CN112846171B - Powder interlayer and method for performing hot isostatic pressing diffusion welding on tungsten target by using same - Google Patents

Powder interlayer and method for performing hot isostatic pressing diffusion welding on tungsten target by using same Download PDF

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CN112846171B
CN112846171B CN202110008313.1A CN202110008313A CN112846171B CN 112846171 B CN112846171 B CN 112846171B CN 202110008313 A CN202110008313 A CN 202110008313A CN 112846171 B CN112846171 B CN 112846171B
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welding
powder
tungsten target
back plate
copper back
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CN112846171A (en
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贾倩
丁照崇
李勇军
曹晓萌
曲鹏
李利利
庞欣
熊晓东
滕海涛
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Grikin Advanced Material Co Ltd
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    • B22F1/0003
    • 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
    • B22F7/00Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/06Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
    • B22F7/062Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts
    • B22F7/064Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts using an intermediate powder layer
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/003Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/12Alloys based on aluminium with copper as the next major constituent
    • 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)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Pressure Welding/Diffusion-Bonding (AREA)
  • Powder Metallurgy (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention provides a powder layer for tungsten target hot isostatic pressing diffusion welding, which is composed of 15-25% of Ti powder, 15-25% of Cu powder and 50-70% of Al powder by mass. The Ti and Cu components can play a role in transition of physical property difference between the W target and the Cu back plate; the Al component can play a role in releasing thermal stress and reducing the final deformation of the tungsten target, and finally the welding assembly with the welding strength of more than 150MPa, the welding rate of more than 99.7 percent and the surface deformation of the W target of less than 1mm is obtained.

Description

Powder interlayer and method for performing hot isostatic pressing diffusion welding on tungsten target by using same
Technical Field
The invention relates to the technical field of magnetron sputtering target material manufacturing, in particular to a method for carrying out hot isostatic pressing diffusion welding on a tungsten target material by using a powder intermediate layer.
Background
The high-purity tungsten target material is widely applied to the manufacture of advanced memory chips due to the characteristics of high density and low resistivity, and is a key material for the manufacture of advanced memory chips such as 3D NAND flash and the like. The tungsten film layer in the current advanced storage chip is mainly prepared by deposition of a magnetron sputtering tungsten target, high-speed particles bombard and etch the surface of the target in the sputtering coating process, and if heat cannot be effectively conducted, the surface temperature of the target can be sharply increased, so that a back plate needs to be welded on the back surface of the target to quickly conduct heat. The commonly used backing plates include a Cu alloy backing plate and an Al alloy backing plate, but since the W target is used for high-power sputter coating, a Cu alloy backing plate with higher strength and better heat conductivity is required to conduct heat. With the increasing integration level of advanced memory chips, the gradual miniaturization of devices and the reduction of line width, the increase of sputtering power puts higher demands on the welding strength of a tungsten target and a Cu alloy back plate. The diffusion welding has the advantages of high welding rate, high welding strength and the like, ensures the integral strength and good electric and heat conducting performance of the target material, prevents the target material from being detached and even falling, and is particularly suitable for welding the target material for high-power and high-efficiency sputtering coating. The difference of physical properties between the tungsten target blank and the copper alloy back plate is large, and the thermal stress is large and difficult to release during diffusion welding, so that the target is large in overall deformation and even cracked.
The current common tungsten target diffusion welding mode generally adopts the mode of adding Al, adding a Ti intermediate layer or simultaneously adding an Al-Ti intermediate layer for transition, but the three intermediate layers have advantages and disadvantages respectively. The Al intermediate layer can release stress and reduce the deformation of the W target after diffusion welding, but the material property difference among the three materials of W-Al-Cu is large, and the welding strength of the W target assembly after final diffusion welding is not high and is generally about 50MPa. The mode of adding the Ti intermediate layer can play a good transition role, the welding strength of the finally obtained tungsten target diffusion welding assembly can reach about 100MPa, but the welding thermal stress cannot be well released, and the finally obtained tungsten target is large in deformation and even possibly torn or broken. Meanwhile, the mode of adding the Al-Ti intermediate layer can obtain the tungsten target welding assembly which has higher strength and smaller deformation than the mode of adding the Al intermediate layer only and adding the Ti intermediate layer only, but the tungsten target welding assembly is limited by the characteristics of Ti and Al compact materials, and cannot obtain a large-size diffusion welding tungsten target with the welding strength of more than 150MPa and the deformation of less than 1mm, and the process is more complicated.
