CN118291936A - Preparation method of diamond laser heat sink substrate - Google Patents
Preparation method of diamond laser heat sink substrate Download PDFInfo
- Publication number
- CN118291936A CN118291936A CN202410383931.8A CN202410383931A CN118291936A CN 118291936 A CN118291936 A CN 118291936A CN 202410383931 A CN202410383931 A CN 202410383931A CN 118291936 A CN118291936 A CN 118291936A
- Authority
- CN
- China
- Prior art keywords
- heat sink
- boron nitride
- electroplating
- plating
- diamond
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000758 substrate Substances 0.000 title claims abstract description 71
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 50
- 239000010432 diamond Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000007747 plating Methods 0.000 claims abstract description 90
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical class N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000010931 gold Substances 0.000 claims abstract description 57
- 229910052737 gold Inorganic materials 0.000 claims abstract description 51
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000000919 ceramic Substances 0.000 claims abstract description 34
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 12
- JCXKHYLLVKZPKE-UHFFFAOYSA-N benzotriazol-1-amine Chemical compound C1=CC=C2N(N)N=NC2=C1 JCXKHYLLVKZPKE-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000010949 copper Substances 0.000 claims description 77
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 68
- 229910052802 copper Inorganic materials 0.000 claims description 68
- 238000009713 electroplating Methods 0.000 claims description 56
- 238000000034 method Methods 0.000 claims description 54
- 238000012546 transfer Methods 0.000 claims description 31
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 29
- 230000008569 process Effects 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 238000004544 sputter deposition Methods 0.000 claims description 21
- 238000000227 grinding Methods 0.000 claims description 19
- 238000004519 manufacturing process Methods 0.000 claims description 19
- 229920002120 photoresistant polymer Polymers 0.000 claims description 19
- 229910052582 BN Inorganic materials 0.000 claims description 18
- 238000005498 polishing Methods 0.000 claims description 18
- 238000005488 sandblasting Methods 0.000 claims description 17
- 229910045601 alloy Inorganic materials 0.000 claims description 15
- 239000000956 alloy Substances 0.000 claims description 15
- 238000011161 development Methods 0.000 claims description 15
- 229910052759 nickel Inorganic materials 0.000 claims description 14
- 239000006260 foam Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 239000010936 titanium Substances 0.000 claims description 11
- -1 1-butyl-3-methylimidazole tetrafluoroborate Chemical compound 0.000 claims description 9
- 238000005530 etching Methods 0.000 claims description 9
- JBANFLSTOJPTFW-UHFFFAOYSA-N azane;boron Chemical compound [B].N JBANFLSTOJPTFW-UHFFFAOYSA-N 0.000 claims description 8
- MSNOMDLPLDYDME-UHFFFAOYSA-N gold nickel Chemical compound [Ni].[Au] MSNOMDLPLDYDME-UHFFFAOYSA-N 0.000 claims description 8
- 238000004026 adhesive bonding Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 238000004381 surface treatment Methods 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- 230000008719 thickening Effects 0.000 claims description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- WJRBRSLFGCUECM-UHFFFAOYSA-N hydantoin Chemical compound O=C1CNC(=O)N1 WJRBRSLFGCUECM-UHFFFAOYSA-N 0.000 claims description 6
- 229940091173 hydantoin Drugs 0.000 claims description 6
- 239000002608 ionic liquid Substances 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 10
- 239000004065 semiconductor Substances 0.000 abstract description 9
- 229910052751 metal Inorganic materials 0.000 abstract description 8
- 239000002184 metal Substances 0.000 abstract description 8
- 238000005260 corrosion Methods 0.000 abstract description 7
- 230000007797 corrosion Effects 0.000 abstract description 7
- 239000000377 silicon dioxide Substances 0.000 abstract description 7
- 238000012986 modification Methods 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 5
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 5
- 239000003112 inhibitor Substances 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 5
- 230000017525 heat dissipation Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000005299 abrasion Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 3
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000005282 brightening Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- WUUZKBJEUBFVMV-UHFFFAOYSA-N copper molybdenum Chemical compound [Cu].[Mo] WUUZKBJEUBFVMV-UHFFFAOYSA-N 0.000 description 1
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007648 laser printing Methods 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
- C04B41/90—Coating or impregnation for obtaining at least two superposed coatings having different compositions at least one coating being a metal
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/02—Electroplating of selected surface areas
- C25D5/022—Electroplating of selected surface areas using masking means
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/16—Electroplating with layers of varying thickness
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/52—After-treatment of electroplated surfaces by brightening or burnishing
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S5/00—Semiconductor lasers
- H01S5/02—Structural details or components not essential to laser action
- H01S5/024—Arrangements for thermal management
- H01S5/02476—Heat spreaders, i.e. improving heat flow between laser chip and heat dissipating elements
- H01S5/02484—Sapphire or diamond heat spreaders
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Ceramic Engineering (AREA)
- Structural Engineering (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Optics & Photonics (AREA)
- Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
Abstract
The invention relates to the technical field of heat sink substrates, in particular to a preparation method of a diamond laser heat sink substrate. The invention uses the high thermal conductivity of the diamond material to apply the diamond material to the high-power semiconductor laser, can obviously improve the radiating effect of the laser, and greatly improves the application range of the laser. The invention also carries out magnetron sputtering treatment on the diamond ceramic chip, and the seed Ti layer and the seed Cu layer are sputtered, and then the metal layer is electroplated, so that the diamond ceramic chip can be better applied to the field of semiconductor lasers. According to the invention, the substrate after gold plating is also plated with the modified nano boron nitride layer, the nano boron nitride has excellent heat conduction performance, and the nano boron nitride is compounded with silicon dioxide, so that the corrosion resistance and wear resistance of the substrate can be improved by compounding the silicon dioxide; meanwhile, a corrosion inhibitor 1-aminobenzotriazole is added for further modification, so that the corrosion resistance of the substrate is further improved.
Description
Technical Field
The invention relates to the technical field of heat sink substrates, in particular to a preparation method of a diamond laser heat sink substrate.
