CN114232090B - Diamond, optical property improvement method and manufacturing method thereof - Google Patents
Diamond, optical property improvement method and manufacturing method thereof Download PDFInfo
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- CN114232090B CN114232090B CN202111575391.6A CN202111575391A CN114232090B CN 114232090 B CN114232090 B CN 114232090B CN 202111575391 A CN202111575391 A CN 202111575391A CN 114232090 B CN114232090 B CN 114232090B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/04—Diamond
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/36—Removing material
- B23K26/38—Removing material by boring or cutting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/70—Auxiliary operations or equipment
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Metallurgy (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
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- Optics & Photonics (AREA)
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- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
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- Crystals, And After-Treatments Of Crystals (AREA)
- Laser Beam Processing (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The application discloses a diamond, an optical property improvement method and a manufacturing method thereof. The optical property improving method includes: coating optical modification paint on at least part of the surface of diamond to be treated to form an optical modification film on the surface of the diamond, wherein the light transmittance of the optical modification film is lower than 50%; and cutting at least part of the area of the diamond not covered by the optical modified film by laser. The coating on the surface of the diamond can prevent the divergence phenomenon of laser caused by uneven refractive index of the diamond, avoids the phenomenon that the energy of the laser is transmitted to the defect position or stress concentration position of the diamond, further effectively eliminates the cracking phenomenon, and the optical modified film also has the functions of heat conduction and toughening, can timely conduct the local heat of the surface of the diamond, so that the temperature uniformity degree of the cut surface of the diamond is improved, and the toughening effect of the optical modified film ensures that microscopic cracks can not be expanded into macroscopic cracks, thereby further avoiding the cracking of the diamond.
Description
Technical Field
The application relates to the technical field of diamond material manufacturing, in particular to diamond, an optical property improvement method and a manufacturing method thereof.
Background
Diamond is the hardest substance naturally occurring in nature, a mineral composed of carbon elements, and an allotrope of graphite. Has wide application in the fields of grinding tool abrasive materials, semiconductors, new materials and the like.
Because of the reserves of natural diamond, the industry currently mainly utilizes synthetic methods to prepare diamond, and the synthetic methods of diamond are various, including ultra-high pressure method, chemical vapor deposition method, physical vapor deposition method and the like. Among them, microwave Plasma Chemical Vapor Deposition (MPCVD) is the preferred method for producing high quality diamond. This is due to the advantages of good controllability of microwave excited plasma, high plasma density, no electrode pollution, etc.
Whether natural diamond or artificial synthetic diamond, the diamond needs to be cut in practical application, and common cutting methods include laser cutting, wire cutting and the like, wherein the laser cutting has the advantages of high cutting speed, good economy, convenience in use and the like.
In the prior art, a plurality of laser cutting devices for cutting diamond are available, and the laser cutting devices such as red light, green light and the like are of various types, and even a plurality of devices are automatically operated, however, the diamond laser cutting devices and the method in the prior art can not effectively prevent the phenomenon of cracking of the diamond in the cutting process.
Disclosure of Invention
In view of the shortcomings of the prior art, it is an object of the present application to provide a diamond, a method for improving its optical properties, and a method for manufacturing the same.
In order to achieve the purpose of the application, the technical scheme adopted by the application comprises the following steps:
in a first aspect, the present application provides a method of improving optical properties of diamond comprising:
coating optical modification paint on at least part of the surface of diamond to be treated to form an optical modification film on the surface of the diamond, wherein the light transmittance of the optical modification film is lower than 50%; and
cutting at least part of the area of the diamond not covered by the optical modified film by laser.
In a second aspect, the present application also provides a method of manufacturing diamond, comprising:
growing diamond by a chemical vapor process, the diamond including single crystal diamond and polycrystalline bodies bonded to the single crystal diamond;
the polycrystalline body bonded to the single crystal diamond is cut off by the above method.
In some preferred embodiments, the single crystal diamond is preferably prepared by MPCVD, which has advantages of fast growth speed, low cost and good uniformity, but is prone to generate polycrystal around it, which affects the purity of the single crystal diamond, so that cutting off the polycrystal growing around the single crystal diamond is particularly required.
