CN113770360B - Chromium silicon alloy sputtering target material and preparation method thereof - Google Patents
Chromium silicon alloy sputtering target material and preparation method thereof Download PDFInfo
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- CN113770360B CN113770360B CN202111048524.4A CN202111048524A CN113770360B CN 113770360 B CN113770360 B CN 113770360B CN 202111048524 A CN202111048524 A CN 202111048524A CN 113770360 B CN113770360 B CN 113770360B
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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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—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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Abstract
The invention provides a chromium silicon alloy sputtering target material and a preparation method thereof, wherein the preparation method comprises the following steps: (1) Screening the chromium-silicon alloy raw material with the purity of more than or equal to 99.98 percent to obtain chromium-silicon alloy powder; (2) Carrying out vacuum hot-pressing sintering treatment on the chromium-silicon alloy powder obtained in the step (1) to obtain a chromium-silicon alloy target blank; (3) Machining the chromium-silicon alloy target blank obtained in the step (2) to obtain a chromium-silicon alloy sputtering target material; the vacuum hot-pressed sintering treatment in the step (2) comprises a first heat preservation treatment, a second heat preservation treatment and a heat preservation and pressure maintaining treatment which are sequentially carried out, and the pressurizing process of the heat preservation and pressure maintaining treatment is divided into at least 2 pressurizing stages. The preparation method provided by the invention ensures the high density of the target material, improves the uniformity of the microstructure and the sputtering performance, simplifies the process flow, improves the production efficiency, reduces the production cost and widens the application range.
Description
Technical Field
The invention belongs to the technical field of sputtering targets, relates to a chromium-silicon alloy sputtering target, and particularly relates to a chromium-silicon alloy sputtering target and a preparation method thereof.
Background
In recent years, 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 chromium silicon targets are 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.
CN 105331939a discloses a silicon-containing alloy target and a preparation method thereof, wherein the preparation method comprises five steps of prealloyed powder preparation, cold isostatic pressing treatment after die filling, degassing treatment after re-covering, hot isostatic pressing treatment and machining treatment. Although the preparation method can prepare the target material with low impurity element content, high purity, high density, fine grains and uniform microstructure, the preparation method needs at least two die filling treatments and comprises the pressing treatment of combining cold isostatic pressing, degassing and hot isostatic pressing, and has the defects of complex process, higher energy consumption and higher cost.
CN 110257781a discloses a chromium aluminum silicon nickel quaternary alloy target and a preparation method thereof, wherein the preparation method comprises the steps of powder mixing, cold isostatic pressing pre-pressing after die filling, crushing of pre-pressed alloy blocks into metal particles, vacuum sintering pre-alloying, crushing of pre-alloyed blocks into metal powder, degassing treatment after packaging, hot isostatic pressing treatment and machining. Although the chromium aluminum silicon nickel quaternary alloy target prepared by the preparation method has the advantages of high compactness, no air holes, no looseness and segregation, fine grains, uniform structure and the like, and can be suitable for sputtering hard coatings required by various tools and dies, the process flow of the invention is too complex, the application range is limited, and the risk of oxidation of products is increased by multi-step operation.
Therefore, how to provide a chromium silicon alloy sputtering target and a preparation method thereof, ensure the high density of the target, improve the uniformity of microstructure and sputtering performance, simplify the process flow, improve the production efficiency, reduce the production cost and widen the application range, and become the urgent problem 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 the chromium-silicon alloy sputtering target material and the preparation method thereof, wherein the preparation method ensures the high density of the target material, improves the microstructure uniformity and the sputtering performance, simplifies the process flow, improves the production efficiency, reduces the production cost and widens the application range.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a chromium silicon alloy sputtering target, the method comprising the steps of:
(1) Screening the chromium-silicon alloy raw material with the purity of more than or equal to 99.98 percent to obtain chromium-silicon alloy powder;
(2) Performing vacuum hot-pressing sintering treatment on the chromium-silicon alloy powder obtained in the step (1) at the sintering temperature of 1000-1300 ℃ and the pressing pressure of 30-40MPa to obtain a chromium-silicon alloy target blank;
(3) And (3) machining the chromium-silicon alloy target blank obtained in the step (2) to obtain the chromium-silicon alloy sputtering target material.