Background
The high-power semiconductor laser has the advantages of high photoelectric efficiency, easy modulation, small volume, light weight and the like, and is widely applied to the aspects of laser communication, laser printing, medical instruments and the like. With the development of high-power semiconductor lasers, when the high-power semiconductor lasers work, a great amount of heat is generated in an active area, so that the output power and the electro-optical conversion efficiency of the lasers are reduced, and even the service lives of the lasers are shortened or the lasers are disabled. At present, the most main heat dissipation mode of the semiconductor laser is to dissipate heat through a heat sink, and a transitional heat sink is added on the basis of a copper heat sink, and common transitional heat sink materials comprise aluminum nitride, aluminum oxide, beryllium oxide, tungsten copper alloy, molybdenum copper alloy and the like.
At present, the commonly used heat dissipation material of the high-power semiconductor laser is aluminum nitride heat sink which is used as transition heat sink to be sintered on copper heat sink, but the heat conductivity of the aluminum nitride material is only 230/(K.m), the heat dissipation effect is limited, and the application range of the high-power laser is limited.
In order to solve the problems and improve the heat dissipation effect of the substrate, the invention provides a preparation method of a diamond laser heat sink substrate.
Disclosure of Invention
The invention aims to provide a preparation method of a diamond laser heat sink substrate, which aims to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: a preparation method of a diamond laser heat sink substrate.
The preparation method of the diamond laser heat sink substrate comprises the following steps:
Step one: taking diamond ceramic chips, cleaning, then performing magnetron sputtering treatment, and sputtering a seed Ti layer and a seed Cu layer in sequence to obtain sputtered ceramic chips;
Step two: electroplating the sputtered ceramic chip with the thickness of 3-4 μm, and performing pattern transfer on the ceramic chip plated with the bottom copper for one time by film pasting, exposure, development, flash etching and film removal; after the primary pattern is manufactured, performing secondary pattern transfer manufacturing through film pasting, exposure and development procedures;
Step three: copper plating and thickening are carried out on the secondary pattern transfer developing area through electroplating;
Step four: after copper plating, grinding and polishing the copper surface, wherein the copper thickness after polishing is 76 mu m, and the roughness Ra is 0.18 mu m; removing the residual dry film in the product pattern space, and then performing sand blasting treatment;
Step five: carrying out surface treatment on the product by using a nickel-gold electroplating process, wherein the nickel plating thickness is controlled to be 1-4 mu m, and the gold plating thickness is controlled to be 1-2 mu m; after gold plating, performing third pattern transfer by gluing, exposing and developing to expose the area needing to be electroplated with AuSn, and covering the rest positions by photoresist; plating AuSn alloy on the surface of the product by an electroplating process, wherein the AuSn alloy has a thickness of 4.0 mu m and an Au content of 73%;
step six: and removing the photoresist again after the AuSn electroplating is finished, and electroplating a gold-plated layer on the surface, wherein the thickness of the gold-plated layer is 0.05 mu m, so as to obtain a gold-plated substrate, and scribing to obtain the diamond laser heat sink substrate.
More preferably, in the first step, the magnetron sputtering treatment process comprises the following steps: firstly sputtering a titanium layer with the thickness of 100-200nm on a ceramic substrate, and then sputtering a copper layer with the thickness of 1.5-2.5 mu m; the sputtering pressure is 2.0X10 -1Pa-3.0×10-1 Pa, the sputtering temperature is 200 ℃ to 280 ℃, the sputtering current is 10A to 20A, the sputtering voltage is 600V to 800V, the sputtering power is 10KW to 20KW, the sputtering time is 1500s, and the sputtering time is 5000s.
More optimally, in the second step, the technological parameters of the bottom copper electroplating are as follows: the concentration of the copper plating solution CuSO 4 is 80-120g/L, the concentration of H 2SO4 is 10% -14%, the concentration of CL ions is 50-100ppm, the concentration of the leveling agent is 8-12ml/L, the concentration of the brightening agent is 0.05-0.1ml/L, the temperature is 20-28 ℃, the current density is 1A/dm 2, and the electroplating time is 15min.
More optimally, in the third step, the process parameters of the thick copper electroplating are as follows: copper plating solution CuSO 4 with concentration of 80-120g/L, H 2SO4 with concentration of 10-14%, CL ion with concentration of 50-100ppm, leveler with concentration of 8-12ml/L, brightening agent with concentration of 0.05-0.1ml/L, temperature of 20-28 ℃, current density of 2-3A/dm2, electroplating time of 3-5H;
More optimally, the nickel ion concentration of the nickel plating solution is 70-90g/L, the nickel chloride concentration is 10-14g/L, the boric acid concentration is 30-40g/L, the PH value is 3.45-4.5, the temperature is 50-60 ℃, the cylinder opening agent concentration is 3-7ml/L, the wetting agent concentration is 3-5ml/L, the nickel plating current density is 0.5A/dm 2, and the nickel plating time is 50-60min;
Gold plating process parameters: the concentration of gold ions is 3-5g/L, the PH value is 4.5-5.5, the gold plating temperature is 50-60 ℃, the gold plating current density is 0.1A/dm 2, and the gold plating time is 20-30min;
Technological parameters of AuSn alloy plating: the concentration of gold ions is 8-12g/L, the concentration of tin is 8-15g/L, the PH value is 3.8-4.2, the temperature is 40-44 ℃, the current density is 0.4A/dm < 2 >, and the electroplating time is 20-25min.
Preferably, the gold ion concentration is 3-5g/L, the PH value is 4.5-5.5, the gold plating temperature is 50-60 ℃, the gold plating current density is 0.1A/dm 2, and the gold plating time is 1-2min.
More optimally, in the step six, a modified nano boron nitride layer is also plated on the substrate after gold plating; the preparation method comprises the following steps: and (3) placing the substrate subjected to gold plating into a preplating solution, carrying out ultrasonic auxiliary preplating for 1-1.5h at 65-70 ℃, wherein the preplating current density is 10mA/cm 2, the ultrasonic power is 300W, and obtaining the preplating substrate, and scribing, so as to obtain the diamond laser heat sink substrate.
More preferably, the preplating solution comprises the following components: 1-butyl-3-methylimidazole tetrafluoroborate ionic liquid is used as a solvent, chloroauric acid is 50-65g/L, hydantoin is 5-7g/L, and modified nano boron nitride is 6-8g/L.
