CN107226624A - It is a kind of for etching solution of electro-conductive glass and preparation method thereof - Google Patents
It is a kind of for etching solution of electro-conductive glass and preparation method thereof Download PDFInfo
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- CN107226624A CN107226624A CN201710645039.2A CN201710645039A CN107226624A CN 107226624 A CN107226624 A CN 107226624A CN 201710645039 A CN201710645039 A CN 201710645039A CN 107226624 A CN107226624 A CN 107226624A
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- etching solution
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- conductive glass
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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
Abstract
The invention discloses a kind of for etching solution of electro-conductive glass and preparation method thereof, the etching solution includes the raw material of following parts by weight：30~50 parts of hydrofluoric acid, 20~30 parts of phosphoric acid, 5~10 parts of calcirm-fluoride, 1~6 part of ammonium sulfate, 1~6 part of magnesium sulfate, 5~10 parts of potassium phosphate, 1~6 part of potassium hydrogen fluoride, 6~12 parts of sodium metasilicate, 5~10 parts of sodium fluoborate, 1~5 part of agar, 1~6 part of sodium alginate, 1~3 part of nano silicon, 0.2~0.6 part of antifreezing agent, 0.01~0.05 part of anion surfactant, 40~60 parts of sulfuric acid solution, 120~160 parts of deionized water.The etching solution of the present invention can be dissolved and be etched by the impurity to conducting glass substrate surface, reach the technique effect for removing substrate surface impurity, so as to effectively solve the problem of substrate reduces yield because graininess is adhered to.
Description
Technical field
The present invention relates to etching solution technical field, and in particular to a kind of etching solution and its preparation side for electro-conductive glass
Method.
Background technology
, it is necessary to use electro-conductive glass in the preparation process of flat-panel monitor.As manufacturer is increasing
Using the method that electro-conductive glass is thinned, electro-conductive glass be etched into for it is important the problem of.Usually used thining method
There are two kinds, one kind is physical method, i.e., be polished grinding using polishing powder, this method thinned time is long, the bad control of precision
System, product yield is low；Another method is the chemical method for etching using etching solution, and this method thinned time is short, equipment investment
It is small, and the composition of reducer is simple, has been increasingly becoming dominant technical approach.
The etching solution of prior art is very fast to the etch-rate of substrate, and etch quantity is not easily controlled, and what is had can not be effectively molten
Silicate is solved, some meetings produce stronger ionization, cause etch-rate to be difficult to control, etching solution can produce a large amount of gas sometimes
Bubble.Accordingly, it is desirable to provide a kind of etching solution and the method for etching electro-conductive glass, can effectively go the removal of impurity, product is improved qualified
Rate, while guarantee can be provided to the thickness control of conducting glass substrate.
The content of the invention
It is an object of the invention to overcoming above-mentioned the deficiencies in the prior art there is provided a kind of etching solution for electro-conductive glass and
Its preparation method, the etching solution can be dissolved and be etched by the impurity to conducting glass substrate surface, reach removal base
The technique effect of plate surface impurity, so as to effectively solve the problem of substrate reduces yield because graininess is adhered to.
The present invention solves technical problem and adopted the following technical scheme that：
A kind of etching solution for electro-conductive glass, includes the raw material of following parts by weight：30~50 parts of hydrofluoric acid, phosphoric acid 20~30
Part, 5~10 parts of calcirm-fluoride, 1~6 part of ammonium sulfate, 1~6 part of magnesium sulfate, 5~10 parts of potassium phosphate, 1~6 part of potassium hydrogen fluoride, silicic acid
6~12 parts of sodium, 5~10 parts of sodium fluoborate, 1~5 part of agar, 1~6 part of sodium alginate, 1~3 part of nano silicon, antifreezing agent
0.2~0.6 part, 0.01~0.05 part of anion surfactant, 40~60 parts of sulfuric acid solution, 120~160 parts of deionized water；
Wherein, the mass concentration of sulfuric acid solution is 10~20%.
