CN110964967B - Back plate with low thermal expansion coefficient and manufacturing method thereof - Google Patents

Back plate with low thermal expansion coefficient and manufacturing method thereof Download PDF

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CN110964967B
CN110964967B CN201911336373.5A CN201911336373A CN110964967B CN 110964967 B CN110964967 B CN 110964967B CN 201911336373 A CN201911336373 A CN 201911336373A CN 110964967 B CN110964967 B CN 110964967B
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thermal expansion
back plate
aln
powder
expansion coefficient
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CN110964967A (en
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丁照崇
李勇军
曹晓萌
张延宾
李利利
贾倩
庞欣
滕海涛
陈明
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Grikin Advanced Material Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C29/00Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/16Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on nitrides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • B22F3/15Hot isostatic pressing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • C22C1/051Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C29/00Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/005Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3407Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Powder Metallurgy (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses a back plate with a low thermal expansion coefficient and a manufacturing method thereof, belonging to the technical field of magnetron sputtering target material manufacturing. The back plate is prepared from high-thermal-conductivity Al or Cu metal powder and low-thermal-expansion AlN powder by mixing, powder mixing, pressure sintering and machining. The thermal expansion coefficient of the back plate is not more than 10 multiplied by 10‑6K‑1Thermal conductivity of not less than 200 W.m‑1·K‑1Diameter, diameter
Figure DDA0002331020360000011
The relative density is more than 99 percent, and the high-reliability welding composition can be realized with the series target materials with low thermal expansion.