More optimally, the preparation method of the modified nano boron nitride comprises the following steps: mixing nano boron nitride, deionized water and ethanol uniformly, adding tetraethyl orthosilicate and a silane coupling agent KH550, reacting for 5-6 hours, adding 1-aminobenzotriazole, performing ultrasonic dispersion for 1-2 hours, filtering, washing and drying to obtain modified nano boron nitride.
More optimally, the preparation method of the nano boron nitride comprises the following steps: taking ammonia borane, and preserving the temperature for 1-1.5 hours at 1090-1110 ℃ to obtain boron nitride foam; adding absolute ethyl alcohol to immerse the boron nitride foam, carrying out ultrasonic treatment for 1-2min, carrying out suction filtration and drying to obtain the nano boron nitride.
Compared with the prior art, the invention has the following beneficial effects:
(1) The diamond heat sink material has high heat conductivity, the highest heat conductivity can reach 2000W/(K.m), and is a material with good heat conductivity. The invention uses the high thermal conductivity of the diamond material to apply the diamond material to the high-power semiconductor laser, can obviously improve the radiating effect of the laser, and greatly improves the application range of the laser. The invention also carries out magnetron sputtering treatment on the diamond ceramic chip, and the seed Ti layer and the seed Cu layer are sputtered, and then the metal layer is electroplated, so that the diamond ceramic chip can be better applied to the field of semiconductor lasers.
(2) The modified nano boron nitride layer is also plated on the substrate after gold plating, the nano boron nitride has excellent heat conduction performance, and the heat conductivity can reach 2000W/(K.m), and the nano boron nitride is prepared by using ammonia borane as a precursor and then sintering at 1090-1110 ℃; the nano boron nitride has the transverse dimension of 30 mu m, the thickness of 1.5nm and the specific surface area of larger, and can load more 1-amino benzotriazole and silicon dioxide; according to the invention, tetraethyl orthosilicate is used, silicon dioxide is compounded on nano boron nitride, and the silicon dioxide can be compounded to improve the corrosion resistance of the substrate; meanwhile, a corrosion inhibitor 1-aminobenzotriazole is added for further modification, so that the corrosion resistance of the substrate is further improved.
(3) The method of the invention preferentially carries out primary pattern transfer manufacture on the electroplated bottom copper, completes the etching of the required pattern (reserves the electroplated lead), and carries out secondary pattern manufacture, thereby avoiding the problems of product side wall extension and surface roughness abnormality caused by grinding etching after the plating of the thick copper; meanwhile, the unique nickel plating cathode and anode design can obviously provide nickel plating thickness uniformity.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention. In the drawings:
FIG. 1 is a schematic view of a diamond tile according to example 1 of the present invention;
FIG. 2 is a schematic view of a substrate after magnetron sputtering according to example 1 of the present invention;
FIG. 3 is a schematic diagram of a substrate after a pattern transfer according to embodiment 1 of the present invention;
FIG. 4 is a schematic diagram of a substrate after a secondary pattern transfer according to embodiment 1 of the present invention;
FIG. 5 is a schematic view of a substrate after plating thick copper according to example 1 of the present invention;
FIG. 6 is a schematic view of a substrate after nickel-gold plating according to example 1 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The purchasing manufacturers of all the raw materials to which the present invention relates are not limited in any way, and exemplary ones include: boron nitride: available from Shanghai Source leaf Biotechnology Co., ltd., model: s40088; ammonia borane: available from zheng jiex chemical products limited, model: JACS-13774-81-7.
Example 1: the preparation method of the diamond laser heat sink substrate comprises the following steps:
step one: taking 50.8mm multiplied by 0.3mm round diamond ceramic chips, cleaning, and then performing magnetron sputtering treatment, wherein a sputtered metal seed layer is a Ti layer and a Cu layer, so as to obtain sputtered ceramic chips;
step two: carrying out electroplating bottom copper treatment on the sputtered ceramic chip, wherein the thickness of the electroplating bottom copper is 3 mu m;
Step three: carrying out primary pattern transfer manufacturing on the ceramic chip plated with the bottom copper through film pasting, exposure, development, flash etching and film removal, and leaving an electroplating lead after the primary pattern manufacturing is finished, so as to provide a conductive effect for the subsequent electroplating process; after the primary pattern is manufactured, performing secondary pattern transfer manufacturing through film pasting, exposure and development procedures;
Step four: copper plating is carried out on the secondary pattern transfer developing area for thickening, and the copper plating thickness is 100 mu m;
Step five: after copper plating, grinding and polishing the copper surface by using double-sided grinding equipment, wherein the copper thickness after polishing is 76 mu m, and the roughness Ra is 0.18 mu m; after the copper surface is polished, removing the film of the product by using an organic film removing liquid, and removing the residual dry film in the pattern space of the product; after the film removal is completed, carrying out sand blasting treatment on the product by using a horizontal sand blasting mode to remove grinding and polishing marks of the product;
Step six: after sand blasting, carrying out surface treatment on the product by using an electroplated nickel-gold process, wherein the nickel plating thickness is 2 mu m, and the gold plating thickness is 1.2 mu m;
step seven: after gold plating, performing third pattern transfer by gluing, exposing and developing to expose the area needing to be electroplated with AuSn, and covering the rest positions by photoresist; plating AuSn alloy on the surface of the product by an electroplating process, wherein the AuSn alloy has a thickness of 4.0 mu m and an Au content of 73%;
Step eight: removing photoresist by using an organic stripping solution again after AuSn electroplating is completed; after photoresist removal, a layer of thin gold is added on the surface of the product in an electroplating mode, wherein the thickness of the gold-plated layer is 0.05 mu m, and a substrate after gold plating is obtained; scribing to obtain the diamond laser heat sink substrate.