Technical scheme
The invention aims to solve the technical problem of providing a powder interlayer and a method for carrying out hot isostatic pressing diffusion welding on a tungsten target by using the powder interlayer, wherein the powder interlayer consists of Ti, al and Cu, and the components of the Ti and the Cu can play a role in transition of the difference of physical properties of a W target and a Cu back plate; the Al component can play a role in releasing thermal stress and reducing the final deformation of the tungsten target, and finally the welding assembly with the welding strength of more than 150MPa, the welding rate of more than 99.7 percent and the surface deformation of the W target of less than 1mm is obtained.
Based on the powder layer, the powder layer for hot isostatic pressing diffusion welding of the tungsten target comprises 15-25% of Ti powder, 15-25% of Cu powder and 50-70% of Al powder by mass.
The invention also provides a tungsten target welding assembly which is composed of a tungsten target, the above-mentioned middle powder layer and a copper back plate.
And the welding strength of the tungsten target welding assembly is more than 150MPa.
Wherein the welding rate of the tungsten target welding assembly is more than 99.7%.
Wherein the target surface deformation of the tungsten target welding assembly is <1mm.
The invention also provides a tungsten target hot isostatic pressing diffusion welding method, which comprises the following steps:
firstly, preparing raw materials including a tungsten target blank, a copper back plate and a sheath;
acid cleaning, namely, carrying out acid cleaning on the tungsten target blank and the copper back plate to remove a surface oxide layer and expose fresh surfaces of the tungsten target blank and the copper back plate;
thirdly, preparing a middle powder layer, weighing Ti powder, cu powder and Al powder required by the corresponding middle layer volume in the corresponding sheath volume according to the proportion, and putting the powders into a powder mixing machine for mixing for 2-5 h;
fourthly, placing the copper back plate into a sheath, paving the middle powder layer obtained in the third step on the copper back plate, and placing the tungsten target blank on the middle powder layer;
fifthly, sealing welding, namely performing degassing sealing welding on the sample sheath obtained in the fourth step;
sixthly, performing hot isostatic pressing diffusion welding, wherein the capsule subjected to degassing sealing welding is subjected to hot isostatic pressing diffusion welding at the welding temperature of 400-650 ℃, the welding pressure of 120-160 MPa and the time of 2-6 hours to obtain a welding assembly of the tungsten target material, the powder intermediate layer and the copper back plate;
and seventhly, machining, namely machining the obtained welding assembly of the tungsten target, the intermediate layer and the copper back plate to remove the sheath, and finally obtaining the tungsten target welding assembly.
Advantageous effects
Compared with the prior art, the technical scheme has the following advantages:
(1) The welding strength is high: the technical scheme adopts the powder intermediate layer containing Ti, al and Cu components, which can play a good physical property transition role, and the finally obtained welding strength is more than 150MPa.
(2) The deformation is small: the Al component in the powder intermediate layer can release thermal stress generated in the welding process, and the diffusion welding is carried out in a powder pressing welding mode, so that the displacement of the W target and the Cu back plate can be adjusted through the powder intermediate layer in the diffusion welding process, and finally the tungsten target diffusion welding assembly with small deformation is obtained.
(3) Is suitable for a high-power sputtering machine table, and ensures that the target cannot be detached and dropped in the sputtering process.
Drawings
FIG. 1 is a tungsten target-interlayer-copper backing plate weld assembly provided by the present invention;
FIG. 2 is a flow chart of a hot isostatic pressing diffusion welding method for a tungsten target according to the present invention.
Detailed Description
The powder layer for hot isostatic pressing diffusion welding of the tungsten target comprises 15-25% of Ti powder, 15-25% of Cu powder and 50-70% of Al powder by mass.
The invention also provides a tungsten target welding assembly which is composed of a tungsten target, the above-mentioned middle powder layer and a copper back plate.
The welding strength of the tungsten target welding assembly is larger than 150Mpa.
The welding rate of the tungsten target welding assembly is more than 99.7%.
The target surface deformation of the tungsten target welding assembly is less than 1mm.
