CN113070742A - Polishing method for removing subsurface damage on surface of optical element - Google Patents
Polishing method for removing subsurface damage on surface of optical element Download PDFInfo
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- CN113070742A CN113070742A CN202110429742.6A CN202110429742A CN113070742A CN 113070742 A CN113070742 A CN 113070742A CN 202110429742 A CN202110429742 A CN 202110429742A CN 113070742 A CN113070742 A CN 113070742A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B13/00—Machines or devices designed for grinding or polishing optical surfaces on lenses or surfaces of similar shape on other work; Accessories therefor
Abstract
The invention relates to a polishing method for removing subsurface damage on the surface of an optical element, which is characterized by comprising the following steps: the method comprises the following steps: performing classical polishing on the optical element; step two: the classically polished optical element was subjected to vacuum plasma polishing. The invention adopts the composite polishing technology of classical polishing and plasma polishing, can obviously eliminate the surface and sub-surface damage of the optical element, and the composite polishing technology can effectively overcome the problems of the surface and sub-surface damage of the optical element caused by classical polishing and low polishing efficiency of plasma polishing, namely, the classical polishing is combined with the plasma polishing, and the polishing efficiency and the removal of the damaged layer can be considered at the same time.
Description
Technical Field
The invention belongs to the technical field of optical processing, and particularly relates to a polishing method for removing subsurface damage on the surface of an optical element.
Background
Aiming at the applications of inertial confinement nuclear fusion, remote imaging detection and the like, the optical element needs to meet the requirements of ultra-smoothness and low loss, and the manufacturing method of the optical element needs to meet the requirements of eliminating surface defects and subsurface damage. Subsurface damage to an optical element is a defect such as microcracks, fractures, deformations, etc., that are latent below the surface of the optical element, which can cause scattering of light and loss of signal, and increase the damage threshold of the laser. For high performance optical components, there are generally stringent requirements for subsurface damage conditions.
In order to reduce the sub-surface damage to the optical element in the polishing process, the invention discloses a polishing device and a method without sub-surface damage in Chinese invention patent application with the patent number of CN202011006458.X (with the publication number of CN 112192323A). The polishing device comprises a plasma generating device, a magnetic field device, a high-energy charged ion beam binding cavity and a processing and polishing vacuum cavity, wherein the high-energy charged ion beam generated by the plasma generating device is bound and isolated in the high-energy charged ion binding cavity outside a polishing area in the processing and polishing vacuum cavity through the magnetic field generated by the magnetic field device, and free radical plasma active groups generated by the plasma generating device enter the polishing area in the processing and polishing vacuum cavity to realize polishing and the like; the patent effectively reduces the number of high-energy charged ions in the process cavity, greatly reduces the bombardment sputtering effect of the high-energy ions on the surface of the optical element, can effectively remove the subsurface damage layer of the optical element, obviously improves the surface quality of the optical element and the like.
However, the method of vacuum plasma polishing is too inefficient, and for polishing optical elements, both polishing precision and polishing efficiency are required.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art and provides a polishing method for removing subsurface damage on the surface of an optical element, which has high polishing efficiency and high polishing precision.
The technical scheme adopted by the invention for solving the technical problems is as follows: a polishing method for removing subsurface damage from the surface of an optical element, comprising the steps of:
the method comprises the following steps: performing classical polishing on the optical element;
step two: the classically polished optical element was subjected to vacuum plasma polishing.
In order to achieve a better polishing effect, the first step comprises the following steps:
(1.1) pre-polishing the optical element;
(1.2) pressurizing the optical element to 4-8 Mpa, and controlling the rotating speed of a machine tool spindle to be 30-40 rpm, so that the optical element to be measured is pressed on a polishing die soaked with polishing liquid through mechanical pressure;
(1.3) preheating the polishing die, so that the asphalt layer on the polishing die is softened by heating and the plasticity is increased;
(1.4) adding a polishing liquid to the polishing mold, thereby forming a liquid film between the optical element and the polishing mold, the liquid film serving as a mass transfer and pressure transfer function;
(1.5) starting polishing for 60-90 min.
