CN117342883A - Method for preparing IGBT ceramic copper-clad substrate by hot isostatic pressing sintering - Google Patents
Method for preparing IGBT ceramic copper-clad substrate by hot isostatic pressing sintering Download PDFInfo
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- CN117342883A CN117342883A CN202311298648.7A CN202311298648A CN117342883A CN 117342883 A CN117342883 A CN 117342883A CN 202311298648 A CN202311298648 A CN 202311298648A CN 117342883 A CN117342883 A CN 117342883A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 89
- 239000000758 substrate Substances 0.000 title claims abstract description 52
- 238000005245 sintering Methods 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000001513 hot isostatic pressing Methods 0.000 title claims abstract description 31
- 229910052751 metal Inorganic materials 0.000 claims abstract description 26
- 239000002184 metal Substances 0.000 claims abstract description 26
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000005219 brazing Methods 0.000 claims abstract description 16
- 239000000945 filler Substances 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 10
- 238000007731 hot pressing Methods 0.000 claims abstract description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 23
- 239000010936 titanium Substances 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000005086 pumping Methods 0.000 claims description 5
- 239000000428 dust Substances 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- AHGIVYNZKJCSBA-UHFFFAOYSA-N [Ti].[Ag].[Cu] Chemical compound [Ti].[Ag].[Cu] AHGIVYNZKJCSBA-UHFFFAOYSA-N 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- 229910010293 ceramic material Inorganic materials 0.000 claims description 2
- 238000009792 diffusion process Methods 0.000 claims description 2
- MZFIXCCGFYSQSS-UHFFFAOYSA-N silver titanium Chemical compound [Ti].[Ag] MZFIXCCGFYSQSS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 238000005253 cladding Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000010949 copper Substances 0.000 abstract description 27
- 229910052802 copper Inorganic materials 0.000 abstract description 11
- 239000004065 semiconductor Substances 0.000 abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 229910000679 solder Inorganic materials 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001755 magnetron sputter deposition Methods 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 244000137852 Petrea volubilis Species 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000002490 spark plasma sintering Methods 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 229910004339 Ti-Si Inorganic materials 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 229910010978 Ti—Si Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000011268 mixed slurry Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 229910017945 Cu—Ti Inorganic materials 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram 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
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 238000007666 vacuum forming Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
- C04B37/021—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles in a direct manner, e.g. direct copper bonding [DCB]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/48—Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
- H01L21/4814—Conductive parts
- H01L21/4846—Leads on or in insulating or insulated substrates, e.g. metallisation
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- 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
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Physics & Mathematics (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Mechanical Engineering (AREA)
- Ceramic Products (AREA)
Abstract
The invention belongs to the field of active metal brazing, and discloses a method for preparing an IGBT ceramic copper-clad substrate by hot isostatic pressing sintering. According to the invention, the active metal brazing filler metal is added under specific conditions to bond the ceramic and copper, so that the wettability of the bonding of the ceramic and copper can be effectively improved, and the high-strength tight connection between the ceramic and the metal copper can be realized by adopting a hot-pressing sintering furnace to perform vacuum sheathing and hot isostatic pressing sintering processes, so that the problem of low bonding strength of the ceramic copper-clad substrate in a high-power semiconductor device can be effectively solved. Solves the problems of complicated steps and long time consumption in preparing the ceramic copper-clad substrate.
Description
Technical Field
The invention belongs to the field of active metal brazing, and relates to a method for preparing an IGBT ceramic copper-clad substrate by hot isostatic pressing sintering.
Background
With the continuous development of technology, the ceramic copper-clad substrate in the electronic power device such as an IGBT chip plays a key role in connecting the internal heat dissipation channel and the external heat dissipation channel, and simultaneously has the functions of electric interconnection, mechanical support and the like. Ceramics are ideal packaging and heat dissipating materials due to their excellent mechanical properties, low expansion coefficient, low dielectric constant and high temperature resistance. However, since the thermal expansion coefficients of ceramics and metals have a large difference, a large amount of residual thermal stress is generated, the bonding strength and the service life are greatly reduced, and the application of the ceramic in the field of high-power semiconductor devices is severely limited.
