CN112266178B - Glass etching method - Google Patents
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- CN112266178B CN112266178B CN202011240798.9A CN202011240798A CN112266178B CN 112266178 B CN112266178 B CN 112266178B CN 202011240798 A CN202011240798 A CN 202011240798A CN 112266178 B CN112266178 B CN 112266178B
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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 provides a glass etching method, which adopts alkali and alcohol organic substance solution with the carbon number less than or equal to 10 as etching solution and adopts ultrasound as an auxiliary way, so that the roughness of the inner wall of the etched glass is greatly reduced, the roughness can reach less than or equal to 6nm, the glass etching method can be widely applied to etching of various kinds of glass, and the application prospect is wide.
Description
Technical Field
The invention relates to the technical field of etching, in particular to a glass etching method.
Background
The glass is a transparent solid at normal temperature, forms a continuous network structure when being melted, and is a silicate-based non-metallic material which gradually increases in viscosity and hardens without crystallizing during cooling. The main component of ordinary glass is silica. The etching of the glass can enable common glass to be presented to the public in forms of coquettish, glacier texture and the like, and can also provide conditions for new application of the glass. The traditional glass etching adopts etching solution containing fluorine.
CN104341111A provides a regeneration method of glass etching solution and a glass etching method, which utilizes potassium ion compound to perform stirring reaction with aged glass etching solution, and removes soluble glass slag in the aged solution by filtration. And carrying out ion exchange treatment on the aging liquid to obtain metal ions. In addition, a proper amount of hydrofluoric acid is added into the aging liquid, and then the glass etching liquid meeting the glass etching requirement is regenerated. The invention also provides a glass etching method, which can remove soluble glass slag in the glass etching solution by using potassium ion compounds in the glass etching process and improve the etching rate of glass etching; but this method does not address the issue of post-etching surface finish of the glass.
CN104926145A discloses a glass etching process, in which the etching solution used only comprises water, hydrofluoric acid, sulfuric acid, nitric acid, sodium nitrite and acetic acid, but the problem of surface smoothness after etching is not involved, and the toxicity and environmental pollution are serious by using hydrofluoric acid.
In order to overcome the toxicity of hydrofluoric acid or fluorine-containing substances in the conventional fluorine-containing etching solution, research has been conducted on a fluorine-free etching solution. CN111116047A discloses a method for manufacturing matte glass, which adopts fluorine-free alkaline etching solution and catalyst to etch the matte layer; the glass substrate after etching is subjected to strengthening treatment, but the method produces misted glass and cannot ensure the surface smoothness after etching.
Therefore, the existing etching for the glass has the problems that the etching solution is high in acidity or toxicity, and the surface smoothness after etching is not realized.
Therefore, it is necessary to develop a glass etching method to solve the problem of surface smoothness after etching existing glass.
Disclosure of Invention
In view of the problems in the prior art, the invention provides the glass etching method, the glass etching method does not need to adopt fluorine-containing substances, is more environment-friendly and harmless, greatly reduces the roughness of the inner wall of the etched glass, can reach the roughness less than or equal to 6nm under better conditions, can be widely applied to etching of various glasses, and has wide application prospect.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a glass etching method, which comprises the following steps: etching the glass by adopting an etching solution under an ultrasonic condition; the etching solution contains alkali and alcohol organic matters with the carbon atom number less than or equal to 10.
The method adopts the alcohol organic matter with the carbon atom number less than or equal to 10 and the alkali as the etching solution, wherein the hydroxyl in the alcohol organic matter can break the hydrogen bond between water molecules, reduce the viscosity of the etching solution, improve the mass transfer effect of the alkali in the etching solution and further promote the etching reaction, and the alcohol organic matter with the carbon atom number less than or equal to 10 is selected and can have better intersolubility with water. The invention also promotes the contact and mass transfer of the etching solution and the etched glass by adopting the ultrasonic for assistance, promotes the etching, thereby keeping the etching degree of each part of the glass consistent and improving the surface finish of the inner wall of the etched glass.
The organic alcohol in the present invention is an organic alcohol having 10 or less carbon atoms, and may be, for example, 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the carbon number of the alcohol organic substance is 2-4.
In the invention, the alcohol organic matter is preferably alcohol with 2-4 carbon atoms, has better intersolubility with water and larger polarity, and is more favorable for breaking hydrogen bonds between water molecules and promoting mass transfer of alkali in the etching solution.