In order to achieve a better polishing effect, the second step includes the following steps:
(2.1) opening a vacuum chamber, putting the optical element subjected to classical polishing, and pumping the vacuum chamber to the background pressure;
(2.2) filling a process gas into the plasma source, wherein the process gas is Ar gas, oxygen gas and SF6Gas, carrier gas is Ar and O2The reaction gas is SF6Ar and O2As a substrate gas to provide an active atmosphere for other chemical gas plasma reactions during polishing, SF6The fluorine-containing plasma can reduce the surface roughness of the optical element;
(2.3) maintaining the pressure of the vacuum chamber at 20-40 Pa to make the reaction gas SF6The volatility is higher, and the purity of chemical components in a processed area is ensured;
(2.4) turning on a radio frequency power supply, wherein the frequency is 80-100 MHz, and the radio frequency power influences the removal rate of the plasma to the optical element, and the amplification is more gentle when the frequency is higher or lower than the frequency;
(2.5) starting polishing for 20-30 min;
(2.6) stopping filling the process gas after polishing is finished, and pumping the vacuum chamber to the background pressure;
(2.7) opening the vacuum chamber and taking out the processed optical element;
(2.8) pumping the vacuum chamber to a state of 0-5 Pa.
In order to increase the removal rate, in the step (1.1), the pre-polishing method comprises the following steps: firstly, coating a polar solvent on the surface of an optical element, then placing the optical element on a spin coater to rotate, and then washing the optical element for 5-10 min by using deionized water.
Preferably, the polar solvent is methyl ether or ethylene glycol. The polar solvent can remove pollutants on the surface of the optical element, and the dimethyl ether has strong polarity and can improve the removal rate. The applicant has made a comparative experiment in the experimental process, and compared with a non-polar chemical solvent isopropanol, the polar solvent has a good effect, and dimethyl ether has a better effect in the polar solvent.
In step (1.3), the polishing mold is preheated by: and putting the polishing die into warm water for 4-5 min.
Preferably, in the step (1.4), the polishing solution is a triethanolamine solution with a concentration of 30% to 50%.
Preferably, in the step (2.2), Ar and O2The flow rate is 50sccm, SF6The flow rate was 10 sccm. The removal rate increases with increasing oxygen flow, but oxygen reachesBy 50sccm, the removal rate is not increased but decreased in Ar and O2The proportion is close to 1: 1, the removal rate of the optical element reaches a maximum.
In order to further improve the removal efficiency of the impurities on the surface of the optical element, in the step (1.1), before the pre-polishing, the optical element is polished by a grinding plate, and a water-soluble cooling liquid is added in the polishing process for cooling, cleaning and lubricating.
Compared with the prior art, the invention has the advantages that: the invention adopts the composite polishing technology of classical polishing and plasma polishing, can obviously eliminate the surface and sub-surface damage of the optical element, and the composite polishing technology can effectively overcome the problems of the surface and sub-surface damage of the optical element caused by classical polishing and low polishing efficiency of plasma polishing, namely, the classical polishing is combined with the plasma polishing, and the polishing efficiency and the removal of the damaged layer can be considered at the same time.
Detailed Description
The present invention will be described in further detail with reference to examples.
In the following examples and comparative examples, samples of fused silica optical elements having a bore diameter of 300mm were selected, and the initial surface roughness of the samples was Ra2.45nm, where Ra is an index for measuring the surface roughness and is the arithmetic mean deviation of the profile, and Rvmax represents the maximum depth of subsurface damage.
Example 1
The initial surface roughness of the optical element of the preferred embodiment is Ra2.45nm, and the polishing method for removing subsurface damage on the surface of the optical element comprises the following steps:
the method comprises the following steps: performing classical polishing on the optical element, wherein the first step further comprises the following steps:
(1.1) pre-polishing the optical element, wherein the pre-polishing method comprises the following steps: firstly, coating polar solvent methyl ether on the surface of an optical element, then placing the optical element on a spin coater, rotating for 2min at the speed of 3000r/min, and then washing the optical element for 5min by using deionized water;
(1.2) pressurizing the optical element to 4Mpa, and controlling the rotating speed of a machine tool spindle to be 30 rpm;
(1.3) preheating the polishing die, wherein the method for preheating the polishing die comprises the following steps: putting the polishing mould into warm water at 50 ℃ for 5 min;
(1.4) adding polishing solution into the polishing mould, wherein the polishing solution is cooling solution of 30% triethanolamine solution (dissolving triethanolamine in water);
(1.5) polishing was started for 60 min.