In recent years, in order to solve the problems of poor bonding strength between ceramics and metals and low service life of ceramic copper-clad substrates, improvement by brazing with an active metal added as a brazing filler metal has been a growing research focus. The principle is as follows: chemical reactions occur at the interface to form new compounds to achieve binding, and thus the binding strength is enhanced. And the brazing temperature can be greatly reduced by adding the proper active metal brazing filler metal, the residual stress is reduced, and the service life is prolonged. However, at present, the ceramic copper-clad substrate is usually prepared by combining active metal solder with ceramic through a vacuum magnetron sputtering method, a molten salt reaction method and the like, and then combining the ceramic after surface treatment with copper. Xin et al propose a method for preparing nano Cu/Ti-Si 3 N 4 Novel method for ceramic copper-clad substrate by vacuum magnetron sputtering method on Si 3 N 4 Depositing nano active metal Ti on the surface of ceramic as transition layer, and then mixing nano copper powder with Si in SPS vacuum furnace 3 N 4 Ceramic burnerThe knots were formed under this condition with a maximum peel strength of only 4.29N/mm. The low peel strength is due to the fact that the Ti layer deposited by vacuum magnetic sputtering is too thin to be Si 3 N 4 The ceramic reaction is insufficient, the process is tedious and the time-consuming is long. (Xin C, huang L, zeng Q, et al A novel nano Cu/Ti-Si 3 N 4 ceramic substrates fabricated by spark plasma sinteringand its bonding mechanism[J]Vacus, 2021,187:110093.DOI:10.1016/j. Vacus.2021.110093.) Paik et al are incubated at 1250 ℃ for 90min to form an oxide layer with a thickness of 1-4 μm on the surface of AlN ceramic, and the maximum peel strength between Cu and AlN ceramic reaches 5.67N/mm, and the peel strength is not high because the oxidation process cannot completely eliminate micropore holes between copper and AlN ceramic, and the difference of thermal expansion coefficients still exists between the oxide layer and Cu, which seriously affects the reliability of a substrate and the application of the module in the aspect of packaging high-power devices. (Entezarian M, drew RA L. Direct bonding ofcopperto aluminum nitride [ J)].Materials Science and Engineering:A,1996,212(2):206-212.DOI:10.1016/0921-5093(96)10190-8.)。
These methods are cumbersome, time consuming, costly, and do not have high bond strength. Therefore, there is a need for a simple and efficient method for preparing ceramic copper clad substrates to reduce experimental steps, shorten preparation time, and enhance bonding strength.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a method for preparing an IGBT ceramic copper-clad substrate by hot isostatic pressing sintering, which aims to solve the problems of complicated steps and long time consumption in preparing the ceramic copper-clad substrate. And the ceramic copper-clad substrate with high bonding strength is prepared by applying pressure and gradient heating from all directions through a hot isostatic pressing sintering furnace.
According to the invention, the active metal brazing filler metal is added under specific conditions to bond the ceramic and copper, so that the wettability of the bonding of the ceramic and copper can be effectively improved, and the high-strength tight connection between the ceramic and the metal copper can be realized by adopting a hot-pressing sintering furnace to perform vacuum sheathing and hot isostatic pressing sintering processes, so that the problem of low bonding strength of the ceramic copper-clad substrate in a high-power semiconductor device can be effectively solved.
The above object of the present invention is achieved by the following technical solutions:
a method for preparing an IGBT ceramic copper-clad substrate by hot isostatic pressing sintering comprises the following steps:
s1, sequentially placing polished and cleaned ceramics, brazing filler metal, cu foil and titanium foil into a sheath die, and vacuumizing in a hot-pressing sintering furnace to obtain a piece to be welded with high vacuum degree;
s2, placing the piece to be welded subjected to the vacuum sheathing in the step 1 into a hot isostatic pressing sintering furnace for brazing, namely the ceramic copper-clad substrate.
Further, the ceramic in step S1 is Si 3 N 4 Any one of AlN or other ceramic materials with the thickness of 0.30-5.00 mm; the brazing filler metal is any one of silver-copper-titanium alloy, silver-titanium alloy or other titanium-containing alloy, and the thickness is 0.03-0.10 mm; the thickness of the Cu foil is 0.02-5.00 mm; the titanium foil is industrial pure titanium alloy with the thickness of 0.10-0.50 mm.
Further, the titanium foil obtained by cutting in the step S1 is polished by sand paper to remove an oxide layer, and finally is wiped clean by dust-free paper adhered with absolute ethyl alcohol.