In a third aspect, the present application also provides a diamond obtained by the above method.
Based on the technical scheme, compared with the prior art, the application has the beneficial effects that:
the method for improving the optical properties of the diamond reduces the light transmittance and refractive index of the diamond by utilizing the optical modified film, has the functions of heat conduction and toughening, and reduces the stress caused by laser cutting, thereby avoiding the cracking problem during laser cutting.
The above description is only an overview of the technical solutions of the present application, and in order to enable those skilled in the art to more clearly understand the technical means of the present application, the present application may be implemented according to the content of the specification, and the following description is given of the preferred embodiments of the present application with reference to the detailed drawings.
Drawings
FIG. 1 is an image of a diamond crack during cutting provided by an exemplary embodiment of the present application;
FIG. 2 is an image of a diamond crack during cutting provided by an exemplary embodiment of the present application;
FIG. 3 is an image of a diamond crack during cutting provided by an exemplary embodiment of the present application;
fig. 4 is an image of a cut diamond end product provided by an exemplary embodiment of the present application.
Detailed Description
In view of the shortcomings in the prior art, the inventor of the present application has long studied and practiced in a large number of ways to propose the technical scheme of the present application. The technical scheme, the implementation process, the principle and the like are further explained as follows.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application, however, the present application may be practiced otherwise than as described herein, and therefore the scope of the present application is not limited to the specific embodiments disclosed below.
The embodiment of the application provides a method for improving optical properties of diamond, which comprises the following steps:
coating optical modification paint on at least part of the surface of diamond to be treated to form an optical modification film on the surface of the diamond, wherein the light transmittance of the optical modification film is lower than 50%; and cutting at least part of the area of the diamond not covered by the optical modified film by laser.
Because the optical modified film has the shading characteristic, the coating on the surface of the diamond can prevent the divergence phenomenon of laser caused by uneven refractive index of the diamond, and the phenomenon that the energy of the laser is transmitted to the defect or stress concentration of the diamond is avoided, so that the cracking phenomenon of the diamond in the laser cutting process is effectively stopped.
The diamond to be cut can be prepared by a physical or chemical vapor deposition method, and can also be prepared by a high-temperature and high-pressure growth process. For example, for MPCVD grown diamond, which includes single crystal diamond and polycrystalline diamond attached around the single crystal diamond, the main purpose of cutting may typically be to cut away the polycrystalline diamond around the single crystal diamond to obtain pure single crystal diamond. For diamond grown at high temperature and high pressure, various defects are liable to occur in the body thereof during the growth, and the main purpose of cutting is to remove edge portions including defects, so as to obtain a core portion having a size as large as possible and a quality as high as possible.
In some embodiments, the diamond comprises single crystal diamond and polycrystalline bodies bonded to the single crystal diamond, the method comprising: the interface between the single crystal diamond and the polycrystal is taken as a boundary, and the surface of the single crystal diamond is covered with the optical modified film; the polycrystalline body bonded to the single crystal diamond is cut off along the boundary using a laser.
In some embodiments, the diamond may comprise CVD diamond or high temperature high pressure diamond.
In some embodiments, the CVD diamond may comprise CVD single crystal diamond.
In some embodiments, the optically modified coating comprises 20 to 45wt% polymeric film-forming material, 20 to 30wt% inorganic pigment, 0 to 5wt% dispersant, and 30 to 50wt% solvent, wherein the polymeric film-forming material comprises: any one or a combination of two or more of polyurethane, polyacrylic resin, and epoxy resin, and not limited thereto, the inorganic pigment includes: any one or a combination of two or more of titanium white, lithopone, zinc oxide and antimony white, and is not limited thereto.
The optical modified film formed by the components can improve the optical characteristics of the diamond, is more suitable for laser cutting, has the functions of heat conduction and toughening, and can timely conduct local heat on the surface of the diamond, so that the temperature uniformity degree of the cut surface of the diamond is improved, and meanwhile, in the optical modified film, micro cracks can not be expanded into macro cracks due to the toughening effect brought by the polymer film forming substances, and the cracking of the diamond is further avoided.