After classical polishing, Ra is 1.85nm, and Rvmax is 89.6 nm; then, the following vacuum plasma polishing was performed;
step two: and performing vacuum plasma polishing on the classically polished optical element, wherein the second step comprises the following steps:
(2.1) opening a vacuum chamber, putting the optical element subjected to classical polishing, and pumping the vacuum chamber to the background pressure;
(2.2) filling a process gas into the plasma source, wherein the process gas is Ar gas, oxygen gas and SF6Gas, Ar and O2The flow rate is 50sccm, SF6The flow rate is 10 sccm;
(2.3) maintaining the pressure of the vacuum chamber at an operating pressure of 20 Pa;
(2.4) turning on a radio frequency power supply, wherein the frequency is 100 MHz;
(2.5) starting polishing for 20 min;
(2.6) stopping filling the process gas after polishing is finished, and pumping the vacuum chamber to the background pressure;
(2.7) opening the vacuum chamber and taking out the processed optical element;
(2.8) the vacuum chamber is pumped to a state of 5Pa, and the polishing is finished.
Ra of the final optical element was 0.89nm, Rvmax was 7.367 nm; from the above, the greatest subsurface damage depth of classical polishing is 89.6nm, the subsurface damage is severe, and after plasma polishing, the greatest subsurface damage depth is reduced to 7.367nm, and the subsurface damage density is relieved. Thus, plasma polishing can greatly reduce subsurface damage caused by classical polishing.
Example 2
Example 2 differs from example 1 in that:
in the step one (1.5), the polishing time is 90min, and the steps are the same as those in the step one of the example 1; after classical polishing, Ra is 1.69nm, Rvmax is 87.3 nm;
in step two (2.5), the polishing time is 30min, and the steps are the same as those in step two of example 1; after plasma polishing, Ra was 0.84nm and Rvmax was 5.367 nm.
As can be seen from the comparison between example 1 and example 2, the subsurface damage cannot be continuously and effectively eliminated by simply prolonging the polishing time of the classical polishing, and although Ra of the sample does not change much relative to the classical polishing after the plasma polishing, Rvmax changes significantly and the density of the surface damage layer is greatly reduced; with a moderately prolonged plasma polishing time, a surface with a smaller damage depth can be obtained.
Example 3
The initial surface roughness of the optical element of the preferred embodiment is Ra2.45nm, and the polishing method for removing subsurface damage on the surface of the optical element comprises the following steps:
the method comprises the following steps: performing classical polishing on the optical element, wherein the first step further comprises the following steps:
(1.1) pre-polishing the optical element, wherein the pre-polishing method comprises the following steps: firstly, coating polar solvent methyl ether on the surface of an optical element, then placing the optical element on a spin coater, rotating for 2min at the speed of 3000r/min, and then washing the optical element for 10min by using deionized water;
(1.2) pressurizing the optical element to 4Mpa, and controlling the rotating speed of a machine tool spindle to be 30 rpm;
(1.3) preheating the polishing die, wherein the method for preheating the polishing die comprises the following steps: putting the polishing mould into warm water at 50 ℃ for 5 min;
(1.4) adding polishing solution into the polishing mould, wherein the polishing solution is cooling solution of 30% triethanolamine solution (dissolving triethanolamine in water);
(1.5) polishing was started for 60 min.
After classical polishing, Ra is 1.92nm, and Rvmax is 110.70 nm;
step two: and performing vacuum plasma polishing on the classically polished optical element, wherein the second step comprises the following steps:
(2.1) opening a vacuum chamber, putting the optical element subjected to classical polishing, and pumping the vacuum chamber to the background pressure;
(2.2) filling a process gas into the plasma source, wherein the process gas is Ar gas, oxygen gas and SF6Gas, Ar and O2The flow rate is 50sccm, SF6The flow rate is 10 sccm;
(2.3) maintaining the pressure of the vacuum chamber at an operating pressure of 20 Pa;
(2.4) turning on a radio frequency power supply, wherein the frequency is 80 MHz;
(2.5) starting polishing for 20 min;
(2.6) stopping filling the process gas after polishing is finished, and pumping the vacuum chamber to the background pressure;
(2.7) opening the vacuum chamber and taking out the processed optical element;
(2.8) pumping the vacuum chamber to a state of 0-5 Pa, and finishing polishing.
The Ra of the final optical element was 0.92nm, and Rvmax was 12.14 nm.
