CN114799175B - Chromium silicon carbon alloy target and preparation method thereof - Google Patents

Chromium silicon carbon alloy target and preparation method thereof Download PDF

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CN114799175B
CN114799175B CN202210458591.1A CN202210458591A CN114799175B CN 114799175 B CN114799175 B CN 114799175B CN 202210458591 A CN202210458591 A CN 202210458591A CN 114799175 B CN114799175 B CN 114799175B
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sintering
chromium
powder
silicon
heating
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CN114799175A (en
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姚力军
潘杰
王学泽
周友平
杨慧珍
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Ningbo Jiangfeng Electronic Material Co Ltd
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Ningbo Jiangfeng Electronic Material Co Ltd
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • 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
    • C22C27/06—Alloys based on chromium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
    • C22C32/0063—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides based on SiC
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Ceramic Products (AREA)

Abstract

The invention provides a chromium silicon carbon alloy target and a preparation method thereof, wherein vacuum hot-pressing sintering is completed through first heating, first sintering, second heating, second sintering, third heating, third sintering, first pressurizing, second pressurizing and pressure maintaining, so that the problems of insufficient density, holes in the target and uneven components of the target are solved; the chromium silicon carbon alloy target material prepared by the preparation method has the purity of more than or equal to 99.9 percent, the compactness of more than or equal to 99 percent, the microcosmic uniformity and the excellent sputtering performance.

Description

Chromium silicon carbon alloy target and preparation method thereof
Technical Field
The invention belongs to the technical field of target preparation, and particularly relates to a chromium silicon carbon alloy target and a preparation method thereof.
Background
Along with the rapid progress of the 5G technology, the demand of the communication and chip industries for high-purity chromium silicon targets is greatly increased, however, the chromium silicon targets produced by various enterprises at present have the defects of low density and uneven microstructure, and cannot meet the requirement of the high-end electronic industry on the quality of the targets, so that the method is only suitable for manufacturing low-end products. In addition, most of chromium silicon targets have high production cost and complex flow, the production efficiency cannot be improved, and the requirements of wider industry fields cannot be met.
CN111058004a discloses a chromium-silicon alloy sputtering target material and a preparation method thereof, the preparation method comprises: (1) Filling chromium-silicon alloy powder with a target mass ratio into a mould, sealing, and performing compaction treatment; (2) Degassing the die subjected to compaction in the step (1); (3) Carrying out hot isostatic pressing treatment on the die subjected to the degassing in the step (2) at the temperature of 1000-1350 ℃ to obtain a chromium silicon alloy sputtering target crude product; and (4) obtaining the chromium silicon alloy sputtering target material after machining.
CN104227000a discloses a production method of chromium target material, which comprises the following specific steps: (1) Uniformly mixing metal chromium powder with the granularity of 60-320 meshes and metal chromium powder with the granularity of 320-500 meshes, and drying for later use, wherein the mass ratio of the metal chromium powder with the granularity of 60-320 meshes to the metal chromium powder with the granularity of 320-500 meshes is 5:3-9:2; (2) Adding the metal chromium powder mixed in the step (1) into a cold pressing mold, performing cold pressing molding by using 700 Mpa-1000 Mpa pressure, maintaining the pressure for 10 s-120 s, and pressing a solid cylinder chromium target blank with the size of phi 50 multiplied by 5.0 mm-phi 120 multiplied by 6.8 mm; (3) Coating the surface of the chromium target blank by using coating paper, loading the chromium target blank into a hot-pressing die, and loading the chromium target blank into a furnace; (4) Vacuumizing to 0-15 pa, heating to 300-400 ℃, preserving heat for 10-30 min, continuously heating to 600-800 ℃, stopping heating, starting a hot pressing facility, aligning the upper and lower pressure heads of the hot pressing facility, and pre-pressing the chromium target blank for 60-90 s under the pressure of 8-12 Mpa; closing the hot-pressing facility, continuously heating to 1300-1600 ℃, preserving heat for 30-120 min, and powering off; (5) Starting a hot-pressing facility, hot-pressing and forming by using 20-100 Mpa pressure, maintaining the pressure for 10-100 min, cooling to be less than or equal to 100 ℃, and discharging from a furnace to obtain the chromium target. The target is only suitable for preparing pure chromium targets, and does not use chromium silicon carbon targets.
Therefore, how to provide a chromium silicon carbon alloy sputtering target material and a preparation method thereof, ensure the high density of the target material, improve the uniformity of microstructure and sputtering performance, improve the production efficiency, reduce the production cost and widen the application range, and become the problem which needs to be solved by the current technicians in the field.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a chromium silicon carbon alloy target and a preparation method thereof, and the vacuum hot-press sintering is completed through first heating, first sintering, second heating, second sintering, third heating, third sintering, first pressurizing, second pressurizing and pressure maintaining, so that the problems of insufficient density, holes in the target and uneven components of the target are solved; the chromium silicon carbon alloy target material prepared by the preparation method has the purity of more than or equal to 99.9 percent, the compactness of more than or equal to 99 percent, the microcosmic uniformity and the excellent sputtering performance.