The invention also provides a tungsten target hot isostatic pressing diffusion welding method, which comprises the following steps:
firstly, preparing raw materials including a tungsten target blank, a copper back plate and a sheath;
acid cleaning, namely, carrying out acid cleaning on the tungsten target blank and the copper back plate to remove a surface oxide layer and expose fresh surfaces of the tungsten target blank and the copper back plate;
thirdly, preparing a middle powder layer, weighing Ti powder, cu powder and Al powder in corresponding sheath volumes in proportion, and putting the powder into a powder mixing machine for mixing for 2-5 hours;
fourthly, placing the copper back plate into a sheath, paving the middle powder layer obtained in the third step on the copper back plate, and placing the tungsten target blank on the middle powder layer;
fifthly, sealing welding, namely performing degassing sealing welding on the sample sheath obtained in the fourth step;
sixthly, performing hot isostatic pressing diffusion welding, namely performing hot isostatic pressing diffusion welding on the sheath subjected to degassing sealing welding at the welding temperature of 400-650 ℃, at the welding pressure of 120-160 MPa for 2-6 h to obtain a welding assembly of the tungsten target material-powder intermediate layer-copper back plate;
and seventhly, machining, namely machining the obtained welding assembly of the tungsten target, the intermediate layer and the copper back plate to remove the sheath, and finally obtaining the tungsten target welding assembly.
The following embodiments are described in detail to solve the technical problems by applying technical means to the present invention, and the implementation process of achieving the technical effects can be fully understood and implemented.
Example 1
Preparing required raw materials such as a tungsten target blank, a copper back plate and a sheath;
acid washing: acid washing the tungsten target blank and the copper back plate, removing a surface oxide layer, and exposing fresh surfaces of the tungsten target material and the copper back plate;
weighing intermediate layer powder: weighing Ti powder, cu powder and Al powder with corresponding sheath volumes, wherein the mass percentages of the corresponding powders are respectively 15%, 15% and 70%;
mixing powder: putting the weighed powder into a powder mixing machine for mixing for 4 hours;
placing a welding assembly: placing the prepared copper back plate into a sheath, then laying the mixed powder of Ti-Cu-Al on the copper back plate, and finally placing the tungsten target material on the Ti-Cu-Al powder;
degassing and sealing welding: degassing and sealing the sheath;
diffusion welding: performing hot isostatic pressure diffusion welding on the sheath subjected to degassing sealing welding at the welding temperature of 500 ℃, at the welding pressure of 120MPa for 6h to obtain a welding assembly of the tungsten target material, the intermediate layer and the copper back plate;
and (3) machining: and machining the obtained welding assembly of the tungsten target, the powder intermediate layer and the copper back plate to remove the sheath, and finally obtaining the tungsten target welding assembly.
Example 2 to example 4
The difference from example 1 is that the powder intermediate layer has different composition ratios of Ti, cu and Al, as shown in the following table.
Comparative example 1
Preparing required raw materials such as a tungsten target blank, a copper back plate, a pure Al intermediate layer and the like;
acid washing: acid cleaning is carried out on the tungsten target blank, the copper back plate and the Al intermediate layer, the surface oxide layer is removed, and the fresh surfaces of the tungsten target material and the copper back plate are exposed;
degassing and sealing welding: placing the cleaned tungsten target blank, the cleaned copper back plate and the cleaned Al intermediate layer into a sheath in the order of the tungsten target blank, the cleaned Al intermediate layer and the cleaned Al intermediate layer from top to bottom for degassing and sealing welding;
hot isostatic pressing diffusion welding: placing the tungsten target blank-Al intermediate layer-copper back plate sample subjected to degassing sealing welding into a hot isostatic pressing furnace for hot isostatic pressing diffusion welding at the welding temperature of 500 ℃, the welding pressure of 120MPa and the time of 6 hours to obtain a tungsten target blank-Al intermediate layer-copper back plate assembly subjected to hot isostatic pressing diffusion welding;
and (3) machining: and (4) machining the tungsten target blank-Al intermediate layer-copper back plate assembly to remove the sheath, and finally obtaining the tungsten target material hot isostatic pressing diffusion welding assembly.
Comparative example 2
Preparing required raw materials such as a tungsten target blank, a copper back plate, a Ti intermediate layer and the like;
acid washing: acid washing the tungsten target blank, the copper back plate and the Ti intermediate layer, removing a surface oxide layer, and exposing fresh surfaces of the tungsten target material and the copper back plate;
degassing and sealing welding: placing the cleaned tungsten target blank, the cleaned copper back plate and the cleaned Ti intermediate layer in a sheath in the order of the tungsten target blank, the cleaned Ti intermediate layer and the cleaned Ti intermediate layer from top to bottom for degassing and sealing welding;
hot isostatic pressing diffusion welding: and (3) placing the tungsten target blank-Ti intermediate layer-copper back plate sample subjected to degassing sealing welding into a hot isostatic pressing furnace for hot isostatic pressing diffusion welding, wherein the welding temperature is 500 ℃, the welding pressure is 120MPa, and the time is 6 hours. Obtaining a tungsten target blank-Ti intermediate layer-copper back plate assembly subjected to hot isostatic pressing diffusion welding;
and (3) machining: and (4) machining the tungsten target blank-Ti intermediate layer-copper back plate assembly to remove the sheath, and finally obtaining the tungsten target material hot isostatic pressing diffusion welding assembly.
