CN113355650B - AlN-diamond heat sink, preparation method and application thereof, and semiconductor laser packaging part - Google Patents
AlN-diamond heat sink, preparation method and application thereof, and semiconductor laser packaging part Download PDFInfo
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 135
- 239000010432 diamond Substances 0.000 title claims abstract description 135
- 239000004065 semiconductor Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000004806 packaging method and process Methods 0.000 title abstract description 5
- 238000005498 polishing Methods 0.000 claims abstract description 36
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000000151 deposition Methods 0.000 claims abstract description 27
- 238000004544 sputter deposition Methods 0.000 claims abstract description 22
- 230000008021 deposition Effects 0.000 claims abstract description 19
- 238000000227 grinding Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 12
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 7
- 239000011733 molybdenum Substances 0.000 claims abstract description 7
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- 239000012298 atmosphere Substances 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 229910001218 Gallium arsenide Inorganic materials 0.000 claims description 10
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 235000010333 potassium nitrate Nutrition 0.000 claims description 5
- 239000004323 potassium nitrate Substances 0.000 claims description 5
- 229910001018 Cast iron Inorganic materials 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000007800 oxidant agent Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 238000000861 blow drying Methods 0.000 claims description 2
- 238000007664 blowing Methods 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- 238000010891 electric arc Methods 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000008646 thermal stress Effects 0.000 abstract description 4
- 239000010408 film Substances 0.000 description 31
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000001237 Raman spectrum Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
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- 238000010899 nucleation Methods 0.000 description 2
- 230000002572 peristaltic effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 238000004630 atomic force microscopy Methods 0.000 description 1
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- 230000015572 biosynthetic process Effects 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
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- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000003698 laser cutting Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
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- 229910000679 solder Inorganic materials 0.000 description 1
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- 230000003746 surface roughness Effects 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/272—Diamond only using DC, AC or RF discharges
-
- 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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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- 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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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- 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
- C23C14/0617—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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- 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
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/01—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes on temporary substrates, e.g. substrates subsequently removed by etching
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/503—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using dc or ac discharges
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- C—CHEMISTRY; METALLURGY
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
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- 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
- H01S5/02469—Passive cooling, e.g. where heat is removed by the housing as a whole or by a heat pipe without any active cooling element like a TEC
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Abstract
The invention discloses an AlN-diamond heat sink, a preparation method and application thereof and a semiconductor laser packaging piece, wherein the preparation method of the AlN-diamond heat sink comprises the following steps: step 1, grinding, cleaning and drying the surface of a molybdenum sheet; step 2, depositing a diamond film on the surface of the molybdenum substrate by a direct current arc plasma jet chemical vapor deposition method, and then cooling to normal temperature to separate the diamond thick film from the molybdenum sheet; step 3, polishing the self-supporting diamond film by using a chemical mechanical polishing method to obtain a diamond sheet with a flattened surface, and cleaning and drying the diamond sheet; step 4, carrying out reverse sputtering treatment on the diamond sheet with the flattened surface; and 5, depositing an AlN film on the surface of the diamond sheet subjected to the reverse sputtering treatment by direct current sputtering, and after the deposition is finished, performing N 2 And reducing the atmosphere to normal temperature to obtain the AlN-diamond heat sink. The heat conductivity of the diamond sheet in the AlN-diamond heat sink is high, and the AlN film is used as a buffer layer, so that the thermal stress of the device can be reduced.
Description
Technical Field
The invention relates to the technical field of preparation processes of high-power semiconductor laser heat sinks, in particular to an AlN-diamond heat sink, a preparation method and application thereof and a semiconductor laser.
Background
The semiconductor laser has the advantages of high photoelectric conversion efficiency, small volume, strong adjustability, convenient use and the like, and is widely applied to the fields of solid laser pumping, material processing, medical cosmetology, military and the like. As the output power of semiconductor lasers has been increasing, the reliability of semiconductor lasers, in particular, as solid-state lasers, is becoming an important factor that limits their development.
