CN104045241B - A kind of micro-fluorine glass etching finishing method - Google Patents

A kind of micro-fluorine glass etching finishing method Download PDF

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CN104045241B
CN104045241B CN201410265784.0A CN201410265784A CN104045241B CN 104045241 B CN104045241 B CN 104045241B CN 201410265784 A CN201410265784 A CN 201410265784A CN 104045241 B CN104045241 B CN 104045241B
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etching
glass
sodium
micro
etch
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CN104045241A (en
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刘存海
张佳
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Chen Feng
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Abstract

The invention discloses a kind of micro-fluorine glass etching finishing method, after sodium fluoride and sodium sulfate grind respectively, and sodium dihydrogen phosphate, water, activating agent are made into etching solution according to the part by weight mixing of 10:7 8:1:5 6:5 and perform etching.The present invention is compared with the prior art and has the advantage that one, avoids directly using a large amount of Fluohydric acid., and the medicine used reclaims and is simply entirely capable of realizing recycling.Two, etch-rate is fast, and the degree of depth is big, uniformity good, safety is high, can reach production real requirement.Three, meet the theory of environmental protection and sustainable development, reach the requirement that cleaning produces, carry out processing method for the waste water designed by technique, make the waste water processed reach the standard of national discharge.

Description

A kind of micro-fluorine glass etching finishing method
Technical field
The present invention relates to the glass etching polishing technology of chemical processing field, a kind of micro-fluorine glass etching Finishing method.
Background technology
The polish of the glass pieces such as glass apparatus, instrument, electronic material display screen is the needs of current scientific development.As What improves the preci-sion and accuracy of glass pieces is to put the major subjects in face of specialty researcher.Particularly at electronic material Glass pieces in terms of display needs the etching technique of high precision and high accuracy to complete, traditional Fluohydric acid. sulphuric acid erosion Lithography will be on the verge of to eliminate owing to producing serious environmental pollution, and the glass etching technology arisen at the historic moment mainly has: fluorination Ammonium sulfuric acid process, sodium fluoride sulfuric acid process, ammonium fluoride acid system etc., although these methods greatly reduce the danger to human body Evil, but the effect of its etching is far away from Fluohydric acid. sulfuric acid process.
Glass is a kind of Inorganic Non-metallic Materials, has a long history and good characteristic, and its purposes is quite varied, relates to Every aspect to life.Glass etching polishing technology is indispensable part during glass post-processing processes, and has act foot light The status of weight.Glass, after etch-polish, in addition to having the performance of glass self, also has the spy that simple glass does not has Property.Glass etching polishing technology can be applicable to electronic product glass substrate and the polishing of basal plane, precision glass instrument and instrument Polishing, the making of glass precision optics workpiece, glass product scale, building and ornament materials, the high-end art work etc..
In recent years, glass product deep development is increasingly paid close attention to by everybody with utilizing.From environmental science and sustainable development Exhibition reality set out, seek a kind of environmental protection, respond well etching technique be our purpose.Along with economic technology Development, etch-polish technology will constantly bring forth new ideas, and glass etching simultaneously will incorporate multi-functional, intelligent and environmental friendliness etc. and manage Read, develop more new product containing high-tech composition.
Summary of the invention
The technical problem to be solved is with micro-fluorine catalytic cycle etch-polish technology generation of a kind of environmental protection Technology glass surface being etched for traditional direct Fluohydric acid., and erosion effect is than directly corroding more with Fluohydric acid. Uniformly, the degree of depth of erosion is big, decreases the pollution to environment, meets the requirement of green production.
Micro-fluorine glass etching polishing technology is that the Trace Fluoride utilizing reaction to produce carries out fast-etching to glass, through this technology Glass basal plane after etching, can reach the effect of seamless etching, i.e. glass basal plane after etching and the primary basic phase of glass basal plane Kiss.Be under-etching of glass product resistance to answer intensity big (proof stress intensity far beyond HF-H2SO4 method, mechanical grinding etc., at present Domestic existing glass polishing technology) etching solution can be recycled, and waste liquid can reach discharge after treatment, therefore it is raw to be by cleaning The effective method produced.
Technical scheme is as follows:
A kind of micro-fluorine glass etching finishing method, after sodium fluoride and sodium sulfate grind respectively, and sodium dihydrogen phosphate, water, work Property agent mix according to the part by weight of 10:7-8:1:5-6:5 and be made into etching solution and perform etching.
Described micro-fluorine glass etching finishing method, described activating agent is ammonium sulfate or sodium tetraborate.
Described micro-fluorine glass etching finishing method, described activating agent replaces with thickening agent, and described thickening agent is starch, will After sodium fluoride and sodium sulfate grind respectively, and sodium dihydrogen phosphate, water, starch are made into according to the part by weight mixing of 10:8:1:6:5 Etching solution performs etching.
