CN110885963B - Tungsten-nickel alloy target material and preparation method thereof - Google Patents

Tungsten-nickel alloy target material and preparation method thereof Download PDF

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CN110885963B
CN110885963B CN201910955313.5A CN201910955313A CN110885963B CN 110885963 B CN110885963 B CN 110885963B CN 201910955313 A CN201910955313 A CN 201910955313A CN 110885963 B CN110885963 B CN 110885963B
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tungsten
nickel alloy
alloy target
isostatic pressing
treatment
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CN110885963A (en
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刘桂荣
王广达
弓艳飞
杨林
熊宁
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Attl Advanced Materials Co ltd
Advanced Technology and Materials Co Ltd
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Attl Advanced Materials Co ltd
Advanced Technology and Materials Co Ltd
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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
    • C23C14/08—Oxides
    • B22F1/0003—
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B22F3/15—Hot isostatic pressing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C03C17/23—Oxides
    • C03C17/245—Oxides by deposition from the vapour phase
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/04—Alloys based on tungsten or molybdenum
    • 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
    • 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
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • 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
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/21—Oxides
    • C03C2217/23—Mixtures
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/70—Properties of coatings
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/15—Deposition methods from the vapour phase
    • C03C2218/154—Deposition methods from the vapour phase by sputtering

Abstract

The invention discloses a preparation method of a tungsten-nickel alloy target material and the tungsten-nickel alloy target material prepared by the method. The preparation method of the tungsten-nickel alloy target comprises the following steps: the preparation method comprises the following steps: mixing tungsten powder and nickel powder to obtain mixed powder; a press forming step: carrying out compression molding treatment on the mixed powder to obtain a prefabricated blank; sintering: sintering the prefabricated blank to obtain a sintered blank; hot isostatic pressing treatment: carrying out hot isostatic pressing treatment on the sintered blank to obtain a hot isostatic pressing blank; a heat treatment step: and carrying out heat treatment on the hot isostatic pressing blank, and then rapidly cooling to obtain the tungsten-nickel alloy target. The invention adopts the processes of low-temperature sintering and hot isostatic pressing to carry out densification treatment, the compactness of the tungsten-nickel alloy target material reaches more than 99.8 percent and is isotropic, the average particle size of the tungsten phase is less than 30 microns, and the tungsten-nickel alloy target material can be widely applied to the aspect of glass coating.