To achieve the purpose, the invention adopts the following technical scheme:
the invention aims at providing a preparation method of a chromium silicon carbon alloy target, which comprises the following steps:
(1) Mixing chromium silicon alloy powder, silicon carbide powder and chromium powder to obtain a mixture;
(2) Carrying out vacuum hot-pressing sintering on the mixture obtained in the step (1) to obtain a chromium silicon carbon alloy target;
the vacuum hot-pressing sintering comprises a first heating, a first sintering, a second heating, a second sintering, a third heating, a third sintering, a first pressurizing, a second pressurizing and a pressure maintaining which are sequentially carried out.
According to the invention, the vacuum hot-pressing sintering is completed through the first heating, the first sintering, the second heating, the second sintering, the first pressurizing, the second pressurizing and the pressure maintaining, so that the problems of insufficient density, holes in the target material and uneven components are solved; the chromium silicon carbon alloy target material prepared by the preparation method has the purity of more than or equal to 99.9 percent, the compactness of more than or equal to 99 percent, the microcosmic uniformity and the excellent sputtering performance.
It is worth noting that in the invention, the purpose of the first temperature rise is to remove volatile impurity elements on the surface of the powder, promote the contact of the surface of the powder and increase interaction; in the first sintering process, the temperature in the die is uniform, so that alloying reaction is generated between the powder, and the internal structure is more uniform; when the temperature is raised for the second time, the temperature is raised continuously to enable the powder to further interact, and the contact gap between the powder is reduced; in the second sintering process, the temperature in the die is uniform, and the powder can fully react, so that the powder gap is reduced as much as possible, and preparation is made for subsequent pressurization; the compactness of the target blank is increased by pressurization; the performance uniformity and the compactness of the target blank are improved under the constant temperature and constant pressure.
In a preferred embodiment of the present invention, the chromium content in the chromium-silicon alloy powder in the step (1) is 50-70%, for example, 50%,5254%,56%,58%,60%,62%,64%,66%,68%,70%, etc., and the balance is silicon.
The particle size of the chromium silicon alloy powder in the step (1) is preferably not more than 75. Mu.m, for example, 15. Mu.m, 20. Mu.m, 25. Mu.m, 30. Mu.m, 35. Mu.m, 40. Mu.m, 50. Mu.m, 55. Mu.m, 60. Mu.m, 65. Mu.m, 70. Mu.m, 75. Mu.m, etc., but is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value ranges are equally applicable.
The grain size of the silicon carbide powder in the step (1) is preferably not more than 20. Mu.m, for example, 2. Mu.m, 4. Mu.m, 6. Mu.m, 8. Mu.m, 10. Mu.m, 12. Mu.m, 14. Mu.m, 16. Mu.m, 18. Mu.m, 20. Mu.m, etc., but is not limited to the above-mentioned values, and other non-mentioned values within the above-mentioned range are equally applicable.
The particle size of the chromium powder in the step (1) is preferably not more than 10. Mu.m, for example, 1. Mu.m, 2. Mu.m, 3. Mu.m, 4. Mu.m, 5. Mu.m, 6. Mu.m, 7. Mu.m, 8. Mu.m, 9. Mu.m, 10. Mu.m, etc., but not limited to the values recited, and other non-recited values within the above-mentioned range are applicable.
Preferably, the purity of the chromium silicon alloy powder, the silicon carbide powder and the chromium powder in the step (1) is equal to or higher than 99.95%, for example, 99.95%,99.98%,99.99%,99.992%,99.995%,99.998%,99.999%, etc., but the present invention is not limited to the above-mentioned values, and other non-mentioned values in the above-mentioned value ranges are equally applicable.
As a preferable technical scheme of the invention, in the mixture in the step (1), the silicon content is 40-55wt%, for example, 40wt%,42wt%,46wt%,48wt%,50wt%,52wt%,54wt%,55wt%, etc., the carbon content is 2-12wt%, for example, 2wt%,4wt%,6wt%,8wt%,10wt%,12wt%, etc., and the balance is chromium; however, the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned numerical ranges are equally applicable.
Preferably, the mixing of step (1) is performed in a shielding gas.
Preferably, the shielding gas comprises nitrogen and/or argon.
Preferably, the mixing in step (1) is performed by ball milling.
Preferably, the ball ratio of the ball mill is (5-8): 1, for example, 5:1,5.5:1,6:1,6.5:1,7:1,7.5:1,8:1, etc., but the ball ratio is not limited to the recited values, and other non-recited values within the above-mentioned range are equally applicable.
Preferably, the mixing of step (1) is performed in a polyurethane liner powder mixer.
Preferably, the mixing time in step (1) is not less than 36 hours, for example, 36 hours, 38 hours, 40 hours, 45 hours, 50 hours, 55 hours, 60 hours, 65 hours, 70 hours, 80 hours, 90 hours, etc., but not limited to the recited values, and other non-recited values within the above range are equally applicable.
As a preferable technical scheme of the invention, before the vacuum hot-pressing sintering in the step (2), the mixture in the step (1) is sequentially subjected to die filling and prepressing.
Preferably, the mold used in the molding comprises a graphite mold.