At present, cu or AlN is mostly adopted as a heat sink for packaging a semiconductor laser. Although Cu has good thermal conductivity, its thermal expansion coefficient is as high as 17.8ppmK ～1 And the GaAs semiconductor laser linear array is about 5.8ppmK ～1 Resulting in a mismatch in the coefficient of thermal expansion, resulting in large thermal stresses. The large thermal stress not only easily causes the bending of the semiconductor laser linear array, but also easily causes the cracking of the solder layer. Although the thermal expansion coefficient of AlN is close to that of GaAs device, its thermal conductivity is only 170W m -1 K -1 The heat generated by the device is difficult to be led out, so that the output power of the semiconductor laser is reduced, and the aging and the failure of the device can be accelerated when the device works under the condition of high temperature for a long time.
Disclosure of Invention
The invention aims to solve the problem of low AlN thermal conductivity existing in the prior art, and provides an AlN-diamond heat sink which comprises a CVD diamond layer and an AlN film deposited on the surface of the CVD diamond layer, wherein the CVD diamond has extremely high thermal conductivity (up to 1800 Wm) -1 K -1 ) And an AlN film is deposited on the surface of the buffer layer to serve as a buffer layer.
The invention also aims to provide a preparation method of the AlN-diamond heat sink, which comprises the steps of firstly preparing a CVD diamond layer by taking a molybdenum sheet as a substrate, and then depositing an AlN film after carrying out reverse sputtering treatment on the diamond layer.
The AlN-diamond heat sink is applied to a semiconductor laser, the CVD diamond layer has good thermal conductivity and is beneficial to leading out heat generated in the working of a GaAs semiconductor laser, and the AlN film is used as a buffer layer and can effectively improve the matching degree of the thermal expansion coefficients of a GaAs device and the diamond heat sink, so that the thermal stress of the device is reduced.
It is another object of the invention to provide a semiconductor laser package assembled with the AlN-diamond heatsink.
The technical scheme adopted for realizing the purpose of the invention is as follows:
a preparation method of the AlN-diamond heat sink comprises the following steps:
step 4, carrying out reverse sputtering treatment on the surface of the diamond sheet to remove surface oxygen components and introduce nitrogen elements to obtain the diamond sheet after the reverse sputtering treatment;
and 5, depositing an AlN film on the surface of the diamond sheet subjected to the reverse sputtering treatment by direct current sputtering, and after the deposition is finished, performing N 2 And reducing the atmosphere to normal temperature to obtain the AlN-diamond heat sink.
In the above technical solution, the grinding process in step 1 specifically includes: taking diamond micro powder as an abrasive, and mechanically grinding the surface of the molybdenum sheet for 10-20 min; the cleaning in the step 1 specifically comprises the following steps: putting the polished molybdenum sheet into deionized water for ultrasonic cleaning for 5-15 min; the drying in the step 1 specifically comprises the following steps: blow-drying with flowing nitrogen.
In the above technical solution, the specific steps of the direct current Arc Plasma jet chemical vapor deposition (DC Arc Plasma jet CVD) method in step 2 are as follows: putting the pretreated molybdenum sheet into a vacuum chamber, vacuumizing the background to be lower than 0.01-0.001 Pa, and introducing H 2 Ar and CH 4 Performing diamond film deposition, wherein CH is contained in the mixed gas 4 The concentration is 0.5-1.5%, the chamber pressure is 4-5 kPa, the pump pressure is 12-20 kPa, the substrate temperature is 900-1100 ℃, the electric arc power is 10-30 kW, and the deposition time is 10-24 h.