Preferably, the etching solution includes the raw material of following parts by weight：42 parts of hydrofluoric acid, 25 parts of phosphoric acid, 8 parts of calcirm-fluoride,
2 parts of ammonium sulfate, 3 parts of magnesium sulfate, 6 parts of potassium phosphate, 3 parts of potassium hydrogen fluoride, 10 parts of sodium metasilicate, 7 parts of sodium fluoborate, 3 parts of agar, marine alga
Sour 5 parts of sodium, 2 parts of nano silicon, 0.5 part of antifreezing agent, 0.02 part of anion surfactant, 50 parts of sulfuric acid solution, go from
Sub- 150 parts of water.
Preferably, the antifreezing agent be ethylene glycol, glycerine, diethylene glycol (DEG), butyl glycol ether, 2-Butoxyethyl acetate,
One or more combinations in dimethyl sulfoxide.
Preferably, the anion surfactant is neopelex, dodecyl sodium sulfate, fatty alcohol ether
One or more combinations in sodium sulphate, ethoxylated fatty-acid methyl ester sodium sulfonate.
The preparation method of the above-mentioned etching solution for electro-conductive glass, comprises the following steps：
（1）Under condition of ice bath, sulfuric acid solution is slowly dropped in deionized water using constant pressure funnel, 30 are mixed
After~50min, hydrofluoric acid, phosphoric acid are slow added into, after stirring, ultrasonically treated 5~10min in supersonic cleaning machine is put into,
Obtain mixed acid solution；
（2）By mixed acid solution, calcirm-fluoride, ammonium sulfate, magnesium sulfate, potassium phosphate, potassium hydrogen fluoride, sodium metasilicate, sodium fluoborate, fine jade
Fat, sodium alginate, nano silicon, antifreezing agent, anion surfactant are sequentially added in reactor, it is warming up to 100~
150 DEG C, stir after 30~50min, ageing obtains the etching solution in 30~50 hours.
Preferably, the ultrasonically treated frequency range is 30~40KHz, and ultrasonic power is 600W, and ultrasonic temperature is 40
~60 DEG C.
Preferably, the reactor uses acid-resistant stainless steel reactor, and speed of agitator is 60~80r/min.
Preferably, the step（2）It is warming up to after 135 DEG C, stirring 40min, ageing obtains the etching solution in 42 hours.
Compared with prior art, the present invention has following beneficial effect：
（1）The etching solution of the present invention, can be dissolved and be etched by the impurity to conducting glass substrate surface, reach removal
The technique effect of substrate surface impurity, so as to effectively solve the problem of substrate reduces yield because graininess is adhered to.
（2）The etching solution of the present invention, have selected a variety of fluorine-containing materials, such as hydrofluoric acid, calcirm-fluoride, potassium hydrogen fluoride, fluoboric acid
Sodium, the source as fluorine ion, reasonable mixture ratio, synergy have adjusted etching solution activity, prevent that reaction is too fast or excessively slow, match somebody with somebody
A variety of sulfate, phosphate, agar, sodium alginate are closed, nano silicon plays slow releasing function, prevents the continuation of erosional surface
Corrosion, advantageously forms uniform trickle hair side, reduces the thickness of etching face, keep the picture of display screen truly attractive in appearance.
（3）The present invention is by the performance cooperative compensating of each raw material, electro-conductive glass light transmittance and atomization after etching solution processing
Degree is higher, and thickness qualities are stable, and surface is difficult to leave cut, with good economic benefit.
Embodiment
Invention is described in further detail below in conjunction with specific embodiment.
Embodiment 1
A kind of etching solution for electro-conductive glass, includes the raw material of following parts by weight：42 parts of hydrofluoric acid, 25 parts of phosphoric acid, calcirm-fluoride 8
Part, 2 parts of ammonium sulfate, 3 parts of magnesium sulfate, 6 parts of potassium phosphate, 3 parts of potassium hydrogen fluoride, 10 parts of sodium metasilicate, 7 parts of sodium fluoborate, 3 parts of agar,
5 parts of sodium alginate, 2 parts of nano silicon, 0.5 part of antifreezing agent glycerine, anion surfactant DBSA
0.02 part of sodium, 50 parts of sulfuric acid solution, 150 parts of deionized water；Wherein, the mass concentration of sulfuric acid solution is 20%.