The vacuum hot-pressed sintering treatment in the step (2) comprises a first heat preservation treatment, a second heat preservation treatment and a heat preservation and pressure maintaining treatment which are sequentially carried out, and the pressurizing process of the heat preservation and pressure maintaining treatment is divided into at least 2 pressurizing stages.
According to the invention, the sintering temperature and the pressing pressure of the vacuum hot-pressing sintering treatment are reasonably controlled, the density of the obtained chromium-silicon alloy sputtering target material is increased to more than 99%, the first heat preservation treatment, the second heat preservation treatment and the heat preservation and pressure maintaining treatment are sequentially carried out, the pressurizing process of the heat preservation and pressure maintaining treatment is divided into at least 2 pressurizing stages, the uniformity and the sputtering stability of crystal grains in the target material are further improved, the cracking phenomenon of the target material is avoided, and the microstructure is uniform and has no pores.
In the present invention, the purity of the chromium silicon alloy raw material in the step (1) is not less than 99.98%, for example, 99.98%, 99.99% or 99.999%, but is not limited to the values listed, and other values not listed in the range are equally applicable.
In the present invention, the sintering temperature in the step (2) is 1000 to 1300 ℃, for example, 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃, 1200 ℃, 1250 ℃, or 1300 ℃, but the sintering temperature is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value range are applicable.
In the present invention, the pressing pressure in the step (2) is 30 to 40MPa, and may be, for example, 30MPa, 31MPa, 32MPa, 33MPa, 34MPa, 35MPa, 36MPa, 37MPa, 38MPa, 39MPa or 40MPa, 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 mass ratio of the silicon element in the chromium silicon alloy raw material in the step (1) is 50% -55%, for example, 50%, 50.5%, 51%, 51.5%, 52%, 52.5%, 53%, 53.5%, 54%, 54.5% or 55%, but is not limited to the recited values, and other non-recited values in the range of the values are equally applicable.
Preferably, the average particle size of the chromium silicon alloy powder in the step (1) is not more than 200. Mu.m, for example, 20. Mu.m, 40. Mu.m, 60. Mu.m, 80. Mu.m, 100. Mu.m, 120. Mu.m, 140. Mu.m, 160. Mu.m, 180. Mu.m, or 200. Mu.m, but not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
Preferably, the vacuum hot-pressing sintering treatment in the step (2) comprises die filling, compaction, vacuumizing, first temperature rising, first heat preservation treatment, second temperature rising, second heat preservation treatment, pressurization, heat preservation and pressure maintaining treatment, pressure removal and cooling which are sequentially performed.
Preferably, the die-filling body is: the chromium-silicon alloy powder is charged into a graphite mold to ensure flatness of 0.5mm or less after the mold is charged, and may be, for example, 0.1mm, 0.15mm, 0.2mm, 0.25mm, 0.3mm, 0.35mm, 0.4mm, 0.45mm or 0.5mm, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the compacting is specifically: the graphite mold is placed in a vacuum sintering furnace and a pressure of 0.8-1.2MPa is applied to the top pressing head, for example, 0.8MPa, 0.85MPa, 0.9MPa, 0.95MPa, 1MPa, 1.05MPa, 1.1MPa, 1.15MPa or 1.2MPa, but the graphite mold is not limited to the recited values, and other non-recited values in the numerical range are applicable.
Preferably, the pressure is applied for a period of time ranging from 4 to 6 minutes, such as 4 minutes, 4.2 minutes, 4.4 minutes, 4.6 minutes, 4.8 minutes, 5 minutes, 5.2 minutes, 5.4 minutes, 5.6 minutes, 5.8 minutes, or 6 minutes, but not limited to the recited values, and other non-recited values within the range are equally applicable.
Preferably, the vacuum is applied to the absolute pressure in the furnace of 100Pa or less, for example, 10Pa, 20Pa, 30Pa, 40Pa, 50Pa, 60Pa, 70Pa, 80Pa, 90Pa or 100Pa, but the vacuum is not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
Preferably, the temperature rising rate of the first temperature rising is 6-8 ℃/min, for example, 6 ℃/min, 6.2 ℃/min, 6.4 ℃/min, 6.6 ℃/min, 6.8 ℃/min, 7 ℃/min, 7.2 ℃/min, 7.4 ℃/min, 7.6 ℃/min, 7.8 ℃/min or 8 ℃/min, but the temperature rising rate is not limited to the recited value, and other non-recited values within the range of the value are equally applicable.