Preferably, the alcohol organic substance is ethanol or isopropanol.
Preferably, the volume concentration of the alcoholic organic substance in the etching solution is 1 to 30%, for example, 1%, 5%, 8%, 11%, 14%, 18%, 21%, 24%, 27%, or 30%, etc., but is not limited to the values listed, and other values not listed in this range are also applicable.
Preferably, the frequency of the ultrasound is 200 to 1000kHz, for example, 200kHz, 250kHz, 280kHz, 300kHz, 350kHz, 370kHz, 400kHz, 450kHz, 460kHz, 500kHz, 550kHz, 600kHz, 650kHz, 700kHz, 750kHz, 800kHz, 900kHz or 1000kHz, etc., but is not limited to the recited values, and other values not recited in this range are also applicable.
Preferably, when the ultrasonic frequency is 200 to 300kHz excluding 300kHz, the volume concentration of the alcoholic organic substance in the etching solution is 10 to 30% excluding 10%, for example, 11%, 15%, 17%, 19%, 22%, 24%, 26%, 28%, or 30%, etc., but not limited to the above-mentioned values, and other values not listed in this range are also applicable.
Preferably, when the ultrasonic frequency is 300 to 500kHz excluding 500kHz, the volume concentration of the alcoholic organic substance in the etching solution is 5 to 10% excluding 5%, for example, 6%, 7%, 8%, 9%, or 10%, but not limited to the above-mentioned values, and other values not listed in this range are also applicable.
The frequency of the ultrasonic wave is matched with the concentration of the alcohol organic matter, wherein the ultrasonic wave generates a bubble cavity effect on the etching solution, and the smaller the generated cavity is along with the increase of the frequency of the ultrasonic wave, the alcohol organic matter with the corresponding volume concentration is matched at the moment, so that the using amount of the alcohol organic matter is reduced, and the roughness of the inner wall of the etched glass is small.
Preferably, the volume concentration of the alcoholic organic substance in the etching solution is 1 to 5%, for example, 1%, 2%, 3%, 4%, or 5% at a frequency of 500 to 1000kHz, but is not limited to the above-mentioned values, and other values not listed in the range are also applicable.
Preferably, the temperature of the etching is 60 to 90 ℃, for example, 60 ℃, 64 ℃, 67 ℃, 70 ℃, 74 ℃, 77 ℃, 80 ℃, 84 ℃, 87 ℃ or 90 ℃, but not limited to the cited values, and other values not listed in the range are also applicable, preferably 80 to 90 ℃.
The etching temperature of the invention is preferably 80-90 ℃, which is more beneficial to improving the mass transfer effect and finally improving the etching speed.
Preferably, the glass comprises any one of, or a combination of at least two of, soda glass, boron glass, or silica glass, with typical non-limiting combinations being combinations of soda glass and boron glass, silica glass and boron glass, and silica glass and soda glass.
Preferably, the base comprises sodium hydroxide and/or potassium hydroxide.
Preferably, the concentration of the base in the water of the etching solution is 30% or more by mass, and may be, for example, 30%, 32%, 34%, 35%, 37%, 39%, 40%, 42%, 44%, or 45% or the like, but is not limited to the values listed, and other values not listed in this range are also applicable.
The mass concentration of the alkali refers to the mass concentration of the alkali solution in water before being mixed with the alcohol organic matter.
As a preferable technical solution of the present invention, the method includes: etching the glass by using an etching solution at the temperature of 60-90 ℃ under an ultrasonic condition;
the etching solution contains alkali and alcohol organic matters with the carbon atom number less than or equal to 10; the mass concentration of the alkali in the water of the etching solution is more than or equal to 30 percent;
wherein when the ultrasonic frequency is 200-300 kHz and does not include 300kHz, the volume concentration of the alcohol organic matters in the etching solution is 10-30% and does not include 10%; when the ultrasonic frequency is 300-500 kHz and does not include 500kHz, the volume concentration of the alcohol organic matters in the etching solution is 5-10% and does not include 5%; when the ultrasonic frequency is 500-1000 kHz, the volume concentration of the alcohol organic matters in the etching solution is 1-5%.
The invention combines the ultrasonic with specific frequency and the etching solution of alcohol organic matter and alkali with specific volume concentration, not only can achieve better etching effect on the glass under the condition of not adopting fluorine-containing substances, but also has higher etching speed, high surface smoothness and low roughness of the inner wall of the etched glass, and has wide application prospect of the etched glass.
