CN111040639A - Chemical mechanical polishing liquid for processing optical surface of Ge-As-Se chalcogenide glass - Google Patents
Chemical mechanical polishing liquid for processing optical surface of Ge-As-Se chalcogenide glass Download PDFInfo
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Abstract
The invention discloses a chemical mechanical polishing solution for processing the optical surface of Ge-As-Se chalcogenide glass, which comprises the following components: polishing powder, a chemical corrosion reagent, an acid-base reagent, a dispersing agent and deionized water; the polishing powder is selected from alumina, diamond powder or cerium oxide; the chemical corrosion reagent is selected from an alkaline reagent or an oxidant, the alkaline reagent is sodium hydroxide, sodium carbonate, sodium bicarbonate, cyclohexylamine, triethylamine or ethylenediamine, and the oxidant is one of hydrogen peroxide, potassium permanganate, ferric chloride and potassium ferrate; the acid-base reagent is used for ensuring the stability of the acidity and the alkalinity of the polishing solution, wherein the acid is one of sulfuric acid, hydrochloric acid, oxalic acid, acetic acid and citric acid; the alkali is selected from one of sodium hydroxide, sodium carbonate, sodium bicarbonate, cyclohexylamine, triethylamine and ethylenediamine; the dispersant is polyphosphate substance, which is used for improving the dispersibility of the polishing powder in turbid liquid. The invention only needs to pertinently adjust the concentration of the chemical corrosion reagent for the chalcogenide glass with different components, and has universality.
Description
Technical Field
The invention belongs to the technical field of precise surface processing of infrared optical materials, and relates to a chemical mechanical polishing solution for optical surface processing of Ge-As-Se chalcogenide glass.
Background
Most of infrared optical elements are crystalline materials such as silicon, germanium, zinc sulfide, zinc selenide and the like, and athermalization treatment is very necessary based on the thermal expansion performance and the temperature-dependent change characteristic of the refractive index. The chalcogenide glass as a common infrared optical material has the characteristics of optical and thermodynamic properties such as small thermo-optic coefficient (dn/dT), large thermal expansion coefficient and the like, can realize athermal matching with other materials, and is beneficial to correction of thermal difference and chromatic aberration of an infrared optical system. The infrared imaging system is widely applied to the infrared imaging fields of infrared thermal imaging, infrared sensing, vehicle-mounted night vision and the like.
The chalcogenide glass material has physical properties of small hardness and large thermal expansion coefficient, and is a solid solution material. The surface shape precision is difficult to control; the surface is easy to damage, more pits and scratches exist, and the grade of surface defects is limited; the processing stability is poor, and even the material cracks and other problems can occur. At present, the processing method of chalcogenide glass mainly comprises the traditional polishing method, single-point diamond turning and precision die pressing. The traditional polishing method is more common, but is influenced by the characteristics of processing auxiliary materials and materials, and the obtained optical surface has more microscopic surface defects; the turning lines are remained on the surface of the single-point diamond turning; the die pressing is suitable for mass production of small-sized parts. Chemical mechanical polishing is one of the methods expected to improve the optical surface quality of chalcogenide glass, and the chemical components of the polishing solution are key factors influencing the surface quality and the material removal rate of the chalcogenide glass. Therefore, how to formulate a reasonable polishing solution for chemical mechanical polishing needs further research.
Disclosure of Invention
Objects of the invention
The purpose of the invention is: the invention provides a chemical mechanical polishing solution for processing optical surfaces of Ge-As-Se chalcogenide glass and a preparation method thereof, wherein the invention selects commonly used alumina polishing powder for polishing infrared optical materials As a film material and utilizes the mechanical grinding function of the alumina polishing powder; meanwhile, chemical reagents are added into the polishing solution to introduce a chemical corrosion effect, so that mechanical grinding and chemical corrosion removal of the material are realized. The method is suitable for polishing the optical surface of the Ge-As-Se chalcogenide glass, and can improve the surface defect condition and reduce the surface roughness value of the chalcogenide glass so As to improve the optical surface quality of the chalcogenide glass.