The target temperature of the first temperature increase is preferably 1000 to 1200 ℃, and may be 1000 ℃, 1020 ℃, 1040 ℃, 1060 ℃, 1080 ℃, 1100 ℃, 1120 ℃, 1140 ℃, 1160 ℃, 1180 ℃, or 1200 ℃, for example, but is not limited to the values listed, and other values not listed in the range are equally applicable.
Preferably, the time of the first heat-preserving treatment is 40-80min, for example, 40min, 45min, 50min, 55min, 60min, 65min, 70min, 75min or 80min, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the second temperature is raised at a temperature-raising rate of 2-4 ℃/min, for example, 2 ℃/min, 2.2 ℃/min, 2.4 ℃/min, 2.6 ℃/min, 2.8 ℃/min, 3 ℃/min, 3.2 ℃/min, 3.4 ℃/min, 3.6 ℃/min, 3.8 ℃/min or 4 ℃/min, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the target temperature of the second temperature rise is 1250-1300 ℃, for example 1250 ℃, 1260 ℃, 1270 ℃, 1280 ℃, 1290 ℃ or 1300 ℃, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the second incubation time is 60-100min, for example, 60min, 65min, 70min, 75min, 80min, 85min, 90min, 95min or 100min, but not limited to the recited values, and other non-recited values within the range are equally applicable.
Preferably, the pressurizing process is divided into 2 pressurizing stages, namely a first pressurizing stage and a second pressurizing stage, which are performed sequentially.
Preferably, the pressurizing rate of the first pressurizing stage is 0.3-0.5MPa/min, for example, but not limited to, the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the target pressure of the first pressurizing stage is 20 to 30MPa, for example, 20MPa, 21MPa, 22MPa, 23MPa, 24MPa, 25MPa, 26MPa, 27MPa, 28MPa, 29MPa or 30MPa, but the target pressure is not limited to the recited values, and other non-recited values within the range are equally applicable.
Preferably, the pressurizing rate of the second pressurizing stage is 0.2-0.3MPa/min, for example, but not limited to, the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the target pressure of the second pressurizing stage is 35-40MPa, for example, 35MPa, 35.5MPa, 36MPa, 36.5MPa, 37MPa, 37.5MPa, 38MPa, 38.5MPa, 39MPa, 39.5MPa or 40MPa, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the time of the heat and pressure maintaining treatment is 100-150min, for example, 100min, 105min, 110min, 115min, 120min, 125min, 130min, 135min, 140min, 145min or 150min, but not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
Preferably, the pressure relief is specifically: the vacuum sintering furnace is charged with nitrogen and/or argon to an absolute pressure of 0.02 to 0.04MPa, for example, 0.02MPa, 0.022MPa, 0.024MPa, 0.026MPa, 0.028MPa, 0.03MPa, 0.032MPa, 0.034MPa, 0.036MPa, 0.038MPa or 0.04MPa, but the present invention is not limited to the above-mentioned values, and other non-mentioned values in the above-mentioned values are equally applicable.
Preferably, the cooling is specifically: when the mold is cooled to a temperature of 200 ℃ or less with the furnace, the mold is taken out and dried to room temperature, for example, 50 ℃, 60 ℃, 80 ℃, 100 ℃, 120 ℃, 140 ℃, 160 ℃, 180 ℃ or 200 ℃, but the mold is not limited to the listed values, and other non-listed values within the range of the values are applicable.
Preferably, the machining in step (3) comprises sequentially performing grinding, cutting, finishing, surface treatment, cleaning, drying and packaging.