The preparation method of the above-mentioned etching solution for electro-conductive glass, comprises the following steps：
（1）Under condition of ice bath, sulfuric acid solution is slowly dropped in deionized water using constant pressure funnel, mixed
After 40min, hydrofluoric acid, phosphoric acid are slow added into, after stirring, ultrasonically treated 8min in supersonic cleaning machine is put into, is mixed
Close acid solution；Ultrasonically treated frequency range is 30~40KHz, and ultrasonic power is 600W, and ultrasonic temperature is 46 DEG C.
（2）By mixed acid solution, calcirm-fluoride, ammonium sulfate, magnesium sulfate, potassium phosphate, potassium hydrogen fluoride, sodium metasilicate, sodium fluoborate,
Agar, sodium alginate, nano silicon, antifreezing agent, anion surfactant sequentially add acid-resistant stainless steel reactor, stir
Mix rotating speed is 60r/min, is warming up to after 135 DEG C, stirring 40min, ageing obtains the etching solution in 42 hours.
Embodiment 2
A kind of etching solution for electro-conductive glass, includes the raw material of following parts by weight：36 parts of hydrofluoric acid, 27 parts of phosphoric acid, calcirm-fluoride 5
Part, 3 parts of ammonium sulfate, 2 parts of magnesium sulfate, 7 parts of potassium phosphate, 5 parts of potassium hydrogen fluoride, 8 parts of sodium metasilicate, 6 parts of sodium fluoborate, 3 parts of agar, sea
5 parts of mosanom, 1 part of nano silicon, 0.2 part of antifreeze glycol, anion surfactant dodecyl sodium sulfate
0.03 part, 50 parts of sulfuric acid solution, 134 parts of deionized water；Wherein, the mass concentration of sulfuric acid solution is 17%.
The preparation method of the above-mentioned etching solution for electro-conductive glass, comprises the following steps：
（1）Under condition of ice bath, sulfuric acid solution is slowly dropped in deionized water using constant pressure funnel, mixed
After 45min, hydrofluoric acid, phosphoric acid are slow added into, after stirring, ultrasonically treated 7min in supersonic cleaning machine is put into, is mixed
Close acid solution；Ultrasonically treated frequency range is 30~40KHz, and ultrasonic power is 600W, and ultrasonic temperature is 48 DEG C.
（2）By mixed acid solution, calcirm-fluoride, ammonium sulfate, magnesium sulfate, potassium phosphate, potassium hydrogen fluoride, sodium metasilicate, sodium fluoborate,
Agar, sodium alginate, nano silicon, antifreezing agent, anion surfactant sequentially add acid-resistant stainless steel reactor, stir
Mix rotating speed is 65r/min, is warming up to after 140 DEG C, stirring 36min, ageing obtains the etching solution in 34 hours.
Embodiment 3
A kind of etching solution for electro-conductive glass, includes the raw material of following parts by weight：42 parts of hydrofluoric acid, 26 parts of phosphoric acid, calcirm-fluoride 7
Part, 3 parts of ammonium sulfate, 5 parts of magnesium sulfate, 8 parts of potassium phosphate, 3 parts of potassium hydrogen fluoride, 10 parts of sodium metasilicate, 6 parts of sodium fluoborate, 3 parts of agar,
5 parts of sodium alginate, 2 parts of nano silicon, 0.5 part of antifreezing agent diethylene glycol (DEG), anion surfactant fatty alcohol-ether sodium sulfate
0.03 part, 52 parts of sulfuric acid solution, 150 parts of deionized water；Wherein, the mass concentration of sulfuric acid solution is 17%.
The preparation method of the above-mentioned etching solution for electro-conductive glass, comprises the following steps：
（1）Under condition of ice bath, sulfuric acid solution is slowly dropped in deionized water using constant pressure funnel, mixed
After 42min, hydrofluoric acid, phosphoric acid are slow added into, after stirring, ultrasonically treated 6min in supersonic cleaning machine is put into, is mixed
Close acid solution；Ultrasonically treated frequency range is 30~40KHz, and ultrasonic power is 600W, and ultrasonic temperature is 55 DEG C.