Further, the ceramics, the brazing filler metal and the Cu foil in the step S1 are respectively put into acetone and absolute ethyl alcohol for ultrasonic cleaning to remove greasy dirt and dust on the surface of the sample, and are dried.
Further, the vacuumizing in the step S1 is as follows: opening the mechanical pump and the pre-pumping valve, then opening the diffusion pump, closing the pre-pumping valve, opening the high vacuum valve, and reducing the vacuum degree to 10 -2 ～10 -3 Pa, performing vacuum sheathing.
Further, in step S1, the wrapping procedure is as follows: (1) uniformly heating from 25 ℃ to 700-800 ℃ at 15-20 ℃/min, and boosting to 6-6.5 MPa; (2) preserving heat and pressure for 30-45 min; (3) and after the sheath is completed, the pressure is removed, and the sheath is taken out after the temperature is reduced to room temperature.
Further, the placing of the piece to be welded in step S2 into the hot isostatic pressing furnace is as follows: and placing the piece to be welded in the crucible, opening the furnace cover of the hot isostatic pressing sintering furnace, placing the piece into the crucible, and screwing the furnace cover.
Further, the sintering process in the hot isostatic pressing furnace in the step S2 is as follows: heating from 25 ℃ to 550-650 ℃ at 10-20 ℃/min, boosting to 80-100 MPa, maintaining for 30-60 min, heating to 700-900 ℃ at 5-10 ℃/min, boosting to 150-200 MPa; maintaining the temperature and pressure at the highest temperature and pressure for 30-60 min; then the temperature is reduced to 200-300 ℃ at 10-20 ℃/min; and finally cooling to room temperature along with the furnace.
And further, cooling to room temperature along with a hot isostatic pressing sintering furnace after sintering, opening a furnace cover to take out a sample, and cutting off a sheath to obtain the ceramic copper-clad substrate.
Compared with the prior art, the invention has the beneficial effects that:
(1) The prepared ceramic copper-clad substrate has the advantages of compact combination of the ceramic and Cu, simple steps and short time consumption, and is prepared by a one-step method.
(2) The prepared ceramic copper-clad substrate has the advantages that chemical reaction occurs between the ceramic and Cu due to the existence of Ag-Cu-Ti solder, novel compound TiN is generated, and the bonding strength is improved.
Drawings
The invention is further illustrated by the following figures and examples:
fig. 1 is a schematic view of a vacuum envelope.
Fig. 2 is a photograph of a part to be welded with a successful sheathing.
Fig. 3 is a photograph of a sample taken from a hot isostatic pressing sintering furnace.
Fig. 4 is a schematic structural diagram of a ceramic copper-clad substrate prepared by the method.
Fig. 5 is an SEM image of a ceramic copper-clad substrate prepared according to the present invention.
Fig. 6 is a point scanning spectrum of a cross section of a ceramic copper-clad substrate prepared in example 1 of the present invention.
Detailed Description
The present invention is described in detail below by way of specific examples, but the scope of the present invention is not limited thereto. Unless otherwise specified, the experimental methods used in the present invention are all conventional methods, and all experimental equipment, materials, reagents, etc. used can be obtained from commercial sources.
Example 1
(1) Si is selected for 3 N 4 Ceramic with a size of 10X 0.35mm 3 The method comprises the steps of carrying out a first treatment on the surface of the The size of the commercially available Ag69.7-Cu27-Ti3.3 solder is 10×10×0.05mm 3 The method comprises the steps of carrying out a first treatment on the surface of the The Cu foils were 10X 0.02mm in size 3 And 10X 0.20mm 3 The method comprises the steps of carrying out a first treatment on the surface of the The titanium foil is an industrial pure titanium alloy and is round with a diameter of 125mm and a thickness of 0.15 mm.
(2) Polishing the cut titanium foil with 1200-mesh sand paper, and finally wiping the titanium foil with dust-free paper adhered with absolute ethyl alcohol; si is mixed with 3 N 4 And respectively placing the ceramic, the Ag69.7-Cu27-Ti3.3 solder and the Cu foil into acetone and absolute ethyl alcohol for ultrasonic cleaning for 5min to remove greasy dirt and dust on the surface of the sample, and drying.