In some embodiments, the optically modified coating further comprises 2-4wt% carbon nanotubes and/or nanowires.
By adding the carbon nano tubes or the nano metal wires in the optical modified coating, on one hand, the blocking capability of the coating to laser can be further improved, on the other hand, the heat conduction capability of the coating can be remarkably improved, and the carbon nano tubes or the nano metal wires can be interwoven in the coating to form a network structure, so that the flexibility of the coating is improved, and the stress generated in the monocrystalline diamond when the monocrystalline diamond is cut by the laser can be better counteracted.
In some embodiments, the carbon nanotubes have a diameter of 10-50nm and a length of 1-10 microns, and the nanowires have a diameter of 5-50nm and a length of 1-10 microns.
In some embodiments, the laser cutting method specifically comprises:
cleaning the surface of the diamond;
coating the optical modified coating on at least part of the surface of the cleaned diamond;
and (3) drying the diamond with the surface coated with the optical modified coating at 50-70 ℃ for 2-10min to form the optical modified film.
Wherein, the optical modification coating can be coated on the surface of the diamond in various modes such as brushing, spin coating, spraying, printing and the like.
In some embodiments, the optically-modified coating completely covers the growth face of the diamond.
In some embodiments, the optically modified film has a thickness of 0.01 to 0.2 μm.
In some embodiments, the laser has a power of 5-15W and a beam diameter of 4-5mm.
In some embodiments, the duration of the cut is less than 15 minutes.
The embodiment of the application also provides a manufacturing method of the diamond, which comprises the following steps:
growing diamond by a chemical vapor process, the diamond including single crystal diamond and polycrystalline bodies bonded to the single crystal diamond;
the polycrystalline body bonded to the single crystal diamond is cut off by the above method.
In some embodiments, the chemical vapor deposition process comprises a microwave plasma chemical vapor deposition process.
In some exemplary embodiments of the present application, a method of avoiding cracking of single crystal diamond when cutting away polycrystalline material surrounding CVD grown single crystal diamond is disclosed. The method is mainly characterized in that before the cutting operation is carried out by laser, an optical modification coating is coated on the surface of the monocrystalline diamond to form an optical modification coating, so that the cracking of the monocrystalline diamond caused by the refraction and stress of the diamond is effectively prevented.
The embodiment of the application also provides the diamond cut or manufactured by the laser cutting method or the manufacturing method.
The technical scheme of the application is further described in detail below through a plurality of embodiments and with reference to the accompanying drawings. However, the examples are chosen to illustrate the application only and are not intended to limit the scope of the application.
Example 1
A method for improving optical properties of diamond, which uses MPCVD grown diamond as diamond to be cut for the purpose of removing polycrystals bonded around single crystal diamond. The method comprises the following steps:
brushing an optical modified coating on the surface of the monocrystalline diamond in the diamond to be cut by taking the interface of the monocrystalline diamond and the polycrystal as a boundary, wherein the optical modified coating contains titanium white powder, polyacrylic acid and benzene in a mass ratio of 1:1:1.2, and then performing coating drying/curing for 5min under the condition of 60 ℃ to form an optical modified film with 40% light transmittance;
setting the power of the laser to 10W, the beam diameter to 4mm, and the continuous working time of the laser, and carrying out laser cutting on the diamond to be cut along the boundary for 2min to obtain the finished single crystal diamond, wherein the shape of one finished single crystal diamond is shown in figure 4. The average cracking rates of a plurality of finished single crystal diamonds counted in this example are shown in table 1.
Example 2
A method for improving optical properties of diamond, which uses diamond grown at high temperature and high pressure as diamond to be cut, wherein the cutting purpose is to remove edge portions or defective portions of the diamond at high temperature and high pressure to maximally secure the quality of a finished diamond at high temperature and high pressure. The method comprises the following steps:
brushing an optical modified coating on the surface of a defect-free area of diamond to be cut by taking the edge of the defect as a boundary, wherein the optical modified coating comprises zinc oxide, epoxy resin, road-blond 32500 and acetone in a mass ratio of 1:0.5:0.6:0.1; then, the coating is dried/cured for 10min at 50 ℃ to form an optical modified film with 20% light transmittance;
setting the power of the laser to 15W, the beam diameter to 5mm, and the continuous working time of the laser to 15min, and performing laser cutting along the defect edge to obtain the finished diamond, wherein the average cracking rate of a plurality of counted finished diamond is shown in table 1.
Example 3
A method for improving optical properties of diamond, substantially the same as in example 1, except that:
setting the laser power to 15W, the beam diameter to 5mm, and the laser duration to 10min, obtaining the finished diamond, and counting the cracking rate of a plurality of finished single crystal diamonds as shown in Table 1.
Example 4
A method for improving optical properties of diamond, substantially the same as in example 1, except that:
drying/curing the coating at 70 ℃ for 2min to form an optical modified film;
the obtained product diamond was subjected to statistics, and the cracking rates of the obtained plurality of product single crystal diamonds are shown in table 1.
Example 5
A method of improving optical properties of diamond comprising the steps of:
coating an optical modified coating on the surface of diamond, wherein the optical modified coating contains antimony white, polyurethane, toluene and road-blogging 32500 in the mass ratio of 1:2:1.5:0.2, and completely coating the surface;
drying/curing the coating at 65 ℃ to form an optical modified film;
the final diamond was obtained, and the cracking rates of a plurality of average final diamonds obtained by statistics are shown in table 1.
Example 6
A method for improving optical properties of diamond, substantially the same as in example 5, except that:
the optical modified coating comprises antimony white, polyurethane, toluene and lubo 32500 with the mass ratio of 1:2:1.5:0.2:0.2 and silver nanowires with the average diameter of 50nm and the average length of 1800 nm.
The average cracking rates of the plurality of finished diamonds obtained by statistics are shown in table 1.
Example 7
A method for improving optical properties of diamond, substantially the same as in example 5, except that:
the optical modified coating comprises antimony white, polyurethane, toluene and road bloodless 32500 with the mass ratio of 1:2:1.5:0.2:0.2 and carbon nano tubes with the average diameter of 40nm and the average length of 1000 nm.
The average cracking rates of the plurality of finished diamonds obtained by statistics are shown in table 1.
Comparative example 1
This comparative example is substantially identical to example 1, with the difference that:
the operation of coating the optical modified coating on the surface of the diamond to be cut is omitted, the diamond to be cut is directly cut, and finally, the obtained photographs of a plurality of finished single crystal diamonds are shown in figures 1-3, wherein the black linear parts are cracks generated by cracking. The average cracking rates of the plurality of finished single crystal diamonds counted in this comparative example are shown in table 1.
Comparative example 2
This comparative example is substantially identical to example 2, with the difference that:
laser cutting was performed at a laser cutting power of 20W and a beam diameter of 6mm, and the statistical cracking rates are shown in Table 1.
TABLE 1 cracking Rate of the cutting diamonds of each example and comparative example
Based on the statistical results, it can be clear that the optical property improvement method provided by the application can effectively reduce the cracking rate of the diamond in the laser cutting process; the optical modified film formed by the optical property improvement method provided by the application needs to be cut by matching with the laser cutting parameters, and the cracking rate can be increased due to improper laser cutting parameters.
It should be understood that the above embodiments are merely for illustrating the technical concept and features of the present application, and are intended to enable those skilled in the art to understand the present application and implement the same according to the present application without limiting the scope of the present application. All equivalent changes or modifications made in accordance with the spirit of the present application should be construed to be included in the scope of the present application.
Claims (9)
1. A laser cutting method of diamond including single crystal diamond and polycrystalline body bonded to the single crystal diamond, comprising:
coating an optical modification coating on the surface of the single crystal diamond by taking the interface of the single crystal diamond and the polycrystal as a boundary to form an optical modification film on the surface of the single crystal diamond, wherein the light transmittance of the optical modification film is lower than 50%; and
cutting and removing polycrystals bonded to the single crystal diamond along the boundary by using laser;
wherein the optically modified coating comprises 20-45wt% of a polymeric film-forming substance, 20-30wt% of an inorganic pigment, 0-5 wt% of a dispersant, and 30-50wt% of a solvent, wherein the polymeric film-forming substance is selected from the group consisting of: any one or a combination of more than two of polyurethane, polyacrylic resin and epoxy resin, wherein the inorganic pigment is selected from the following components: any one or more than two of titanium dioxide, lithopone, zinc oxide and antimony white.