（2）By mixed acid solution, calcirm-fluoride, ammonium sulfate, magnesium sulfate, potassium phosphate, potassium hydrogen fluoride, sodium metasilicate, sodium fluoborate,
Agar, sodium alginate, nano silicon, antifreezing agent, anion surfactant sequentially add acid-resistant stainless steel reactor, stir
Mix rotating speed is 80r/min, is warming up to after 150 DEG C, stirring 50min, ageing obtains the etching solution in 40 hours.
Embodiment 4
A kind of etching solution for electro-conductive glass, includes the raw material of following parts by weight：47 parts of hydrofluoric acid, 23 parts of phosphoric acid, calcirm-fluoride 8
Part, 2 parts of ammonium sulfate, 1 part of magnesium sulfate, 5 parts of potassium phosphate, 3 parts of potassium hydrogen fluoride, 10 parts of sodium metasilicate, 7 parts of sodium fluoborate, 3 parts of agar,
5 parts of sodium alginate, 3 parts of nano silicon, 0.5 part of antifreeze glycol monobutyl ether acetate, anion surfactant ethoxy
0.03 part of base methyl sodiosul foaliphatate, 55 parts of sulfuric acid solution, 150 parts of deionized water；Wherein, the mass concentration of sulfuric acid solution
For 12%.
The preparation method of the above-mentioned etching solution for electro-conductive glass, comprises the following steps：
（1）Under condition of ice bath, sulfuric acid solution is slowly dropped in deionized water using constant pressure funnel, mixed
After 50min, hydrofluoric acid, phosphoric acid are slow added into, after stirring, ultrasonically treated 10min in supersonic cleaning machine is put into, is mixed
Close acid solution；Ultrasonically treated frequency range is 30~40KHz, and ultrasonic power is 600W, and ultrasonic temperature is 60 DEG C.
（2）By mixed acid solution, calcirm-fluoride, ammonium sulfate, magnesium sulfate, potassium phosphate, potassium hydrogen fluoride, sodium metasilicate, sodium fluoborate,
Agar, sodium alginate, nano silicon, antifreezing agent, anion surfactant sequentially add acid-resistant stainless steel reactor, stir
Mix rotating speed is 80r/min, is warming up to after 120 DEG C, stirring 47min, ageing obtains the etching solution in 45 hours.
Embodiment 5
A kind of etching solution for electro-conductive glass, includes the raw material of following parts by weight：50 parts of hydrofluoric acid, 28 parts of phosphoric acid, calcirm-fluoride 6
Part, 3 parts of ammonium sulfate, 2 parts of magnesium sulfate, 8 parts of potassium phosphate, 6 parts of potassium hydrogen fluoride, 11 parts of sodium metasilicate, 8 parts of sodium fluoborate, 4 parts of agar,
5 parts of sodium alginate, 3 parts of nano silicon, 0.5 part of antifreezing agent glycerine, anion surfactant dodecyl sodium sulfate
0.05 part, 60 parts of sulfuric acid solution, 160 parts of deionized water；Wherein, the mass concentration of sulfuric acid solution is 16%.
The preparation method of the above-mentioned etching solution for electro-conductive glass, comprises the following steps：
（1）Under condition of ice bath, sulfuric acid solution is slowly dropped in deionized water using constant pressure funnel, mixed
After 45min, hydrofluoric acid, phosphoric acid are slow added into, after stirring, ultrasonically treated 10min in supersonic cleaning machine is put into, is mixed
Close acid solution；Ultrasonically treated frequency range is 30~40KHz, and ultrasonic power is 600W, and ultrasonic temperature is 60 DEG C.
（2）By mixed acid solution, calcirm-fluoride, ammonium sulfate, magnesium sulfate, potassium phosphate, potassium hydrogen fluoride, sodium metasilicate, sodium fluoborate,
Agar, sodium alginate, nano silicon, antifreezing agent, anion surfactant sequentially add acid-resistant stainless steel reactor, stir
Mix rotating speed is 80r/min, is warming up to after 150 DEG C, stirring 45min, ageing obtains the etching solution in 46 hours.