(3) And (5) assembling. Firstly, placing a layer of titanium foil at the lowest part, and then according to Cu, ag69.7-Cu27-Ti3.3 solder and Si 3 N 4 Sequentially placing Ag69.7-Cu27-Ti3.3 solder and Cu in the middle of the titanium foil, and finally placing a layer of titanium foil on the titanium foil, assembling and placing the titanium foil into a sheathing die.
(4) And (5) vacuum covering. Placing the assembled sheath sample into a hot-pressed sintering furnace, and vacuumizing the furnace chamber to 10 -2 And (3) uniformly heating to 800 ℃ from 25 ℃ at 15 ℃/min, raising the pressure to 6MPa, maintaining the temperature and the pressure for 30min, cooling to room temperature, and taking out the sheath sample.
(5) And (5) sintering by hot isostatic pressing. Placing the sheath sample sintered in the step (4) into a hot isostatic pressing sintering furnace, closing a furnace cover, vacuumizing the furnace chamber to below 10Pa, and repeatedly cleaning the furnace chamber with high-purity argon for three times. Heating from 25deg.C to 600deg.C at 10deg.C/min, increasing pressure to 100MPa, maintaining for 30min, heating to 700deg.C at 5deg.C/min, increasing pressure to 150MPa, and maintaining for 30min to promote Ti to Si 3 N 4 Diffusing the ceramic to form a TiN transition layer; then reducing the temperature to 300 ℃ at 10 ℃/min; and finally cooling to room temperature along with the furnace.
(6) The sample was removed. And (3) cooling the sintered ceramic copper-clad substrate to room temperature along with a hot isostatic pressing sintering furnace after the sintering in the step (5), opening the furnace cover to take out a sample, and cutting off a sheath to obtain the ceramic copper-clad substrate.
The peel strength was 21.16N/mm as measured by peel testing.
TABLE 1 Point scanning energy spectrum element occupancy ratio Table of ceramic copper-clad substrate section prepared in example 1
| Element(s) | Wt％ | At％ |
| N | 29.90 | 63.71 |
| Si | 5.36 | 5.70 |
| Ti | 31.93 | 19.89 |
| Cu | 8.40 | 3.95 |
| Ag | 24.40 | 6.75 |
| Total amount: | 100.00 | 100.00 |
comparative example 1
(1) Si is selected for 3 N 4 And (3) ceramics. TiH is processed by 2 Uniformly mixing powder (69.7 wt%), polyvinyl alcohol (0.3 wt%) and water (30 wt%) to obtain mixed slurry, and adding said mixed slurry into Si 3 N 4 The upper and lower surfaces of the ceramic substrate were coated with TiH 10 μm thick 2 And (3) placing the layers in a drying box and drying for 2 hours at 300 ℃.
(2) Coating TiH under the protection atmosphere of argon 2 Si of layer 3 N 4 Heat treating the ceramic substrate to coat the TiH 2 The Ti metal layer with a thickness of 6 μm is formed by decomposition.
(3) Placing copper foil on the surface of ceramic substrate coated with Ti metal layer, placing into hot-pressing die, vacuum-forming under vacuum condition to 2×10 -4 Pa, applying 5MPa pressure, heating from room temperature to 1000 ℃, and preserving heat for 1h.
(4) The sample was removed and cooled to room temperature. The ceramic copper-clad substrate is obtained.
The peel strength was 11.00N/mm as measured by peel testing.
Comparative example 2
(1) Si is selected for 3 N 4 And (3) ceramics. In Si 3 N 4 Sputtering Ti on two sides of the ceramic substrate by adopting a magnetron sputtering method, and sputtering for 20min at a rate of 25 nm/min; then, cr is subjected to magnetron sputtering at a rate of 25nm/min for 15min, and the resultant is placed in a muffle furnace at an air flow rate of 2.5L/min.
(2) Coating the obtained Si with a coating 3 N 4 The ceramic substrate is placed in a muffle furnace, and is heated to 1300 ℃ from room temperature at a speed of 5 ℃/min under the condition of air flow of 2.5L/min, then is insulated for 60min, is cooled to 500 ℃ at a speed of 3 ℃/min, and is cooled along with the furnace.