As a preferred technical solution of the first aspect of the present invention, the preparation method includes the following steps:
(1) Screening the chromium-silicon alloy raw material with the purity of more than or equal to 99.98 percent to obtain chromium-silicon alloy powder with the average granularity of less than or equal to 200 mu m; the mass ratio of silicon element in the chromium-silicon alloy raw material is 50% -55%;
(2) Carrying out vacuum hot-pressing sintering treatment on the chromium-silicon alloy powder obtained in the step (1) to obtain a chromium-silicon alloy target blank; the vacuum hot-pressing sintering treatment specifically comprises the following steps:
(A) Chromium silicon alloy powder is filled into a graphite mold, and flatness after mold filling is ensured to be less than or equal to 0.5mm;
(B) Placing the graphite mold into a vacuum sintering furnace, and applying pressure of 0.8-1.2MPa on a top pressing head and keeping the pressure for 4-6min;
(C) Vacuumizing until the absolute pressure in the furnace is less than or equal to 100Pa;
(D) Heating to 1000-1200deg.C at a rate of 6-8deg.C/min, and maintaining the temperature for 40-80min;
(E) Heating to 1250-1300 ℃ at a speed of 2-4 ℃/min, and preserving heat for 60-100min;
(F) Pressurizing to 20-30MPa at a rate of 0.3-0.5MPa/min, pressurizing to 35-40MPa at a rate of 0.2-0.3MPa/min, and maintaining the temperature and pressure for 100-150min;
(G) Filling nitrogen and/or argon into the vacuum sintering furnace until the absolute pressure in the furnace is 0.02-0.04MPa;
(H) Cooling the mold along with the furnace to a temperature less than or equal to 200 ℃, taking out the mold and airing to room temperature;
(3) And (3) sequentially carrying out grinding, cutting, finishing, surface treatment, cleaning, drying and packaging on the chromium-silicon alloy target blank obtained in the step (2) to obtain the chromium-silicon alloy sputtering target material.
In a second aspect, the present invention provides a chromium silicon alloy sputtering target prepared by the preparation method according to the first aspect.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the sintering temperature and the pressing pressure of the vacuum hot-pressing sintering treatment are reasonably controlled, the density of the obtained chromium-silicon alloy sputtering target material is increased to more than 99%, the first heat preservation treatment, the second heat preservation treatment and the heat preservation and pressure maintaining treatment are sequentially carried out, the pressurizing process of the heat preservation and pressure maintaining treatment is divided into at least 2 pressurizing stages, the uniformity and the sputtering stability of crystal grains in the target material are further improved, the cracking phenomenon of the target material is avoided, and the microstructure is uniform and has no pores.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments.
Example 1
The embodiment provides a chromium silicon alloy sputtering target material and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Screening the chromium-silicon alloy raw material with the purity of more than or equal to 99.99 percent to obtain chromium-silicon alloy powder with the average granularity of 100 mu m; the mass ratio of silicon element in the chromium-silicon alloy raw material is 52%;
(2) Carrying out vacuum hot-pressing sintering treatment on the chromium-silicon alloy powder obtained in the step (1) to obtain a chromium-silicon alloy target blank; the vacuum hot-pressing sintering treatment specifically comprises the following steps:
(A) Putting chromium-silicon alloy powder into a graphite die, and ensuring the flatness of the die to be 0.3+/-0.1 mm;
(B) Placing the graphite mold into a vacuum sintering furnace, applying pressure of 1MPa on a top pressing head, and keeping for 5min;
(C) Vacuumizing until the absolute pressure in the furnace is 80Pa;
(D) Heating to 1100 ℃ at a speed of 7 ℃/min, and preserving heat for 60min;
(E) Heating to 1270 ℃ at a speed of 3 ℃/min, and preserving heat for 80min;
(F) Pressurizing to 25MPa at a rate of 0.4MPa/min, pressurizing to 38MPa at a rate of 0.25MPa/min, and maintaining the temperature and pressure for 120min;
(G) Filling nitrogen into the vacuum sintering furnace until the absolute pressure in the furnace is 0.03MPa;
(H) Cooling the mold to 150 ℃ along with the furnace, taking out the mold and airing to room temperature;
(3) And (3) grinding, cutting, finishing, surface treatment, cleaning, drying and packaging the chromium-silicon alloy target blank obtained in the step (2) in sequence according to the specified size of a customer to obtain the chromium-silicon alloy sputtering target material.
