CN112025417B - Non-contact ion beam polishing method for surface of optical diamond material - Google Patents
Non-contact ion beam polishing method for surface of optical diamond material Download PDFInfo
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- CN112025417B CN112025417B CN202010841748.XA CN202010841748A CN112025417B CN 112025417 B CN112025417 B CN 112025417B CN 202010841748 A CN202010841748 A CN 202010841748A CN 112025417 B CN112025417 B CN 112025417B
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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
- B24B1/002—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes using electric current
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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
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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
- B24B49/00—Measuring or gauging equipment for controlling the feed movement of the grinding tool or work; Arrangements of indicating or measuring equipment, e.g. for indicating the start of the grinding operation
- B24B49/12—Measuring or gauging equipment for controlling the feed movement of the grinding tool or work; Arrangements of indicating or measuring equipment, e.g. for indicating the start of the grinding operation involving optical means
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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
- B24B9/00—Machines or devices designed for grinding edges or bevels on work or for removing burrs; Accessories therefor
Abstract
The invention discloses a non-contact ion beam polishing method for the surface of an optical diamond material, which is characterized by comprising the following steps: (1) preparing and obtaining an optical-grade diamond material sample by adopting a microwave plasma chemical vapor deposition method; (2) completing sample clamping in a clean room; (3) starting an ion source until the ion source is stable; (4) polishing a layer of diamond material sample surface to obtain a clean surface; (5) carrying out large-area uniform etching and polishing by adopting high-energy wide-beam ion beams, wherein the beam pressure is 1200-1500V, and the diameter of the ion beams is 20-50 mm; (6) performing micro-area precision polishing by adopting low-energy narrow-beam ion beams, wherein the beam pressure is 600-800V, and the diameter of the ion beams is 2-15 mm; (7) and taking out the sample after polishing to obtain the diamond material with the nanoscale smooth surface. Compared with the prior art, the method can obtain the nano-level smooth surface.
Description
Technical Field
The invention relates to the technical field of precision manufacturing, in particular to a non-contact ion beam polishing method for the surface of an optical diamond material.
Background
The diamond has excellent optical performance, the transmittance of the diamond can reach more than 70 percent in the wave band range from visible light to micron wave, and the diamond is widely used in the aspect of infrared window materials by matching with high hardness and high stability of the diamond. The artificially manufactured diamond film has a transmittance similar to that of natural diamond in an infrared band, which can reach 71%, and thus is widely used in the optical field. The microwave loss of the optical-grade diamond film is less than or equal to 2.0x10-5(140GHz)。One of the key factors influencing microwave loss is the roughness of the surface of the film, the larger the roughness of the surface of the film is, the stronger the scattering of the surface is, and the larger the loss of incident waves is, and researches show that the optical transmittance of the diamond film can meet the application requirements only if the roughness reaches below 3 mu m. Diamond films prepared by CVD all have a tendency to grow in a preferred orientation, and the resulting film surfaces are generally very rough and far from meeting the use conditions of optical devices.
In order to obtain a highly accurate optical-grade diamond film, a method currently adopted is to polish a diamond film produced by CVD so that its surface roughness satisfies requirements. The polishing method mainly studied at present for the surface of diamond is mainly contact polishing, which comprises the following steps: mechanical polishing, chemical polishing, and chemically assisted mechanical polishing, etc. The contact type mechanical polishing process has difficult parameter control, has a plurality of elements influencing the surface quality of the film, and is limited by the polishing principle: mechanical polishing cannot polish large areas and complex curved surfaces; the main disadvantages of thermochemical polishing are the complex equipment and process, the poor processing stability and the high cost.
Ion beam polishing is a non-contact polishing method capable of removing defects, scratches, etc. on the surface of an element, and specifically, refer to the invention patent "method for reducing surface contamination of an ion beam polished optical element" of patent application No. 201910844111.3 (publication No. CN 110712094A).