(3) Placing the flat Cu layer on a ceramic backing plate for pre-oxidation, and forming a copper alloy layer on O 2 Preserving heat for 20min at 800 ℃ in 160ppm atmosphere, and cooling to room temperature along with a furnace; then the oxidation surface of the Cu layer is thermally oxidized with Si 3 N 4 The surfaces of the ceramic substrate covered with the oxide layer are bonded together and placed on O 2 And (3) preserving heat for 15min at 1075 ℃ in the atmosphere with the content of 35ppm to obtain the ceramic copper-clad substrate.
The peel strength was 4.00N/mm as measured by peel testing.
Comparative example 3
The difference from example 1 is that no active metal filler metal was added.
(1) Si is selected for 3 N 4 Ceramic with a size of 10X 0.35mm 3 The method comprises the steps of carrying out a first treatment on the surface of the The Cu foils were 10X 0.02mm in size 3 And 10X 0.20mm 3 The method comprises the steps of carrying out a first treatment on the surface of the The titanium foil is an industrial pure titanium alloy, and is a circle with a diameter of 125mm and a thickness of 0.15 mm.
(2) Polishing the cut titanium foil with 1200-mesh sand paper, and finally wiping the titanium foil with dust-free paper adhered with absolute ethyl alcohol; si is mixed with 3 N 4 And respectively placing the ceramic and the Cu foil into acetone and absolute ethyl alcohol for ultrasonic cleaning for 5min to remove greasy dirt and dust on the surface of the sample, and drying.
(3) And (5) assembling. Firstly, a layer of titanium foil is placed at the lowest part, and then Cu and Si are used as the materials 3 N 4 And placing Cu in the middle of the titanium foil in sequence, and finally placing a layer of titanium foil on the titanium foil, assembling and placing the titanium foil into a sheath die.
(4) And (5) vacuum covering. Placing the assembled sheath sample into a hot-pressed sintering furnace, and vacuumizing the furnace chamber to 10 -2 And (3) uniformly heating to 800 ℃ from 25 ℃ at 15 ℃/min, raising the pressure to 6MPa, maintaining the temperature and the pressure for 30min, cooling to room temperature, and taking out the sheath sample.
(5) And (5) sintering by hot isostatic pressing. Placing the sheath sample sintered in the step (4) into a hot isostatic pressing sintering furnace, closing a furnace cover, vacuumizing the furnace chamber to below 10Pa, and repeatedly cleaning the furnace chamber with high-purity argon for three times. Firstly, vacuumizing the furnace chamber to below 10Pa, and then repeatedly cleaning the furnace chamber with high-purity argon for three times. Heating from 25 ℃ to 600 ℃ at 10 ℃/min, boosting to 100MPa, maintaining for 30min, heating to 700 ℃ at 5 ℃/min, boosting to 150MPa, maintaining for 30min, and then reducing to 300 ℃ at 10 ℃/min; and finally cooling to room temperature along with the furnace.
(6) The sample was removed. And (3) cooling the sintered ceramic copper-clad substrate to room temperature along with a hot isostatic pressing sintering furnace after the sintering in the step (5), opening the furnace cover to take out a sample, and cutting off a sheath to obtain the ceramic copper-clad substrate.
The peel strength was 2.06N/mm as measured by peel testing.
Comparative example 4
(1) Si with purity of more than 99.99wt% is selected 3 N 4 Ceramic is used as the substrate material. The Ti/TiN/Ti/TiN/Ti nano multilayer film is adopted as a transition layer and deposited on Si by a Physical Vapor Deposition (PVD) method 3 N 4 A ceramic surface.
(2) Vacuum sintering the nano Cu powder onto ceramic with Ti/TiN/Ti/TiN/Ti nano multilayer film deposited on the surface by using a spark plasma sintering furnace. The applied pressure is 30MPa in the sintering process, the temperature is raised to 600 ℃, and the heat preservation and pressure maintaining are carried out for 200s.
(3) The sample was removed. And cooling to room temperature after sintering is completed, and preparing the ceramic copper-clad substrate.
The peel strength was 5.39N/mm as measured by peel testing.
Comparative example 5
(1) Si with purity of more than 99.99wt% is selected 3 N 4 Ceramic is used as the substrate material. Ti is deposited on the surface of the ceramic by adopting a vacuum magnetron sputtering method.
(2) Vacuum sintering the nano Cu powder onto the ceramic with Ti deposited on the surface by using a spark plasma sintering furnace. The applied pressure is 30MPa in the sintering process, the temperature is raised to 600 ℃, and the heat preservation and pressure maintaining are carried out for 200s.