Example 2: the preparation method of the diamond laser heat sink substrate comprises the following steps:
step one: taking 50.8mm multiplied by 0.3mm round diamond ceramic chips, cleaning, and then performing magnetron sputtering treatment, wherein a sputtered metal seed layer is a Ti layer and a Cu layer, so as to obtain sputtered ceramic chips;
step two: carrying out electroplating bottom copper treatment on the sputtered ceramic chip, wherein the thickness of the electroplating bottom copper is 3 mu m;
Step three: carrying out primary pattern transfer manufacturing on the ceramic chip plated with the bottom copper through film pasting, exposure, development, flash etching and film removal, and leaving an electroplating lead after the primary pattern manufacturing is finished, so as to provide a conductive effect for the subsequent electroplating process; after the primary pattern is manufactured, performing secondary pattern transfer manufacturing through film pasting, exposure and development procedures;
Step four: copper plating is carried out on the secondary pattern transfer developing area for thickening, and the copper plating thickness is 100 mu m;
Step five: after copper plating, grinding and polishing the copper surface by using double-sided grinding equipment, wherein the copper thickness after polishing is 76 mu m, and the roughness Ra is 0.18 mu m; after the copper surface is polished, removing the film of the product by using an organic film removing liquid, and removing the residual dry film in the pattern space of the product; after the film removal is completed, carrying out sand blasting treatment on the product by using a horizontal sand blasting mode to remove grinding and polishing marks of the product;
Step six: after sand blasting, carrying out surface treatment on the product by using an electroplated nickel-gold process, wherein the nickel plating thickness is 2 mu m, and the gold plating thickness is 1.2 mu m;
step seven: after gold plating, performing third pattern transfer by gluing, exposing and developing to expose the area needing to be electroplated with AuSn, and covering the rest positions by photoresist; plating AuSn alloy on the surface of the product by an electroplating process, wherein the AuSn alloy has a thickness of 4.0 mu m and an Au content of 73%;
Step eight: removing photoresist by using an organic stripping solution again after AuSn electroplating is completed; after photoresist removal, a layer of thin gold is added on the surface of the product in an electroplating mode, wherein the thickness of the gold-plated layer is 0.05 mu m, and a substrate after gold plating is obtained;
step nine: placing the substrate after gold plating into a preplating solution, carrying out ultrasonic auxiliary preplating for 1.2h at 66 ℃, wherein the preplating current density is 10mA/cm 2, the ultrasonic power is 300W, and obtaining a substrate, scribing and obtaining a diamond laser heat sink substrate;
(1) The composition of the preplating solution is as follows: taking 1-butyl-3-methylimidazole tetrafluoroborate ionic liquid as a solvent, 60g/L chloroauric acid, 6g/L hydantoin and 7g/L modified nano boron nitride;
(2) Preparation of modified nano boron nitride:
taking 10g of ammonia borane, and preserving heat for 1.2 hours at 1095 ℃ to obtain boron nitride foam; adding absolute ethyl alcohol to immerse the boron nitride foam, carrying out ultrasonic treatment for 1min, carrying out suction filtration and drying to obtain nano boron nitride;
Taking 5g of nano boron nitride, 100mL of deionized water and 400mL of ethanol, uniformly mixing, adding 15mL of tetraethyl orthosilicate and 0.3g of silane coupling agent KH550, reacting for 5.5h, adding 4g of 1-aminobenzotriazole, performing ultrasonic dispersion for 1.5h, filtering, washing and drying to obtain the modified nano boron nitride.
Example 3: the preparation method of the diamond laser heat sink substrate comprises the following steps:
step one: taking 50.8mm multiplied by 0.3mm round diamond ceramic chips, cleaning, and then performing magnetron sputtering treatment, wherein a sputtered metal seed layer is a Ti layer and a Cu layer, so as to obtain sputtered ceramic chips;
step two: carrying out electroplating bottom copper treatment on the sputtered ceramic chip, wherein the thickness of the electroplating bottom copper is 3 mu m;
Step three: carrying out primary pattern transfer manufacturing on the ceramic chip plated with the bottom copper through film pasting, exposure, development, flash etching and film removal, and leaving an electroplating lead after the primary pattern manufacturing is finished, so as to provide a conductive effect for the subsequent electroplating process; after the primary pattern is manufactured, performing secondary pattern transfer manufacturing through film pasting, exposure and development procedures;
Step four: copper plating is carried out on the secondary pattern transfer developing area for thickening, and the copper plating thickness is 100 mu m;
Step five: after copper plating, grinding and polishing the copper surface by using double-sided grinding equipment, wherein the copper thickness after polishing is 76 mu m, and the roughness Ra is 0.18 mu m; after the copper surface is polished, removing the film of the product by using an organic film removing liquid, and removing the residual dry film in the pattern space of the product; after the film removal is completed, carrying out sand blasting treatment on the product by using a horizontal sand blasting mode to remove grinding and polishing marks of the product;
Step six: after sand blasting, carrying out surface treatment on the product by using an electroplated nickel-gold process, wherein the nickel plating thickness is 2 mu m, and the gold plating thickness is 1.2 mu m;
step seven: after gold plating, performing third pattern transfer by gluing, exposing and developing to expose the area needing to be electroplated with AuSn, and covering the rest positions by photoresist; plating AuSn alloy on the surface of the product by an electroplating process, wherein the AuSn alloy has a thickness of 4.0 mu m and an Au content of 73%;
Step eight: removing photoresist by using an organic stripping solution again after AuSn electroplating is completed; after photoresist removal, a layer of thin gold is added on the surface of the product in an electroplating mode, wherein the thickness of the gold-plated layer is 0.05 mu m, and a substrate after gold plating is obtained;
Step nine: placing the substrate after gold plating into a preplating solution, carrying out ultrasonic auxiliary preplating for 1h at 65 ℃, wherein the preplating current density is 10mA/cm 2, the ultrasonic power is 300W, obtaining the substrate, and scribing to obtain the diamond laser heat sink substrate;
(1) The composition of the preplating solution is as follows: taking 1-butyl-3-methylimidazole tetrafluoroborate ionic liquid as a solvent, wherein the solvent is 50g/L of chloroauric acid, 5g/L of hydantoin and 6g/L of modified nano boron nitride;
(2) Preparation of modified nano boron nitride:
Taking 10g of ammonia borane, and preserving heat for 1h at 1090 ℃ to obtain boron nitride foam; adding absolute ethyl alcohol to immerse the boron nitride foam, carrying out ultrasonic treatment for 1min, carrying out suction filtration and drying to obtain nano boron nitride;
Taking 5g of nano boron nitride, 100mL of deionized water and 400mL of ethanol, uniformly mixing, adding 15mL of tetraethyl orthosilicate and 0.3g of silane coupling agent KH550, reacting for 5h, adding 4g of 1-aminobenzotriazole, performing ultrasonic dispersion for 1h, filtering, washing and drying to obtain the modified nano boron nitride.