However, when the non-contact ion beam polishing method is applied to polishing the surface of an optical diamond material, a nano-level smooth surface cannot be obtained, and the high-precision application requirement of the diamond film cannot be met.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for polishing the surface of the optical diamond material with a nanoscale smooth surface by a non-contact ion beam, aiming at the current situation of the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows: a non-contact ion beam polishing method for the surface of an optical diamond material is characterized by comprising the following steps:
(1) preparing and obtaining an optical-grade diamond material sample by adopting a microwave plasma chemical vapor deposition method;
(2) finishing sample clamping in the ultraclean room, then putting the sample into a sample frame of a secondary chamber of ion beam polishing equipment, closing the secondary chamber, and then transferring the sample to a main chamber;
(3) starting an ion source until the ion source is stable;
(4) polishing a layer of diamond material sample surface to obtain a clean surface;
(5) carrying out large-area uniform etching and polishing by adopting high-energy wide-beam ion beams, wherein the beam pressure is 1200-1500V, and the diameter of the ion beams is 20-50 mm;
(6) performing micro-area precision polishing by adopting low-energy narrow-beam ion beams, wherein the beam pressure is 600-800V, and the diameter of the ion beams is 2-15 mm;
(7) and taking out the sample after polishing to obtain the diamond material with the nanoscale smooth surface.
Preferably, step (4) is achieved by:
A. controlling the ion beam to vertically enter the Faraday cup, collecting data at equal intervals in the scanning direction, and determining the current density parameter of the ion beam;
B. controlling an ion beam to vertically enter the surface of a sample, performing a scanning experiment on the sample, measuring the polishing conditions of the surface of the sample before and after the experiment by an interferometer, and obtaining a removal function after Gaussian fitting;
C. setting the material removal amount in the experimental process, and calculating the residence time of the ion beam by adopting a numerical simulation method according to a removal function;
D. and loading an ion beam residence time program file and starting polishing.
Preferably, the ion source reaches a steady state in step (3) after 1-2 hours of starting.
Preferably, the polishing time of the high-energy wide-beam ion beam and the low-energy narrow-beam ion beam in steps (5) and (6) is determined according to the sample size:
wherein T is processing time, C is a proportionality constant, R is the radius of a processing element, B is an edge extension distance, v is the moving speed of the ion source during processing, and dx is the step length.
Preferably, the Ra value of the diamond material obtained in the step (7) is 3-40 nm.
Compared with the prior art, the invention has the advantages that:
(1) adopting an ion beam polishing technology, accelerating argon ions by an accelerator to obtain energy of hundreds to tens of thousands of electron volts, bombarding the surface of a sample by the ions carrying energy, contacting surface atoms and transferring the energy, and separating from the surface when the energy of the atoms is higher than the surface constraint energy to realize the removal of materials without introducing new pollutants or impurity elements;
(2) the surface layer is conventionally polished, large-area uniform etching polishing is carried out by combining high-energy wide-beam ion beams, micro-area precise polishing is carried out by low-energy narrow-beam ion beams, and finally the surface of the optical diamond material is polished to be nano-scale, so that the surface quality of the optical diamond material is greatly improved.
Drawings
FIG. 1 is a schematic diagram of an ion beam polishing process according to an embodiment of the present invention;
FIG. 2 is a graph showing ion beam polishing removal function of diamond in example 1 of the present invention;
FIG. 3 is a picture of the surface topography of the diamond material obtained after polishing in example 1 of the present invention;
fig. 4 is a picture of the surface roughness of the diamond material obtained after polishing in example 1 of the present invention.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
Example 1:
(1) preparing and obtaining an optical-grade diamond material sample by adopting a microwave plasma chemical vapor deposition method, wherein the schematic diagram of the ion beam polishing process is shown in figure 1;
(2) finishing sample clamping in the ultraclean room, then putting the sample into a sample frame of a secondary chamber of ion beam polishing equipment, closing the secondary chamber, and then transferring the sample to a main chamber;
(3) starting an ion source, wherein the ion source reaches a stable state after being started for 1-2 hours;
(4) polishing a layer of diamond material sample surface to obtain a clean surface, and specifically realizing the following steps:
A. controlling the ion beam to vertically enter the Faraday cup, collecting data at equal intervals in the scanning direction, and determining the current density parameter of the ion beam;
B. controlling the ion beam to vertically enter the surface of the sample, performing a scanning experiment on the sample, measuring the sample polishing conditions before and after the experiment by an interferometer, and obtaining a removal function (shown in figure 2) by Gaussian fitting;
C. setting the material removal amount in the experimental process, and calculating the residence time of the ion beam by adopting a numerical simulation method according to a removal function;
D. loading an ion beam residence time program file, and starting polishing;
(5) adopting high-energy wide-beam ion beams to carry out large-area uniform etching and polishing, wherein the beam pressure is 1300V, and the diameter of the ion beams is 30 mm;
(6) performing micro-area precision polishing by adopting low-energy narrow-beam ion beams, wherein the beam pressure is 700V, and the diameter of the ion beams is 10 mm;
wherein, the polishing time of the high-energy wide-beam ion beam and the low-energy narrow-beam ion beam is determined according to the sample size:
the ion beam processing time T is proportional to the element radius R and the boundary Border (B), inversely proportional to the ion beam movement step dx and the movement speed v, and the specific relation is expressed as:
wherein T is processing time, C is a proportionality constant, R is the radius of a processing element, B is an edge extension distance, v is the moving speed of the ion source during processing, and dx is the step length;
(7) and taking out a sample from the auxiliary vacuum chamber after polishing, and detecting the surface appearance and the surface roughness Ra of the polished diamond material by using a laser confocal microscope and an atomic force microscope.