(II) technical scheme
In order to solve the above technical problems, the present invention provides a chemical mechanical polishing solution for optical surface processing of Ge-As-Se chalcogenide glass, comprising: polishing powder, a chemical corrosion reagent, an acid-base reagent, a dispersing agent and deionized water; the polishing powder is one of alumina, diamond powder and cerium oxide for polishing infrared materials; the chemical corrosion reagent is selected from an alkaline reagent or an oxidant, the alkaline reagent is one of sodium hydroxide, sodium carbonate, sodium bicarbonate, cyclohexylamine, triethylamine and ethylenediamine, and the oxidant is one of hydrogen peroxide, potassium permanganate, ferric chloride and potassium ferrate; the acid-base reagent is used for ensuring the stability of the acidity and the alkalinity of the polishing solution, wherein the acid is one of sulfuric acid, hydrochloric acid, oxalic acid, acetic acid and citric acid; the alkali is selected from one of sodium hydroxide, sodium carbonate, sodium bicarbonate, cyclohexylamine, triethylamine and ethylenediamine; the dispersant is polyphosphate substance, which is used for improving the dispersibility of the polishing powder in turbid liquid.
Wherein, the polishing powder is aluminum oxide polishing powder, the chemical corrosion reagent is hydrogen peroxide, the acid-base reagent is sulfuric acid, and the dispersing agent is sodium hexametaphosphate.
Wherein, the content of each component in 1000mL of polishing solution is as follows: 30-70 g/L of aluminum oxide polishing powder; 0.5-50 g/L of sulfuric acid; 0.1-1 g/L sodium hexametaphosphate; 40-250 g/L of hydrogen peroxide and the balance of deionized water.
Wherein, 1000mL of polishing solution comprises the following components: 147.49ml of 30 wt% H2O2Stock solution, 0.27ml of 98 wt% H2SO4Stock solution, 50g of W0.3 alumina polishing powder, 1g of sodium hexametaphosphate and 852.24ml of deionized water.
Wherein, 1000mL of polishing solution comprises the following components: 294.99ml of 30 wt% H2O2 stock solution, 0.27ml of 98 wt% H2SO4 stock solution, 50g of W0.3 alumina polishing powder, 1g of sodium hexametaphosphate and 704.74ml of deionized water.
Wherein, 1000mL of polishing solution comprises the following components: 442.48ml of 30 wt% H2O2 stock solution, 0.27ml of 98 wt% H2SO4 stock solution, 50g of W0.3 alumina polishing powder, 1g of sodium hexametaphosphate and 557.25ml of deionized water.
Wherein, 1000mL of polishing solution comprises the following components: 589.97ml of 30 wt% H2O2 stock solution, 0.27ml of 98 wt% H2SO4 stock solution, 50g of W0.3 alumina polishing powder, 1g of sodium hexametaphosphate and 409.76ml of deionized water.
The preparation method of the chemical mechanical polishing solution for processing the optical surface of the Ge-As-Se chalcogenide glass comprises the following steps:
weighing alumina polishing powder with a preset weight, adding the alumina polishing powder into deionized water while stirring, and performing ultrasonic dispersion for 5-10 min;
weighing sodium hexametaphosphate with preset weight, and adding the sodium hexametaphosphate into the solution while stirring;
measuring a sulfuric acid stock solution with a preset volume, and adding the sulfuric acid stock solution into the solution along the wall of a container to a set pH value;
measuring a hydrogen peroxide stock solution with a preset volume, and adding the hydrogen peroxide stock solution into the solution while stirring.
(III) advantageous effects
The chemical mechanical polishing solution for the optical surface processing of the Ge-As-Se chalcogenide glass and the preparation method thereof, which are provided by the technical scheme, can reduce the number of surface defects of the chalcogenide glass after polishing and reduce the surface roughness value of the chalcogenide glass. The chemical reagents (acid, alkali, oxidant and dispersant) involved in the test are all inorganic substances which are easy to dissolve in water, the concentration of the chemical reagents can be directly controlled by a weighing mode, and the preparation is convenient. In addition, the invention only needs to pertinently adjust the concentration of the chemical corrosion reagent for the chalcogenide glass with different components, and has universality. Moreover, the method only changes the chemical components of the polishing solution, has no special requirements on instruments and equipment, and can be directly used by operators.
Drawings
FIG. 1 is a schematic representation of a microscopic image of a chemical mechanical polishing test sample.
Detailed Description
In order to make the objects, contents and advantages of the present invention clearer, the following detailed description of the embodiments of the present invention will be made in conjunction with the accompanying drawings and examples.