The post-treatment of the etched glass is not particularly limited in the present invention, and any method and manner for post-treatment of the etched glass known to those skilled in the art may be used, for example, the steps such as cleaning and the like may be adopted, and thus, the details are not described herein.
The etched glass has smooth surface and can be widely used in optical glass.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) the etching solution adopted by the glass etching method provided by the invention does not contain fluorine, and is more environment-friendly and harmless;
(2) the glass etching method provided by the invention combines specific etching solution and ultrasound, greatly reduces the roughness of the inner wall surface of the etched glass, the roughness is less than or equal to 16nm, the roughness is less than or equal to 6nm under better conditions, improves the smoothness of the etched surface, and the etching rate is more than 70 mu m/h.
Drawings
FIG. 1 is a test chart of surface roughness after etching by the glass etching method provided in example 1 of the present invention.
FIG. 2 is a test chart of surface roughness after etching by the glass etching method provided in comparative example 1 of the present invention.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
First, an embodiment
Example 1
The embodiment provides a glass etching method, which comprises the following steps:
etching the sodium glass by using an etching solution under the ultrasonic condition of 75 ℃ and the frequency of 200 kHz; the etching solution contains 20% ethanol by volume concentration and 38% sodium hydroxide by mass concentration in water.
The test chart of the roughness of the surface of the glass after etching in the embodiment is shown in fig. 1, and it can be seen from fig. 1 that the surface of the glass after etching is smooth and has small roughness.
Example 2
This example provides a glass etching method similar to that of example 1 except that the etching solution contains 5 vol% ethanol.
Example 3
This example provides a glass etching method similar to that of example 1, except that the etching solution contains 10 vol% ethanol.
Example 4
This example provides a glass etching method similar to that of example 1, except that the etching solution contains 15 vol% ethanol.
Example 5
This example provides a glass etching method similar to that of example 1, except that the etching solution contained 25% by volume of ethanol.
Example 6
This example provides a glass etching method similar to that of example 1, except that the etching solution contains 30 vol% ethanol.
Example 7
This example provides a glass etching method similar to that of example 1 except that the etching solution contained hexanol at a volume concentration of 20%.
Example 8
This example provides a glass etching method which is the same as that of example 1 except that the etching solution contains 20% by volume of octanol.
Example 9
The embodiment provides a glass etching method, which comprises the following steps:
etching the sodium glass by using an etching solution under the ultrasonic condition of 80 ℃ and the frequency of 40 kHz; the etching solution contains 5% ethanol by volume concentration and 35% sodium hydroxide by mass concentration in water.
Example 10
This example provides a glass etching process which is the same as that of example 9 except for the ultrasonic condition at a frequency of 60 kHz.
Example 11
This example provides a glass etching process identical to that of example 9 except for the ultrasonic condition at a frequency of 80 kHz.
Example 12
This example provides a glass etching process identical to that of example 9 except for the ultrasonic condition at a frequency of 100 kHz.
Example 13
The embodiment provides a glass etching method, which comprises the following steps:
etching boron glass by using an etching solution under the ultrasonic conditions of 72 ℃ and 300kHz frequency; the etching solution contains 10% volume concentration of isopropanol and 32% mass concentration of potassium hydroxide in water.
Example 14
This example provides a glass etching method similar to that of example 13 except that the etching solution contained 3% by volume of isopropyl alcohol.
Example 15
The embodiment provides a glass etching method, which comprises the following steps:
etching boron glass by using an etching solution under the ultrasonic conditions of 90 ℃ and 480kHz frequency; the etching solution contained 5.5% by volume of isopropyl alcohol and 34% by mass of sodium hydroxide in water.
Example 16
The embodiment provides a glass etching method, which comprises the following steps:
etching boron glass by using an etching solution under the ultrasonic conditions of 80 ℃ and 700kHz frequency; the etching solution contained 3% by volume isopropyl alcohol and 34% by mass potassium hydroxide in water.
Example 17
This example provides a glass etching method similar to that of example 16, except that the etching solution contained isopropyl alcohol at a volume concentration of 0.1%.
Example 18
The embodiment provides a glass etching method, which comprises the following steps:
etching boron glass by using an etching solution under the ultrasonic conditions of 75 ℃ and 500kHz frequency; the etching solution contains 5% ethanol by volume concentration and 36% sodium hydroxide by mass concentration in water.