Embodiment 6
A kind of etching solution for electro-conductive glass, includes the raw material of following parts by weight：50 parts of hydrofluoric acid, 30 parts of phosphoric acid, calcirm-fluoride
10 parts, 6 parts of ammonium sulfate, 6 parts of magnesium sulfate, 10 parts of potassium phosphate, 6 parts of potassium hydrogen fluoride, 12 parts of sodium metasilicate, 10 parts of sodium fluoborate, agar 5
Part, 6 parts of sodium alginate, 3 parts of nano silicon, 0.6 part of antifreeze glycol monobutyl ether acetate, anion surfactant ten
0.05 part of dialkyl benzene sulfonic acids sodium, 53 parts of sulfuric acid solution, 158 parts of deionized water；Wherein, the mass concentration of sulfuric acid solution is 15%.
The preparation method of the above-mentioned etching solution for electro-conductive glass, comprises the following steps：
（1）Under condition of ice bath, sulfuric acid solution is slowly dropped in deionized water using constant pressure funnel, mixed
After 42min, hydrofluoric acid, phosphoric acid are slow added into, after stirring, ultrasonically treated 10min in supersonic cleaning machine is put into, is mixed
Close acid solution；Ultrasonically treated frequency range is 30~40KHz, and ultrasonic power is 600W, and ultrasonic temperature is 50 DEG C.
（2）By mixed acid solution, calcirm-fluoride, ammonium sulfate, magnesium sulfate, potassium phosphate, potassium hydrogen fluoride, sodium metasilicate, sodium fluoborate,
Agar, sodium alginate, nano silicon, antifreezing agent, anion surfactant sequentially add acid-resistant stainless steel reactor, stir
Mix rotating speed is 80r/min, is warming up to after 150 DEG C, stirring 50min, ageing obtains the etching solution in 46 hours.
Described above is only the preferred embodiment of the present invention, and protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical schemes belonged under thinking of the present invention belong to protection scope of the present invention.It should be pointed out that for the art
Those of ordinary skill for, some improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (8)
1. a kind of etching solution for electro-conductive glass, it is characterised in that include the raw material of following parts by weight：Hydrofluoric acid 30~50
Part, 20~30 parts of phosphoric acid, 5~10 parts of calcirm-fluoride, 1~6 part of ammonium sulfate, 1~6 part of magnesium sulfate, 5~10 parts of potassium phosphate, hydrogen fluoride
1~6 part of potassium, 6~12 parts of sodium metasilicate, 5~10 parts of sodium fluoborate, 1~5 part of agar, 1~6 part of sodium alginate, nano silicon
1~3 part, 0.2~0.6 part of antifreezing agent, 0.01~0.05 part of anion surfactant, 40~60 parts of sulfuric acid solution, deionization
120~160 parts of water；Wherein, the mass concentration of sulfuric acid solution is 10~20%.
2. the etching solution according to claim 1 for electro-conductive glass, it is characterised in that the etching solution includes following heavy
Measure the raw material of part：42 parts of hydrofluoric acid, 25 parts of phosphoric acid, 8 parts of calcirm-fluoride, 2 parts of ammonium sulfate, 3 parts of magnesium sulfate, 6 parts of potassium phosphate, hydrogen fluoride
3 parts of potassium, 10 parts of sodium metasilicate, 7 parts of sodium fluoborate, 3 parts of agar, 5 parts of sodium alginate, 2 parts of nano silicon, 0.5 part of antifreezing agent,
0.02 part of anion surfactant, 50 parts of sulfuric acid solution, 150 parts of deionized water.
3. the etching solution according to claim 1 for electro-conductive glass, it is characterised in that the antifreezing agent be ethylene glycol,
One or more combinations in glycerine, diethylene glycol (DEG), butyl glycol ether, 2-Butoxyethyl acetate, dimethyl sulfoxide.
4. the etching solution according to claim 1 for electro-conductive glass, it is characterised in that the anion surfactant
For in neopelex, dodecyl sodium sulfate, fatty alcohol-ether sodium sulfate, ethoxylated fatty-acid methyl ester sodium sulfonate
One or more combinations.