The chemical mechanical polishing solution for processing the optical surface of Ge-As-Se chalcogenide glass comprises the following components: polishing powder, a chemical corrosion reagent, an acid-base reagent, a dispersing agent and deionized water.
Wherein, polishing powder: the common aluminum oxide (white corundum), diamond powder, cerium oxide and the like for polishing infrared materials can be selected, the requirements of infrared optical surfaces on the grade of surface defects, cost control and the like are fully considered, and the aluminum oxide polishing powder is preferred.
Chemical corrosion reagent: the Ge-As-Se chalcogenide glass can chemically react with alkaline reagents (including sodium hydroxide, sodium carbonate, sodium bicarbonate, cyclohexylamine, triethylamine, ethylenediamine and the like), oxidants (including hydrogen peroxide, potassium permanganate, ferric chloride, potassium ferrate and the like) and the like. In order to facilitate monitoring of the processing process and achieve the purposes of guaranteeing personal safety and environmental protection, the hydrogen peroxide which is colorless and tasteless and has nontoxic decomposition products is preferably used as a chemical corrosion reagent.
Acid-base reagent: the pH of the solution plays a crucial role in the stability of the polishing solution, and the acid can be selected from: sulfuric acid, hydrochloric acid, oxalic acid, acetic acid, citric acid, and the like; alkalies: sodium hydroxide, sodium carbonate, sodium bicarbonate, cyclohexylamine, triethylamine, ethylenediamine, and the like. The acidic substance is added in the scheme, so that the dispersion stability of the polishing powder can be improved, the decomposition rate of hydrogen peroxide can be slowed down, the pH value of the solution can be accurately controlled, the pH stability of the solution can be ensured, and sulfuric acid is preferably selected.
Dispersing agent: the dispersant can improve the dispersibility of the polishing powder in turbid liquid, and is usually polyphosphate substances. The invention selects sodium hexametaphosphate as the dispersant of the alumina polishing solution.
The content of each component in the polishing solution can be properly adjusted according to the content of three elements Ge-As-Se in the chalcogenide glass to be processed, and the content of the added reagent meets the following mass percentage range:
the content of each substance in 1000mL of polishing solution is as follows: 1. 30-70 g/L of aluminum oxide polishing powder; 2. 0.5-50 g/L of sulfuric acid; 3. 0.1-1 g/L sodium hexametaphosphate; 4. 40-250 g/L of hydrogen peroxide and the balance of deionized water.
The components of the polishing powder are sequentially added into the polishing solution according to a certain sequence and content, and the polishing solution is subjected to ultrasonic treatment for 3-5 minutes by using an ultrasonic machine and then can be used.
The chemical mechanical polishing solution in each example of the invention has the composition and content shown in the attached table 1.
TABLE 1 accompanying the chemical mechanical polishing liquid compositions and contents
Comparative example
Weighing 50g of aluminum oxide polishing powder with the particle size of W0.3, adding the aluminum oxide polishing powder into 1000ml of deionized water while stirring, and performing ultrasonic dispersion for 5-10 min;
and (3) carrying out effect analysis:
mixing wafer Ge of phi 40mm10As40Se50The chalcogenide glass sample is placed on a polishing machine, the rotating speed of a main shaft is controlled to be 37rpm, the swing speed of a swing shaft is controlled to be 25rpm, the eccentricity is 10mm, the polishing time is 30min, the condition of surface layer defects of the finally obtained surface is shown in the attached figure 1- (a), and the surface roughness is shown in the attached table 2.
Example 1
Weighing 50g of alumina polishing powder with the particle size of W0.3, adding the alumina polishing powder into 852.24ml of deionized water while stirring, and performing ultrasonic dispersion for 5-10 min;
weighing 1g of sodium hexametaphosphate, and adding the solution while stirring;
measuring 0.27ml of 98% sulfuric acid stock solution, and adding the sulfuric acid stock solution into the solution along the wall of a container until the pH value is about 2;
147.49ml of a 30% strength stock solution of hydrogen peroxide were weighed out and added to the above solution with stirring.
And (3) carrying out effect analysis:
mixing wafer Ge of phi 40mm10As40Se50Putting the chalcogenide glass sample on a polishing machine, controlling the rotating speed of a main shaft to be 37rpm, the swing speed of a swing shaft to be 25rpm, the eccentricity to be 10mm, and polishingThe time is 30min, the surface layer defect condition of the finally obtained surface is shown in attached figure 1- (b), and the surface roughness is shown in attached table 2.