The pre-compaction pressure is preferably < 2MPa, and may be, for example, 0.1MPa,0.3MPa,0.5MPa,0.7MPa,0.9MPa,1MPa,1.2MPa,1.5MPa,1.7MPa,1.9MPa, etc., but is not limited to the values recited, and other values not recited in the above-mentioned numerical ranges are equally applicable. Preferably, the milling balls used in the ball milling include zirconia balls.
Preferably, the pre-pressing time is 3 to 10min, for example, 3min,4min,5min,6min,7min,8min,9min,10min, etc., but the pre-pressing time is not limited to the listed values, and other non-listed values within the above-mentioned range are equally applicable.
In a preferred embodiment of the present invention, the degree of vacuum in the vacuum hot press sintering in the step (2) is not more than 100Pa, and may be, for example, 10Pa,20Pa,30Pa,40Pa,50Pa,60Pa,70Pa,80Pa,90Pa,100Pa, etc., but is not limited to the values recited above, and other values not recited in the above-mentioned ranges are equally applicable.
In a preferred embodiment of the present invention, the temperature rising rate of the first temperature rising in the step (2) is 5 to 10 ℃/min, for example, 5 ℃/min,5.5 ℃/min,6 ℃/min,6.5 ℃/min,7 ℃/min,7.5 ℃/min,8 ℃/min,8.5 ℃/min,9 ℃/min,9.5 ℃/min,10 ℃/min, etc., but the temperature rising rate is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value ranges are equally applicable.
Preferably, the end temperature of the first temperature increase in step (2) is the same as the temperature of the first sintering.
Preferably, the temperature of the first sintering in the step (2) is 500 to 600 ℃, for example, 500 ℃,510 ℃,520 ℃,530 ℃,540 ℃,550 ℃,560 ℃,570 ℃,580 ℃,590 ℃,600 ℃, etc., but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned numerical ranges are equally applicable.
It is worth to be noted that, the temperature of the first sintering is 500-600 ℃, if the temperature is higher than 600 ℃, the energy consumption is increased; if the temperature is lower than 500 ℃, the impurity elements on the surface of the powder cannot be sufficiently removed, the interaction between the powders is affected, meanwhile, the temperature is too low, the interaction between the powders is weak, the subsequent pressurizing effect is further affected, and the density is lower.
Preferably, the time of the first sintering in the step (2) is 0.5 to 1h, for example, 0.5h,0.6h,0.7h,0.8h,0.9h,1h, etc., but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value ranges are equally applicable.
Preferably, the heating rate of the second heating in the step (2) is 5 to 10 ℃/min, for example, 5 ℃/min,5.5 ℃/min,6 ℃/min,6.5 ℃/min,7 ℃/min,7.5 ℃/min,8 ℃/min,8.5 ℃/min,9 ℃/min,9.5 ℃/min,10 ℃/min, etc., but not limited to the recited values, and other non-recited values within the above range are equally applicable.
Preferably, the end temperature of the second elevated temperature of step (2) is the same as the temperature of the second sintering.
Preferably, the temperature of the second sintering in the step (2) is 800 to 900 ℃, for example, 800 ℃,810 ℃,820 ℃,830 ℃,840 ℃,850 ℃,860 ℃,870 ℃,880 ℃,890 ℃,900 ℃, etc., but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned numerical ranges are equally applicable.
Preferably, the second sintering time in the step (2) is 0.5 to 1h, for example, 0.5h,0.6h,0.7h,0.8h,0.9h,1h, etc., but not limited to the listed values, and other non-listed values in the above-mentioned value ranges are equally applicable.
It is worth to say that, the temperature of the second sintering is 800-900 ℃, if the temperature is higher than 900 ℃, the energy consumption is increased; if the temperature is lower than 800 ℃, incomplete reaction between the powders can be caused, and a large number of gaps still exist, so that the compactness of the target is affected.
In a preferred embodiment of the present invention, the temperature rising rate of the third temperature rising in the step (2) is 1 to 5 ℃/min, and may be, for example, 1 ℃/min,1.5 ℃/min,2 ℃/min,2.5 ℃/min,3 ℃/min,3.5 ℃/min,4 ℃/min,4.5 ℃/min,5 ℃/min, etc., but not limited to the above-mentioned values, and other values not mentioned in the above-mentioned range of values are equally applicable.
Preferably, the end temperature of the third elevated temperature of step (2) is the same as the temperature of the third sintering.
Preferably, the temperature of the third sintering in the step (2) is 1150-1350 ℃, for example 1150 ℃,1170 ℃,1190 ℃,1200 ℃,1220 ℃,1240 ℃,1260 ℃,1280 ℃,1300 ℃,1330 ℃,1350 ℃, etc., but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned numerical ranges are equally applicable.
It is worth to say that, the temperature of the third sintering is 1150-1350 ℃, if the temperature is higher than 1350 ℃, the density is insufficient; if the temperature is lower than 1150 ℃, the alloy target blank is over-burned, the internal stress is increased, and then cracking is generated.
Preferably, the time of the third sintering in the step (2) is equal to or longer than 1h, for example, 1h,1.5h,2h,3h,4h,5h,6h,7h,8h,9h,10h, etc., but the present invention is not limited to the above-mentioned values, and other values not shown in the above-mentioned value ranges are equally applicable.
Preferably, in the step (2), the pressure in the mold is maintained to be equal to or less than 6MPa in the first temperature rise, the first sintering, the second temperature rise, the second sintering, the third temperature rise, and the third sintering, and for example, 1MPa,2MPa,3MPa,4MPa,5MPa,6MPa, etc., but the present invention is not limited to the above-mentioned values, and other non-mentioned values in the above-mentioned numerical ranges are also applicable.
In a preferred embodiment of the present invention, the first pressurizing rate in the step (2) is 0.1 to 0.3MPa/h, for example, 0.1MPa/h,0.12MPa/h,0.15MPa/h,0.18MPa/h,0.2MPa/h,0.23MPa/h,0.25MPa/h,0.27MPa/h,0.3MPa/h, etc., but the first pressurizing rate is not limited to the above-mentioned values, and other non-mentioned values in the above-mentioned value ranges are equally applicable.
The end point pressure of the first pressurization in the step (2) is preferably 15 to 22MPa, and may be, for example, 15MPa,16MPa,17MPa,18MPa,19MPa,20MPa,21MPa,22MPa, etc., but is not limited to the values listed, and other values not listed in the above-mentioned value ranges are equally applicable.
Preferably, the second pressurizing rate in the step (2) is 0.01-0.1 MPa/h, for example, 0.01MPa/h,0.02MPa/h,0.04MPa/h,0.05MPa/h,0.06MPa/h,0.7MPa/h,0.09MPa/h,0.1MPa/h, etc., but not limited to the values listed, and other non-listed values in the above-mentioned value ranges are equally applicable.
Preferably, the end pressure of the second pressurization of step (2) is the same as the pressure of the holding pressure.
The pressure of the holding pressure in the step (2) is preferably 28 to 38MPa, and may be 28 to 38MPa, 29MPa,30MPa,31MPa,32MPa,33MPa,34MPa,35MPa,36MPa,37MPa,38MPa, etc., but the pressure is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned numerical ranges are equally applicable.
Preferably, the pressure maintaining time in the step (2) is 60 to 180min, for example, 60min,70min,80min,90min,100min,110min,120min,130min,140min,150min,160min,170min,180min, etc., but not limited to the values listed, and other values not listed in the above-mentioned value ranges are equally applicable.
As a preferable technical scheme of the invention, the preparation method comprises the following steps:
(1) Mixing chromium silicon alloy powder, silicon carbide powder and chromium powder in a polyurethane lining powder mixer, controlling the mixing time to be more than or equal to 36 hours to obtain a mixture, controlling the silicon content in the mixture to be 40-55wt%, the carbon content to be 2-12wt% and the balance to be chromium;
wherein, the chromium content in the chromium-silicon alloy powder is 50-70 percent, and the rest is silicon; the grain diameter of the chromium silicon alloy powder is less than or equal to 75 mu m; the grain diameter of the silicon carbide powder is less than or equal to 20 mu m; the grain diameter of the chromium powder is less than or equal to 10 mu m; the purities of the chromium silicon alloy powder, the silicon carbide powder and the chromium powder are all more than or equal to 99.95 percent; mixing is carried out under nitrogen and/or argon; the mixing mode is ball milling; ball ratio of ball milling is (5-8): 1;
(2) Filling the mixture in the step (1) into a mold, wherein the mold adopted in the mold filling process comprises a graphite mold; prepressing for 3-10 min under the pressure less than 2 MPa; vacuum hot-pressing sintering is carried out under the vacuum degree of less than or equal to 100Pa, and the chromium silicon carbon alloy target is obtained;
wherein, the vacuum hot press sintering includes: first heating at a heating rate of 5-10 ℃/min, and first sintering at 500-600 ℃ for 0.5-1 h; carrying out second heating at a heating rate of 5-10 ℃/min, and carrying out second sintering at 800-900 ℃ for 0.5-1 h; heating up at a heating rate of 1-5 ℃/min, and sintering at 1150-1350 ℃ for more than or equal to 1h; controlling the pressure in the die to be less than or equal to 6MPa during the first temperature rise, the first sintering, the second temperature rise, the second sintering, the third temperature rise and the third sintering; the first pressurization is carried out to 15 to 22MPa at the rate of 0.1 to 0.3MPa/h, then the second pressurization is carried out to 28 to 38MPa at the rate of 0.01 to 0.1MPa/h, and the pressure is maintained for 60 to 180 minutes.
The second object of the invention is to provide a chromium silicon carbon alloy target material, which is prepared by the preparation method according to one of the objects.
The numerical ranges recited herein include not only the above-listed point values, but also any point values between the above-listed numerical ranges that are not listed, and are limited in space and for the sake of brevity, the present invention is not intended to be exhaustive of the specific point values that the stated ranges include.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the preparation method of the chromium silicon carbon alloy target material, vacuum hot-pressing sintering is completed through first heating, first sintering, second heating, second sintering, third heating, third sintering, first pressurizing, second pressurizing and pressure maintaining, so that the problems of insufficient density, holes in the target material and uneven components of the target material are solved;
(2) The purity of the chromium silicon carbon alloy target material is more than or equal to 99.9%, the compactness is more than or equal to 99%, the microcosmic uniformity is good, and the sputtering performance is excellent.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides a chromium silicon carbon alloy target and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Mixing chromium silicon alloy powder, silicon carbide powder and chromium powder in a polyurethane lining powder mixer, controlling the mixing time to be 40 hours to obtain a mixture, controlling the silicon content in the mixture to be 40wt%, the carbon content to be 10wt% and the balance to be chromium;
wherein, the chromium content in the chromium-silicon alloy powder is 60 percent, and the rest is silicon; the grain diameter of the chromium-silicon alloy powder is 70 mu m; the grain diameter of the silicon carbide powder is 16 mu m; the grain diameter of the chromium powder is 5 mu m; the purities of the chromium silicon alloy powder, the silicon carbide powder and the chromium powder are all 99.99 percent; mixing in argon; the mixing mode is ball milling; ball ratio of ball milling is 6:1;
(2) Filling the mixture in the step (1) into a mold, wherein the mold adopted in the mold filling process comprises a graphite mold; pre-pressing for 5min under the pressure of 1.5 MPa; performing vacuum hot-pressing sintering under the vacuum degree of 50Pa to obtain a chromium silicon carbon alloy target;
wherein, the vacuum hot press sintering includes: first heating at a heating rate of 10 ℃/min, and first sintering at 600 ℃ for 0.8h; carrying out second heating at a heating rate of 10 ℃/min, and carrying out second sintering at 900 ℃ for 0.8h; heating up at a heating rate of 5 ℃/min, and sintering at 1200 ℃ for 2 hours; controlling the pressure in the die to be 6MPa during the first temperature rise, the first sintering, the second temperature rise, the second sintering, the third temperature rise and the third sintering; the first pressurization was carried out to 22MPa at a rate of 0.3MPa/h, followed by the second pressurization to 35MPa at a rate of 0.06MPa/h, and the pressure was maintained for 120min.
Example 2
The embodiment provides a chromium silicon carbon alloy target and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Mixing chromium silicon alloy powder, silicon carbide powder and chromium powder in a polyurethane lining powder mixer, controlling the mixing time to be 36 hours to obtain a mixture, controlling the silicon content in the mixture to be 55wt%, the carbon content to be 2wt% and the balance to be chromium;
wherein, the chromium content in the chromium-silicon alloy powder is 50 percent, and the rest is silicon; the grain diameter of the chromium silicon alloy powder is 75 mu m; the grain diameter of the silicon carbide powder is 20 mu m; the grain diameter of the chromium powder is 10 mu m; the purities of the chromium silicon alloy powder, the silicon carbide powder and the chromium powder are all 99.95 percent; mixing is carried out under nitrogen; the mixing mode is ball milling; ball ratio of ball milling is 8:1;
(2) Filling the mixture in the step (1) into a mold, wherein the mold adopted in the mold filling process comprises a graphite mold; prepressing for 10min under the pressure of 0.8 MPa; performing vacuum hot-pressing sintering under the vacuum degree of 100Pa to obtain a chromium silicon carbon alloy target;
wherein, the vacuum hot press sintering includes: carrying out first heating at a heating rate of 5 ℃/min, and carrying out first sintering at 500 ℃ for 1h; carrying out second heating at a heating rate of 5 ℃/min, and carrying out second sintering at 800 ℃ for 1h; carrying out third heating at a heating rate of 3 ℃/min, and carrying out third sintering at 1350 ℃ for 1h; controlling the pressure in the die to be 3MPa during the first temperature rise, the first sintering, the second temperature rise, the second sintering, the third temperature rise and the third sintering; the first pressurization was carried out to 18MPa at a rate of 0.1MPa/h, followed by the second pressurization to 28MPa at a rate of 0.01MPa/h, and the pressure was maintained for 180min.
Example 3
The embodiment provides a chromium silicon carbon alloy target and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Mixing chromium silicon alloy powder, silicon carbide powder and chromium powder in a polyurethane lining powder mixer, controlling the mixing time to be 48 hours to obtain a mixture, and controlling the silicon content in the mixture to be 50wt%, the carbon content to be 12wt% and the balance to be chromium;
wherein, the chromium content in the chromium-silicon alloy powder is 70 percent, and the rest is silicon; the grain diameter of the chromium silicon alloy powder is 75 mu m; the grain diameter of the silicon carbide powder is 20 mu m; the grain diameter of the chromium powder is 10 mu m; the purities of the chromium silicon alloy powder, the silicon carbide powder and the chromium powder are all 99.99 percent; mixing in argon; the mixing mode is ball milling; ball ratio of ball milling is 5:1;
(2) Filling the mixture in the step (1) into a mold, wherein the mold adopted in the mold filling process comprises a graphite mold; pre-pressing for 3min under the pressure of 1.8 MPa; performing vacuum hot-pressing sintering under the vacuum degree of 100Pa to obtain a chromium silicon carbon alloy target;
wherein, the vacuum hot press sintering includes: carrying out first heating at a heating rate of 8 ℃/min, and carrying out first sintering at 550 ℃ for 0.5h; carrying out second heating at a heating rate of 8 ℃/min, and carrying out second sintering at 550 ℃ for 0.5h; carrying out third heating at a heating rate of 1 ℃/min, and carrying out third sintering for 3h at 1150 ℃; controlling the pressure in the die to be 5MPa during the first temperature rise, the first sintering, the second temperature rise, the second sintering, the third temperature rise and the third sintering; the first pressurization was carried out to 15MPa at a rate of 0.2MPa/h, followed by the second pressurization to 38MPa at a rate of 0.1MPa/h, and the pressure was maintained for 60 minutes.
Example 4
The embodiment provides a chromium silicon carbon alloy target and a preparation method thereof, and the preparation method described in reference to embodiment 1 is different only in that: the temperature of the third sintering in the step (2) is 1000 ℃.
Example 5
The embodiment provides a chromium silicon carbon alloy target and a preparation method thereof, and the preparation method described in reference to embodiment 1 is different only in that: the temperature of the third sintering in the step (2) is 1500 ℃.
Example 6
The embodiment provides a chromium silicon carbon alloy target and a preparation method thereof, and the preparation method described in reference to embodiment 1 is different only in that: and (3) maintaining the pressure in the step (2) to be 25MPa.
Example 7
The embodiment provides a chromium silicon carbon alloy target and a preparation method thereof, and the preparation method described in reference to embodiment 1 is different only in that: and (3) maintaining the pressure of 42MPa in the step (2).
Comparative example 1
The comparative example provides a chromium silicon carbon alloy target and a preparation method thereof, and the preparation method described with reference to the embodiment 1 is only different in that: the vacuum hot-pressed sintering in the step (2) comprises heating, sintering, first pressurizing, second pressurizing and pressure maintaining which are sequentially carried out; namely, the step (2) is as follows:
(2) Filling the mixture in the step (1) into a mold, wherein the mold adopted in the mold filling process comprises a graphite mold; pre-pressing for 5min under the pressure of 1.5 MPa; performing vacuum hot-pressing sintering under the vacuum degree of 50Pa to obtain a chromium silicon carbon alloy target;
wherein, the vacuum hot press sintering includes: heating at a heating rate of 10 ℃/min, and sintering at 1200 ℃ for 2h; controlling the temperature rise and the sintering to be 6MPa in the die; the first pressurization was carried out to 22MPa at a rate of 0.3MPa/h, followed by the second pressurization to 35MPa at a rate of 0.06MPa/h, and the pressure was maintained for 120min.
Comparative example 2
The comparative example provides a chromium silicon carbon alloy target and a preparation method thereof, and the preparation method described with reference to the embodiment 1 is only different in that: the vacuum hot-pressing sintering in the step (2) comprises sequentially performing first heating, first sintering, second heating, second sintering, third heating, third sintering, pressurizing and maintaining pressure; namely, the step (2) is as follows:
(2) Filling the mixture in the step (1) into a mold, wherein the mold adopted in the mold filling process comprises a graphite mold; pre-pressing for 5min under the pressure of 1.5 MPa; performing vacuum hot-pressing sintering under the vacuum degree of 50Pa to obtain a chromium silicon carbon alloy target;
wherein, the vacuum hot press sintering includes: first heating at a heating rate of 10 ℃/min, and first sintering at 600 ℃ for 0.8h; carrying out second heating at a heating rate of 10 ℃/min, and carrying out second sintering at 900 ℃ for 0.8h; heating up at a heating rate of 5 ℃/min, and sintering at 1200 ℃ for 2 hours; controlling the pressure in the die to be 6MPa during the first temperature rise, the first sintering, the second temperature rise, the second sintering, the third temperature rise and the third sintering; pressurizing to 35MPa at a rate of 0.3MPa/h, and maintaining the pressure for 25min.
Comparative example 3
The comparative example provides a chromium silicon carbon alloy target and a preparation method thereof, and the preparation method described with reference to the embodiment 1 is only different in that: the vacuum hot-pressing sintering in the step (2) comprises a first heating, a first sintering, a second heating, a second sintering, a third heating and a third sintering which are sequentially carried out; namely, the step (2) is as follows:
(2) Filling the mixture in the step (1) into a mold, wherein the mold adopted in the mold filling process comprises a graphite mold; pre-pressing for 5min under the pressure of 1.5 MPa; performing vacuum hot-pressing sintering under the vacuum degree of 50Pa to obtain a chromium silicon carbon alloy target;
wherein, the vacuum hot press sintering includes: first heating at a heating rate of 10 ℃/min, and first sintering at 600 ℃ for 0.8h; carrying out second heating at a heating rate of 10 ℃/min, and carrying out second sintering at 900 ℃ for 0.8h; heating up at a heating rate of 5 ℃/min, and sintering at 1200 ℃ for 2 hours; and controlling the pressure in the die to be 6MPa during the first temperature rise, the first sintering, the second temperature rise, the second sintering, the third temperature rise and the third sintering.
The performance of the chromium silicon carbon alloy targets obtained in the above examples and comparative examples was tested, and the test contents and methods are as follows:
density: actual density ρ Actual practice is that of And theoretical density ρ Theory of The ratio of (a) is the density, i.e., density=ρ Actual practice is that of /ρ Theory of 100% of the chromium silicon carbon alloy target material, and testing the actual density of the chromium silicon carbon alloy target material by adopting a wide-range solid density tester;
conductivity fluctuation: the chromium silicon carbon alloy target is detected by using a conductivity meter, and the larger the conductivity fluctuation is, the worse the target uniformity is, the fluctuation is generally more than +/-10%, and the target structure is considered to be uneven.
The test results of the chromium silicon carbon alloy targets obtained in the above examples and comparative examples are shown in table 1.
TABLE 1
Project Density is% Conductivity fluctuation%
Example 1 99.7 4.1
Example 2 99.8 3.8
Example 3 99.3 5.9
Example 4 96.1 14.0
Example 5 99.9 (presence of cracking) -
Example 6 97.5 13.7
Example 7 99.7 4.7
Comparative example 1 97.2 11.3
Comparative example 2 98.0 10.6
Comparative example 3 90.9 15.9
From table 1, the following points can be found:
(1) It can be seen from examples 1-3 that the preparation method of the chromium-silicon-carbon alloy target material of the invention completes vacuum hot-press sintering through first heating, first sintering, second heating, second sintering, third heating, third sintering, first pressurizing, second pressurizing and pressure maintaining, and solves the problems of insufficient density, holes in the interior and uneven components of the target material; the density of the obtained chromium-silicon-carbon alloy target material is more than or equal to 99%, the conductivity fluctuation is small, and the microcosmic uniformity is realized;
(2) Comparing example 1 with examples 4 and 5, it can be seen that the density is reduced due to the fact that the temperature of the third sintering in step (2) in example 4 is 1000 ℃ which is lower than the preferred 1150-1350 ℃ according to the invention; because the temperature of the third sintering in the step (2) in the embodiment 5 is 1500 ℃ which exceeds 1150-1350 ℃ which is preferable in the invention, the overburning is caused, the internal stress is increased, and the cracking is generated;
(3) Comparing example 1 with examples 6 and 7, it can be seen that, since the pressure of the pressure maintaining in step (2) in example 6 is 25MPa and is lower than the preferred 28-38 MPa of the present invention, the density of the obtained chromium-silicon-carbon alloy target is reduced, the fluctuation of conductivity is increased, and the target is uneven; in the embodiment 7, the pressure of the pressure maintaining in the step (2) is 42MPa, which exceeds the preferable pressure of 28-38 MPa, the influence on density and conductivity fluctuation is not great, but the excessively high pressure can increase energy consumption and reduce economic benefit in actual production;
(4) Comparing example 1 with comparative examples 1 to 3, it can be seen that the vacuum hot press sintering of step (2) of comparative example 1 includes sequentially heating, sintering, first pressurizing, second pressurizing, and pressure maintaining; since comparative example 1 did not perform temperature rise and sintering in stages, the density was lowered to some extent, and the target was not uniform; the vacuum hot-pressed sintering in the step (2) in the comparative example 2 comprises sequentially performing first heating, first sintering, second heating, second sintering, third heating, third sintering, pressurizing and maintaining pressure; since comparative example 2 was not subjected to the staged pressurization, the density of the target was lowered to some extent, and the target was not uniform; the vacuum hot press sintering in the step (2) in the comparative example 3 comprises a first heating, a first sintering, a second heating, a second sintering, a third heating and a third sintering which are sequentially performed; since the first pressurization, the second pressurization and the pressure maintaining are omitted in comparative example 3, the density of the target material is greatly reduced, and the target material is not uniform.
While the foregoing is directed to embodiments of the present invention, other and further details of the invention may be had by the present invention, it should be understood that the foregoing description is merely illustrative of the present invention and that no limitations are intended to the scope of the invention, except insofar as modifications, equivalents, improvements or modifications are within the spirit and principles of the invention.

Claims (33)

1. The preparation method of the chromium silicon carbon alloy target is characterized by comprising the following steps of:
(1) Mixing chromium silicon alloy powder, silicon carbide powder and chromium powder to obtain a mixture;
(2) Carrying out vacuum hot-pressing sintering on the mixture obtained in the step (1) to obtain a chromium silicon carbon alloy target;
the vacuum hot-pressing sintering comprises a first heating, a first sintering, a second heating, a second sintering, a third heating, a third sintering, a first pressurizing, a second pressurizing and a pressure maintaining which are sequentially carried out;
the temperature of the first sintering in the step (2) is 500-600 ℃;
the time of the first sintering in the step (2) is 0.5-1 h;
the temperature of the second sintering in the step (2) is 800-900 ℃;
the second sintering time in the step (2) is 0.5-1 h;
the temperature of the third sintering in the step (2) is 1150-1350 ℃;
and (3) the time of the third sintering in the step (2) is more than or equal to 1h.
2. The method according to claim 1, wherein the chromium-silicon alloy powder in step (1) contains 50 to 70% of chromium and the balance silicon.
3. The method according to claim 1, wherein the chromium-silicon alloy powder in the step (1) has a particle diameter of 75 μm or less.
4. The method according to claim 1, wherein the silicon carbide powder in the step (1) has a particle diameter of 20 μm or less.
5. The method according to claim 1, wherein the chromium powder in the step (1) has a particle diameter of 10 μm or less.
6. The method according to claim 1, wherein the purity of the chromium silicon alloy powder, the silicon carbide powder and the chromium powder in the step (1) is not less than 99.95%.
7. The method according to claim 1, wherein the mixture in step (1) has a silicon content of 40 to 55wt%, a carbon content of 2 to 12wt% and the balance chromium.
8. The method of claim 1, wherein the mixing in step (1) is performed in a shielding gas.
9. The method of claim 8, wherein the shielding gas comprises nitrogen and/or argon.
10. The method of claim 1, wherein the mixing in step (1) is by ball milling.
11. The method according to claim 10, wherein the ball ratio of the ball mill is (5-8): 1.
12. The method of claim 1, wherein the mixing of step (1) is performed in a polyurethane liner powder mixer.
13. The method according to claim 1, wherein the mixing time in step (1) is not less than 36 hours.
14. The method according to claim 1, wherein the mixture of step (1) is sequentially subjected to die filling and prepressing before the vacuum hot press sintering of step (2).
15. The method of claim 14, wherein the mold used in the molding comprises a graphite mold.
16. The method of claim 14, wherein the pre-compaction is at a pressure of < 2MPa.
17. The method of claim 16, wherein the pre-pressing time is 3 to 10 minutes.
18. The method according to claim 1, wherein the degree of vacuum in the vacuum hot-press sintering in the step (2) is not more than 100Pa.
19. The method according to claim 1, wherein the first temperature rise in step (2) is performed at a temperature rise rate of 5 to 10 ℃/min.
20. The method of claim 1, wherein the first elevated end point temperature of step (2) is the same as the first sintering temperature.
21. The method according to claim 1, wherein the second temperature rise in step (2) is performed at a temperature rise rate of 5 to 10 ℃/min.
22. The method of claim 1, wherein the second elevated temperature of step (2) has an end temperature that is the same as the second sintering temperature.
23. The method according to claim 1, wherein the third temperature rise in step (2) is performed at a temperature rise rate of 1 to 5 ℃/min.
24. The method according to claim 1, wherein the third elevated temperature in step (2) has an end temperature identical to the third sintering temperature.
25. The method according to claim 1, wherein the first temperature rise, the first sintering, the second temperature rise, the second sintering, the third temperature rise and the third sintering in the step (2) are all performed while maintaining the pressure in the mold to be equal to or less than 6MPa.
26. The method of claim 1, wherein the first pressurization in step (2) is at a rate of 0.1 to 0.3MPa/h.
27. The method according to claim 1, wherein the first pressurization in step (2) has an end pressure of 15 to 22MPa.
28. The method of claim 1, wherein the second pressurization in step (2) is performed at a rate of 0.01 to 0.1MPa/h.
29. The production method according to claim 1, wherein the second pressurization end pressure of step (2) is the same as the holding pressure.
30. The method according to claim 1, wherein the pressure of the holding pressure in the step (2) is 28 to 38MPa.
31. The method according to claim 1, wherein the dwell time in step (2) is 60 to 180 minutes.
32. The preparation method according to claim 1, characterized in that the preparation method comprises the steps of:
(1) Mixing chromium silicon alloy powder, silicon carbide powder and chromium powder in a polyurethane lining powder mixer, controlling the mixing time to be more than or equal to 36 hours to obtain a mixture, controlling the silicon content in the mixture to be 40-55wt%, the carbon content to be 2-12wt% and the balance to be chromium;
wherein, the chromium content in the chromium-silicon alloy powder is 50-70 percent, and the rest is silicon; the grain diameter of the chromium silicon alloy powder is less than or equal to 75 mu m; the grain diameter of the silicon carbide powder is less than or equal to 20 mu m; the grain diameter of the chromium powder is less than or equal to 10 mu m; the purities of the chromium silicon alloy powder, the silicon carbide powder and the chromium powder are all more than or equal to 99.95 percent; mixing is carried out under nitrogen and/or argon; the mixing mode is ball milling; ball ratio of ball milling is (5-8): 1;
(2) Filling the mixture in the step (1) into a mold, wherein the mold adopted in the mold filling process comprises a graphite mold; prepressing for 3-10 min under the pressure less than 2 MPa; vacuum hot-pressing sintering is carried out under the vacuum degree of less than or equal to 100Pa, and the chromium silicon carbon alloy target is obtained;
wherein, the vacuum hot press sintering includes: first heating at a heating rate of 5-10 ℃/min, and first sintering at 500-600 ℃ for 0.5-1 h; carrying out second heating at a heating rate of 5-10 ℃/min, and carrying out second sintering at 800-900 ℃ for 0.5-1 h; heating up at a heating rate of 1-5 ℃/min, and sintering at 1150-1350 ℃ for more than or equal to 1h; controlling the pressure in the die to be less than or equal to 6MPa during the first temperature rise, the first sintering, the second temperature rise, the second sintering, the third temperature rise and the third sintering; the first pressurization is carried out to 15 to 22MPa at the rate of 0.1 to 0.3MPa/h, then the second pressurization is carried out to 28 to 38MPa at the rate of 0.01 to 0.1MPa/h, and the pressure is maintained for 60 to 180 minutes.
33. A chrome silicon carbon alloy target, characterized in that the chrome silicon carbon alloy target is prepared by the preparation method of any one of claims 1-32.
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