Example 2
The embodiment provides a chromium silicon alloy sputtering target material and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Screening the chromium-silicon alloy raw material with the purity of more than or equal to 99.98 percent to obtain chromium-silicon alloy powder with the average granularity of 150 mu m; the mass ratio of silicon element in the chromium-silicon alloy raw material is 50%;
(2) Carrying out vacuum hot-pressing sintering treatment on the chromium-silicon alloy powder obtained in the step (1) to obtain a chromium-silicon alloy target blank; the vacuum hot-pressing sintering treatment specifically comprises the following steps:
(A) Putting chromium-silicon alloy powder into a graphite die, and ensuring the flatness of the die to be 0.3+/-0.1 mm;
(B) Placing the graphite mold into a vacuum sintering furnace, applying pressure of 0.8MPa on a top pressing head, and keeping for 6min;
(C) Vacuumizing until the absolute pressure in the furnace is 90Pa;
(D) Heating to 1000 ℃ at a speed of 6 ℃/min, and preserving heat for 80min;
(E) Heating to 1250 ℃ at a rate of 2 ℃/min, and preserving heat for 100min;
(F) Pressurizing to 20MPa at a rate of 0.3MPa/min, pressurizing to 35MPa at a rate of 0.2MPa/min, and maintaining the temperature and pressure for 150min;
(G) Argon is filled into the vacuum sintering furnace until the absolute pressure in the furnace is 0.02MPa;
(H) Cooling the mold to 150 ℃ along with the furnace, taking out the mold and airing to room temperature;
(3) And (3) grinding, cutting, finishing, surface treatment, cleaning, drying and packaging the chromium-silicon alloy target blank obtained in the step (2) in sequence according to the specified size of a customer to obtain the chromium-silicon alloy sputtering target material.
Example 3
The embodiment provides a chromium silicon alloy sputtering target material and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Screening the chromium-silicon alloy raw material with the purity of more than or equal to 99.98 percent to obtain chromium-silicon alloy powder with the average granularity of 200 mu m; the mass ratio of silicon element in the chromium-silicon alloy raw material is 55%;
(2) Carrying out vacuum hot-pressing sintering treatment on the chromium-silicon alloy powder obtained in the step (1) to obtain a chromium-silicon alloy target blank; the vacuum hot-pressing sintering treatment specifically comprises the following steps:
(A) Putting chromium-silicon alloy powder into a graphite die, and ensuring the flatness of the die to be 0.4+/-0.1 mm;
(B) Placing the graphite mold into a vacuum sintering furnace, and applying pressure of 1.2MPa on a top pressing head and keeping for 4min;
(C) Vacuumizing until the absolute pressure in the furnace is 100Pa;
(D) Raising the temperature to 1200 ℃ at the speed of 8 ℃/min, and preserving the temperature for 40min;
(E) Raising the temperature to 1300 ℃ at the speed of 4 ℃/min, and preserving the temperature for 60min;
(F) Pressurizing to 30MPa at a rate of 0.5MPa/min, pressurizing to 40MPa at a rate of 0.3MPa/min, and maintaining the temperature and pressure for 100min;
(G) Charging nitrogen into the vacuum sintering furnace until the absolute pressure in the furnace is 0.04MPa;
(H) Cooling the mold to 200 ℃ along with the furnace, taking out the mold and airing to room temperature;
(3) And (3) grinding, cutting, finishing, surface treatment, cleaning, drying and packaging the chromium-silicon alloy target blank obtained in the step (2) in sequence according to the specified size of a customer to obtain the chromium-silicon alloy sputtering target material.
Example 4
The present embodiment provides a chromium silicon alloy sputtering target and a preparation method thereof, and the preparation method changes the heat preservation time in the step (D) to 30min, and the other conditions are the same as those in the embodiment 1, so that no description is repeated here.
Example 5
The present embodiment provides a chromium silicon alloy sputtering target and a preparation method thereof, and the preparation method changes the heat preservation time in the step (E) to 50min, and the other conditions are the same as those in the embodiment 1, so that no description is repeated here.
Example 6
The present embodiment provides a chromium silicon alloy sputtering target and a preparation method thereof, and the preparation method is the same as that of embodiment 1 except that the heat preservation and pressure maintaining time in the step (F) is changed to 90min, so that no description is repeated here.
Comparative example 1
The comparative example provides a chromium silicon alloy sputtering target and a preparation method thereof, and the preparation method is the same as that of example 1 except that the temperature of the target temperature for heating in the step (D) is changed to 900 ℃, so that no description is repeated here.
Comparative example 2
The comparative example provides a chromium silicon alloy sputtering target and a preparation method thereof, and the preparation method is the same as that of example 1 except that the target temperature for heating in step (E) is changed to 1400 ℃, so that the description thereof is omitted.
Comparative example 3
The comparative example provides a chromium silicon alloy sputtering target and a preparation method thereof, and the preparation method is the same as that of example 1 except that the final pressing pressure of the pressing in the step (F) is changed to 28MPa, so that the description thereof is omitted.