The present invention is compared with the prior art and has the advantage that one, avoids directly using a large amount of Fluohydric acid., the medicine used Reclaim and be simply entirely capable of realizing recycling.Two, etch-rate is fast, and the degree of depth is big, uniformity good, safety is high, can reach production Real requirement.Three, meet the theory of environmental protection and sustainable development, reach the requirement that cleaning produces, for designed by technique Waste water carry out processing method, make the waste water processed reach the standard of national discharge.
Accompanying drawing explanation
Fig. 1 to Fig. 7 is the scanning electron microscopic picture of the embodiment of the present invention.
Detailed description of the invention
Sample is analyzed (depth of erosion: weigh the weight difference of glass print before and after corroding with analytical balance and compare (the hyaloid sheet specification selected by experiment is identical);Surface smoothness and the concavo-convex uniformity: see with SM-6390 type scanning electron microscope Examine).
Below in conjunction with specific embodiment, the present invention is described in detail.
Example 1:
After sodium fluoride (inorganic salt 1) and sodium sulfate (inorganic salt 2) grind respectively, and sodium dihydrogen phosphate, water are with 10:8:1:1 Part by weight, be made into etching solution.Again etching solution is coated on the glass that pretreatment is good.After placing 1 hour under 25OC, to glass Glass surface is carried out.By scanning electron microscope, its surface topography is observed.Pre-treatment step: ultrasonic washing (low frequency) Acid elution (the arbitrary proportion mixed liquor of dichromic acid and sulphuric acid) organic solvent-acetone soaks 3 minutes distilled water washs and adds Heat posted protective layer.
Such as Fig. 1, finding that etching surface is uneven, turning white in surface, has side etching phenomenon, and etch depth is the least.
Experimental data: etch first 17.4801 grams and etch latter 17.4431 grams
After before depth of erosion: m etching ,-m etches=17.4801-17.4431=0.0370
Example 2:
1. take sodium fluoride and after sodium sulfate grinds respectively, and sodium dihydrogen phosphate, water and starch (thickness of regulation solution) with The ratio of 10:8:1:1:5, is made into etching solution, then etching solution is coated on the glass that pretreatment is good.Place 1 hour under 28OC After, glass surface is carried out.By scanning electron microscope, its surface topography is observed, such as Fig. 2.
Experimental data: etch first 17.0375 grams;Etch latter 17.4063 grams;
After before depth of erosion: m etching ,-m etches=17.0375-17.4063=0.0375;
2. take sodium fluoride and after sodium sulfate grinds respectively, and sodium dihydrogen phosphate, water and starch (thickness of regulation solution) with The ratio of 10:8:1:6:5, is made into etching solution, then etching solution is coated on the glass that pretreatment is good.Place 1 hour under 28OC After, it is carried out glass surface its surface topography being observed, such as Fig. 3 by scanning electron microscope.
Experimental data: etch first 17.0577 grams;Etch latter 17.0103 grams;
After before depth of erosion: m etching ,-m etches=17.0577-17.0103=0.0474;
Compared by Fig. 2 and Fig. 3, find the etching solution effect more excellent (such as Fig. 3) being made in the ratio of 10:8:1:6:5, erosion Quarter, surface was more uniform, did not substantially have lateral erosion, and etch depth is bigger.
Example 3:
1. take sodium fluoride and after sodium sulfate grinds respectively, and sodium dihydrogen phosphate, water, activating agent sodium tetraborate be with 10:8:1: The ratio of 1:5 is made into etching solution, then after etching solution is coated in placing 1 hour under 28OC on the glass that pretreatment is good, to glass Surface is carried out.By scanning electron microscope, its surface topography is observed, such as Fig. 4.
Experimental data: etch first 17.2908 grams;Etch latter 17.1773 grams;
After before depth of erosion: m etching ,-m etches=17.2908-1773=0.1135;
2. take sodium fluoride and after sodium sulfate grinds respectively, and sodium dihydrogen phosphate, water, activating agent sodium tetraborate be with 10:8:1: The ratio of 6:5, is made into etching solution, then etching solution is coated on the glass that pretreatment is good.After placing 1 hour under 28OC, to glass Glass surface is carried out.By scanning electron microscope, its surface topography is observed, such as Fig. 5.
Experimental data: etch first 17.6257 grams;Etch latter 17.4890 grams;
After before depth of erosion: m etching ,-m etches=17.6257-17.4890=0.1367;
Contrasted by Fig. 4 and Fig. 5, find to be made into etching solution (such as Fig. 5), surface smoothness in the ratio of 10:8:1:6:5 The most preferably being improved with the concavo-convex uniformity, etch depth is bigger.
Example 4:
1. take sodium fluoride and after sodium sulfate grinds respectively, and etching solution (is played dispersion to make by sodium dihydrogen phosphate, water, ammonium sulfate With) with the ratio of 10:8:1:3:5, be made into etching solution, then etching solution be coated on the glass that pretreatment is good.1 is placed under 28OC After hour, glass surface is carried out.By scanning electron microscope, its surface topography is observed, such as Fig. 6.
Experimental data: etch first 17.8512 grams;Etch latter 17.2797 grams;
After before depth of erosion: m etching ,-m etches=17.8512-17.2797=0.5715;
2. take sodium fluoride and after sodium sulfate grinds respectively, and etching solution (is played dispersion to make by sodium dihydrogen phosphate, water, ammonium sulfate With) ratio of 10:7:1:5:5, it is made into etching solution, then etching solution is coated on the glass that pretreatment is good to place 1 under 28OC little Shi Hou, is carried out glass surface.By scanning electron microscope, its surface topography is observed, such as Fig. 7.
Experimental data: etch first 17.3937 grams;Etch latter 16.6074 grams;
After before depth of erosion: m etching ,-m etches=17.3937-16.6074=0.7863;
Contrasted by Fig. 6 and Fig. 7, find to be made into etching solution (such as Fig. 7), sample table after etching with the ratio of 10:7:1:5:5 Face is more uniform, does not substantially have lateral erosion, and etch depth is big, and whole structure is excellent.
It should be appreciated that for those of ordinary skills, can be improved according to the above description or be converted, And all these modifications and variations all should belong to the protection domain of claims of the present invention.