Example 4: the preparation method of the diamond laser heat sink substrate comprises the following steps:
step one: taking 50.8mm multiplied by 0.3mm round diamond ceramic chips, cleaning, and then performing magnetron sputtering treatment, wherein a sputtered metal seed layer is a Ti layer and a Cu layer, so as to obtain sputtered ceramic chips;
step two: carrying out electroplating bottom copper treatment on the sputtered ceramic chip, wherein the thickness of the electroplating bottom copper is 3 mu m;
Step three: carrying out primary pattern transfer manufacturing on the ceramic chip plated with the bottom copper through film pasting, exposure, development, flash etching and film removal, and leaving an electroplating lead after the primary pattern manufacturing is finished, so as to provide a conductive effect for the subsequent electroplating process; after the primary pattern is manufactured, performing secondary pattern transfer manufacturing through film pasting, exposure and development procedures;
Step four: copper plating is carried out on the secondary pattern transfer developing area for thickening, and the copper plating thickness is 100 mu m;
Step five: after copper plating, grinding and polishing the copper surface by using double-sided grinding equipment, wherein the copper thickness after polishing is 76 mu m, and the roughness Ra is 0.18 mu m; after the copper surface is polished, removing the film of the product by using an organic film removing liquid, and removing the residual dry film in the pattern space of the product; after the film removal is completed, carrying out sand blasting treatment on the product by using a horizontal sand blasting mode to remove grinding and polishing marks of the product;
Step six: after sand blasting, carrying out surface treatment on the product by using an electroplated nickel-gold process, wherein the nickel plating thickness is 2 mu m, and the gold plating thickness is 1.2 mu m;
step seven: after gold plating, performing third pattern transfer by gluing, exposing and developing to expose the area needing to be electroplated with AuSn, and covering the rest positions by photoresist; plating AuSn alloy on the surface of the product by an electroplating process, wherein the AuSn alloy has a thickness of 4.0 mu m and an Au content of 73%;
Step eight: removing photoresist by using an organic stripping solution again after AuSn electroplating is completed; after photoresist removal, a layer of thin gold is added on the surface of the product in an electroplating mode, wherein the thickness of the gold-plated layer is 0.05 mu m, and a substrate after gold plating is obtained;
Step nine: placing the substrate after gold plating into a preplating solution, carrying out ultrasonic auxiliary preplating for 1.5h at 70 ℃, wherein the preplating current density is 10mA/cm 2, the ultrasonic power is 300W, and obtaining a substrate, scribing and obtaining a diamond laser heat sink substrate;
(1) The composition of the preplating solution is as follows: taking 1-butyl-3-methylimidazole tetrafluoroborate ionic liquid as a solvent, 65g/L of chloroauric acid, 7g/L of hydantoin and 8g/L of modified nano boron nitride;
(2) Preparation of modified nano boron nitride:
taking 10g of ammonia borane, and preserving heat for 1.5 hours at the temperature of 1110 ℃ to obtain boron nitride foam; adding absolute ethyl alcohol to immerse the boron nitride foam, carrying out ultrasonic treatment for 1min, carrying out suction filtration and drying to obtain nano boron nitride;
Taking 5g of nano boron nitride, 100mL of deionized water and 400mL of ethanol, uniformly mixing, adding 15mL of tetraethyl orthosilicate and 0.3g of silane coupling agent KH550, reacting for 6h, adding 4g of 1-aminobenzotriazole, performing ultrasonic dispersion for 2h, filtering, washing and drying to obtain the modified nano boron nitride.
Comparative example 1: the preparation method of nano boron nitride is different, and the rest is the same as in example 2:
The preparation method of the nanometer boron nitride comprises the following steps:
Taking 10g of boron nitride, ball milling for 24 hours at the speed of 600r/m, immersing the boron nitride foam in absolute ethyl alcohol, performing ultrasonic treatment for 2 hours, centrifuging, filtering and drying to obtain nano boron nitride.
Comparative example 2: the modification treatment of nano boron nitride was not performed, and the rest was the same as in example 2:
step one: taking 50.8mm multiplied by 0.3mm round diamond ceramic chips, cleaning, and then performing magnetron sputtering treatment, wherein a sputtered metal seed layer is a Ti layer and a Cu layer, so as to obtain sputtered ceramic chips;
step two: carrying out electroplating bottom copper treatment on the sputtered ceramic chip, wherein the thickness of the electroplating bottom copper is 3 mu m;
Step three: carrying out primary pattern transfer manufacturing on the ceramic chip plated with the bottom copper through film pasting, exposure, development, flash etching and film removal, and leaving an electroplating lead after the primary pattern manufacturing is finished, so as to provide a conductive effect for the subsequent electroplating process; after the primary pattern is manufactured, performing secondary pattern transfer manufacturing through film pasting, exposure and development procedures;
Step four: copper plating is carried out on the secondary pattern transfer developing area for thickening, and the copper plating thickness is 100 mu m;
Step five: after copper plating, grinding and polishing the copper surface by using double-sided grinding equipment, wherein the copper thickness after polishing is 76 mu m, and the roughness Ra is 0.18 mu m; after the copper surface is polished, removing the film of the product by using an organic film removing liquid, and removing the residual dry film in the pattern space of the product; after the film removal is completed, carrying out sand blasting treatment on the product by using a horizontal sand blasting mode to remove grinding and polishing marks of the product;
Step six: after sand blasting, carrying out surface treatment on the product by using an electroplated nickel-gold process, wherein the nickel plating thickness is 2 mu m, and the gold plating thickness is 1.2 mu m;
step seven: after gold plating, performing third pattern transfer by gluing, exposing and developing to expose the area needing to be electroplated with AuSn, and covering the rest positions by photoresist; plating AuSn alloy on the surface of the product by an electroplating process, wherein the AuSn alloy has a thickness of 4.0 mu m and an Au content of 73%;
Step eight: removing photoresist by using an organic stripping solution again after AuSn electroplating is completed; after photoresist removal, a layer of thin gold is added on the surface of the product in an electroplating mode, wherein the thickness of the gold-plated layer is 0.05 mu m, and a substrate after gold plating is obtained;
step nine: placing the substrate after gold plating into a preplating solution, carrying out ultrasonic auxiliary preplating for 1.2h at 66 ℃, wherein the preplating current density is 10mA/cm 2, the ultrasonic power is 300W, and obtaining a substrate, scribing and obtaining a diamond laser heat sink substrate;
(1) The composition of the preplating solution is as follows: taking 1-butyl-3-methylimidazole tetrafluoroborate ionic liquid as a solvent, 60g/L chloroauric acid, 6g/L hydantoin and 7g/L nano boron nitride;
(2) Preparation of nano boron nitride:
Taking 10g of ammonia borane, and preserving heat for 1.2 hours at 1095 ℃ to obtain boron nitride foam; adding absolute ethyl alcohol to immerse the boron nitride foam, carrying out ultrasonic treatment for 1min, carrying out suction filtration and drying to obtain the nano boron nitride.