Comparative example 4
The comparative example provides a chromium silicon alloy sputtering target and a method for producing the same, and the method for producing the same is the same as that of example 1 except that the final pressing pressure in the step (F) is changed to 45MPa, so that the description thereof will not be repeated here.
Comparative example 5
The comparative example provides a chromium silicon alloy sputtering target and a method for producing the same except that step (F) is changed to: pressurizing to 38MPa at a rate of 0.4MPa/min, maintaining the temperature and the pressure for 120min, and keeping the rest conditions in the same manner as in the embodiment 1, so that no description is given here.
Comparative example 6
The embodiment provides a chromium silicon alloy sputtering target material and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Screening the chromium-silicon alloy raw material with the purity of more than or equal to 99.99 percent to obtain chromium-silicon alloy powder with the average granularity of 100 mu m; the mass ratio of silicon element in the chromium-silicon alloy raw material is 52%;
(2) Carrying out vacuum hot-pressing sintering treatment on the chromium-silicon alloy powder obtained in the step (1) to obtain a chromium-silicon alloy target blank; the vacuum hot-pressing sintering treatment specifically comprises the following steps:
(A) Putting chromium-silicon alloy powder into a graphite die, and ensuring the flatness of the die to be 0.3+/-0.1 mm;
(B) Placing the graphite mold into a vacuum sintering furnace, applying pressure of 1MPa on a top pressing head, and keeping for 5min;
(C) Vacuumizing until the absolute pressure in the furnace is 80Pa;
(D) Heating to 1270 ℃ at a speed of 7 ℃/min, pressurizing to 38MPa at a speed of 0.4MPa/min, and maintaining the temperature and pressure for 260min;
(E) Filling nitrogen into the vacuum sintering furnace until the absolute pressure in the furnace is 0.03MPa;
(F) Cooling the mold to 150 ℃ along with the furnace, taking out the mold and airing to room temperature;
(3) And (3) grinding, cutting, finishing, surface treatment, cleaning, drying and packaging the chromium-silicon alloy target blank obtained in the step (2) in sequence according to the specified size of a customer to obtain the chromium-silicon alloy sputtering target material.
The results of performance testing of the tungsten carbide targets obtained in examples 1 to 6 and comparative examples 1 to 6 are shown in Table 1.
TABLE 1
In the table, the density of the target is measured by an Archimedes drainage method; measuring the purity of the target material by a GDMS method; and observing whether the microstructure has pores or not by combining with a scanning electron microscope photograph of the surface of the target.
As can be seen from table 1: the chromium-silicon alloy sputtering target material obtained in the examples 1-6 has excellent performance, the density is more than or equal to 99%, the cracking phenomenon is avoided, and the microstructure is uniform and bubble-free; comparative examples 1-4 show that unreasonable setting of sintering temperature and pressing pressure in the vacuum hot-pressed sintering treatment can bring adverse effects to the target performance; comparative example 5 the pressurizing process was changed to 1 pressurizing stage on the basis of example 1, resulting in a significant decrease in the density of the target, and a certain number of air holes were present in the microstructure; comparative example 6 the heating process and the pressurizing process were performed simultaneously on the basis of example 1, i.e., the first heat-preserving treatment and the second heat-preserving treatment were removed, and the overall properties of the target material were also lowered, affecting the microstructure uniformity thereof.
Therefore, the sintering temperature and the pressing pressure of the vacuum hot-pressing sintering treatment are reasonably controlled, the compactness of the obtained chromium-silicon alloy sputtering target material is increased to more than 99%, the first heat preservation treatment, the second heat preservation treatment and the heat preservation and pressure maintaining treatment are sequentially carried out, the pressurizing process of the heat preservation and pressure maintaining treatment is divided into at least 2 pressurizing stages, the uniformity and the sputtering stability of crystal grains in the target material are further improved, the cracking phenomenon of the target material is avoided, and the microstructure is uniform and has no air holes.