Description

Back plate with low thermal expansion coefficient and manufacturing method thereof
Technical Field
The invention belongs to the technical field of magnetron sputtering target material manufacturing, and particularly relates to a back plate with a low thermal expansion coefficient and a manufacturing method thereof.
Background
At present, the materials of the back plate for the magnetron sputtering target material mostly adopt Al alloy and Cu alloy, such as Al alloy with grades of 6061, 5052, 2024 and the like, and oxygen-freeCu alloy such as copper, CuZn, CuCr, etc. The Al alloy and Cu alloy back plate has good thermal conductivity which is usually more than 150 W.m-1·K-1The heat generated in the sputtering process can be quickly led out, so that the target and the back plate are prevented from being detached and cracked. But for W and W alloy, Mo and Mo alloy, Cr and Cr alloy, Ru and Ru alloy, Si and Si alloy, Al2O3The target materials are brittle and have low thermal expansion coefficient (mostly less than 10 multiplied by 10)-6K-1) Al alloy and Cu alloy (having a thermal expansion coefficient of 15 to 25) x 10-6K-1) The thermal expansion difference of the back plate is large. In the process of brazing and diffusion welding of the target and the back plate, along with the increase of welding temperature and welding area, the thermal stress caused by the difference of thermal expansion coefficients is larger, so that the integral deformation and even the fragmentation of the target are easily caused.
Disclosure of Invention
Aiming at the problems, the invention prepares the back plate with low thermal expansion coefficient, the back plate material is composed of AlN and Al or Cu, and the thermal expansion coefficient is less than or equal to 10 multiplied by 10-6K-1Thermal conductivity of not less than 200 W.m-1·K-1Diameter of
Figure BDA0002331020340000011
The relative density is more than 99 percent.
A method of manufacturing a back sheet having a low coefficient of thermal expansion comprising the steps of:
1) taking Al or Cu metal powder and AlN powder as raw materials;
2) proportioning and uniformly mixing the powder raw materials in the step 1) according to a proportion to obtain mixed powder: the mass content of AlN in the mixed powder is 60-80 wt%, and the balance is Al or Cu;
3) performing pressure sintering on the mixed powder in the step 2) to obtain a back plate blank, wherein the sintering temperature is 600-1050 ℃, the pressure is 100-150 MPa, and the heat preservation time is 2-6 h;
4) machining the backboard blank in the step 3), and then welding the backboard blank with a series of low-thermal-expansion targets to finally obtain the welding composite target.
The pressure sintering mode in the step 3) is hot isostatic pressing sintering.
The materials of the low-thermal expansion series target material in the step 4) are W and W alloy, Mo and Mo alloy, Cr and Cr alloy, Ru and Ru alloy, Si and Si alloy and Al2O3
The welding in the step 4) comprises brazing and diffusion welding.
The invention has the beneficial effects that:
1. the back plate of the present invention has both low thermal expansion of ceramic material and high heat conductivity of metal material. Aiming at low thermal expansion series target materials such as refractory metals, ceramics and the like, compared with the traditional Al or Cu alloy back plate, the low thermal expansion of the back plate reduces the property difference with the target materials, reduces the thermal stress between the target materials and the back plate during brazing and diffusion welding, and fundamentally solves the difficult problems that the whole welded composite target is easy to deform and crack;
2. the high heat conductivity of the back plate can quickly lead out heat generated in the sputtering process, and the desoldering cracking caused by overheating of the target material is avoided, so that the requirement of high-power sputtering coating can be met, and the use reliability of the target material is improved.
3. The back plate comprises Al or Cu with good ductility, and can realize large-area and high-density molding and subsequent machining by adopting pressure sintering molding, the relative density reaches over 99 percent, and the diameter reaches
Figure BDA0002331020340000012
Thereby satisfying 8 and 12 inches of substrate coating.
Drawings
FIG. 1 is a schematic view of a welded composite target according to the present invention;
FIG. 2 is a flow chart of the fabrication of a backing plate and a bonded composite target;
wherein: a-welding a composite target, 1-a back plate, 2-a target material and 3-a welding surface.
Detailed Description
In order to solve the problems of the prior art, it is desirable to manufacture a back plate having a low thermal expansion coefficient, a good thermal conductivity and a good electrical conductivity. However, most of materials with low thermal expansion coefficient in the natural world are oxide, carbide, nitride and other ceramic materials, and the ceramic materials are hard and brittle, insulating and non-conducting, poor in heat conduction and difficult to be directly used as target backing plates. While table 1 is a few of the current low coefficient of thermal expansion, high thermal conductivity ceramic materials. Compared with the manufacturing cost, the thermal conductivity, the linear expansion coefficient and the like, the AlN material is relatively good, but the AlN is also an insulating and non-conducting material. Therefore, the production process, raw materials and proportion are optimized, Al or Cu metal powder and AlN powder are used as raw materials, and the backboard blank is obtained through pressure sintering, so that the backboard has low thermal expansion coefficient, high thermal conductivity and electric conductivity.
TABLE 1 comparison of ceramic materials with low thermal expansion coefficient and high thermal conductivity
Figure BDA0002331020340000021
A backboard with low thermal expansion coefficient is made of AlN and Al or Cu, and the thermal expansion coefficient is less than or equal to 10 multiplied by 10-6K-1Thermal conductivity of not less than 200 W.m-1·K-1Diameter of
Figure BDA0002331020340000022
The relative density is more than 99 percent.
A method of manufacturing a back sheet having a low coefficient of thermal expansion comprising the steps of:
1) taking Al or Cu metal powder and AlN powder as raw materials;
2) proportioning and uniformly mixing the powder raw materials in the step 1) according to a proportion to obtain mixed powder: the mass content of AlN in the mixed powder is 60-80 wt%, and the balance is Al or Cu;
3) carrying out hot isostatic pressing sintering on the mixed powder in the step 2) to obtain a back plate blank, wherein the sintering temperature is 600-1050 ℃, the pressure is 100-150 MPa, and the heat preservation time is 2-6 h;
4) machining the back plate 1 blank in the step 3), and then mixing with a series of low-thermal-expansion targets, such as: w and W alloy, Mo and Mo alloy, Cr and Cr alloy, Ru and Ru alloy, Si and Si alloy, Al2O3And (3) carrying out brazing or diffusion welding on the target material 2, and finally obtaining a welded composite target A, wherein the welding surface 3 is shown in figure 1.
The invention is described in further detail below with reference to the following figures and specific examples:
as shown in fig. 1, a typical welding composite target is shown, the target and the back plate are combined by surface contact welding, and when the difference between the thermal expansion coefficients of the target and the back plate is small, the overall welding composite target can be greatly reduced, and the welding composite reliability can be improved. FIG. 2 is a flow chart of the fabrication of a backing plate and a bonded composite target, with the performance results of the specific examples shown in Table 2.
TABLE 2 Performance results for a Low CTE backing sheet
Figure BDA0002331020340000031
As can be seen from the results in Table 2, the thermal expansion coefficient of the back sheet according to the present invention is not more than 10X 10-6K-1And a thermal conductivity of not less than 200 W.m-1·K-1. When the back plate 1 is welded and compounded with a low-thermal expansion series target material 2 (such as refractory metal, ceramic and the like), the welding surface 3 is as shown in the figure, so that the welding compound target A is small in overall deformation and free of cracking, heat generated in the sputtering process can be rapidly led out, the requirement of high-power sputtering coating is met, and the use reliability of the target material is greatly improved.