Example 4
The initial surface roughness of the optical element of the preferred embodiment is Ra2.45nm, and the polishing method for removing subsurface damage on the surface of the optical element comprises the following steps:
the method comprises the following steps: performing classical polishing on the optical element, wherein the first step further comprises the following steps:
(1.1) pre-polishing the optical element, wherein the pre-polishing method comprises the following steps: firstly, coating polar solvent methyl ether on the surface of an optical element, then placing the optical element on a spin coater, rotating for 2min at the speed of 3000r/min, and then washing the optical element for 5min by using deionized water;
(1.2) pressurizing the optical element to 5Mpa, and controlling the rotating speed of a machine tool spindle to 35 rpm;
(1.3) preheating the polishing die, wherein the method for preheating the polishing die comprises the following steps: putting the polishing mould into warm water at 50 ℃ for 5 min;
(1.4) adding polishing solution into the polishing mould, wherein the polishing solution is cooling solution of 30% triethanolamine solution (dissolving triethanolamine in water);
(1.5) polishing was started for 60 min.
After classical polishing, Ra is 1.89nm, and Rvmax is 100.57 nm;
step two: and performing vacuum plasma polishing on the classically polished optical element, wherein the second step comprises the following steps:
(2.1) opening a vacuum chamber, putting the optical element subjected to classical polishing, and pumping the vacuum chamber to the background pressure;
(2.2) filling a process gas into the plasma source, wherein the process gas is Ar gas, oxygen gas and SF6Gas, Ar and O2The flow rate is 50sccm, SF6The flow rate is 10 sccm;
(2.3) maintaining the pressure of the vacuum chamber at an operating pressure of 30 Pa;
(2.4) turning on a radio frequency power supply, wherein the frequency is 90 MHz;
(2.5) starting polishing for 20 min;
(2.6) stopping filling the process gas after polishing is finished, and pumping the vacuum chamber to the background pressure;
(2.7) opening the vacuum chamber and taking out the processed optical element;
(2.8) the vacuum chamber is pumped to a state of 5Pa, and the polishing is finished.
Ra of the final optical element was 0.87nm, Rvmax was 9.37 nm; from the above, it can be seen that the surface roughness of the optical element is not greatly affected by changing the pressure and rotation speed of the classical polishing method, the pressure of the vacuum plasma and the power supply frequency, but Rvmax is significantly changed and the depth of the surface damage layer is greatly reduced.
Example 5
Example 5 differs from example 1 only in that:
before the optical element is pre-polished in the step (1.1), the optical element is polished, and water-soluble cooling liquid is added in the polishing process for cooling, cleaning and lubricating.
The method specifically comprises the following steps: a fine grinding piece with diamond granularity of W28 is used as a grinding tool and is arranged on a main shaft of a grinding machine to rotate at high speed so as to grind an optical element, and meanwhile, water-soluble cooling liquid (mainly water and a small amount of triethanolamine) with the concentration of 50% is added for cooling, cleaning and lubricating.
Compared with embodiment 1, the embodiment has greatly improved removal efficiency of impurities on the surface of the optical element.
Comparative example 1
The polishing method of the optical member of this comparative example included the steps of:
(1.1) pre-polishing the optical element, wherein the pre-polishing method comprises the following steps: firstly, coating polar solvent methyl ether on the surface of an optical element, then placing the optical element on a spin coater, rotating for 3min at the speed of 3000r/min, and then washing the optical element for 15min by using deionized water;
(1.2) pressurizing the optical element to 4Mpa, and controlling the rotating speed of a machine tool spindle to be 30 rpm;
(1.3) preheating the polishing die, wherein the method for preheating the polishing die comprises the following steps: putting the polishing mould into warm water at 50 ℃ for 5 min;
(1.4) adding polishing solution into the polishing mould, wherein the polishing solution is cooling solution of 30% triethanolamine solution (dissolving triethanolamine in water);
(1.5) polishing was started for 4 h. After treatment, the polished surface roughness of the optical element is less than 0.86nm, and the maximum subsurface damage depth Rvmax of the optical element can reach 12.5 nm.
From the above, the polishing method of the optical element only adopts the classical polishing method, and in the classical polishing process, the subsurface damage depth can be obviously reduced by properly prolonging the polishing time, but the efficiency is reduced and the damage cannot be continuously reduced by simply depending on the prolonging of the polishing time.
Comparative example 2
The polishing method of the optical member of this comparative example included the steps of:
(2.1) opening a vacuum chamber, putting the optical element subjected to classical polishing, and pumping the vacuum chamber to the background pressure;
(2.2) filling a process gas into the plasma source, wherein the process gas is Ar gas, oxygen gas and SF6Gas, Ar and O2The flow rate is 50sccm, SF6The flow rate is 10 sccm;
(2.3) maintaining the pressure of the vacuum chamber at an operating pressure of 20 Pa;
(2.4) turning on a radio frequency power supply, wherein the frequency is 100 MHz;
(2.5) starting polishing for 2 h;
(2.6) stopping filling the process gas after polishing is finished, and pumping the vacuum chamber to the background pressure;
(2.7) opening the vacuum chamber and taking out the processed optical element;
(2.8) the vacuum chamber is pumped to a state of 5Pa, and the polishing is finished.