Claims (2)

1. a micro-fluorine glass etching finishing method, it is characterised in that after sodium fluoride and sodium sulfate grind respectively, and biphosphate Sodium, water, activating agent are made into etching solution according to the weight ratio mixing of 10:7-8:1:5-6:5 and perform etching, and described activating agent is sulphuric acid Ammonium or sodium tetraborate.
Micro-fluorine glass etching finishing method the most according to claim 1, it is characterised in that described activating agent replaces with thickening Agent, described thickening agent is starch, and after sodium fluoride and sodium sulfate being ground respectively, and sodium dihydrogen phosphate, water, starch press 10:8:1: The weight ratio mixing of 6:5 is made into etching solution and is etched.
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CN105330166B (en) * 2015-11-24 2018-03-06 陈锋 A kind of glass frosting liquid of environment-friendly type and preparation method thereof
CN113526876B (en) * 2020-04-16 2023-01-31 郑州恒昊光学科技有限公司 Method for manufacturing glass with ice slush effect

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1277944A (en) * 1999-06-22 2000-12-27 杨全月 Etching paste for automobile glass and the use thereof
CN101560058A (en) * 2008-04-15 2009-10-21 株式会社东进世美肯 Cleaning and etching composition for glass substrate for liquid crystal display device and method for etching glass substrate using the same
CN103000509A (en) * 2011-09-09 2013-03-27 东友精细化工有限公司 Method for manufacturing display device and etching solution composition

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DE10228116A1 (en) * 2002-06-24 2004-01-29 Sälzle, Erich, Dr. Process for polishing glass objects

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1277944A (en) * 1999-06-22 2000-12-27 杨全月 Etching paste for automobile glass and the use thereof
CN101560058A (en) * 2008-04-15 2009-10-21 株式会社东进世美肯 Cleaning and etching composition for glass substrate for liquid crystal display device and method for etching glass substrate using the same
CN103000509A (en) * 2011-09-09 2013-03-27 东友精细化工有限公司 Method for manufacturing display device and etching solution composition

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