In the above technical solution, the chemical mechanical polishing method in step 3 specifically includes the steps of:
(1) Preparing a polishing solution: adding polyethylene glycol into deionized water as a solvent, adding potassium nitrate as an oxidant, taking diamond powder as an abrasive, and fully stirring and mixing to form the polishing solution, wherein the mass ratio of the polyethylene glycol to the deionized water to the potassium nitrate to the diamond powder is (1-2): 10: (3.0-3.5): (1-2);
(2) Polishing in a diamond polishing machine, namely taking a cast iron grinding disc as the grinding disc, dropping polishing solution at the speed of 150-250 ml/h (by using a peristaltic pump) for 500-600 min by taking the pressure between the grinding disc and the self-supporting diamond film as 8-12 psi, the rotating speed of the polishing disc as 100-200 rpm and the temperature of the polishing disc as 100-150 ℃, and obtaining the diamond sheet with a flattened surface after polishing.
In the above technical solution, after polishing in step 3, cutting (YAG laser cutting) is performed to obtain a diamond wafer with a predetermined size, and then cleaning and drying are performed.
In the above technical solution, the cleaning in the step 3 specifically includes: firstly, placing a diamond sheet with a flattened surface in concentrated nitric acid, carrying out ultrasonic treatment for 30min at the temperature of 50-90 ℃, and then carrying out ultrasonic cleaning in deionized water, acetone and deionized water in sequence, wherein the drying in the step 3 is as follows: blowing the glass by flowing nitrogen.
In the aboveIn the technical scheme, the reverse sputtering treatment in the step 4 comprises the following specific steps: putting the diamond wafer into a sample chamber of a magnetron sputtering system, and vacuumizing the background to (0.5-1) x 10 ～3 Pa, introduction of Ar and N 2 Mixed gas of Ar and N 2 The flow ratio is 1.
In the above technical solution, the dc sputtering deposition in step 5 specifically comprises the following steps: transferring the diamond sheet after the reverse sputtering treatment to a deposition chamber, and vacuumizing the background to (0.5-1) x 10 ～5 Pa, introducing Ar and N 2 Mixed gas of Ar and N 2 The flow ratio is 1.
In another aspect of the invention, the AlN-diamond heat sink obtained by the preparation method comprises a diamond sheet and an AlN film deposited on the diamond sheet.
In the above technical solution, the diamond sheet has a thickness of 100 to 200 μm, and the AlN film has a thickness of 10 to 20 μm.
In another aspect of the invention, the AlN-diamond heat sink is used in a semiconductor laser.
In the above technical solution, the semiconductor laser is a GaAs semiconductor laser or a third generation semiconductor laser GaN.
In another aspect of the invention, a semiconductor laser package, the GaAs device or GaN device of the semiconductor laser is packaged on the AlN-diamond heat sink.
Compared with the prior art, the invention has the beneficial effects that:
1. the AlN-diamond heat sink not only has excellent heat dissipation performance of diamond, but also reduces the difference of thermal expansion coefficients between the heat sink and the linear array of the semiconductor laser, and is favorable for improving the reliability of the semiconductor laser, and the specific thermal conductivity of the AlN-diamond heat sink is 1373Wm -1 K -1 About 25 ℃, the thermal expansion coefficient of the AlN-diamond heat sink is about 2.09X 10 -6 。
The AlN-diamond heat sink has good insulating property, can be suitable for packaging the semiconductor laser of the existing water-cooling micro-channel heat sink, avoids electrochemical corrosion of the inner wall of the water channel of the micro-channel, and prolongs the service life of the micro-channel heat sink.
3. The invention can convert the oxygen termination surface into the nitrogen termination surface by carrying out the reverse sputtering treatment process on the surface of the diamond sheet, thereby being beneficial to improving the crystallization quality of AlN film formation and the bonding strength between the AlN film and the diamond film.
Drawings
FIG. 1 is an SEM photograph of a free-standing CVD diamond film;
FIG. 2 is a Raman spectrum of a free-standing CVD diamond film;
FIG. 3 is an AFM scan of a surface of a diamond wafer with a planarized surface;
FIG. 4 is an XPS energy spectrum of a reverse sputter treated diamond wafer surface;
FIG. 5 is an SEM of a section of an AlN/diamond plate;
fig. 6 is an XRD pattern of AlN/diamond wafer.