Example 2
Weighing 50g of alumina polishing powder with the particle size of W0.3, adding the alumina polishing powder into 704.74ml of deionized water while stirring, and performing ultrasonic dispersion for 5-10 min;
weighing 1g of sodium hexametaphosphate, and adding the solution while stirring;
measuring 0.27ml of 98% sulfuric acid stock solution, and adding the sulfuric acid stock solution into the solution along the wall of a container until the pH value is about 2;
294.99ml of a 30% strength stock solution of hydrogen peroxide were weighed out and added to the above solution with stirring.
And (3) carrying out effect analysis:
mixing wafer Ge of phi 40mm10As40Se50And (3) putting the chalcogenide glass sample on a polishing machine, controlling the rotating speed of a main shaft to be 37rpm, the swinging speed of a swing shaft to be 25rpm, the eccentricity to be 10mm and the polishing time to be 30min, and finally obtaining the surface layer defect condition of the surface as shown in the attached diagram 1- (c) and the surface roughness as shown in the attached table 2.
Example 3
Weighing 50g of alumina polishing powder with the particle size of W0.3, adding the alumina polishing powder into 557.25ml of deionized water while stirring, and performing ultrasonic dispersion for 5-10 min;
weighing 1g of sodium hexametaphosphate, and adding the solution while stirring;
measuring 0.27ml of 98% sulfuric acid stock solution, and adding the sulfuric acid stock solution into the solution along the wall of a container until the pH value is about 2;
442.48ml of a 30% strength stock solution of hydrogen peroxide were weighed out and added to the above solution with stirring.
And (3) carrying out effect analysis:
mixing wafer Ge of phi 40mm10As40Se50The chalcogenide glass sample is placed on a polishing machine, the rotating speed of a main shaft is controlled to be 37rpm, the swing speed of a swing shaft is controlled to be 25rpm, the eccentricity is 10mm, the polishing time is 30min, the condition of surface layer defects of the finally obtained surface is shown in the attached diagram 1- (d), and the surface roughness is shown in the attached diagram 2.
Example 4
Weighing 50g of alumina polishing powder with the particle size of W0.3, adding the alumina polishing powder into 409.76ml of deionized water while stirring, and performing ultrasonic dispersion for 5-10 min;
weighing 1g of sodium hexametaphosphate, and adding the solution while stirring;
measuring 0.27ml of 98% sulfuric acid stock solution, and adding the sulfuric acid stock solution into the solution along the wall of a container until the pH value is about 2;
589.97ml of a 30% strength stock solution of hydrogen peroxide were weighed out and added to the above solution with stirring.
And (3) carrying out effect analysis:
mixing wafer Ge of phi 40mm10As40Se50The chalcogenide glass sample is placed on a polishing machine, the rotating speed of a main shaft is controlled to be 37rpm, the swing speed of a swing shaft is controlled to be 25rpm, the eccentricity is 10mm, the polishing time is 30min, the condition of surface layer defects of the finally obtained surface is shown in the attached figure 1- (e), and the surface roughness is shown in the attached table 2.
TABLE 2 influence of different hydrogen peroxide concentrations on surface roughness after polishing
Example summary analysis: polishing Effect of comparative examples 1 to 4 for Ge10As40Se50The chalcogenide glass sample can obtain the best effect when the concentration of hydrogen peroxide is about 10 wt% -15 wt%, and the corresponding surface defects are the minimum and the surface roughness is the minimum.
Finally, it should be noted that: when the technical scheme provided by the invention selects the easily-decomposed oxidants such as hydrogen peroxide, although the weak acid is added to reduce the decomposition rate, the easily-decomposed oxidants can be gradually decomposed along with the storage time, so that the excessive polishing solution is not suitable to be prepared and stored in a low-temperature environment every time so as to prevent the oxidants from decomposing and losing efficacy.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A chemical mechanical polishing solution for processing an optical surface of Ge-As-Se chalcogenide glass is characterized by comprising the following components: polishing powder, a chemical corrosion reagent, an acid-base reagent, a dispersing agent and deionized water; the polishing powder is one of alumina, diamond powder and cerium oxide for polishing infrared materials; the chemical corrosion reagent is selected from an alkaline reagent or an oxidant, the alkaline reagent is one of sodium hydroxide, sodium carbonate, sodium bicarbonate, cyclohexylamine, triethylamine and ethylenediamine, and the oxidant is one of hydrogen peroxide, potassium permanganate, ferric chloride and potassium ferrate; the acid-base reagent is used for ensuring the stability of the acidity and the alkalinity of the polishing solution, wherein the acid is one of sulfuric acid, hydrochloric acid, oxalic acid, acetic acid and citric acid; the alkali is selected from one of sodium hydroxide, sodium carbonate, sodium bicarbonate, cyclohexylamine, triethylamine and ethylenediamine; the dispersant is polyphosphate substance, which is used for improving the dispersibility of the polishing powder in turbid liquid.