Example 19
The embodiment provides a glass etching method, which comprises the following steps:
etching boron glass by using an etching solution under the ultrasonic conditions of 90 ℃ and 1000kHz frequency; the etching solution contains 1% by volume of isopropanol and 38% by mass of sodium hydroxide in water.
Second, comparative example
Comparative example 1
This comparative example provides a glass etching method similar to that of example 1 except that the etching solution contained no ethanol.
The test chart of the roughness of the etched glass surface of the comparative example is shown in FIG. 2, and it can be seen from FIG. 2 that the etched glass surface of the comparative example 1 has poor smoothness and high roughness.
Comparative example 2
This comparative example provides a glass etching process which is the same as example 1 except that ultrasound is not used.
Comparative example 3
This comparative example provides a glass etching process that is the same as example 1 except that ethanol is replaced with dodecyl alcohol.
Third, test and results
The test method comprises the following steps: the roughness of the inner wall surface of the glass after etching of the above examples and comparative examples was measured by an atomic force microscope, and the results are shown in table 1.
TABLE 1
The results of the etching rate tests conducted on examples 1 to 6 are shown in Table 2.
TABLE 2
| Time of day rate (μm/h) | |
| Example 1 | 130 |
| Example 2 | 260 |
| Example 3 | 208 |
| Example 4 | 156 |
| Example 5 | 104 |
| Example 6 | 78 |
From tables 1 and 2, the following points can be seen:
(1) it can be seen from the comprehensive examples 1 to 19 that the glass etching method provided by the invention adopts the solution of alkali and alcohol organic matters with the carbon number less than or equal to 10 as the etching solution and adopts ultrasound as an auxiliary, so that the roughness of the inner wall of the etched glass is greatly reduced, the roughness can reach less than or equal to 16nm, the etching rate is more than 70 μm/h, and the roughness and the etching rate of the etched inner wall can be considered at the same time;
(2) it can be seen from the comprehensive examples 1 to 6 that, in the examples 1 and 3 to 6, when the ultrasonic frequency is 200kHz, the volume concentration of ethanol is more than 10%, compared with the volume concentration of ethanol of 5% in the example 2, the roughness of the examples 1 and 3 to 6 of the market water is less than 6nm, and the roughness of the example 2 reaches 6.4nm, thereby showing that the roughness of the inner wall of the etched glass is further reduced by combining the specific ultrasonic frequency and the concentration of organic alcohol;
(3) it can be seen from the combination of examples 1, 7 to 8 and comparative example 3 that ethanol is used in example 1, and compared with hexanol and octanol respectively used in examples 7 to 8 and dodecyl alcohol used in comparative example 3, the roughness of example 1 is 5.1nm, the roughness of examples 7 to 8 is 5.8 and 6.4nm respectively, and the roughness of comparative example 3 is up to 19.2nm, which indicates that the roughness of the inner wall of the etched glass is reduced by controlling the number of carbon atoms of organic alcohol within a specific range;
(4) it can be seen from the combination of the example 1 and the comparative examples 1 to 2 that, in the example 1, the roughness is much lower than that in the comparative examples 1 to 2 when the ultrasound and the ethanol are combined and compared with the comparative examples 1 to 2 without the ultrasound and the ethanol respectively, so that the roughness of the inner wall after etching is greatly reduced by combining the ultrasound and the addition of the organic alcohol, the mass concentration of the alkali in the etching solution is reduced to a certain extent by the addition of the alcohol, and the method can also guarantee a higher etching rate and has an obvious effect.
In conclusion, the glass etching method provided by the invention adopts the solution of alkali and alcohol organic matters with the carbon number less than or equal to 10 as the etching solution and the ultrasonic with the specific frequency as an auxiliary, so that the roughness of the inner wall of the etched glass is greatly reduced, the roughness can reach less than or equal to 6nm under the better condition, and the glass etching method has wide application in optical glass.
The applicant states that the present invention is described by the above embodiments to explain the detailed structural features of the present invention, but the present invention is not limited to the above detailed structural features, that is, it is not meant to imply that the present invention must be implemented by relying on the above detailed structural features. It should be understood by those skilled in the art that any modifications, equivalent substitutions of selected elements of the present invention, additions of auxiliary elements, selection of specific forms, etc., are intended to fall within the scope and disclosure of the present invention.