Fig. 7 is the thermal conductivity of AlN/diamond wafer.
Fig. 8 is the expansion coefficient of AlN/diamond wafer.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Example 1
A preparation method of an AlN-diamond heat sink comprises the following steps:
s1: the molybdenum sheet with a flat surface is selected for pretreatment, and the diameter of the molybdenum sheet is 75mm, and the thickness of the molybdenum sheet is 10mm. Using diamond micro powder with the particle size of 1 mu m as an abrasive, and mechanically grinding the surface of the molybdenum sheet for 10min. After grinding treatment, the molybdenum sheet is placed in deionized water for ultrasonic cleaning for 10min, and then blown dry by flowing nitrogen gas, so as to obtain the pretreated molybdenum sheet.
S2: and (3) taking the molybdenum sheet after pretreatment in the step (S1) as a substrate for growing the diamond film, and depositing the self-supporting diamond film by a direct current Arc Plasma jet chemical vapor deposition (DC Arc Plasma jet CVD) device. Specifically, the method comprises the following steps: putting the pretreated molybdenum sheet into a vacuum chamber, vacuumizing the background of the vacuum chamber to 0.01Pa, and introducing H 2 Ar and CH 4 Mixed gas of (2), starting to deposit a diamond film, CH 4 The concentration is 1%, the chamber pressure is 4KPa, the pump pressure is 15Pa, the substrate temperature is 1000 ℃, the arc power is 30kW, and the deposition time is 10h. After the deposition is finished, the temperature is reduced to normal temperature, the diamond thick film is separated from the molybdenum sheet, the self-supporting diamond film is prepared, the thickness is 100-200 mu m, and the appearance of the self-supporting diamond film is observed by a scanning electron microscope SEM (scanning electron microscope), as shown in figure 1. FIG. 2 is a Raman spectrum of a sample, wherein the wave number is 1332cm ～1 The characteristic peak of diamond appears, and the scattering peak of components such as graphite or amorphous carbon is not seen, which indicates that the diamond has high quality.
S3: and (3) carrying out surface planarization treatment on the self-supporting diamond film prepared in the step (S2) by a chemical mechanical polishing technology. The grinding disc of the diamond polishing machine is a cast iron grinding disc, the pressure between the grinding disc and the diamond film is 10psi, the rotating speed of the polishing disc is set to be 150rpm, the temperature of the polishing disc is set to be 150 ℃, a peristaltic pump is used for dropwise adding polishing liquid at the speed of 200ml/h, and the polishing time is 600min, so that the diamond sheet with the flattened surface is obtained. The surface morphology of the surface-flattened diamond wafer was tested by atomic force microscopy and had a roughness of only 1.8nm, as shown in fig. 3. Preparation of the used polishing solution: 200g of polyethylene glycol is added into 1000ml of deionized water as a solvent, 310g of potassium nitrate is used as an oxidizing agent, and diamond powder is used as an abrasive, and the mixture is fully stirred and mixed to form a highly-dispersed and stable solution.
S4: the diamond sheet with the planarized surface obtained in step S3 was cut into 10.8X 4.5mm pieces by a YAG laser cutter 2 And (4) size. Then cleaning, specifically, placing in concentrated nitric acid, performing ultrasonic treatment at 90 deg.C for 30min, sequentially performing ultrasonic cleaning in deionized water, acetone and deionized water for 10min, and adopting flowing nitrogenAnd drying the diamond sheet to obtain the cleaned diamond sheet.
S5: and (4) carrying out reverse sputtering treatment on the surface of the cleaned diamond sheet obtained in the step (S4). Putting the diamond chip into a sample chamber of a magnetron sputtering system, and vacuumizing the background to 1 x 10 ～3 Pa, introducing Ar and N 2 Mixed gas of (2), ar and N 2 The flow ratio is 1. The elemental composition of the diamond wafer reverse-sputtered by XPS test is shown in fig. 4, and it can be seen that the atomic ratio of N element is about 22.6%, indicating that the sample is an N-terminated surface.