(3) The sample was removed. And cooling to room temperature after sintering is completed, and preparing the ceramic copper-clad substrate.
The peel strength was 4.29N/mm as measured by peel testing.
Performance test: the peel strength of the ceramic copper-clad substrate prepared by the different processes is compared, and the comparison result is shown in Table 2:
table 2 peel strength table of ceramic copper clad substrates prepared by different processes
The above-described embodiments are only preferred embodiments of the invention, and not all embodiments of the invention are possible. Any obvious modifications thereof, which would be apparent to those skilled in the art without departing from the principles and spirit of the present invention, should be considered to be included within the scope of the appended claims.
Claims (7)
1. The method for preparing the IGBT ceramic copper-clad substrate by hot isostatic pressing sintering is characterized by comprising the following steps of: s1, sequentially placing polished and cleaned ceramics, brazing filler metal, cu foil and titanium foil into a sheath die, and vacuumizing in a hot-pressing sintering furnace to obtain a piece to be welded with high vacuum degree;
s2, placing the piece to be welded subjected to the vacuum sheathing in the step 1 into a hot isostatic pressing sintering furnace for brazing, namely the ceramic copper-clad substrate.
2. The method for manufacturing a copper-clad ceramic substrate for an IGBT as claimed in claim 1, wherein said ceramic in step S1 is Si 3 N 4 Any one of AlN or other ceramic materials with the thickness of 0.30-5.00 mm; the brazing filler metal is any one of silver-copper-titanium alloy, silver-titanium alloy or other titanium-containing alloy, and the thickness is 0.03-0.10 mm; the thickness of the Cu foil is 0.02-5.00 mm; the titanium foil is industrial pure titanium alloy with the thickness of 0.10-0.50 mm.
3. The method for preparing the IGBT ceramic copper-clad substrate by hot isostatic pressing sintering according to claim 2, wherein the ceramic, the brazing filler metal and the Cu sheet in the step S1 are respectively put into acetone and absolute ethyl alcohol for ultrasonic cleaning to remove greasy dirt and dust on the surface of a sample, and are dried.
4. A method for preparing a copper-clad IGBT ceramic substrate by hot isostatic pressing sintering as claimed in claim 3, wherein the vacuum pumping in step S1 is: opening the mechanical pump and the pre-pumping valve, then opening the diffusion pump, closing the pre-pumping valve, opening the high vacuum valve, and reducing the vacuum degree to 10 -2 ～10 -3 Pa, performing vacuum sheathing.
5. The method for preparing the IGBT ceramic copper-clad substrate by hot isostatic pressing sintering according to claim 4, wherein the cladding procedure in step S1 is: (1) uniformly heating from 25 ℃ to 700-800 ℃ at 15-20 ℃/min, and boosting to 6-6.5 MPa; (2) preserving heat and pressure for 30-45 min; (3) and after the sheath is completed, the pressure is removed, and the sheath is taken out after the temperature is reduced to room temperature.
6. The method for preparing the IGBT ceramic copper-clad substrate by hot isostatic pressing sintering according to claim 5, wherein the placing of the part to be welded in the hot isostatic pressing sintering furnace in step S2 is: and placing the piece to be welded in the crucible, opening the furnace cover of the hot isostatic pressing sintering furnace, placing the piece into the crucible, and screwing the furnace cover.
7. The method for preparing the IGBT ceramic copper-clad substrate by hot isostatic pressing sintering according to claim 6, wherein the sintering process in the hot isostatic pressing sintering furnace in step S2 is: heating from 25 ℃ to 550-650 ℃ at 10-20 ℃/min, boosting to 80-100 MPa, maintaining for 30-60 min, heating to 700-900 ℃ at 5-10 ℃/min, boosting to 150-200 MPa; maintaining the temperature and pressure at the highest temperature and pressure for 30-60 min; then the temperature is reduced to 200-300 ℃ at 10-20 ℃/min; and finally cooling to room temperature along with the furnace.
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| CN202311298648.7A CN117342883A (en) | 2023-10-09 | 2023-10-09 | Method for preparing IGBT ceramic copper-clad substrate by hot isostatic pressing sintering |
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| CN202311298648.7A CN117342883A (en) | 2023-10-09 | 2023-10-09 | Method for preparing IGBT ceramic copper-clad substrate by hot isostatic pressing sintering |
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