Comparative example 3
Preparing required raw materials such as a tungsten target blank, a copper back plate, a pure Al intermediate layer and the like;
acid washing: acid cleaning is carried out on the tungsten target blank, the copper back plate and the Al intermediate layer, the surface oxide layer is removed, and the fresh surfaces of the tungsten target material and the copper back plate are exposed;
film coating: and plating a Ti film on the surfaces of the tungsten target blank, the copper back plate and the Al intermediate layer.
Degassing and sealing welding: placing the cleaned tungsten target blank, the cleaned copper back plate and the cleaned Al intermediate layer into a sheath in the order of the tungsten target blank, the cleaned Al intermediate layer and the cleaned Al intermediate layer from top to bottom for degassing and sealing welding;
hot isostatic pressing diffusion welding: placing the tungsten target blank, the Ti-Al intermediate layer and the copper back plate sample subjected to degassing sealing welding into a hot isostatic pressing furnace for hot isostatic pressing diffusion welding at the welding temperature of 500 ℃ under the welding pressure of 120MPa for 6 hours to obtain a tungsten target blank-Al intermediate layer-copper back plate assembly subjected to hot isostatic pressing diffusion welding;
and (3) machining: and machining the tungsten target blank, the Ti-Al intermediate layer and the copper back plate assembly to remove the sheath, and finally obtaining the tungsten target material hot isostatic pressing diffusion welding assembly.
The results are compared and shown in Table 1.
TABLE 1 tungsten target interlayer principal Components and Properties
Figure BDA0002883950820000061
As can be seen from comparison of examples and comparative examples, if only an Al intermediate layer is used, the average weld strength is significantly reduced and the amount of weld deformation of the assembly is higher than that of the assembly formed by the Al, ti, cu powder intermediate layer. If only a Ti intermediate layer is used, the amount of weld distortion of the assembly will be significantly higher than for assemblies formed with intermediate layers of Al, ti, cu powders. The Ti-Al intermediate layer is adopted, the welding strength of the welding assembly is lower than that of the welding assembly formed by the Al, ti and Cu powder intermediate layers, and the welding deformation of the welding assembly is larger than that of the welding assembly formed by the Al, ti and Cu powder intermediate layers.
All of the above mentioned intellectual property rights are not intended to be restrictive to other forms of implementing the new and/or new products. Those skilled in the art will appreciate that this important information can be used to modify the above to achieve similar performance. However, all modifications or alterations are based on the new products of the invention and belong to the reserved rights.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.

Claims (2)

1. A method of hot isostatic pressure diffusion welding, comprising:
firstly, preparing raw materials including a tungsten target blank, a copper back plate and a sheath;
acid cleaning, namely, carrying out acid cleaning on the tungsten target blank and the copper back plate to remove a surface oxide layer and expose fresh surfaces of the tungsten target blank and the copper back plate;
thirdly, preparing a middle powder layer, weighing Ti powder, cu powder and Al powder required by the corresponding middle layer volume in the corresponding sheath volume according to the proportion, and putting the powder into a powder mixing machine for mixing for 2-5 h, wherein the mass ratio of the powder is 15-25% of the Ti powder, 15-25% of the Cu powder and 50-70% of the Al powder;
fourthly, placing the copper back plate into a sheath, paving the middle powder layer obtained in the third step on the copper back plate, and placing the tungsten target blank on the middle powder layer;
fifthly, sealing welding, namely performing degassing sealing welding on the sample sheath obtained in the fourth step;
sixthly, performing hot isostatic pressing diffusion welding, wherein the capsule subjected to degassing sealing welding is subjected to hot isostatic pressing diffusion welding at the welding temperature of 400-650 ℃, the welding pressure of 120-160 MPa and the time of 2-6 hours to obtain a welding assembly of the tungsten target material, the powder intermediate layer and the copper back plate;
and seventhly, machining, namely machining the obtained welding assembly of the tungsten target, the intermediate layer and the copper back plate to remove the sheath, and finally obtaining the tungsten target welding assembly.
2. A tungsten target welded assembly produced by the hot isostatic pressing diffusion welding process of claim 1, wherein: consists of a tungsten target, the middle powder layer as claimed in claim 1 and a copper back plate;
the welding strength of the welding assembly is more than 150Mpa, the welding rate is more than 99.7%, and the surface deformation of the target material is less than 1mm.
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