S6: transferring the diamond sheet subjected to the reverse sputtering treatment obtained in the step S5 to a deposition chamber, and vacuumizing the background to 1 × 10 ～5 Pa, introduction of Ar and N 2 The AlN film was deposited by dc sputtering. In the deposition process, al with the purity of 99.999 percent is used as a target material, ar and N 2 The flow ratio is 1. After the deposition is finished, at N 2 And slowly reducing the temperature to normal temperature in the atmosphere, thereby preparing the AlN/diamond piece, namely the AlN-diamond heat sink. FIG. 5 is a cross-sectional profile of a sample of AlN/diamond plate with an AlN film layer of about 10.2 μm thickness. The crystal orientation of the sample was measured by X-ray diffraction, and as shown in fig. 6, a diffraction peak in which AlN (002) orientation is conspicuous was present at a diffraction angle of 36.7 °, indicating that the deposited AlN had good film-forming quality.
The AlN-diamond heat sink of the present invention was prepared with process parameter adjustments in accordance with the teachings of the present invention and exhibited substantially the same performance as example 1.
Example 2
The AlN-diamond heat sink obtained by the preparation method comprises a diamond sheet and an AlN film layer deposited on the surface of the diamond sheet, wherein the thickness of the diamond sheet is 100-200 mu m, and the thickness of the AlN film layer is 10.2 mu m.
As shown in fig. 6, the thermal conductivity of the diamond microchannel heat sink is measured by using a photothermal deflection thin film thermal conductivity test system, and the phase σ of the detected light deflection quantity is in a linear relationship with the distance r from the heat source.
The heat conduction coefficient is calculated by the formula:
wherein,
that is, the slope of the graph, ω is the modulation frequency of the detection light, and the thermal conductivity α is obtained, so that the thermal conductivity K is:
K＝ρ·C ρ ·α (2)
where p is the density of the measurement object, C ρ Is its specific heat capacity. The thermal conductivity of the AlN-diamond heat sink is calculated to be 1373Wm -1 K -1 ，
As shown in FIG. 7, the AlN-diamond heatsink has a coefficient of thermal expansion of about 2.09X 10 at 25 deg.C -6 。
Example 3
The AlN-diamond heat sink is applied to a semiconductor laser, and the semiconductor laser can be a GaAs semiconductor laser or a third-generation semiconductor laser GaN.
A GaAs device or a GaN device of the semiconductor laser is packaged on the AlN-diamond heat sink.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of the AlN-diamond heat sink is characterized by comprising the following steps:
step 1, grinding the surface of a molybdenum sheet, cleaning and drying to obtain a pretreated molybdenum sheet;
step 2, taking the pretreated molybdenum sheet as a molybdenum substrate, depositing a diamond film on the surface of the molybdenum substrate by a direct current arc plasma jet chemical vapor deposition method, and cooling to normal temperature after deposition to separate the diamond film from the molybdenum substrate to prepare a self-supporting diamond film;
step 3, polishing the self-supporting diamond film by using a chemical mechanical polishing method to obtain a diamond sheet with a flattened surface, and cleaning and drying to obtain the diamond sheet;
step 4, carrying out reverse sputtering treatment on the surface of the diamond sheet to remove surface oxygen components and introduce nitrogen elements to obtain the diamond sheet subjected to reverse sputtering treatment; the reverse sputtering treatment in the step 4 comprises the following specific steps: putting the diamond chip into a sample introduction chamber of a magnetron sputtering system, and vacuumizing the background to (0.5 to 1) x 10 ~3 Pa, introducing Ar and N 2 Mixed gas of (2), ar and N 2 The flow ratio is 1;
and 5, depositing an AlN film on the surface of the diamond sheet subjected to the reverse sputtering treatment by direct current sputtering, and after the deposition is finished, performing N 2 And reducing the atmosphere to normal temperature to obtain the AlN-diamond heat sink.