2. The chemical mechanical polishing solution for optical surface processing of Ge-As-Se chalcogenide glass according to claim 1, wherein the polishing powder is alumina polishing powder, the chemical corrosion reagent is hydrogen peroxide, the acid-base reagent is sulfuric acid, and the dispersing agent is sodium hexametaphosphate.
3. The chemical mechanical polishing solution for optical surface processing of Ge-As-Se chalcogenide glass according to claim 2, wherein 1000mL of the polishing solution comprises the following components: 30-70 g/L of aluminum oxide polishing powder; 0.5-50 g/L of sulfuric acid; 0.1-1 g/L sodium hexametaphosphate; 40-250 g/L of hydrogen peroxide and the balance of deionized water.
4. The chemical mechanical polishing solution for optical surface processing of Ge-As-Se chalcogenide glass according to claim 3, wherein 1000mL of the polishing solution comprises the following components: 147.49ml of 30 wt% H2O2Stock solution, 0.27ml of 98 wt% H2SO4Stock solution, 50g of W0.3 alumina polishing powder, 1g of sodium hexametaphosphate and 852.24ml of sodium hexametaphosphateAnd (4) ionized water.
5. The chemical mechanical polishing solution for optical surface processing of Ge-As-Se chalcogenide glass according to claim 3, wherein 1000mL of the polishing solution comprises the following components: 294.99ml of 30 wt% H2O2 stock solution, 0.27ml of 98 wt% H2SO4 stock solution, 50g of W0.3 alumina polishing powder, 1g of sodium hexametaphosphate and 704.74ml of deionized water.
6. The chemical mechanical polishing solution for optical surface processing of Ge-As-Se chalcogenide glass according to claim 3, wherein 1000mL of the polishing solution comprises the following components: 442.48ml of 30 wt% H2O2 stock solution, 0.27ml of 98 wt% H2SO4 stock solution, 50g of W0.3 alumina polishing powder, 1g of sodium hexametaphosphate and 557.25ml of deionized water.
7. The chemical mechanical polishing solution for optical surface processing of Ge-As-Se chalcogenide glass according to claim 3, wherein 1000mL of the polishing solution comprises the following components: 589.97ml of 30 wt% H2O2 stock solution, 0.27ml of 98 wt% H2SO4 stock solution, 50g of W0.3 alumina polishing powder, 1g of sodium hexametaphosphate and 409.76ml of deionized water.
8. A method for preparing a chemical mechanical polishing solution for processing an optical surface of Ge-As-Se chalcogenide glass according to any one of claims 4 to 7, characterized in that the process is As follows:
weighing alumina polishing powder with a preset weight, adding the alumina polishing powder into deionized water while stirring, and performing ultrasonic dispersion for 5-10 min;
weighing sodium hexametaphosphate with preset weight, and adding the sodium hexametaphosphate into the solution while stirring;
measuring a sulfuric acid stock solution with a preset volume, and adding the sulfuric acid stock solution into the solution along the wall of a container to a set pH value;
measuring a hydrogen peroxide stock solution with a preset volume, and adding the hydrogen peroxide stock solution into the solution while stirring.
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| CN111748285A (en) * | 2020-06-22 | 2020-10-09 | 宁波日晟新材料有限公司 | Ferrate-containing silicon carbide polishing solution and preparation method and application thereof |
| CN112680111A (en) * | 2020-12-24 | 2021-04-20 | 广东先导先进材料股份有限公司 | Polishing solution for glass and application thereof |
| CN116042098A (en) * | 2023-02-08 | 2023-05-02 | 广东粤港澳大湾区黄埔材料研究院 | Nano alumina polishing solution and application thereof in polishing of infrared chalcogenide glass |
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