Claims (1)

1. A method of making a backing plate having a low coefficient of thermal expansion, comprising the steps of:
1) taking Al or Cu metal powder and AlN powder as raw materials;
2) mixing the powder raw materials in the step 1) according to a mass ratio of Al: AlN 35: 75, mixing materials and uniformly mixing to obtain mixed powder;
3) carrying out hot isostatic pressing sintering on the mixed powder in the step 2) to obtain a back plate blank, wherein the sintering temperature is 600 ℃, the pressure is 120MPa, and the heat preservation time is 4 h;
4) machining the back plate blank in the step 3), and then brazing or diffusion welding the back plate blank with a series of low-thermal-expansion target materials to finally obtain a welding composite target;
the thermal expansion coefficient of the back plate is 8.7 multiplied by 10-6K-1The thermal conductivity was 245 W.m-1·K-1Diameter of
Figure FDA0003057139310000011
The relative density is 99.5%;
or
According to the proportion of Al: AlN 20: 80, mixing materials; in the step 3, the sintering temperature is 650 ℃, the pressure is 150MPa, and the heat preservation time is 6 h; the thermal expansion coefficient of the resulting back sheet was 8.5X 10-6K-1The thermal conductivity was 205 W.m-1·K-1Diameter of
Figure FDA0003057139310000012
The relative density is 99.4%;
or
Taking Cu metal powder and AlN powder as raw materials, and mixing the following raw materials in percentage by weight: AlN ═ 40: 60, burdening; in the step 3, the sintering temperature is 850 ℃, the pressure is 120MPa, and the heat preservation time is 3 h; the thermal expansion coefficient of the resulting back sheet was 9.2X 10-6K-1The thermal conductivity of the coating was 295 W.m- 1.K-1Diameter of
Figure FDA0003057139310000013
The relative density is 99.6%;
or
Taking Cu metal powder and AlN powder as raw materials, and mixing the following raw materials in percentage by weight: 30 parts of AlN: 70, preparing materials; in the step 3, the sintering temperature is 950 ℃, the pressure is 100MPa, and the heat preservation time is 5 h; the thermal expansion coefficient of the resulting back sheet was 8.1X 10-6K-1The thermal conductivity was 285 W.m- 1.K-1Diameter of
Figure FDA0003057139310000014
The relative density is 99.2%.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10321776A (en) * 1997-05-19 1998-12-04 Nisshin Steel Co Ltd Radiator member for semiconductor element
CN107604192A (en) * 2017-08-25 2018-01-19 巩义市泛锐熠辉复合材料有限公司 A kind of preparation method of aluminium nitride/aluminium composite material
CN109267020A (en) * 2018-09-29 2019-01-25 有研新材料股份有限公司 A kind of preparation method and application of aluminium nitrogen scandium alloy target

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10321776A (en) * 1997-05-19 1998-12-04 Nisshin Steel Co Ltd Radiator member for semiconductor element
CN107604192A (en) * 2017-08-25 2018-01-19 巩义市泛锐熠辉复合材料有限公司 A kind of preparation method of aluminium nitride/aluminium composite material
CN109267020A (en) * 2018-09-29 2019-01-25 有研新材料股份有限公司 A kind of preparation method and application of aluminium nitrogen scandium alloy target

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