Description

Tungsten-nickel alloy target material and preparation method thereof
Technical Field
The invention belongs to the technical field of refractory metal material powder metallurgy, and particularly relates to a tungsten-nickel alloy target material and a preparation method thereof.
Background
The electrochromic intelligent glass has adjustability of light absorption and transmission under the action of an electric field, can selectively absorb or reflect external heat radiation and internal heat diffusion, and is a development direction of energy-saving building materials. The electrochromic intelligent glass can regulate the light intensity in the automobile and the airplane with lower voltage and lower power, and is already applied to some high-grade cars and airplanes.
The tungsten-nickel alloy target is already popularized and applied as an electrochromic glass sputtering coating target, a tungsten-nickel alloy oxide layer is generated on the surface of glass by the tungsten-nickel alloy target, oxidation-reduction reaction is carried out under the action of voltage, and the color is changed. The currently applied tungsten-nickel target is manufactured by a thermal spraying process, the density of the sputtering target is only about 90%, and nickel elements in the target are not uniformly distributed, so that the sputtering performance of a product is influenced, and the quality of an electrochromic layer is influenced. The patent CN105849633A adopts powder mixing, forming, sintering and forging treatment processes to prepare the tubular target, the density can reach 99.97%, but the prepared alloy microstructure has certain grain directionality due to the adoption of the forging process.
Disclosure of Invention
Aiming at the defects and defects in the prior art, the invention provides the preparation method of the tungsten-nickel alloy target, which is simple in process and suitable for batch production, and mainly adopts low-temperature sintering and hot isostatic pressing treatment, so that the density of the prepared nickel alloy target reaches over 99.8 percent and is isotropic, and the average particle size of a tungsten phase is less than 30 microns.
The second objective of the present invention is to provide a tungsten-nickel alloy target.
The technical scheme adopted by the invention for solving the technical problem is as follows:
a preparation method of a tungsten-nickel alloy target material comprises the following steps:
the preparation method comprises the following steps: mixing tungsten powder and nickel powder to obtain mixed powder;
a press forming step: carrying out compression molding treatment on the mixed powder to obtain a prefabricated blank;
sintering: sintering the prefabricated blank to obtain a sintered blank;
hot isostatic pressing treatment: carrying out hot isostatic pressing treatment on the sintered blank to obtain a hot isostatic pressing blank;
a heat treatment step: and carrying out heat treatment on the hot isostatic pressing blank, and rapidly cooling to obtain the tungsten-nickel alloy target.
In the above method for preparing a tungsten-nickel alloy target, as a preferred embodiment, the heat treatment step further includes a machining step, so as to obtain a finished tungsten-nickel alloy target.
In the above method for preparing a tungsten-nickel alloy target, as a preferred embodiment, in the raw material preparation step, the tungsten powder accounts for 40 to 86 wt% (e.g., 42%, 45%, 50%, 60%, 70%, 80%, 83%, 85%) of the mixed powder, and the nickel powder accounts for 14 to 60 wt% (e.g., 16%, 20%, 30%, 40%, 50%, 55%, 58%) of the mixed powder.
In the above method for preparing a tungsten-nickel alloy target, as a preferred embodiment, the tungsten powder has a fisher average particle size of 2.0 to 3.0 μm (e.g., 2.2 μm, 2.4 μm, 2.6 μm, 2.8 μm), the nickel powder has a fisher average particle size of 2.3 to 3.5 μm (e.g., 2.5 μm, 2.7 μm, 3 μm, 3.2 μm, 3.4 μm), the mixing time is preferably 8 to 20 hours (e.g., 9 hours, 10 hours, 12 hours, 14 hours, 16 hours, 18 hours, 19 hours), and if the mixing time is too short, the mixing is not uniform; if the mixing time is too long, the phenomenon of uneven mixing is also formed.
In the above method for preparing a tungsten-nickel alloy target, as a preferred embodiment, in the step of press forming, the press forming treatment adopts a cold isostatic pressing process; more preferably, the pressure of the cold isostatic pressing is 150-220 MPa (such as 160MPa, 170MPa, 180MPa, 190MPa, 200MPa, 210MPa), and the time (pressure maintaining time) of the cold isostatic pressing is 12-25 min (such as 14min, 16min, 18min, 20min, 22min, 24 min); further preferably, the preform has a relative density of 55 to 65% (e.g. 56%, 58%, 60%, 62%, 64%); further, the mixed powder is filled into a soft film and is put into a cold isostatic press for the press forming treatment. The cold isostatic pressing can be used for conveniently carrying out sheath sealing of hot isostatic pressing on the blank, is beneficial to production operation, and can also reduce the problems of pollution, oxidation and the like of powder.