The surface topography picture and the surface roughness picture of the diamond material obtained in example 1 are shown in fig. 3 and 4, respectively, and it can be seen that the Ra value of the diamond material was measured to be 3.7 nm.
Example 2:
(1) preparing and obtaining an optical-grade diamond material sample by adopting a microwave plasma chemical vapor deposition method, wherein the schematic diagram of the ion beam polishing process is shown in figure 1;
(2) finishing sample clamping in the ultraclean room, then putting the sample into a sample frame of a secondary chamber of ion beam polishing equipment, closing the secondary chamber, and then transferring the sample to a main chamber;
(3) starting an ion source, wherein the ion source reaches a stable state after being started for 1-2 hours;
(4) polishing a layer of diamond material sample surface to obtain a clean surface, and specifically realizing the following steps:
A. controlling the ion beam to vertically enter the Faraday cup, collecting data at equal intervals in the scanning direction, and determining the current density parameter of the ion beam;
B. controlling an ion beam to vertically enter the surface of a sample, performing a scanning experiment on the sample, measuring the polishing conditions of the sample before and after the experiment by an interferometer, and obtaining a removal function after Gaussian fitting;
C. setting the material removal amount in the experimental process, and calculating the residence time of the ion beam by adopting a numerical simulation method according to a removal function;
D. loading an ion beam residence time program file, and starting polishing;
(5) performing large-area uniform etching and polishing by adopting high-energy wide-beam ion beams, wherein the beam pressure is 1200V, and the diameter of the ion beams is 30 mm;
(6) performing micro-area precision polishing by adopting low-energy narrow-beam ion beams, wherein the beam pressure is 600V, and the diameter of the ion beams is 4 mm;
wherein the polishing time of the high-energy wide-beam ion beam and the low-energy narrow-beam ion beam is determined according to the sample size:
the ion beam processing time T is proportional to the element radius R and the boundary Border (B), inversely proportional to the ion beam movement step dx and the movement speed v, and the specific relation is expressed as:
wherein T is processing time, C is a proportionality constant, R is the radius of a processing element, B is an edge extension distance, v is the moving speed of the ion source during processing, and dx is the step length;
(7) and taking out a sample from the auxiliary vacuum chamber after polishing, and detecting the surface appearance and the surface roughness Ra of the polished diamond material by using a laser confocal microscope to detect that the Ra value of the diamond material is 30.5 nm.
Example 3:
(1) preparing and obtaining an optical-grade diamond material sample by adopting a microwave plasma chemical vapor deposition method, wherein the schematic diagram of the ion beam polishing process is shown in figure 1;
(2) completing sample clamping in the ultra-clean room, then putting the sample into a sample frame of an auxiliary chamber of ion beam polishing equipment, closing the auxiliary chamber, and then transferring the sample to a main chamber;
(3) starting an ion source, wherein the ion source reaches a stable state after being started for 1-2 hours;
(4) polishing a layer of diamond material sample surface to obtain a clean surface, and specifically realizing the following steps:
A. controlling the ion beam to vertically enter the Faraday cup, and acquiring data at equal intervals in the scanning direction to determine the current density parameter of the ion beam;
B. controlling an ion beam to vertically enter the surface of a sample, performing a scanning experiment on the sample, measuring the polishing conditions of the sample before and after the experiment by an interferometer, and obtaining a removal function after Gaussian fitting;
C. setting the material removal amount in the experimental process, and calculating the residence time of the ion beam by adopting a numerical simulation method according to a removal function;
D. loading an ion beam residence time program file, and starting polishing;
(5) adopting high-energy wide-beam ion beams to carry out large-area uniform etching and polishing, wherein the beam pressure is 1500V, and the diameter of the ion beams is 20 mm;
(6) performing micro-area precision polishing by adopting low-energy narrow-beam ion beams, wherein the beam pressure is 800V, and the diameter of the ion beams is 8 mm;
wherein, the polishing time of the high-energy wide-beam ion beam and the low-energy narrow-beam ion beam is determined according to the sample size:
the ion beam processing time T is proportional to the element radius R and the boundary Border (B), inversely proportional to the ion beam movement step dx and the movement speed v, and the specific relation is expressed as:
wherein T is processing time, C is a proportionality constant, R is the radius of a processing element, B is an edge extension distance, v is the moving speed of the ion source during processing, and dx is the step length;
(7) and taking out a sample from the auxiliary vacuum chamber after polishing, and detecting the surface appearance and the surface roughness Ra of the polished diamond material by using a laser confocal microscope to detect that the Ra value of the diamond material is 15.2 nm.
