | 2021-04-08 | 2021-04-08 | Preparation method of electronic grade mixed acid etching solution |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008066706A (en) * | 2006-09-08 | 2008-03-21 | Samsung Electronics Co Ltd | Etching solution supply unit, etching apparatus, and etching method |
| CN101215099A (en) * | 2008-01-16 | 2008-07-09 | 京东方科技集团股份有限公司 | Flat glass substrate attenuation etching liquid |
| CN102643027A (en) * | 2012-04-26 | 2012-08-22 | 深圳南玻显示器件科技有限公司 | Glass etching liquid and glass etching method |
| CN108004550A (en) * | 2017-12-29 | 2018-05-08 | 深圳市华星光电技术有限公司 | Etching solution and its application for copper/molybdenum film layer |
| CN108585530A (en) * | 2018-04-20 | 2018-09-28 | 广东红日星实业有限公司 | A kind of glass etching liquid and preparation method thereof |
| CN109321253A (en) * | 2018-11-28 | 2019-02-12 | 湖北兴福电子材料有限公司 | A kind of etching solution of Silicon Wafer |
-
2021
- 2021-04-08 CN CN202110376327.9A patent/CN113072306A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008066706A (en) * | 2006-09-08 | 2008-03-21 | Samsung Electronics Co Ltd | Etching solution supply unit, etching apparatus, and etching method |
| CN101215099A (en) * | 2008-01-16 | 2008-07-09 | 京东方科技集团股份有限公司 | Flat glass substrate attenuation etching liquid |
| CN102643027A (en) * | 2012-04-26 | 2012-08-22 | 深圳南玻显示器件科技有限公司 | Glass etching liquid and glass etching method |
| CN108004550A (en) * | 2017-12-29 | 2018-05-08 | 深圳市华星光电技术有限公司 | Etching solution and its application for copper/molybdenum film layer |
| CN108585530A (en) * | 2018-04-20 | 2018-09-28 | 广东红日星实业有限公司 | A kind of glass etching liquid and preparation method thereof |
| CN109321253A (en) * | 2018-11-28 | 2019-02-12 | 湖北兴福电子材料有限公司 | A kind of etching solution of Silicon Wafer |
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