Experiment:
Taking the diamond laser heat sink substrates prepared in the examples 1 to 4 and the comparative examples 1 to 2 to perform thermal conductivity test; referring to GB/T1771-2007, salt spray resistance is carried out on a substrate at 37 ℃, the test time is 2400h, and the concentration of sodium chloride is 60g/L; using a vertical universal friction and wear testing machine to test wear resistance, selecting GCr15 as a counter-grinding material, wherein the load is 15N, the rotating speed of a turntable is 100r/min, the wear time is 30min, measuring the mass of a sample before and after the abrasion, and calculating the abrasion loss; the data obtained are shown in the following table:
Conclusion:
As can be seen from the data on the table, the diamond heat sink material prepared by sputtering the seed Ti layer, the seed Cu layer and the electroplated metal layer in the embodiment 1 of the invention has high heat conductivity, can improve the heat dissipation effect of the laser, and has the heat conductivity of 1731W/(K.m). In the embodiment 2-4, the substrate after gold plating is also plated with the modified nano boron nitride layer, so that the heat conduction performance is improved, and meanwhile, the corrosion resistance of the copper-clad plate is improved; comparative example 1 nanometer boron nitride was prepared by a different method, and the nanometer boron nitride prepared by the method had a small specific surface area, and the grafted 1-aminobenzotriazole and silica became less and the abrasion resistance became worse. Comparative example 2 did not modify the nano boron nitride, did not load silica thereon, and had poor abrasion resistance.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a diamond laser heat sink substrate is characterized by comprising the following steps: the method comprises the following steps:
Step one: taking diamond ceramic chips, cleaning, then performing magnetron sputtering treatment, and sputtering a seed Ti layer and a seed Cu layer in sequence to obtain sputtered ceramic chips;
Step two: electroplating the sputtered ceramic chip with copper, and performing pattern transfer on the ceramic chip plated with copper for one time through film pasting, exposure, development, flash etching and film removal; after the primary pattern is manufactured, performing secondary pattern transfer manufacturing through film pasting, exposure and development procedures;
Step three: copper plating and thickening are carried out on the secondary pattern transfer developing area through electroplating;
step four: after copper plating, grinding and polishing the copper surface, removing the residual dry film in the product pattern space, and then performing sand blasting;
step five: carrying out surface treatment on the product by using an electroplated nickel gold process; after gold plating, performing third pattern transfer by gluing, exposing and developing to expose the area needing to be electroplated with AuSn, and covering the rest positions by photoresist; plating AuSn alloy on the surface of the product through an electroplating process;
step six: and removing the photoresist again after the AuSn electroplating is finished, electroplating a gold layer on the surface to obtain a gold-plated substrate, and scribing to obtain the diamond laser heat sink substrate.
2. The method for preparing the diamond laser heat sink substrate according to claim 1, wherein the method comprises the following steps: in the first step, the magnetron sputtering treatment process is as follows: firstly sputtering a titanium layer with the thickness of 100-200nm on a ceramic substrate, and then sputtering a copper layer with the thickness of 1.5-2.5 mu m; the sputtering pressure is 2.0X10 -1Pa-3.0×10-1 Pa, the sputtering temperature is 200 ℃ to 280 ℃, the sputtering current is 10A to 20A, the sputtering voltage is 600V to 800V, the sputtering power is 10KW to 20KW, the sputtering time is 1500s, and the sputtering time is 5000s.
3. The method for preparing the diamond laser heat sink substrate according to claim 1, wherein the method comprises the following steps: in the second step, the technological parameters of the bottom copper electroplating are as follows: the temperature is 20-28 ℃, the current density is 1A/dm 2, and the electroplating time is 15min.
4. The method for preparing the diamond laser heat sink substrate according to claim 1, wherein the method comprises the following steps: in the third step, the technological parameters of the thick copper electroplating are as follows: the temperature is 20-28 ℃, the current density is 2-3A/dm < 2 >, and the electroplating time is 3-5h.
5. The method for preparing the diamond laser heat sink substrate according to claim 1, wherein the method comprises the following steps: in the fifth step, nickel plating process parameters: the temperature is 50-60 ℃, the nickel plating current density is 0.5A/dm 2, and the nickel plating time is 50-60min;
Gold plating process parameters: the gold plating current density is 0.1A/dm 2, and the gold plating time is 20-30min;
technological parameters of AuSn alloy plating: the temperature is 40-44 ℃, the current density is 0.4A/dm < 2 >, and the electroplating time is 20-25min.
6. The method for preparing the diamond laser heat sink substrate according to claim 1, wherein the method comprises the following steps: in the fifth step, gold plating process parameters: the temperature is 50-60 ℃, the gold plating current density is 0.1A/dm 2, and the gold plating time is 1-2min.
7. The method for preparing the diamond laser heat sink substrate according to claim 1, wherein the method comprises the following steps: step six, plating a modified nano boron nitride layer on the substrate after gold plating; the preparation method comprises the following steps: and (3) placing the substrate subjected to gold plating into a preplating solution, carrying out ultrasonic auxiliary preplating for 1-1.5h at 65-70 ℃, wherein the preplating current density is 10mA/cm 2, the ultrasonic power is 300W, and obtaining the preplating substrate, and scribing, so as to obtain the diamond laser heat sink substrate.