5. the preparation method of the etching solution for electro-conductive glass according to any one of Claims 1 to 4, it is characterised in that
Comprise the following steps：
（1）Under condition of ice bath, sulfuric acid solution is slowly dropped in deionized water using constant pressure funnel, 30 are mixed
After~50min, hydrofluoric acid, phosphoric acid are slow added into, after stirring, ultrasonically treated 5~10min in supersonic cleaning machine is put into,
Obtain mixed acid solution；
（2）By mixed acid solution, calcirm-fluoride, ammonium sulfate, magnesium sulfate, potassium phosphate, potassium hydrogen fluoride, sodium metasilicate, sodium fluoborate, fine jade
Fat, sodium alginate, nano silicon, antifreezing agent, anion surfactant are sequentially added in reactor, it is warming up to 100~
150 DEG C, stir after 30~50min, ageing obtains the etching solution in 30~50 hours.
6. the preparation method of the etching solution according to claim 5 for electro-conductive glass, it is characterised in that at the ultrasound
The frequency range of reason is 30~40KHz, and ultrasonic power is 600W, and ultrasonic temperature is 40~60 DEG C.
7. the preparation method of the etching solution according to claim 5 for electro-conductive glass, it is characterised in that the reactor
Using acid-resistant stainless steel reactor, speed of agitator is 60~80r/min.
8. the preparation method of the etching solution according to claim 5 for electro-conductive glass, it is characterised in that the step
（2）It is warming up to after 135 DEG C, stirring 40min, ageing obtains the etching solution in 42 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710645039.2A CN107226624A (en) | 2017-08-01 | 2017-08-01 | It is a kind of for etching solution of electro-conductive glass and preparation method thereof |
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| CN201710645039.2A CN107226624A (en) | 2017-08-01 | 2017-08-01 | It is a kind of for etching solution of electro-conductive glass and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107640907A (en) * | 2017-10-27 | 2018-01-30 | 惠州市清洋实业有限公司 | A kind of preprocess method of glass thinning |
| CN107935400A (en) * | 2017-11-24 | 2018-04-20 | 无锡南理工新能源电动车科技发展有限公司 | A kind of display screen glass substrate etching solution based on nano silicon dioxide |
| CN113955947A (en) * | 2021-12-03 | 2022-01-21 | 蓝思科技（长沙）有限公司 | Glass etching solution, preparation method and etching method |
| CN114455858A (en) * | 2022-01-27 | 2022-05-10 | 醴陵旗滨电子玻璃有限公司 | Glass strengthening method, glass substrate, and etching material for glass |
| CN115636592A (en) * | 2021-12-31 | 2023-01-24 | 深圳市海风润滑技术有限公司 | High-stability frosting powder and preparation method thereof |
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| CN105349114A (en) * | 2015-10-27 | 2016-02-24 | 中国科学院深圳先进技术研究院 | Boron nitride doped composite material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107640907A (en) * | 2017-10-27 | 2018-01-30 | 惠州市清洋实业有限公司 | A kind of preprocess method of glass thinning |
| CN107935400A (en) * | 2017-11-24 | 2018-04-20 | 无锡南理工新能源电动车科技发展有限公司 | A kind of display screen glass substrate etching solution based on nano silicon dioxide |
| CN113955947A (en) * | 2021-12-03 | 2022-01-21 | 蓝思科技（长沙）有限公司 | Glass etching solution, preparation method and etching method |
| CN115636592A (en) * | 2021-12-31 | 2023-01-24 | 深圳市海风润滑技术有限公司 | High-stability frosting powder and preparation method thereof |
| CN114455858A (en) * | 2022-01-27 | 2022-05-10 | 醴陵旗滨电子玻璃有限公司 | Glass strengthening method, glass substrate, and etching material for glass |
| CN114455858B (en) * | 2022-01-27 | 2024-02-27 | 湖南旗滨电子玻璃股份有限公司 | Glass strengthening method, glass substrate and etching material for glass |
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Application publication date: 20171003 |