2. The method according to claim 1, wherein the grinding treatment in step 1 is specifically: taking diamond micro powder as an abrasive, and mechanically grinding the surface of the molybdenum sheet for 10-20 min; the cleaning in the step 1 specifically comprises the following steps: placing the polished molybdenum sheet in deionized water for ultrasonic cleaning for 5-15min; the drying in the step 1 specifically comprises the following steps: blow-drying with flowing nitrogen.
3. The preparation method according to claim 1, wherein the dc arc plasma jet chemical vapor deposition method in the step 2 comprises the following specific steps: putting the pretreated molybdenum sheet into a vacuum chamber, vacuumizing the background to be lower than 0.01-0.001 Pa, and introducing H 2 Ar and CH 4 Performing diamond film deposition, wherein CH is contained in the mixed gas 4 The concentration is 0.5% -1.5%, and the cavityThe chamber pressure is 4-5 kPa, the pump pressure is 12-20 kPa, the substrate temperature is 900-1100 ℃, the electric arc power is 10-30 kW, and the deposition time is 15-24 h.
4. The method according to claim 1, wherein the chemical mechanical polishing method in the step 3 comprises the following steps:
(1) Preparing a polishing solution: adding polyethylene glycol into deionized water as a solvent, adding potassium nitrate as an oxidant, taking diamond powder as an abrasive, and fully stirring and mixing to form a polishing solution, wherein the mass ratio of the polyethylene glycol to the deionized water to the potassium nitrate to the diamond powder is (1-2): 10: (3.0 to 3.5): (1-2);
(2) Polishing in a diamond polishing machine, namely taking a cast iron grinding disc as a grinding disc, wherein the pressure between the grinding disc and a self-supporting diamond film is 8-12psi, the rotation speed of the polishing disc is 100-200rpm, the temperature of the polishing disc is 100-150 ℃, polishing solution is dripped at the speed of 150-250ml/h, the polishing time is 500-600min, and a diamond sheet with a flattened surface is obtained after polishing;
after polishing in the step 3, cutting to obtain a diamond sheet with a preset size, and then cleaning and drying;
the cleaning in the step 3 specifically comprises the following steps: firstly, placing a diamond sheet with a flattened surface in concentrated nitric acid, carrying out ultrasonic treatment for 30min at the temperature of 50-90 ℃, and then carrying out ultrasonic cleaning in deionized water, acetone and deionized water in sequence, wherein the drying in the step 3 is as follows: blowing the glass by flowing nitrogen.
5. The preparation method according to claim 1, wherein the direct current sputtering deposition in the step 5 comprises the following specific steps: transferring the diamond sheet after the reverse sputtering treatment to a deposition chamber, and vacuumizing the background to (0.5 to 1) x 10 ~5 Pa, introduction of Ar and N 2 Mixed gas of (2), ar and N 2 The flow ratio is 10W, and the deposition time is 300-400 min.
6. The AlN-diamond heat sink obtained by the production method according to any one of claims 1 to 5, comprising a diamond sheet and an AlN film deposited on the diamond sheet.
7. The AlN-diamond heatsink of claim 6, wherein the diamond table has a thickness of 100 to 200 μm and the AlN film has a thickness of 10 to 20 μm.
8. Use of the AlN-diamond heatsink of claim 6 in a semiconductor laser.
9. Use according to claim 8, wherein the semiconductor laser is a GaAs semiconductor laser or a third generation semiconductor laser GaN.
10. A semiconductor laser package wherein a GaAs device or GaN device of a semiconductor laser is packaged on the AlN-diamond heat sink of claim 6.
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| US20100314627A1 (en) * | 2009-06-16 | 2010-12-16 | Chien-Min Sung | DIAMOND GaN DEVICES AND ASSOCIATED METHODS |
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| US20100314627A1 (en) * | 2009-06-16 | 2010-12-16 | Chien-Min Sung | DIAMOND GaN DEVICES AND ASSOCIATED METHODS |
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