In the above method for preparing a tungsten-nickel alloy target, as a preferred embodiment, in the sintering step, the temperature of the sintering treatment is 1300 to 1500 ℃ (for example, 1320 ℃, 1350 ℃, 1380 ℃, 1400 ℃, 1420 ℃, 1450 ℃, 1480 ℃), if the temperature of the sintering treatment is too low, the densification is insufficient, and if the temperature of the sintering treatment is too high, the nickel is melted, thereby affecting the performance of the product; the time (heat preservation time) of the sintering treatment is 1-3 h (such as 1.2h, 1.5h, 2h and 2.5 h); the sintering is carried out under a protective atmosphere, preferably, the protective atmosphere is hydrogen so as to reduce the oxygen content more effectively than other atmospheres or vacuum; preferably, the relative density of the sintered compact is 95% or more.
If the hot isostatic pressing is directly carried out on the raw material powder without carrying out cold isostatic pressing and sintering, the blank has irregular appearance and possibly causes uneven density.
In the above method for preparing a tungsten-nickel alloy target, as a preferred embodiment, in the hot isostatic pressing step, the hot isostatic pressing temperature is 1000 to 1250 ℃ (such as 1010 ℃, 1020 ℃, 1050 ℃, 1080 ℃, 1120 ℃, 1150 ℃, 1200 ℃, 1220 ℃, 1240 ℃) and the pressure is 80 to 150MPa (such as 85MPa, 90MPa, 100MPa, 1150MPa, 120MPa, 130MPa, 140MPa, 145MPa), and the holding time is 1 to 4 hours (such as 1.2 hours, 1.5 hours, 2 hours, 2.5 hours, 3 hours, 3.5 hours); more preferably, the hot isostatic pressing treatment temperature is 1100-1250 ℃ (such as 1120 ℃, 1150 ℃, 1180 ℃, 1220 ℃, 1230 ℃ and 1245 ℃), and if the hot isostatic pressing treatment temperature is too low, the density is improved, and if the hot isostatic pressing treatment temperature is too high, the material grain distortion energy is too large, and the mechanical property is reduced.
In the above method for preparing a tungsten-nickel alloy target, as a preferred embodiment, in the heat treatment step, the temperature of the heat treatment is 900-; preferably, the heat treatment is performed in a vacuum quenching furnace, and more preferably, the vacuum degree in the vacuum quenching furnace is 10-1～10-3Pa, and further preferably, the vacuum degree in the vacuum quenching furnace is 10-2Pa。
In the above method for preparing a tungsten-nickel alloy target, as a preferred embodiment, in the heat treatment step, the rapid cooling rate is 3 to 7 ℃/s (e.g., 4 ℃/s, 5 ℃/s, 6 ℃/s).
A tungsten-nickel alloy target material prepared by the method.
In the tungsten-nickel alloy target material, as a preferred embodiment, the tungsten-nickel alloy target material comprises 40-86% of tungsten, 14-60% of nickel and inevitable impurities in percentage by weight; preferably, the compactness of the tungsten-nickel alloy target material reaches more than 99.8 percent and is isotropic.
Compared with the prior art, the invention has the following positive effects:
(1) the raw materials of the invention are produced by using the conventional tungsten powder and nickel powder sold in the market, are easy to purchase, do not need special powder treatment, and reduce the workload.
(2) The preparation method is a powder metallurgy process, and is simple and easy to operate.
(3) The method adopts the processes of low-temperature sintering and hot isostatic pressing for densification, the compactness of the tungsten-nickel alloy target material reaches more than 99.8 percent and is isotropic, the average particle size of a tungsten phase is less than 30 micrometers, and the tungsten-nickel alloy target material can be widely applied to the aspect of glass coating.
(4) The preparation method provided by the invention has the advantages that the steps are mutually matched, particularly, the tungsten-nickel alloy target material with high density, isotropy and stable performance is prepared by adopting the processes of low-temperature sintering, hot isostatic pressing and rapid cooling after heat treatment, the yield is high and can reach more than 97%, and the method is favorable for industrial production.
Drawings
For a more clear description of the invention, reference is made herein to the accompanying drawings, which form a further part hereof. Wherein:
fig. 1 is a microstructure diagram of a tungsten-nickel alloy target material obtained in example 3 of the present application.
Detailed Description
In order to highlight the objects, technical solutions and advantages of the present invention, the present invention is further illustrated by the following examples, which are presented by way of illustration of the present invention and are not intended to limit the present invention. The technical solution of the present invention is not limited to the specific embodiments listed below, and includes any combination of the specific embodiments.
Example 1
(1) Preparing raw materials: mixing tungsten powder with the granularity of 2.0 mu m and the weight percentage of 40 percent and nickel powder with the granularity of 2.3 mu m and the weight percentage of 60 percent in a mixer for 8 hours to obtain mixed powder for later use after uniform mixing;
(2) cold isostatic pressing: putting the mixed powder into a soft plastic film, putting the soft plastic film into a cold isostatic press for press forming, wherein the isostatic pressure is 150MPa, the pressure maintaining time is 12 minutes, and the mixed powder is subjected to isostatic press forming to obtain a preformed blank with the relative density of 55 percent;
(3) and (3) sintering: sintering the prefabricated blank in a hydrogen protective atmosphere at 1300 ℃ for 1 hour to obtain a sintered blank;
(4) hot isostatic pressing treatment: carrying out hot isostatic pressing treatment on the sintered blank in an argon atmosphere at the temperature of 1000 ℃, the pressure of 80MPa and the heat preservation time of 1 hour to obtain a hot isostatic pressing blank;
(5) and (3) heat treatment: putting the hot isostatic pressing blank into a vacuum quenching furnace for heat treatment, wherein the heat treatment temperature is 1100 ℃, keeping the temperature for 1 hour, and rapidly cooling at the speed of 5 ℃/s to obtain a final tungsten-nickel alloy blank;
(6) and machining the tungsten-nickel alloy blank to obtain the final tungsten-nickel alloy target.
The density of the tungsten-nickel alloy target finally obtained in the embodiment is tested to be 11.34g/cm by adopting a drainage method3The compactness is 99.9%, the tungsten-nickel alloy target material prepared by the embodiment is isotropic, and the average particle size of tungsten phase observed by microstructure is 25 μm.
Example 2
(1) Preparing raw materials: mixing 86 wt% of tungsten powder with the granularity of 3.0 mu m and 14 wt% of nickel powder with the granularity of 3.5 mu m in a mixer for 20 hours, and uniformly mixing to obtain mixed powder for later use;
(2) cold isostatic pressing: putting the mixed powder into a soft plastic film, putting the soft plastic film into a cold isostatic press for press forming, wherein the isostatic pressure is 220MPa, the pressure maintaining time is 25 minutes, and the mixed powder is subjected to isostatic press forming to obtain a preformed blank with the relative density of 65%;
(3) and (3) sintering: sintering the prefabricated blank in a hydrogen protective atmosphere at 1500 ℃ for 3 hours to obtain a sintered blank;
(4) hot isostatic pressing treatment: carrying out hot isostatic pressing treatment on the sintered blank in an argon atmosphere at 1250 ℃, under 150MPa and for 4 hours to obtain a hot isostatic pressing blank;
(5) and (3) heat treatment: putting the hot isostatic pressing blank into a vacuum quenching furnace for heat treatment, wherein the heat treatment temperature is 1100 ℃, keeping the temperature for 3 hours, and rapidly cooling at the speed of 6 ℃/s to obtain a final tungsten-nickel alloy blank;
(6) and machining the tungsten-nickel alloy blank to obtain the final tungsten-nickel alloy target.
The density of the tungsten-nickel alloy target finally obtained in the embodiment is tested to be 16.57g/cm by adopting a drainage method3The compactness is 99.9%, the tungsten nickel alloy target material prepared in the embodiment is isotropic, and the average particle size of tungsten phase observed in microstructure is 28 μm.
Example 3
(1) Preparing raw materials: tungsten powder with the granularity of 2.5 mu m and the weight percentage of 76.5 percent and nickel powder with the granularity of 3.0 mu m and the weight percentage of 23.5 percent are mixed in a mixer for 15 hours, and mixed powder is obtained for standby after uniform mixing;
(2) cold isostatic pressing: putting the mixed powder into a soft plastic film, putting the soft plastic film into a cold isostatic press for press forming, wherein the isostatic pressure is 200MPa, the pressure maintaining time is 20 minutes, and the mixed powder is subjected to isostatic press forming to obtain a preformed blank with the relative density of 60%;