8. The method for preparing a diamond laser heat sink substrate according to claim 7, wherein: the preplating solution comprises the following components: 1-butyl-3-methylimidazole tetrafluoroborate ionic liquid is used as a solvent, chloroauric acid is 50-65g/L, hydantoin is 5-7g/L, and modified nano boron nitride is 6-8g/L.
9. The method for preparing the diamond laser heat sink substrate according to claim 8, wherein the method comprises the following steps: the preparation method of the modified nano boron nitride comprises the following steps: mixing nano boron nitride, deionized water and ethanol uniformly, adding tetraethyl orthosilicate and a silane coupling agent KH550, reacting for 5-6 hours, adding 1-aminobenzotriazole, performing ultrasonic dispersion for 1-2 hours, filtering, washing and drying to obtain modified nano boron nitride.
10. The method for preparing the diamond laser heat sink substrate according to claim 9, wherein the method comprises the following steps: the preparation method of the nano boron nitride comprises the following steps: taking ammonia borane, and preserving the temperature for 1-1.5 hours at 1090-1110 ℃ to obtain boron nitride foam; adding absolute ethyl alcohol to immerse the boron nitride foam, carrying out ultrasonic treatment for 1-2min, carrying out suction filtration and drying to obtain the nano boron nitride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410383931.8A CN118291936B (en) | 2024-04-01 | 2024-04-01 | Preparation method of diamond laser heat sink substrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410383931.8A CN118291936B (en) | 2024-04-01 | 2024-04-01 | Preparation method of diamond laser heat sink substrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN118291936A true CN118291936A (en) | 2024-07-05 |
| CN118291936B CN118291936B (en) | 2024-09-06 |
Family
ID=91675355
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410383931.8A Active CN118291936B (en) | 2024-04-01 | 2024-04-01 | Preparation method of diamond laser heat sink substrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN118291936B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN119725265A (en) * | 2025-03-04 | 2025-03-28 | 山东大学 | Insulating substrate based on diamond ceramic layer and preparation method thereof |
| CN119843275A (en) * | 2025-03-18 | 2025-04-18 | 湖南良诚新材料科技有限公司 | Method for preparing diamond coating by laser cladding |
Citations (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09162198A (en) * | 1995-12-07 | 1997-06-20 | Nec Corp | Semiconductor device |
| US20080041560A1 (en) * | 2002-04-02 | 2008-02-21 | Paradis Leo R | Diamond heat sink |
| WO2009052817A2 (en) * | 2007-10-26 | 2009-04-30 | Dirk Lorenzen | Corrosion-resistant microchannel heat sink and semiconductor cooling device comprising said microchannel heat sink |
| KR20100025502A (en) * | 2009-11-18 | 2010-03-09 | 이환철 | Insulated metal components and method of manufacturing the same |
| JP2010129762A (en) * | 2008-11-27 | 2010-06-10 | Sony Corp | Semiconductor laser element and semiconductor laser device |
| US20110117338A1 (en) * | 2008-04-29 | 2011-05-19 | Ben Poquette | Open pore ceramic matrix coated with metal or metal alloys and methods of making same |
| WO2012145750A2 (en) * | 2011-04-22 | 2012-10-26 | The Nano Group, Inc. | Electroplated lubricant-hard-ductile nanocomposite coatings and their applications |
| CN104947068A (en) * | 2015-06-10 | 2015-09-30 | 哈尔滨工业大学 | Preparation method of diamond heat sink piece |
| WO2015147401A1 (en) * | 2014-03-25 | 2015-10-01 | 새솔다이아몬드공업 주식회사 | Method for manufacturing pad conditioner and pad conditioner |
| CN105986158A (en) * | 2015-02-12 | 2016-10-05 | 中国科学院宁波材料技术与工程研究所 | High-thermal-conductivity diamond-metal composite material and preparation method thereof |
| US20170009350A1 (en) * | 2015-07-06 | 2017-01-12 | Carbodeon Ltd Oy | Metallic coating and a method for producing the same |
| US20170151755A1 (en) * | 2015-12-01 | 2017-06-01 | Materion Corporation | Metal-on-ceramic substrates |
| US20170176495A1 (en) * | 2015-12-21 | 2017-06-22 | Intel Corporation | Coated Probe Tips for Plunger Pins of an Integrated Circuit Package Test System |
| CN111133640A (en) * | 2017-09-26 | 2020-05-08 | 欧司朗Oled股份有限公司 | Semiconductor laser diode and semiconductor device |
| RU2746861C1 (en) * | 2020-07-24 | 2021-04-21 | Сергей Константинович Есаулов | Method for producing a composite metal-dispersed coating, dispersed system for precipitation of composite metal-dispersed coating and method of its production |
| CN116403912A (en) * | 2023-03-06 | 2023-07-07 | 汕尾市栢林电子封装材料有限公司 | Method for preparing aluminum nitride/tungsten copper gold tin heat sink |
| CN116574997A (en) * | 2023-04-21 | 2023-08-11 | 航天科工(长沙)新材料研究院有限公司 | Method for metallizing diamond surface |
| CN117165942A (en) * | 2023-09-08 | 2023-12-05 | 合肥圣达电子科技实业有限公司 | Plating process of diamond/copper composite material |
| CN117646174A (en) * | 2023-10-09 | 2024-03-05 | 苏州智芯联电子科技有限公司 | Heat sink and preparation method thereof |
-
2024
- 2024-04-01 CN CN202410383931.8A patent/CN118291936B/en active Active
Patent Citations (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09162198A (en) * | 1995-12-07 | 1997-06-20 | Nec Corp | Semiconductor device |
| US20080041560A1 (en) * | 2002-04-02 | 2008-02-21 | Paradis Leo R | Diamond heat sink |
| WO2009052817A2 (en) * | 2007-10-26 | 2009-04-30 | Dirk Lorenzen | Corrosion-resistant microchannel heat sink and semiconductor cooling device comprising said microchannel heat sink |
| US20110117338A1 (en) * | 2008-04-29 | 2011-05-19 | Ben Poquette | Open pore ceramic matrix coated with metal or metal alloys and methods of making same |