2. The laser cutting method of claim 1, wherein the diamond comprises chemical vapor deposited diamond or high temperature high pressure grown diamond.
3. The laser cutting method according to claim 2, wherein the optically modified paint further comprises 2-4wt% of carbon nanotubes and/or nano wires, wherein the carbon nanotubes have a diameter of 10-50nm and a length of 1-10 microns, and the nano wires have a diameter of 5-50nm and a length of 1-10 microns.
4. The laser cutting method according to claim 2, characterized in that it comprises in particular:
cleaning the surface of the diamond;
coating the optical modified coating on at least part of the surface of the cleaned diamond;
and (3) drying the diamond with the surface coated with the optical modified coating at 50-70 ℃ for 2-10min to form the optical modified film.
5. The laser cutting method according to claim 4, characterized by comprising: and enabling the optical modified film to completely cover the growth surface of the diamond.
6. The laser cutting method according to claim 1, wherein the optically modified film has a thickness of 0.01 to 0.2 μm.
7. The laser cutting method according to claim 1, wherein the power of the laser is 5-15W and the beam diameter is 4-5mm.
8. The laser cutting method of claim 7, wherein the duration of the cutting is less than 15 minutes.
9. A method of manufacturing diamond, comprising:
growing diamond by using a microwave plasma chemical vapor deposition method, wherein the diamond comprises single crystal diamond and polycrystal bonded to the single crystal diamond;
polycrystalline body bonded to the single crystal diamond is cut off by the method of any one of claims 1 to 8.
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Citations (5)
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| JP2012176889A (en) * | 2012-05-10 | 2012-09-13 | Apollo Diamond Inc | System and method for producing synthetic diamond |
| CN110281142A (en) * | 2019-06-20 | 2019-09-27 | 山东大学 | Diamond seed preparation method, diamond seed and monocrystalline |
| CN111733454A (en) * | 2020-05-20 | 2020-10-02 | 西南科技大学 | Separation method of CVD homoepitaxy diamond large single crystal based on boron-doped transition layer |
| CN112025530A (en) * | 2020-11-06 | 2020-12-04 | 苏州香榭轩表面工程技术咨询有限公司 | Nano-diamond cutter and preparation method and application thereof |
| KR20210048950A (en) * | 2019-10-24 | 2021-05-04 | (주)엠티아이 | Coating composition protecting wafer and method of dicing wafer using the same |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6858080B2 (en) * | 1998-05-15 | 2005-02-22 | Apollo Diamond, Inc. | Tunable CVD diamond structures |
| US10077608B2 (en) * | 2011-12-30 | 2018-09-18 | Smith International, Inc. | Thermally stable materials, cutter elements with such thermally stable materials, and methods of forming the same |
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2021
- 2021-12-21 CN CN202111575391.6A patent/CN114232090B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012176889A (en) * | 2012-05-10 | 2012-09-13 | Apollo Diamond Inc | System and method for producing synthetic diamond |
| CN110281142A (en) * | 2019-06-20 | 2019-09-27 | 山东大学 | Diamond seed preparation method, diamond seed and monocrystalline |
| KR20210048950A (en) * | 2019-10-24 | 2021-05-04 | (주)엠티아이 | Coating composition protecting wafer and method of dicing wafer using the same |
| CN111733454A (en) * | 2020-05-20 | 2020-10-02 | 西南科技大学 | Separation method of CVD homoepitaxy diamond large single crystal based on boron-doped transition layer |
| CN112025530A (en) * | 2020-11-06 | 2020-12-04 | 苏州香榭轩表面工程技术咨询有限公司 | Nano-diamond cutter and preparation method and application thereof |
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