(3) and (3) sintering: sintering the prefabricated blank in a hydrogen protective atmosphere at 1400 ℃ for 2 hours to obtain a sintered blank;
(4) hot isostatic pressing treatment: carrying out hot isostatic pressing treatment on the sintered blank in an argon atmosphere at the temperature of 1100 ℃, the pressure of 130MPa and the heat preservation time of 2 hours to obtain a hot isostatic pressing blank;
(5) and (3) heat treatment: putting the hot isostatic pressing blank into a vacuum quenching furnace for heat treatment, wherein the heat treatment temperature is 1100 ℃, keeping the temperature for 2 hours, and rapidly cooling at the speed of 7 ℃/s to obtain the final tungsten-nickel alloy blank;
(6) and machining the tungsten-nickel alloy blank to obtain the final tungsten-nickel alloy target.
The density of the tungsten-nickel alloy target finally obtained in the embodiment is tested to be 15.14g/cm by adopting a drainage method3The density is 100%; referring to fig. 1, the microstructure of the tungsten-nickel alloy target prepared in this example is shown to be isotropic in fig. 1, and the average grain size of tungsten phase observed in the microstructure is 26 μm.
Example 4
(1) Preparing raw materials: mixing tungsten powder with the granularity of 2.6 mu m and the weight percentage of 70 percent and nickel powder with the granularity of 3 mu m and the weight percentage of 30 percent in a mixer for 18 hours, and uniformly mixing to obtain mixed powder for later use;
(2) cold isostatic pressing: putting the mixed powder into a soft plastic film, putting the soft plastic film into a cold isostatic press for press forming, wherein the isostatic pressure is 180MPa, the pressure maintaining time is 16 minutes, and the mixed powder is subjected to isostatic press forming to obtain a preformed blank with the relative density of 58%;
(3) and (3) sintering: sintering the prefabricated blank in a hydrogen protective atmosphere at the sintering temperature of 1350 ℃ for 1.5 hours to obtain a sintered blank;
(4) hot isostatic pressing treatment: carrying out hot isostatic pressing treatment on the sintered blank in an argon atmosphere at the temperature of 1150 ℃, the pressure of 120MPa and the heat preservation time of 1.5 hours to obtain a hot isostatic pressing blank;
(5) and (3) heat treatment: putting the hot isostatic pressing blank into a vacuum quenching furnace for heat treatment, wherein the heat treatment temperature is 1100 ℃, keeping the temperature for 1.5 hours, and rapidly cooling at the speed of 6 ℃/s to obtain a final tungsten-nickel alloy blank;
(6) and machining the tungsten-nickel alloy blank to obtain the final tungsten-nickel alloy target.
The density of the tungsten-nickel alloy target finally obtained in the embodiment is tested to be 14.27g/cm by adopting a drainage method3The density is 99.9%; the tungsten-nickel alloy target material prepared by the embodiment is isotropic, and the average particle size of tungsten phase is 25 μm when microstructure observation is carried out.
Examples 5 to 8
Examples 5 to 8 the same procedures as in example 4 were carried out except that the particle sizes of the raw materials tungsten powder and nickel powder used in step (1) were different from those of example 4. See table 1 for details.
TABLE 1 particle size and target Properties of the raw powders in examples 5-8
Figure BDA0002227088910000071
Examples 9 to 11
Examples 9 to 11 were the same as example 4 except that the hot isostatic pressing process conditions in step (4) were different from those in example 4. See table 2 for details.
TABLE 2 parameters of HIP's and target Properties in examples 9-10
Figure BDA0002227088910000072
Examples 12 to 13
Examples 12 to 13 were the same as example 4 except that the rapid cooling rate in step (5) was different from that in example 4. See table 3 for details.
TABLE 3 fast cooling rates and target Properties after Heat treatment in examples 12-13
Fast cooling rate Density of target material Compactness of target material Average grain size of tungsten phase of target material
Example 12 1℃/s 14.12g/cm3 98.8％ 46μm
Example 13 10℃/s 14.15g/cm3 99％ 32μm
According to the embodiment, the tungsten powder and the nickel powder are uniformly mixed through a material mixing process, then the mixture is sintered at a low temperature in a hydrogen atmosphere, the density of the alloy reaches over 95 percent, and then the densification treatment is performed through a hot isostatic pressing process, so that the density of the alloy can reach over 99.8 percent, nearly reach the theoretical density and is isotropic. The preparation method of the tungsten-nickel alloy target material is simple in production process, high in yield and beneficial to industrial production.

Claims (12)

1. A preparation method of a tungsten-nickel alloy target is characterized by comprising the following steps:
the preparation method comprises the following steps: mixing tungsten powder and nickel powder to obtain mixed powder;
a press forming step: carrying out compression molding treatment on the mixed powder to obtain a prefabricated blank;
sintering: sintering the prefabricated blank to obtain a sintered blank;
hot isostatic pressing treatment: carrying out hot isostatic pressing treatment on the sintered blank to obtain a hot isostatic pressing blank;
a heat treatment step: carrying out heat treatment on the hot isostatic pressing blank, and then rapidly cooling to obtain a tungsten-nickel alloy target material;
in the raw material preparation step, the tungsten powder accounts for 40-86 wt% of the mixed powder, and the nickel powder accounts for 14-60 wt% of the mixed powder; the Fisher average particle size of the tungsten powder is 2.0-3.0 mu m, the Fisher average particle size of the nickel powder is 2.3-3.5 mu m, and the mixing treatment time is 8-20 h;
in the sintering step, the temperature of the sintering treatment is 1300-1420 ℃, the time of the sintering treatment is 1-3 h, and the sintering treatment is carried out in a protective atmosphere; the relative density of the sintered blank is more than 95%;
in the hot isostatic pressing step, the hot isostatic pressing temperature is 1000-1250 ℃, the pressure is 80-150 MPa, and the heat preservation time is 1-4 h;
in the heat treatment step, the temperature of the heat treatment is 900-1300 ℃, and the time is 1-3 h;
in the heat treatment step, the rapid cooling rate is 3-7 ℃/s.
2. The method for preparing a tungsten-nickel alloy target according to claim 1, wherein after the heat treatment step, the method further comprises a machining step, and a finished tungsten-nickel alloy target is obtained through the machining step.
3. The method for preparing a tungsten-nickel alloy target according to claim 1, wherein in the step of press forming, the press forming is performed by a cold isostatic pressing process.
4. The preparation method of the tungsten-nickel alloy target according to claim 3, wherein the pressure of the cold isostatic pressing is 150-220 MPa, and the time of the cold isostatic pressing is 12-25 min.
5. The method for preparing the tungsten-nickel alloy target material according to claim 1, wherein the mixed powder is filled in a soft rubber film and is placed in a cold isostatic press for the press forming treatment.
6. The method for preparing a tungsten-nickel alloy target according to claim 5, wherein the relative density of the preform is 55-65%.
7. The method for preparing a tungsten-nickel alloy target according to any one of claims 1 to 3, wherein the protective atmosphere is hydrogen in the sintering step.
8. The method for preparing the tungsten-nickel alloy target material according to claim 1, wherein the hot isostatic pressing treatment temperature is 1100-1250 ℃.
9. The method for producing a tungsten-nickel alloy target according to any one of claims 1 to 3, wherein in the heat treatment step, the heat treatment is performed in a vacuum quenching furnace having a vacuum degree of 10-1~10- 3Pa。
10. A tungsten-nickel alloy target material prepared by the method of any one of claims 1-9.
11. The tungsten-nickel alloy target according to claim 10, comprising, by weight, 40 to 86% of tungsten, 14 to 60% of nickel, and inevitable impurities.
12. The tungsten-nickel alloy target according to claim 11, wherein the compactness of the tungsten-nickel alloy target is more than 99.8%.
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CN113549881A (en) * 2021-05-31 2021-10-26 洛阳科威钨钼有限公司 Preparation method of tungsten-nickel alloy target material
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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6010583A (en) * 1997-09-09 2000-01-04 Sony Corporation Method of making unreacted metal/aluminum sputter target
CN101360844A (en) * 2006-02-06 2009-02-04 三井金属矿业株式会社 Sputtering target, sputtering target material and process for producing these
CN101514413A (en) * 2009-04-03 2009-08-26 西北有色金属研究院 Preparing method of nickel tungsten base band used for coated conductor
CN102329973A (en) * 2011-09-21 2012-01-25 西安理工大学 Preparation method for Ni-W alloy by using smelting method
WO2013003065A2 (en) * 2011-06-30 2013-01-03 Soladigm, Inc. Sputter target and sputtering methods
CN105849633A (en) * 2013-12-20 2016-08-10 攀时奥地利公司 W-Ni sputter target
CN106119790A (en) * 2016-08-12 2016-11-16 苏州思创源博电子科技有限公司 A kind of tungsten nickel target processing method
CN106119788A (en) * 2016-08-12 2016-11-16 苏州思创源博电子科技有限公司 A kind of modified tungsten nickel target prepares work method

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4954816B2 (en) * 2007-07-18 2012-06-20 山陽特殊製鋼株式会社 Manufacturing method of sputtering target material for Ni-W type intermediate layer

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6010583A (en) * 1997-09-09 2000-01-04 Sony Corporation Method of making unreacted metal/aluminum sputter target
CN101360844A (en) * 2006-02-06 2009-02-04 三井金属矿业株式会社 Sputtering target, sputtering target material and process for producing these
CN101514413A (en) * 2009-04-03 2009-08-26 西北有色金属研究院 Preparing method of nickel tungsten base band used for coated conductor
WO2013003065A2 (en) * 2011-06-30 2013-01-03 Soladigm, Inc. Sputter target and sputtering methods
CN102329973A (en) * 2011-09-21 2012-01-25 西安理工大学 Preparation method for Ni-W alloy by using smelting method
CN105849633A (en) * 2013-12-20 2016-08-10 攀时奥地利公司 W-Ni sputter target
CN106119790A (en) * 2016-08-12 2016-11-16 苏州思创源博电子科技有限公司 A kind of tungsten nickel target processing method
CN106119788A (en) * 2016-08-12 2016-11-16 苏州思创源博电子科技有限公司 A kind of modified tungsten nickel target prepares work method

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