Claims (11)
1. A glass etching method, characterized in that the glass etching method comprises: etching the glass by adopting an etching solution under an ultrasonic condition;
the etching solution contains alkali and alcohol organic matters with the carbon atom number less than or equal to 10;
the frequency of the ultrasonic wave is 200-1000 kHz;
the volume concentration of the alcohol organic matters in the etching solution is 1-30%;
the mass concentration of the alkali in the water of the etching solution is more than or equal to 30 percent.
2. The glass etching method according to claim 1, wherein the number of carbon atoms of the alcohol organic substance is 2 to 4.
3. The glass etching method of claim 1, wherein the alcohol organic comprises ethanol or isopropanol.
4. The glass etching method according to claim 1, wherein when the ultrasonic frequency is 200 to 300kHz and does not include 300kHz, the volume concentration of the alcoholic organic compound in the etching solution is 10 to 30% and does not include 10%.
5. The glass etching method according to claim 1, wherein when the ultrasonic frequency is 300 to 500kHz and 500kHz is excluded, the volume concentration of the alcoholic organics in the etching solution is 5 to 10% and 5% is excluded.
6. The glass etching method according to claim 1, wherein the volume concentration of the alcoholic organic compound in the etching solution is 1 to 5% when the frequency of the ultrasonic wave is 500 to 1000 kHz.
7. The glass etching method according to claim 1, wherein the etching temperature is 60 to 90 ℃.
8. The glass etching method according to claim 7, wherein the etching temperature is 80 to 90 ℃.
9. The glass etching method according to claim 1, wherein the glass comprises any one of sodium glass, boron glass, or silicon glass, or a combination of at least two thereof.
10. The glass etching method of claim 1, wherein the alkali comprises sodium hydroxide and/or potassium hydroxide.
11. The glass etching method according to claim 1, wherein the method comprises: etching the glass by using an etching solution at the temperature of 60-90 ℃ under an ultrasonic condition;
the etching solution contains alkali and alcohol organic matters with the carbon atom number less than or equal to 10; the mass concentration of the alkali in the water of the etching solution is more than or equal to 30 percent;
wherein when the ultrasonic frequency is 200-300 kHz and does not include 300kHz, the volume concentration of the alcohol organic matters in the etching solution is 10-30% and does not include 10%; when the ultrasonic frequency is 300-500 kHz and does not include 500kHz, the volume concentration of the alcohol organic matters in the etching solution is 5-10% and does not include 5%; when the ultrasonic frequency is 500-1000 kHz, the volume concentration of the alcohol organic matters in the etching solution is 1-5%.
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Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4602184A (en) * | 1984-10-29 | 1986-07-22 | Ford Motor Company | Apparatus for applying high frequency ultrasonic energy to cleaning and etching solutions |
| DE10241300A1 (en) * | 2002-09-04 | 2004-03-18 | Merck Patent Gmbh | Etching for silicon surfaces and layers, used in photovoltaic, semiconductor and high power electronics technology, for producing photodiode, circuit, electronic device or solar cell, is thickened alkaline liquid |
| FR2923947B1 (en) * | 2007-11-20 | 2010-06-11 | Inst Polytechnique Grenoble | METHOD AND DEVICE FOR SELECTIVE ETCHING. |
| KR20090081979A (en) * | 2008-01-25 | 2009-07-29 | 소닉스자펜 주식회사 | Etching composition for manufacturing concavo-convex substrate in monocrystalline silicon photovoltaic devices |
| JP5251861B2 (en) * | 2009-12-28 | 2013-07-31 | 信越化学工業株式会社 | Method for producing synthetic quartz glass substrate |
| CN105228788A (en) * | 2012-11-29 | 2016-01-06 | 康宁股份有限公司 | For sacrifice cover layer and the method thereof of laser drill base material |
| JP2017525155A (en) * | 2014-07-30 | 2017-08-31 | コーニング インコーポレイテッド | Ultrasonic bath and method for uniform glass substrate etching |
| CN107531564A (en) * | 2015-02-27 | 2018-01-02 | 康宁股份有限公司 | By laser damage and it is etched in the product that the method for passage is manufactured in glassware and is thus manufactured |
| US20170103249A1 (en) * | 2015-10-09 | 2017-04-13 | Corning Incorporated | Glass-based substrate with vias and process of forming the same |
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