CN105345007B - A kind of preparation method of high dense chrome tungsten alloy target material - Google Patents

A kind of preparation method of high dense chrome tungsten alloy target material Download PDF

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CN105345007B
CN105345007B CN201410404503.5A CN201410404503A CN105345007B CN 105345007 B CN105345007 B CN 105345007B CN 201410404503 A CN201410404503 A CN 201410404503A CN 105345007 B CN105345007 B CN 105345007B
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powder
chromium
alloy target
target material
tungsten
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CN105345007A (en
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张凤戈
姚伟
姜海
张路长
唐培新
何向晖
郝权
赵雷
孙继洲
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Advanced Technology and Materials Co Ltd
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Abstract

The invention belongs to technical field of powder metallurgy material preparation, there is provided a kind of preparation method of high dense chrome tungsten alloy target material.The chromium tungsten alloy target material includes the composition of following atomic percent:Chromium 80~99%, tungsten 1~20%.The preparation method of the chromium tungsten alloy target material is:After tungsten powder is reduced, and chromium powder is prepared by pre-alloyed powder, fills the processing such as jacket, degassing, high temperature insostatic pressing (HIP), machining, obtains the chromium tungsten alloy target material.The chromium tungsten alloy target material density of the present invention high (relative density is not less than 99%), even tissue, crystal grain are tiny (being not more than 50 μm);The plated film fields such as electrode contact material can be used for by the target, preparing has high rigidity, high dieletric strength, low value of damming, the thin-film material of alternative pure tungsten.

Description

A kind of preparation method of high dense chrome tungsten alloy target material
Technical field
The invention belongs to technical field of powder metallurgy material preparation, more particularly to a kind of system of high dense chrome tungsten alloy target material Preparation Method.
Background technology
With continuing to develop for material science, the structure of material is developed into two-dimensional directional gives full play to the offer of material potential A kind of important channel.Membrane science is exploitation new material and the very important field of new device.High-tech Material from body material to Film is shifted, so that plating membrane module is developed rapidly.
Target is the critical material in surface coating technology, and the quality of target performance directly affects the quality of film performance, And the performance of target is mainly determined by target production technology.Current target production method mainly has smelting process and powder metallurgic method. Smelting technology can produce most metal targets, but a small number of targets are because alloying component fusing point gap is too big, the strict control of target requirement The factors such as combinations particle size and can only using powder metallurgical technique prepare.
Hot isostatic pressing technique is to utilize high temperature and high pressure, makes a kind of technique of densifying materials in a sealed container. Because the technology is, using high-pressure inert gas as working media, uniformly to be pressed in workpiece surface, phase is produced to workpiece arbitrary surfaces Same effect, can improve material internal density uniformity.Due to preparing the superiority on material, high temperature insostatic pressing (HIP) is widely used in disappearing Except casting defect, the process such as powder metallurgy densification.
The fusing point of chromium is 1860 DEG C, and the fusing point of tungsten is 3407 DEG C, because chromium, two kinds of melting point metal temperature differences of tungsten are huge, Under the conditions of conventional equipment, preparing chromium tungsten alloy using the method for conventional metallurgical can not realize.The method of ordinary sinter can To prepare chromium tungsten alloy, but the porosity of material is too high, and relative density is unable to reach the use requirement of target.
At present, the main production that CrW targets are carried out using hot pressed sintering both at home and abroad;But it is due to be limited hardly possible by production technology With the big target product of obtained dense structure, dimensions.
The content of the invention
Good it is an object of the invention to provide a kind of compactness, no internal flaw, even tissue, crystal grain is tiny, specification chi Very little big chromium tungsten alloy target material and preparation method thereof.
The purpose of the present invention is achieved through the following technical solutions:
A kind of chromium tungsten alloy target material, includes the composition of following atomic percent:Chromium 80~99%, tungsten 1~20%.
Further, the chromium tungsten alloy target material includes the composition of following atomic percent:Chromium 90%, tungsten 10%.
Further, the relative density of the alloy target material is not less than 99%, and average grain size is not more than 50 μm.
The purpose of the present invention is realized by following another technical scheme:
The preparation method of the chromium tungsten alloy target material, comprises the following steps:
Step one, tungsten powder is subjected to reduction treatment, the tungsten powder after being reduced;
Step 2, pre-alloyed powder is prepared by the tungsten powder and chromium powder after the reduction;
Step 3, dress jacket processing, the jacket filled are carried out by the prealloy powder powder stock;
Step 4, is de-gassed processing, the jacket after being deaerated by the jacket filled;
Step 5, carries out hip treatment, the ingot blank after being suppressed, then remove jacket to the jacket after the degassing Blank after being suppressed;
Step 6, processing is machined out by the blank after the compacting, obtains the chromium tungsten alloy target material.
Further, in the step 2, the pre-alloyed powder is that the tungsten powder after the reduction is ground with chromium powder Powder processing is obtained;Preferably, the milling processing is using the processing of high-energy ball milling powder.
Further, the high-energy ball milling powder processing processing, refers under the conditions of inert gas shielding in high-energy ball milling 4-24h is mixed in machine.
Further, the average grain diameter of the pre-alloyed powder is not more than 50 μm.
Further, in the step one, the reduction treatment is to be passed through hydrogen at 850~950 DEG C.
Further, in the step 4, the temperature of the degassing process is 300~500 DEG C, and the time is 5~30h; Preferably, the vacuum degree control during degassing process is 10-1Pa~10-4Pa。
Further, in the step 5, the holding temperature of the hip treatment is 1250~1450 DEG C, insulation Time is 2~5h, and pressure is 120~150MPa.
Compared to prior art, the present invention has the advantages that:
1st, by the present invention in that the CrW alloy target materials provided with heat and other static pressuring processes have consistency height, (relative density is not Less than 99%), pore-free, the internal flaw such as loose and segregation, even tissue, crystal grain is tiny, and (mean grain size is average crystal grain Size is not more than 50 μm) the advantages of.
2nd, target of the invention using high-energy-milling due to producing pre-alloyed powder, it is possible to is made well mixed CrW pre-alloyed powders, and due to the advantage of heat and other static pressuring processes itself, by the control to raw material quality, can be made Impurity content is low, and target purity is high, consistency is high, crystal grain is tiny, the uniform target material base of microscopic structure.
3rd, because the present invention uses heat and other static pressuring processes, target size is only limited by hot isostatic apparatus operating room size System, it is possible to realize that target size maximizes, target full-size can accomplish 1701mm.
4th, CrW targets prepared by the present invention, available for plated film fields such as electrode contact materials, preparing has high rigidity, height Dieletric strength, low value of damming, the thin-film material of alternative pure tungsten.
Brief description of the drawings
Fig. 1 is the micro-organization chart for the target that the embodiment of the present invention 3 is obtained.
Embodiment
The present invention provides a kind of high dense chrome tungsten alloy target material, and the atomic percent for the composition that the alloy target material is included is: The content (at%) of tungsten (W) is 0<W≤20%, the content (at%) of chromium (Cr) is 80≤Cr<100%, such as the atomic percent of W Content can be 1%, 2%, 2.5%, 3.2%, 4.1%, 4.9%, 5%, 5.2%, 8%, 11%, 14%, 17%, 19% Deng preferred chromium is 90%, and tungsten is 10%.
Wherein, the present invention uses purity to be 99.5%-99.99%'s for 99.9%-99.999% tungsten (W) powder and purity Chromium (Cr) powder, mechanical mixture prepares pre-alloyed powder, pre-alloyed powder is packed into metal capsule, through taking out in a heated condition The processes such as vacuum outgas, hip treatment, machining, obtain consistency high (relative density is not less than 99%), microscopic structure Uniformly, grain size (average grain size) is not more than 50 μm of high-quality CrW targets.The W powder purities for preparing CrW targets can be Between 99.9%~99.999%, used after being reduced through high-purity hydrogen.
According to above-mentioned purpose, the overall technical scheme of the present invention is:Pre-alloyed powder is produced using ball-milling technology, by gained Pre-alloyed powder loads jacket, and degassed rear hip treatment obtains qualified chromium tungsten alloy target material.
The specific steps to the present invention are described in detail below.
The first step, powder reduction step:Tungsten powder is subjected to reduction treatment, the tungsten powder after being reduced;
Specifically, be by particle diameter be 2~10 μm, the tungsten powder that purity is 99.9%~99.999%% be passed through hydrogen also Original, in 850~950 DEG C (such as can be 850 DEG C, 900 DEG C, 930 DEG C, 950 DEG C etc.) be incubated 1~10h (such as can be 2h, 4h, 6h, 8h etc.), reduce O content in W powder raw materials.
Second step, powder preparation step:Tungsten powder and chromium powder after the reduction is handled by milling, pre- conjunction is prepared Bronze end;
Specifically, chromium powder and reduction that average particle diameter size is 99.5%~99.99% for 10~45 μm, purity are used Tungsten powder afterwards, is positioned in milling equipment after being weighed according to the weight ratio corresponding to above-mentioned atomic percent, carries out milling processing 4 ~24h, for example can be exemplarily 4.5h, 6h, 9h, 11h, 15h, 18h, 20h, 22h.Milling processing can use high energy Ball-milling treatment, planetary ball mill processing etc.;Preferably high-energy ball milling powder is handled, and is referred under the conditions of inert gas shielding in high energy 4~24h is mixed in ball mill.The ratio of grinding media to material (mass ratio) that is related to is in milling processing:10:1~50:1, such as can be 10:1、20:1、30:1、40:1、50:1, mill ball used is generally sintered carbide ball.
3rd step, fills jacket step:The pre-alloyed powder that second step is prepared is fitted into metal capsule, is filled Jacket;
Specifically, can be stainless steel capsule or the jacket of other metal materials as metal capsule, than Such as low carbon steel plate jacket, titanium plate jacket.
4th step, de-airing step:The jacket filled is de-gassed processing using degasification furnace, the jacket after being deaerated;
Specifically, the jacket filled for completing dress powder is placed in degasification furnace and is de-gassed processing, degasification furnace selection city Vacuum degassing furnace or well formula resistance degasification furnace are sold, degassing temperature is generally 300~500 DEG C, 5~30h of degassing time.It is exemplary Ground, the degassing temperature can be 310 DEG C, 325 DEG C, 345 DEG C, 375 DEG C, 390 DEG C, 420 DEG C, 450 DEG C, 480 DEG C, 495 DEG C;Institute It can be 5h, 9h, 15h, 20h, 22.5h, 25h, 28h to state degassing time.
It is highly preferred that certain vacuum degree control is carried out during the degassing process, such as can be by vacuum degree control 10- 1Pa~10-4Pa, exemplarily, vacuum can be 10-1Pa、10-2Pa、10-3Pa、10-4Pa。
5th step, high temperature insostatic pressing (HIP) step:Hip treatment is carried out to the jacket after degassing using hot isostatic apparatus, obtained Ingot blank after to compacting, then remove the blank after jacket is suppressed;
Specifically, it is exactly after the jacket soldering and sealing by degassing, to be put into hot isostatic apparatus and be sintered;Sintering process In, holding temperature is 1250~1450 DEG C, and sintering time is 2~5h, and pressure during sintering is 120~150MPa;Exemplarily, The holding temperature can be 1255 DEG C, 1285 DEG C, 1315 DEG C, 1350 DEG C, 1380 DEG C, 1420 DEG C, 1445 DEG C;During the sintering Between can be 2h, 3.5h, 4.0h, 4.5h;The sintering pressure can for 125MPa, 135MPa, 140MPa, 145MPa, 148MPa、150MPa.After sintering, the powder densification in jacket after degassing process, the ingot blank formed after compacting;Remove again Metal capsule is stated, the blank after being suppressed.
6th step, machining steps:Blank after the compacting that is obtained in high temperature insostatic pressing (HIP) step is machined out according to drawing, Required finished product target is obtained after cleaning.
It is only to the exemplary of the present invention that the parameter in the present invention, embodiment is further described below by way of example Illustrate, the invention is not restricted to being specifically defined for these embodiments.
Embodiment 1
In the present embodiment, chromium tungsten alloy target material includes the composition of following atomic percent:Chromium 80%, tungsten 20%;
The preparation method of this example chromium tungsten alloy target material, comprises the following steps:
Powder reduction step:Tungsten powder (8 μm of average grain diameter, purity:99.99%;O content is 500~700ppm) at 850 DEG C At a temperature of be passed through hydrogen, be incubated 5 hours, carry out deoxidation treatment, it is tungsten powder after≤200ppm deoxidation that O content, which is made, that is, is reduced Tungsten powder afterwards;
Powder preparation step:Weight ratio as corresponding to above-mentioned atomic percent weighs tungsten powder and average grain diameter 45 after deoxidation μm 99.95% purity chromium powder, well mixed pre-alloyed powder is produced using high-energy-milling;Ratio of grinding media to material is 20:1, Mill ball is sintered carbide ball, and milling time is 4 hours;The average grain diameter of gained pre-alloyed powder is 30~35 μm;
Fill jacket step:The pre-alloyed powder mixed is fitted into the suitable stainless steel capsule of size;
De-airing step:The stainless steel capsule filled is placed in degasification furnace, 500 DEG C of heating-up temperature, soaking time 20h, Devolatilization vacuum degree is controlled 10-3Pa~10-4Pa;
High temperature insostatic pressing (HIP) step:It is put into hot isostatic apparatus and sinters after the jacket soldering and sealing that degassing is finished, holding temperature is 1450 DEG C, time 5h, pressure 120MPa;The blank after jacket is suppressed is removed again;
Machining steps:Blank after compacting is machined out according to drawing, required finished product target is obtained after cleaning Material.
The target relative density that this example is obtained reaches 99%, average grain size≤40 μm.
Embodiment 2
Chromium tungsten alloy target material includes the composition of following atomic percent:Chromium 90%, tungsten 10%.
The preparation method of this example chromium tungsten target material, comprises the following steps:
Powder reduction step:Tungsten powder (6 μm of average grain diameter, purity:99.999%;O content is≤200ppm) in 850 DEG C of temperature Hydrogen is passed through under degree, 3 hours are incubated, deoxidation treatment is carried out and O content is made for tungsten powder after 70ppm deoxidation, that is, the tungsten after reducing Powder;
Powder preparation step:Weight as corresponding to above-mentioned atomic percent than weigh average grain diameter 35 μm chromium powder, It is put into the tungsten powder (tungsten powder after deoxidation) after reduction in high energy ball mill and mixes 12h, high purity inert gas is passed through in mixed process Protected, ratio of grinding media to material is 30:1, ball material is hard alloy, obtains pre-alloyed powder;The average grain of gained pre-alloyed powder Footpath is 25~30 μm;
Fill jacket step:The pre-alloyed powder mixed is fitted into the suitable metal capsule of size, mild steel can be used Plate jacket or titanium plate jacket;
De-airing step:The jacket filled is placed in degasification furnace, 400 DEG C of heating-up temperature, soaking time 30h;
High temperature insostatic pressing (HIP) step:It is put into hot isostatic apparatus and sinters after the jacket soldering and sealing that degassing is finished, holding temperature is 1350 DEG C, time 3h, pressure 150MPa;The blank after jacket is suppressed is removed again;
Machining steps:Blank after compacting is machined out according to drawing, required finished product target is obtained after cleaning Material.
The target relative density that this example is obtained reaches 99.2%, average grain size≤35 μm.
Embodiment 3
In the present embodiment, chromium tungsten alloy target material includes the composition of following atomic percent:Chromium 95.2%, tungsten 4.8%.
The preparation method of this example chromium tungsten target material, comprises the following steps:
Powder reduction step:Tungsten powder (10 μm of average grain diameter, purity:99.9%;O content is 1000ppm) in 950 DEG C of temperature Under be passed through hydrogen, be incubated 1 hour, it is tungsten powder, that is, the tungsten after reducing after≤300ppm deoxidation to carry out deoxidation treatment and O content is made Powder;
Powder preparation step:Weight as corresponding to above-mentioned atomic percent than weigh average grain diameter 45 μm chromium powder and Tungsten powder, which is put into high energy ball mill, after deoxidation mixes 24h, is vacuumized in mixed process and is filled with high purity inert gas and is protected, Ratio of grinding media to material is 40:1, ball material is hard alloy, obtains pre-alloyed powder;The average grain diameter of gained pre-alloyed powder is 40~45 μm;
Fill jacket step:The pre-alloyed powder mixed is fitted into the suitable metal capsule of size, mild steel can be used Plate jacket or titanium plate jacket;
De-airing step:The jacket filled is placed in degasification furnace, 300 DEG C of heating-up temperature, soaking time 20h, at degassing Certain vacuum degree control is carried out during reason, by vacuum degree control 10-1Pa~10-2Pa;
High temperature insostatic pressing (HIP) step:It is put into hot isostatic apparatus and sinters after the jacket soldering and sealing that degassing is finished, holding temperature is 1250 DEG C, time 4h, pressure 135MPa;The blank after jacket is suppressed is removed again;
Machining steps:Blank after compacting is machined out according to drawing, required finished product target is obtained after cleaning Material.
The target relative density that this example is obtained reaches 99.5%, average grain size≤50 μm.
As shown in figure 1, the obtained target consistency of the present embodiment is high, crystal grain is tiny, microscopic structure is uniform.
Embodiment 4
In the present embodiment, chromium tungsten alloy target material includes the composition of following atomic percent:Chromium 96.8%, tungsten 2.2%.This reality The preparation method of example chromium tungsten target material, comprises the following steps:
Powder reduction step:Tungsten powder (3 μm of average grain diameter, purity:99.99%;O content is 600~900ppm) at 950 DEG C At a temperature of be passed through hydrogen, be incubated 1 hour, it is tungsten powder after≤250ppm deoxidation to carry out deoxidation treatment and O content is made, that is, after reducing Tungsten powder;
Powder preparation step:Weight as corresponding to above-mentioned atomic percent than weigh average grain diameter 25 μm chromium powder and Tungsten powder, which is put into high energy ball mill, after deoxidation mixes 20h, is vacuumized in mixed process and is filled with high purity inert gas and is protected, Ratio of grinding media to material is 35:1, ball material is hard alloy, obtains pre-alloyed powder;The average grain diameter of gained pre-alloyed powder is 20~25 μm;
Fill jacket step:The pre-alloyed powder mixed is fitted into the suitable metal capsule of size, mild steel can be used Plate jacket or titanium plate jacket;
De-airing step:The jacket filled is placed in degasification furnace, 370 DEG C of heating-up temperature, soaking time 16h, at degassing Certain vacuum degree control is carried out during reason, by vacuum degree control 10-2Pa~10-3Pa;
High temperature insostatic pressing (HIP) step:It is put into hot isostatic apparatus and sinters after the jacket soldering and sealing that degassing is finished, holding temperature is 1280 DEG C, time 3.5h, pressure 145MPa;The blank after jacket is suppressed is removed again;
Machining steps:Blank after compacting is machined out according to drawing, required finished product target is obtained after cleaning Material.
The target relative density that this example is obtained reaches 99.6%, average grain size≤35 μm.
Embodiment 5
In the present embodiment, chromium tungsten alloy target material includes the composition of following atomic percent:Chromium 83%, tungsten 17%.
The preparation method of this example chromium tungsten target material, comprises the following steps:
Powder reduction step:Tungsten powder (5 μm of average grain diameter, purity:99.999%;O content is≤300ppm) in 920 DEG C of temperature It is passed through hydrogen under degree, is incubated 2 hours, it is tungsten powder after≤100ppm deoxidation to carry out deoxidation treatment and O content is made, that is, after reducing Tungsten powder;
Powder preparation step:Weight as corresponding to above-mentioned atomic percent than weigh average grain diameter 10 μm chromium powder, It is put into tungsten powder after reduction (tungsten powder after deoxidation) in high energy ball mill and mixes 15h, high purity inert gas is passed through in mixed process and is entered Row protection, ratio of grinding media to material is 40:1, ball material is hard alloy, obtains pre- pre-alloyed powder;The average grain of gained pre-alloyed powder Footpath is 5~10 μm;
Fill jacket step:The pre-alloyed powder mixed is fitted into the suitable metal capsule of size, mild steel can be used Plate jacket or titanium plate jacket;
De-airing step:The jacket filled is placed in degasification furnace, 430 DEG C of heating-up temperature, soaking time 10h;
High temperature insostatic pressing (HIP) step:It is put into hot isostatic apparatus and sinters after the jacket soldering and sealing that degassing is finished, holding temperature is 1400 DEG C, time 2h, pressure 150MPa;The blank after jacket is suppressed is removed again;
Machining steps:Blank after compacting is machined out according to drawing, required finished product target is obtained after cleaning Material.
The target relative density that this example is obtained reaches 99.2%, average grain size≤20 μm.
Embodiment 6
In the present embodiment, chromium tungsten alloy target material includes the composition of following atomic percent::Chromium 98.5%, tungsten 1.5%;This The preparation method of example chromium tungsten alloy target material, comprises the following steps:
Powder reduction step:Tungsten powder (5 μm of average grain diameter, purity:99.9%;O content is 1000~1200ppm) 850 It is passed through hydrogen at a temperature of DEG C, is incubated 5 hours, carry out deoxidation treatment, it is tungsten powder after≤350ppm deoxidation that O content, which is made,;
Powder preparation step:Weight ratio as corresponding to above-mentioned atomic percent weighs tungsten powder and average grain diameter 25 after deoxidation μm 99.95% purity chromium powder, well mixed pre-alloyed powder is produced using high-energy-milling;Ratio of grinding media to material is 25:1, Mill ball is sintered carbide ball, and milling time is 6 hours, obtains pre-alloyed powder;The average grain diameter of gained pre-alloyed powder is ≤20μm;
Fill jacket step:The pre- pre-alloyed powder mixed is fitted into the suitable stainless steel capsule of size;
De-airing step:Stainless steel capsule is placed in degasification furnace, 480 DEG C of heating-up temperature, soaking time 6h;
High temperature insostatic pressing (HIP) step:It is put into hot isostatic apparatus and sinters after the jacket soldering and sealing that degassing is finished, holding temperature is 1360 DEG C, time 5h, pressure 125MPa;The blank after jacket is suppressed is removed again;
Machining steps:Blank after compacting is machined out according to drawing, required finished product target is obtained after cleaning Material.
The target relative density that this example is obtained reaches 99%, and average grain size is 30 μm.
The assay method of each parameter is as follows in above example:Relative density is measured using Archimedes's drainage; Average grain size is analyzed target by optical metallographic microscope.
It should be appreciated that the purposes of these embodiments is merely to illustrate the present invention and is not intended to limitation protection model of the invention Enclose.In addition, it will also be appreciated that after the technology contents of the present invention have been read, those skilled in the art can make each to the present invention Change, modification and/or variation are planted, all these equivalent form of values equally fall within the guarantor that the application appended claims are limited Within the scope of shield.

Claims (8)

1. a kind of preparation method of chromium tungsten alloy target material, it is characterised in that the preparation method of the chromium tungsten alloy target material, including with Lower step:
Step 1: tungsten powder is subjected to reduction treatment, the tungsten powder after being reduced;
Step 2: the tungsten powder and chromium powder after the reduction are prepared into pre-alloyed powder;The pre-alloyed powder is described goes back Tungsten powder after original carries out what milling processing was obtained with chromium powder;The milling processing is using the processing of high-energy ball milling powder;
Step 3: the prealloy powder powder stock is carried out into dress jacket processing, the jacket filled;
Step 4: the jacket filled is de-gassed processing, the jacket after being deaerated;
Step 5: carrying out hip treatment, the ingot blank after being suppressed to the jacket after the degassing, then remove jacket and obtain Blank after compacting;The holding temperature of the hip treatment is 1250~1445 DEG C, and soaking time is 2~5h, and pressure is 120~150MPa;
Step 6: the blank after the compacting is machined out into processing, the chromium tungsten alloy target material is obtained;The chromium tungsten alloy Target includes the composition of following atomic percent:Chromium 80~99%, tungsten 1~20%.
2. the preparation method of chromium tungsten alloy target material according to claim 1, it is characterised in that the chromium tungsten alloy target material includes The composition of following atomic percent:Chromium 90%, tungsten 10%.
3. the preparation method of chromium tungsten alloy target material according to claim 1, it is characterised in that the alloy target material it is relatively close Degree is not less than 99%, and average grain size is not more than 50 μm.
4. the preparation method of chromium tungsten alloy target material according to claim 1, it is characterised in that at the high-energy ball milling powder Reason, refers to mix 4~24h in high energy ball mill under the conditions of inert gas shielding.
5. the preparation method of chromium tungsten alloy target material according to claim 1, it is characterised in that the pre-alloyed powder is averaged Particle diameter is not more than 50 μm.
6. the preparation method of chromium tungsten alloy target material according to claim 1, it is characterised in that described in the step one Reduction treatment is to be passed through hydrogen at 850~950 DEG C.
7. the preparation method of chromium tungsten alloy target material according to claim 1, it is characterised in that described in the step 4 The temperature of degassing process is 300~500 DEG C, and the time is 5~30h.
8. the preparation method of chromium tungsten alloy target material according to claim 7, it is characterised in that the vacuum during degassing process Spend for 10-1Pa~10-4Pa。
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