As can be seen from the above, the polishing method of the optical element employs only the plasma polishing method. Under the condition, the average etching rate can reach 20nm/min, the working time is 2h when the initial surface roughness is 2.45nm, and the polishing surface roughness is lower than 0.86 nm. The maximum subsurface damage depth Rvmax can reach 11.5 nm.
Claims (9)
1. A polishing method for removing subsurface damage from the surface of an optical element, comprising the steps of:
the method comprises the following steps: performing classical polishing on the optical element;
step two: the classically polished optical element was subjected to vacuum plasma polishing.
2. The method of claim 1, wherein: the first step comprises the following steps:
(1.1) pre-polishing the optical element;
(1.2) pressurizing the optical element to 4-8 Mpa, and controlling the rotating speed of a machine tool spindle to be 30-40 rpm;
(1.3) preheating the polishing die;
(1.4) adding polishing liquid into the polishing die;
(1.5) starting polishing for 60-90 min.
3. A polishing method for removing subsurface damage from the surface of an optical element as recited in claim 1 or 2, wherein: the second step comprises the following steps:
(2.1) opening a vacuum chamber, putting the optical element subjected to classical polishing, and pumping the vacuum chamber to the background pressure;
(2.2) filling a process gas into the plasma source, wherein the process gas is Ar gas, oxygen gas and SF6A gas;
(2.3) maintaining the pressure of the vacuum chamber at the working pressure of 20-40 Pa;
(2.4) turning on a radio frequency power supply, wherein the frequency is 80-100 MHz;
(2.5) starting polishing for 20-30 min;
(2.6) stopping filling the process gas after polishing is finished, and pumping the vacuum chamber to the background pressure;
(2.7) opening the vacuum chamber and taking out the processed optical element;
(2.8) pumping the vacuum chamber to a state of 0-5 Pa.
4. A polishing method for removing subsurface damage from the surface of an optical element as recited in claim 2, wherein: in the step (1.1), the pre-polishing method comprises the following steps: firstly, coating a polar solvent on the surface of an optical element, then placing the optical element on a spin coater to rotate, and then washing the optical element for 5-10 min by using deionized water.
5. The polishing method for removing subsurface damage from the surface of an optical element as recited in claim 4, wherein: the polar solvent is methyl ether or ethylene glycol.
6. A polishing method for removing subsurface damage from the surface of an optical element as recited in claim 2, wherein: in the step (1.3), the polishing mold preheating method comprises the following steps: and putting the polishing die into warm water for 4-5 min.
7. A polishing method for removing subsurface damage from the surface of an optical element as recited in claim 2, wherein: in the step (1.4), the polishing solution is a triethanolamine solution with a concentration of 30% -50%.
8. According toA polishing method for removing subsurface damage from the surface of an optical element as recited in claim 3, wherein: in the step (2.2), Ar and O2The flow rate is 50sccm, SF6The flow rate was 10 sccm.
9. A polishing method for removing subsurface damage from the surface of an optical element as recited in claim 2, wherein: in the step (1.1), before the pre-polishing, the optical element is polished by a grinding plate, and a water-soluble cooling liquid is added in the polishing process for cooling, cleaning and lubricating.
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| CN109623581A (en) * | 2019-01-04 | 2019-04-16 | 芜湖启迪半导体有限公司 | A kind of surface polishing method of hard material |
| CN112192323A (en) * | 2020-09-23 | 2021-01-08 | 航天科工微电子系统研究院有限公司 | Polishing equipment and method without subsurface damage |
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2021
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| CN102011106A (en) * | 2010-09-07 | 2011-04-13 | 天津理工大学 | Method for flattening diamond film by using composite process |
| CN109366256A (en) * | 2018-12-10 | 2019-02-22 | 武汉大学 | A kind of composite polishing method based on laser and plasma |
| CN109623581A (en) * | 2019-01-04 | 2019-04-16 | 芜湖启迪半导体有限公司 | A kind of surface polishing method of hard material |
| CN112192323A (en) * | 2020-09-23 | 2021-01-08 | 航天科工微电子系统研究院有限公司 | Polishing equipment and method without subsurface damage |
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Application publication date: 20210706 |