| JP2010129762A (en) * | 2008-11-27 | 2010-06-10 | Sony Corp | Semiconductor laser element and semiconductor laser device |
| KR20100025502A (en) * | 2009-11-18 | 2010-03-09 | 이환철 | Insulated metal components and method of manufacturing the same |
| WO2012145750A2 (en) * | 2011-04-22 | 2012-10-26 | The Nano Group, Inc. | Electroplated lubricant-hard-ductile nanocomposite coatings and their applications |
| WO2015147401A1 (en) * | 2014-03-25 | 2015-10-01 | 새솔다이아몬드공업 주식회사 | Method for manufacturing pad conditioner and pad conditioner |
| CN105986158A (en) * | 2015-02-12 | 2016-10-05 | 中国科学院宁波材料技术与工程研究所 | High-thermal-conductivity diamond-metal composite material and preparation method thereof |
| CN104947068A (en) * | 2015-06-10 | 2015-09-30 | 哈尔滨工业大学 | Preparation method of diamond heat sink piece |
| US20170009350A1 (en) * | 2015-07-06 | 2017-01-12 | Carbodeon Ltd Oy | Metallic coating and a method for producing the same |
| US20170151755A1 (en) * | 2015-12-01 | 2017-06-01 | Materion Corporation | Metal-on-ceramic substrates |
| US20170176495A1 (en) * | 2015-12-21 | 2017-06-22 | Intel Corporation | Coated Probe Tips for Plunger Pins of an Integrated Circuit Package Test System |
| CN111133640A (en) * | 2017-09-26 | 2020-05-08 | 欧司朗Oled股份有限公司 | Semiconductor laser diode and semiconductor device |
| RU2746861C1 (en) * | 2020-07-24 | 2021-04-21 | Сергей Константинович Есаулов | Method for producing a composite metal-dispersed coating, dispersed system for precipitation of composite metal-dispersed coating and method of its production |
| CN116403912A (en) * | 2023-03-06 | 2023-07-07 | 汕尾市栢林电子封装材料有限公司 | Method for preparing aluminum nitride/tungsten copper gold tin heat sink |
| CN116574997A (en) * | 2023-04-21 | 2023-08-11 | 航天科工(长沙)新材料研究院有限公司 | Method for metallizing diamond surface |
| CN117165942A (en) * | 2023-09-08 | 2023-12-05 | 合肥圣达电子科技实业有限公司 | Plating process of diamond/copper composite material |
| CN117646174A (en) * | 2023-10-09 | 2024-03-05 | 苏州智芯联电子科技有限公司 | Heat sink and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| SHANMUGAN SUBRAMANI等: ""Thermal Transient Analysis of High-Power Green LED Fixed on BN Coated Al Substrates as Heatsink"", 《IEEE TRANSACTIONS ON ELECTRON DEVICES》, vol. 61, 9 September 2014 (2014-09-09), pages 3212 - 3216 * |
| 伍垚屹: ""氮化硼纳米片导热网络设计及其在热界面材料中的应用研究"", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》, no. 01, 15 January 2023 (2023-01-15), pages 020 - 1385 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN119725265A (en) * | 2025-03-04 | 2025-03-28 | 山东大学 | Insulating substrate based on diamond ceramic layer and preparation method thereof |
| CN119843275A (en) * | 2025-03-18 | 2025-04-18 | 湖南良诚新材料科技有限公司 | Method for preparing diamond coating by laser cladding |
Also Published As
| Publication number | Publication date |
|---|---|
| CN118291936B (en) | 2024-09-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN118291936B (en) | Preparation method of diamond laser heat sink substrate | |
| CN112111761A (en) | A kind of electrolyte of high elongation electrolytic copper foil and its application | |
| JPH0874061A (en) | Feeding solution and method for feeding for electroless goldplating bath | |
| CN114108051B (en) | Corrosion-resistant mixed acid anodic oxidation process | |
| CN112635772A (en) | Porous copper foil for lithium battery and preparation method and application thereof | |
| KR20050085664A (en) | Plating solutions for electrochemical or chemical deposition of copper interconnects and methods therefor | |
| CN114031769A (en) | Quaternary ammonium salt leveling agent, preparation method thereof, electroplating solution containing quaternary ammonium salt leveling agent and electroplating method | |
| CN110331422A (en) | A kind of ceramic substrate copper electroplating layer thickening method | |
| CN104213171B (en) | Method for manufacturing titanium oxide class ceramic coating on surface of aluminum-alloy piston | |
| CN109898115A (en) | Electro-coppering pre-treating method on a kind of quick aluminum substrate | |
| KR102274074B1 (en) | Copper electroplating compositions and methods of electroplating copper on substrates | |
| CN115279042A (en) | Preparation method of chemically nickel-plated gold DPC ceramic substrate | |
| JP5435484B2 (en) | Method for producing metal-filled microstructure | |
| JP2004526304A (en) | Electrochemical method for polishing copper films on semiconductor substrates | |
| TWI638067B (en) | Method of electroplating photoresist defined features from copper electroplating baths containing reaction products of pyrazole compounds and bisepoxides | |
| CN117646261B (en) | Limited domain electrodeposition method of metal grid line structure for photovoltaic power generation | |
| CN110846710B (en) | Electrochemical polishing method for surface of copper material | |
| CN118910682A (en) | Production process of oxidation-resistant electrolytic copper foil | |
| CN113745007A (en) | A kind of electrochemical corrosion capacity expansion process of tantalum electrolytic capacitor anode foil | |
| CN115142113B (en) | An electrolytic polishing liquid additive, polishing liquid and polishing method for nickel-based alloys | |
| CN220300895U (en) | Simple device for electroplating on semiconductor substrate | |
| CN109853006A (en) | The additive formulations and electro-plating method of electro-coppering under the conditions of a kind of high temperature and high speed | |
| TWI765358B (en) | Manufacturing method of aluminum nitride | |
| CN118579721A (en) | A method for preparing a shrapnel probe | |
| CN111155154B (en) | Double-power-supply double-anode electroplating device and method for filling through hole of glass adapter plate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |