CN105345007A - Preparation method for highly dense chromium-tungsten alloy target - Google Patents
Preparation method for highly dense chromium-tungsten alloy target Download PDFInfo
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Abstract
The invention belongs to the technical field of preparation of powder metallurgy materials and provides a preparation method for a highly dense chromium-tungsten alloy target. The highly dense chromium-tungsten alloy target comprises, by atomic percent, 80%-99% of chromium and 1%-20% of tungsten. The preparation method for the highly dense chromium-tungsten alloy target comprises the steps that after tungsten powder is reduced, the tungsten powder and chromium powder are subjected to treatment of prealloyed powder preparation, packaging and canning, degassing, hot isostatic pressing, machining and the like, and the chromium-tungsten alloy target is obtained. The density of the chromium-tungsten alloy target is high, the relative density is not smaller than 99%, the structure is uniform, and grains are fine and not larger than 50 micrometers; the target can be used in the film coating fields of electrode contact materials and the like and used for preparing thin film materials high in hardness, high in dielectric breakdown strength, low in chopping current and capable of replacing pure tungsten.
Description
Technical field
The invention belongs to technical field of powder metallurgy material preparation, particularly a kind of preparation method of high fine and close chromium tungsten alloy target material.
Background technology
Along with the development of material science, the structure of material develops into two-dimensional directional and gives full play to material potential and provide a kind of important channel.Membrane science is exploitation new material and the very important field of new unit.High-tech Material to film transfer, thus makes plated film device develop rapidly by body material.
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 determines primarily of target production technology.Current target production method mainly contains smelting process and powder metallurgic method.Smelter's artistic skill produces most metal targets, but minority target is because alloying component fusing point gap is too large, target requires the factors such as strict control crystallite dimension and powder metallurgical technique can only be adopted to prepare.
Hot isostatic pressing technique utilizes high temperature and high pressure, makes a kind of technique of densifying materials in a container sealed.Be be working media with high-pressure inert gas due to this technology, evenly exert pressure at surface of the work, identical effect is produced to workpiece arbitrary surfaces, material internal density uniformity can be improved.Owing to preparing the superiority on material, high temperature insostatic pressing (HIP) is widely used in eliminating casting defect, the processes such as powder metallurgy is densified.
The fusing point of chromium is 1860 DEG C, and the fusing point of tungsten is 3407 DEG C, and because chromium, tungsten two kinds of melting point metal temperature difference are huge, under conventional equipment condition, adopting the method for conventional metallurgical to prepare chromium tungsten alloy cannot realize.The method of ordinary sinter can prepare chromium tungsten alloy, but the porosity of material is too high, and relative density cannot reach the instructions for use of target.
At present, the main production adopting hot pressed sintering to carry out CrW target both at home and abroad; But owing to being difficult to obtained dense structure, target product that dimensions is large by production technology restriction.
Summary of the invention
The object of the present invention is to provide a kind of compactness good, without internal flaw, even tissue, crystal grain is tiny, chromium tungsten alloy target material that specification is large and preparation method thereof.
The object of the invention is to be achieved through the following technical solutions:
A kind of chromium tungsten alloy target material, comprises the composition of following atomic percent: chromium 80 ~ 99%, tungsten 1 ~ 20%.
Further, described chromium tungsten alloy target material comprises the composition of following atomic percent: chromium 90%, tungsten 10%.
Further, the relative density of described alloy target material is not less than 99%, and average grain size is not more than 50 μm.
The object of the invention is to be realized by following another technical scheme:
The preparation method of described chromium tungsten alloy target material, comprises the following steps:
Step one, carries out reduction treatment by tungsten powder, obtains the tungsten powder after reducing;
Step 2, prepares pre-alloyed powder by the tungsten powder after described reduction and chromium powder;
Step 3, carries out the process of dress jacket by described prealloy powder powder stock, obtains the jacket filled;
Step 4, carries out degassed process by the described jacket filled, obtain degassed after jacket;
Step 5, to described degassed after jacket carry out hip treatment, obtain suppress after ingot blank, then remove jacket obtain suppress after blank;
Step 6, carries out mechanical process by the blank after described compacting, obtains described chromium tungsten alloy target material.
Further, in described step 2, described pre-alloyed powder is that tungsten powder after described reduction and chromium powder carry out abrasive dust process and obtain; Preferably, described abrasive dust process adopts high-energy ball milling powder process process.
Further, described high-energy ball milling powder process process process, refers to and in high energy ball mill, mix 4-24h under inert gas shielding condition.
Further, the average grain diameter of described pre-alloyed powder is not more than 50 μm.
Further, in described step one, described reduction treatment passes into hydrogen at 850 ~ 950 DEG C.
Further, in described step 4, the temperature of described degassed process is 300 ~ 500 DEG C, and the time is 5 ~ 30h; Preferably, vacuum degree control during described degassed process is 10
-1pa ~ 10
-4pa.
Further, in described step 5, the holding temperature of described hip treatment is 1250 ~ 1450 DEG C, and temperature retention time is 2 ~ 5h, and pressure is 120 ~ 150MPa.
Compared to prior art, the present invention has following beneficial effect:
1, the present invention has the internal flaws such as density high (relative density is not less than 99%), pore-free, loose and segregation by using the CrW alloy target material that provides of heat and other static pressuring processes, even tissue, the advantages such as crystal grain tiny (mean grain size and average grain size are not more than 50 μm).
2, target of the present invention produces pre-alloyed powder owing to adopting high-energy-milling, so the CrW pre-alloyed powder mixed can be obtained, again due to the advantage of heat and other static pressuring processes self, by the control to raw material quality, can impurity content be obtained low, target purity is high, density is high, crystal grain is tiny, the uniform target material base of microscopic structure.
3, because the present invention adopts heat and other static pressuring processes, target size is only by the restriction of hot isostatic apparatus operating room size, and maximize so can realize target size, target full-size can accomplish 1701mm.
4, the CrW target prepared of the present invention, can be used for the plated film fields such as electrode contact material, and preparation has the thin-film material of high rigidity, high withstand voltage intensity, low shut off value, alternative pure tungsten.
Accompanying drawing explanation
Fig. 1 is the micro-organization chart of the target that the embodiment of the present invention 3 obtains.
Detailed description of the invention
The invention provides a kind of high fine and close chromium tungsten alloy target material, the atomic percent of the composition that this alloy target material comprises is: the content (at%) of tungsten (W) is 0<W≤20%, the content (at%) of chromium (Cr) is 80≤Cr<100%, the atomic percentage conc of such as W can be 1%, 2%, 2.5%, 3.2%, 4.1%, 4.9%, 5%, 5.2%, 8%, 11%, 14%, 17%, 19% etc., preferred chromium is 90%, and tungsten is 10%.
Wherein, the present invention adopts purity to be tungsten (W) powder of 99.9%-99.999% and purity to be chromium (Cr) powder of 99.5%-99.99%, mechanical mixture prepares pre-alloyed powder, pre-alloyed powder is packed in metal capsule, through operations such as vacuumize degassing, hip treatment, machineds in a heated condition, obtain density high (relative density is not less than 99%), microscopic structure evenly, grain size (average grain size) is not more than the high-quality CrW target of 50 μm.The W powder purity of preparation CrW target between 99.9% ~ 99.999%, can use after high-purity hydrogen reduction.
According to above-mentioned purpose, the technical scheme of entirety of the present invention is: adopt ball-milling technology to produce pre-alloyed powder, gained pre-alloyed powder is loaded jacket, and after degassed, hip treatment obtains qualified chromium tungsten alloy target material.
Below concrete steps of the present invention are described in detail.
The first step, powder reduction step: tungsten powder is carried out reduction treatment, obtains the tungsten powder after reducing;
Specifically, be be 2 ~ 10 μm by particle diameter, purity be 99.9% ~ 99.999%% tungsten powder pass into hydrogen reducing, in 850 ~ 950 DEG C (can be such as 850 DEG C, 900 DEG C, 930 DEG C, 950 DEG C etc.) insulation, 1 ~ 10h (can be such as 2h, 4h, 6h, 8h etc.), reduce O content in W powder raw material.
Second step, powder preparation step: by the tungsten powder after described reduction and chromium powder by abrasive dust process, prepare pre-alloyed powder;
Specifically, employing average particle diameter size is 10 ~ 45 μm, purity is the chromium powder of 99.5% ~ 99.99% and the tungsten powder after reducing, be positioned in milling equipment after taking according to the weight ratio corresponding to above-mentioned atomic percent, carrying out abrasive dust process 4 ~ 24h, can be such as exemplarily 4.5h, 6h, 9h, 11h, 15h, 18h, 20h, 22h.This abrasive dust process can adopt high-energy ball milling process, planetary ball mill process etc.; Be preferably high-energy ball milling powder process process, refer under inert gas shielding condition and to mix 4 ~ 24h in high energy ball mill.The ratio of grinding media to material (mass ratio) related in abrasive dust process is: 10:1 ~ 50:1, and can be such as 10:1,20:1,30:1,40:1,50:1, mill ball used be generally sintered carbide ball.
3rd step, dress jacket step: the pre-alloyed powder prepared by second step loads in metal capsule, obtains the jacket filled;
Specifically, as metal capsule, can be stainless steel jacket, also can be the jacket of other metal materials, such as low carbon steel plate jacket, titanium plate jacket etc.
4th step, de-airing step: utilize degasification furnace that the jacket filled is carried out degassed process, obtain degassed after jacket;
Specifically, the jacket filled completing dress powder is placed in degasification furnace and carries out degassed process, degasification furnace selects commercially available vacuum degassing furnace or well formula resistance degasification furnace, and degassing temperature is generally 300 ~ 500 DEG C, degassing time 5 ~ 30h.Exemplarily, described 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; Described degassing time can be 5h, 9h, 15h, 20h, 22.5h, 25h, 28h.
More preferably, during described degassed process, carry out certain vacuum degree control, such as can 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: utilize hot isostatic apparatus to carry out hip treatment to the jacket after degassed, obtains the ingot blank after suppressing, then remove jacket obtain compacting after blank;
Specifically, be exactly by after degassed jacket soldering and sealing, put into hot isostatic apparatus and sinter; In sintering process, holding temperature is 1250 ~ 1450 DEG C, and sintering time is 2 ~ 5h, and pressure during sintering is 120 ~ 150MPa; Exemplarily, described 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; Described sintering time can be 2h, 3.5h, 4.0h, 4.5h; Described sintering pressure can be 125MPa, 135MPa, 140MPa, 145MPa, 148MPa, 150MPa.After sintering, the powder densification in the jacket after degassed process, forms the ingot blank after compacting; Remove above-mentioned metal capsule again, obtain the blank after compacting.
6th step, machining steps: carry out machined according to drawing to blank after the compacting obtained in high temperature insostatic pressing (HIP) step, obtains required finished product target after cleaning.
Further describe the present invention below by way of example, the parameter in embodiment is only to exemplary illustration of the present invention, the invention is not restricted to the concrete definition of these embodiments.
Embodiment 1
In the present embodiment, chromium tungsten alloy target material comprises 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 (average grain diameter 8 μm, purity: 99.99%; O content is 500 ~ 700ppm) at 850 DEG C of temperature, pass into hydrogen, be incubated 5 hours, carry out deoxidation treatment, obtained O content is≤deoxidation of 200ppm after tungsten powder, the tungsten powder namely after reduction;
Powder preparation step: the chromium powder taking 99.95% purity of tungsten powder and average grain diameter 45 μm after deoxidation by the weight ratio corresponding to above-mentioned atomic percent, adopts high-energy-milling to produce the pre-alloyed powder mixed; Ratio of grinding media to material is 20:1, and 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;
Dress jacket step: the pre-alloyed powder mixed is loaded in the suitable stainless steel jacket of size;
De-airing step: be placed in degasification furnace by the stainless steel jacket filled, heating-up temperature 500 DEG C, temperature retention time 20h, devolatilization vacuum degree controls 10
-3pa ~ 10
-4pa;
High temperature insostatic pressing (HIP) step: sinter putting into hot isostatic apparatus after degassed complete jacket soldering and sealing, holding temperature is 1450 DEG C, time 5h, pressure 120MPa; Remove jacket again and obtain the blank after suppressing;
Machining steps: according to drawing, machined is carried out to the blank after compacting, obtains required finished product target after cleaning.
The target relative density that this example obtains reaches 99%, average grain size≤40 μm.
Embodiment 2
Chromium tungsten alloy target material comprises 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 (average grain diameter 6 μm, purity: 99.999%; O content is≤200ppm) at 850 DEG C of temperature, pass into hydrogen, be incubated 3 hours, carrying out deoxidation treatment, to obtain O content be tungsten powder after the deoxidation of 70ppm, the tungsten powder after namely reducing;
Powder preparation step: by the weight ratio corresponding to above-mentioned atomic percent take average grain diameter 35 μm chromium powder, with reduction after tungsten powder (after deoxidation tungsten powder) put into high energy ball mill mixing 12h, high purity inert gas protection is passed in mixed process, ratio of grinding media to material is 30:1, ball material is carbide alloy, obtains pre-alloyed powder; The average grain diameter of gained pre-alloyed powder is 25 ~ 30 μm;
Dress jacket step: the pre-alloyed powder mixed is loaded in the suitable metal capsule of size, low carbon steel plate jacket or titanium plate jacket can be adopted;
De-airing step: the jacket filled is placed in degasification furnace, heating-up temperature 400 DEG C, temperature retention time 30h;
High temperature insostatic pressing (HIP) step: sinter putting into hot isostatic apparatus after degassed complete jacket soldering and sealing, holding temperature is 1350 DEG C, time 3h, pressure 150MPa; Remove jacket again and obtain the blank after suppressing;
Machining steps: according to drawing, machined is carried out to the blank after compacting, obtains required finished product target after cleaning.
The target relative density that this example obtains reaches 99.2%, average grain size≤35 μm.
Embodiment 3
In the present embodiment, chromium tungsten alloy target material comprises 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 (average grain diameter 10 μm, purity: 99.9%; O content is 1000ppm) at 950 DEG C of temperature, pass into hydrogen, be incubated 1 hour, carry out deoxidation treatment obtain O content and be≤deoxidation of 300ppm after tungsten powder, the tungsten powder namely after reduction;
Powder preparation step: take average grain diameter tungsten powder after the chromium powder of 45 μm and deoxidation by the weight ratio corresponding to above-mentioned atomic percent and put into high energy ball mill mixing 24h, vacuumize in mixed process and be filled with high purity inert gas protection, ratio of grinding media to material is 40:1, ball material is carbide alloy, obtains pre-alloyed powder; The average grain diameter of gained pre-alloyed powder is 40 ~ 45 μm;
Dress jacket step: the pre-alloyed powder mixed is loaded in the suitable metal capsule of size, low carbon steel plate jacket or titanium plate jacket can be adopted;
De-airing step: the jacket filled is placed in degasification furnace, heating-up temperature 300 DEG C, temperature retention time 20h, during degassed process, carry out certain vacuum degree control, by vacuum degree control 10
-1pa ~ 10
-2pa;
High temperature insostatic pressing (HIP) step: sinter putting into hot isostatic apparatus after degassed complete jacket soldering and sealing, holding temperature is 1250 DEG C, time 4h, pressure 135MPa; Remove jacket again and obtain the blank after suppressing;
Machining steps: according to drawing, machined is carried out to the blank after compacting, obtains required finished product target after cleaning.
The target relative density that this example obtains reaches 99.5%, average grain size≤50 μm.
As shown in Figure 1, the target density that obtains of the present embodiment is high, crystal grain is tiny, microscopic structure is even.
Embodiment 4
In the present embodiment, chromium tungsten alloy target material comprises the composition of following atomic percent: chromium 96.8%, tungsten 2.2%.The preparation method of this example chromium tungsten target material, comprises the following steps:
Powder reduction step: tungsten powder (average grain diameter 3 μm, purity: 99.99%; O content is 600 ~ 900ppm) at 950 DEG C of temperature, pass into hydrogen, be incubated 1 hour, carry out deoxidation treatment obtain O content and be≤deoxidation of 250ppm after tungsten powder, the tungsten powder namely after reduction;
Powder preparation step: take average grain diameter tungsten powder after the chromium powder of 25 μm and deoxidation by the weight ratio corresponding to above-mentioned atomic percent and put into high energy ball mill mixing 20h, vacuumize in mixed process and be filled with high purity inert gas protection, ratio of grinding media to material is 35:1, ball material is carbide alloy, obtains pre-alloyed powder; The average grain diameter of gained pre-alloyed powder is 20 ~ 25 μm;
Dress jacket step: the pre-alloyed powder mixed is loaded in the suitable metal capsule of size, low carbon steel plate jacket or titanium plate jacket can be adopted;
De-airing step: be placed in degasification furnace by the jacket filled, heating-up temperature 370 DEG C, temperature retention time 16h, carries out certain vacuum degree control during degassed process, by vacuum degree control 10
-2pa ~ 10
-3pa;
High temperature insostatic pressing (HIP) step: sinter putting into hot isostatic apparatus after degassed complete jacket soldering and sealing, holding temperature is 1280 DEG C, time 3.5h, pressure 145MPa; Remove jacket again and obtain the blank after suppressing;
Machining steps: according to drawing, machined is carried out to the blank after compacting, obtains required finished product target after cleaning.
The target relative density that this example obtains reaches 99.6%, average grain size≤35 μm.
Embodiment 5
In the present embodiment, chromium tungsten alloy target material comprises 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 (average grain diameter 5 μm, purity: 99.999%; O content is≤300ppm) at 920 DEG C of temperature, pass into hydrogen, be incubated 2 hours, carry out deoxidation treatment obtain O content and be≤deoxidation of 100ppm after tungsten powder, the tungsten powder after namely reducing;
Powder preparation step: by the weight ratio corresponding to above-mentioned atomic percent take average grain diameter 10 μm chromium powder, with reduction after tungsten powder (after deoxidation tungsten powder) put into high energy ball mill mixing 15h, high purity inert gas protection is passed in mixed process, ratio of grinding media to material is 40:1, ball material is carbide alloy, obtains pre-pre-alloyed powder; The average grain diameter of gained pre-alloyed powder is 5 ~ 10 μm;
Dress jacket step: the pre-alloyed powder mixed is loaded in the suitable metal capsule of size, low carbon steel plate jacket or titanium plate jacket can be adopted;
De-airing step: the jacket filled is placed in degasification furnace, heating-up temperature 430 DEG C, temperature retention time 10h;
High temperature insostatic pressing (HIP) step: sinter putting into hot isostatic apparatus after degassed complete jacket soldering and sealing, holding temperature is 1400 DEG C, time 2h, pressure 150MPa; Remove jacket again and obtain the blank after suppressing;
Machining steps: according to drawing, machined is carried out to the blank after compacting, obtains required finished product target after cleaning.
The target relative density that this example obtains reaches 99.2%, average grain size≤20 μm.
Embodiment 6
In the present embodiment, chromium tungsten alloy target material comprises the composition of following atomic percent:: chromium 98.5%, tungsten 1.5%; The preparation method of this example chromium tungsten alloy target material, comprises the following steps:
Powder reduction step: tungsten powder (average grain diameter 5 μm, purity: 99.9%; O content is 1000 ~ 1200ppm) at 850 DEG C of temperature, pass into hydrogen, be incubated 5 hours, carry out deoxidation treatment, obtained O content is≤deoxidation of 350ppm after tungsten powder;
Powder preparation step: the chromium powder taking 99.95% purity of tungsten powder and average grain diameter 25 μm after deoxidation by the weight ratio corresponding to above-mentioned atomic percent, adopts high-energy-milling to produce the pre-alloyed powder mixed; Ratio of grinding media to material is 25:1, and 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≤20 μm;
Dress jacket step: the pre-pre-alloyed powder mixed is loaded in the suitable stainless steel jacket of size;
De-airing step: stainless steel jacket is placed in degasification furnace, heating-up temperature 480 DEG C, temperature retention time 6h;
High temperature insostatic pressing (HIP) step: sinter putting into hot isostatic apparatus after degassed complete jacket soldering and sealing, holding temperature is 1360 DEG C, time 5h, pressure 125MPa; Remove jacket again and obtain the blank after suppressing;
Machining steps: according to drawing, machined is carried out to the blank after compacting, obtains required finished product target after cleaning.
The target relative density that this example obtains reaches 99%, and average grain size is 30 μm.
In above embodiment, the assay method of each parameter is as follows: relative density adopts Archimedes's drainage to measure; Average grain size is analyzed target by optical metallographic microscope.
Should be appreciated that the purposes of these embodiments is only not intended to for illustration of the present invention limit the scope of the invention.In addition; also should understand; after having read technology contents of the present invention, those skilled in the art can make various change, amendment and/or modification to the present invention, and these all equivalent form of values fall within the protection domain that the application's appended claims limits equally.
Claims (10)
1. a chromium tungsten alloy target material, is characterized in that, comprises the composition of following atomic percent: chromium 80 ~ 99%, tungsten 1 ~ 20%.
2. chromium tungsten alloy target material according to claim 1, is characterized in that, comprise the composition of following atomic percent: chromium 90%, tungsten 10%.
3. chromium tungsten alloy target material according to claim 1, it is characterized in that, the relative density of described alloy target material is not less than 99%, and average grain size is not more than 50 μm.
4. the preparation method of the arbitrary described chromium tungsten alloy target material of claims 1 to 3, is characterized in that, comprise the following steps:
Step one, tungsten powder is carried out reduction treatment, obtain the tungsten powder after reducing;
Step 2, the tungsten powder after described reduction and chromium powder are prepared pre-alloyed powder;
Step 3, described prealloy powder powder stock is carried out the process of dress jacket, obtain the jacket filled;
Step 4, the described jacket filled is carried out degassed process, obtain degassed after jacket;
Step 5, to described degassed after jacket carry out hip treatment, obtain suppress after ingot blank, then remove jacket obtain suppress after blank;
Step 6, the blank after described compacting is carried out mechanical process, obtain described chromium tungsten alloy target material.
5. preparation method according to claim 4, is characterized in that, in described step 2, described pre-alloyed powder is that tungsten powder after described reduction and chromium powder carry out abrasive dust process and obtain; Preferably, described abrasive dust process adopts high-energy ball milling powder process process.
6. preparation method according to claim 5, is characterized in that, described high-energy ball milling powder process process, refers in high energy ball mill, to mix 4 ~ 24h under inert gas shielding condition.
7. preparation method according to claim 4, it is characterized in that, the average grain diameter of described pre-alloyed powder is not more than 50 μm.
8. preparation method according to claim 4, it is characterized in that, in described step one, described reduction treatment passes into hydrogen at 850 ~ 950 DEG C.
9. preparation method according to claim 4, it is characterized in that, in described step 4, the temperature of described degassed process is 300 ~ 500 DEG C, and the time is 5 ~ 30h; Preferably, vacuum during described degassed process is 10
-1pa ~ 10-
4pa.
10. preparation method according to claim 4, it is characterized in that, in described step 5, the holding temperature of described hip treatment is 1250 ~ 1450 DEG C, and temperature retention time is 2 ~ 5h, and pressure is 120 ~ 150MPa.
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