Claims (5)
1. A non-contact ion beam polishing method for the surface of an optical diamond material is characterized by comprising the following steps:
(1) preparing and obtaining an optical-grade diamond material sample by adopting a microwave plasma chemical vapor deposition method;
(2) finishing sample clamping in the ultraclean room, then putting the sample into a sample frame of a secondary chamber of ion beam polishing equipment, closing the secondary chamber, and then transferring the sample to a main chamber;
(3) starting an ion source until the ion source is stable;
(4) polishing a layer of diamond material sample surface to obtain a clean surface;
(5) carrying out large-area uniform etching and polishing by adopting high-energy wide-beam ion beams, wherein the beam pressure is 1200-1500V, and the diameter of the ion beams is 20-50 mm;
(6) performing micro-area precision polishing by adopting low-energy narrow-beam ion beams, wherein the beam pressure is 600-800V, and the diameter of the ion beams is 2-15 mm;
(7) and taking out the sample after polishing to obtain the diamond material with the nanoscale smooth surface.
2. A method of surface non-contact ion beam polishing of optical diamond material according to claim 1, wherein: the step (4) is realized by the following mode:
A. controlling the ion beam to vertically enter the Faraday cup, collecting data at equal intervals in the scanning direction, and determining the current density parameter of the ion beam;
B. controlling an ion beam to vertically enter the surface of a sample, performing a scanning experiment on the sample, measuring the polishing conditions of the surface of the sample before and after the experiment by an interferometer, and obtaining a removal function after Gaussian fitting;
C. setting the material removal amount in the experimental process, and calculating the residence time of the ion beam by adopting a numerical simulation method according to a removal function;
D. and loading an ion beam residence time program file and starting polishing.
3. A method of surface non-contact ion beam polishing of optical diamond material according to claim 1, wherein: in the step (3), the ion source reaches a stable state after being started for 1-2 hours.
4. A method of surface non-contact ion beam polishing of optical diamond material according to claim 1, wherein: the polishing time of the high-energy wide-beam ion beam and the low-energy narrow-beam ion beam in the steps (5) and (6) is determined according to the sample size:
wherein T is the processing time, C is a proportionality constant, R is the radius of the processing element, B is the edge extension distance, v is the moving speed of the ion source during processing, and dx is the step length.
5. A method of surface non-contact ion beam polishing of optical diamond material according to claim 1, wherein: the Ra value of the diamond material obtained in the step (7) is 3-40 nm.
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| US7238088B1 (en) * | 2006-01-05 | 2007-07-03 | Apollo Diamond, Inc. | Enhanced diamond polishing |
| CN102896558A (en) * | 2012-10-17 | 2013-01-30 | 中国人民解放军国防科学技术大学 | Calcium fluoride single crystal ultra-precision machining method based on chemico-mechanical polishing and ion beam polishing combined process |
| CN104498887A (en) * | 2014-12-02 | 2015-04-08 | 中国航天科工集团第三研究院第八三五八研究所 | Method for preprocessing nodule defects of ultra-low-loss reflector coating substrate |
| CN109623560B (en) * | 2018-12-14 | 2021-09-14 | 中国兵器科学研究院宁波分院 | Method for determining ion beam polishing process parameters for six-axis motion polishing system |
| CN110253220B (en) * | 2019-06-19 | 2020-10-09 | 中国科学院长春光学精密机械与物理研究所 | Method for polishing metal mirror by diamond single-point vehicle auxiliary ion beam |
| CN110712094B (en) * | 2019-09-06 | 2021-07-23 | 中国兵器科学研究院宁波分院 | Method for reducing ion beam polishing optical element surface pollution |
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| US5403619A (en) * | 1993-01-19 | 1995-04-04 | International Business Machines Corporation | Solid state ionic polishing of diamond |
| JPH10337638A (en) * | 1997-06-09 | 1998-12-22 | Nikon Corp | Shape creating method |
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