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 (20)
1. The preparation method of the chromium silicon alloy sputtering target material is characterized by comprising the following steps of:
(1) Screening the chromium-silicon alloy raw material with the purity of more than or equal to 99.98 percent to obtain chromium-silicon alloy powder;
(2) Performing vacuum hot-pressing sintering treatment on the chromium-silicon alloy powder obtained in the step (1) at the sintering temperature of 1000-1300 ℃ and the pressing pressure of 30-40MPa to obtain a chromium-silicon alloy target blank;
(3) Machining the chromium-silicon alloy target blank obtained in the step (2) to obtain a chromium-silicon alloy sputtering target material;
the vacuum hot-pressed sintering treatment in the step (2) comprises a first heating, a first heat preservation treatment, a second heating, a second heat preservation treatment, pressurizing and heat preservation pressure maintaining treatment which are sequentially carried out, wherein the pressurizing process of the heat preservation pressure maintaining treatment is divided into 2 pressurizing stages, namely a first pressurizing stage and a second pressurizing stage which are sequentially carried out;
the pressurizing rate of the first pressurizing stage is 0.3-0.5MPa/min, and the target pressure is 20-30MPa; the pressurizing rate of the second pressurizing stage is 0.2-0.3MPa/min, and the target pressure is 35-40MPa.
2. The preparation method according to claim 1, wherein the mass ratio of silicon element in the chromium-silicon alloy raw material in the step (1) is 50% -55%.
3. The method according to claim 1, wherein the average particle size of the chromium-silicon alloy powder in the step (1) is 200 μm or less.
4. The method according to claim 1, wherein the vacuum hot-press sintering process in step (2) comprises die-filling, compacting, vacuumizing, first heating, first heat-preserving process, second heating, second heat-preserving process, pressurizing, heat-preserving and pressure-maintaining process, pressure-removing and cooling, which are sequentially performed.
5. The method according to claim 4, wherein the die-filling body comprises: and (3) filling chromium-silicon alloy powder into a graphite die, and ensuring flatness of the die to be less than or equal to 0.5mm.
6. The method according to claim 4, wherein the compacting is in particular: and (3) placing the graphite mould into a vacuum sintering furnace, and applying pressure of 0.8-1.2MPa on a top pressing head.
7. The method according to claim 6, wherein the pressure is applied for 4 to 6 minutes.
8. The method according to claim 4, wherein the vacuum is applied to a furnace absolute pressure of 100Pa or less.
9. The method according to claim 4, wherein the first temperature is raised at a temperature-raising rate of 6 to 8 ℃/min.
10. The method of claim 4, wherein the first elevated target temperature is 1000-1200 ℃.
11. The method according to claim 4, wherein the first heat-retaining treatment is performed for 40 to 80 minutes.
12. The method according to claim 4, wherein the second temperature is raised at a temperature-raising rate of 2 to 4 ℃/min.
13. The method according to claim 4, wherein the target temperature of the second elevated temperature is 1250 to 1300 ℃.
14. The method according to claim 4, wherein the second heat-retaining treatment is performed for 60 to 100 minutes.
15. The method according to claim 4, wherein the time for the heat-retaining and pressure-retaining treatment is 100 to 150 minutes.
16. The method according to claim 4, wherein the pressure release is specifically: and (3) charging nitrogen and/or argon into the vacuum sintering furnace until the absolute pressure in the furnace is 0.02-0.04MPa.
17. The method according to claim 4, wherein the cooling is specifically: and taking out the mould and airing to room temperature after the temperature of the mould is cooled to be less than or equal to 200 ℃ along with the furnace.
18. The method of claim 1, wherein the machining in step (3) comprises sequentially performing grinding, cutting, finishing, surface treatment, cleaning, drying, and packaging.
19. The preparation method according to any one of claims 1 to 18, characterized in that the preparation method comprises the steps of:
(1) Screening the chromium-silicon alloy raw material with the purity of more than or equal to 99.98 percent to obtain chromium-silicon alloy powder with the average granularity of less than or equal to 200 mu m; the mass ratio of silicon element in the chromium-silicon alloy raw material is 50% -55%;
(2) Carrying out vacuum hot-pressing sintering treatment on the chromium-silicon alloy powder obtained in the step (1) to obtain a chromium-silicon alloy target blank; the vacuum hot-pressing sintering treatment specifically comprises the following steps:
(A) Chromium silicon alloy powder is filled into a graphite mold, and flatness after mold filling is ensured to be less than or equal to 0.5mm;
(B) Placing the graphite mold into a vacuum sintering furnace, and applying pressure of 0.8-1.2MPa on a top pressing head and keeping the pressure for 4-6min;
(C) Vacuumizing until the absolute pressure in the furnace is less than or equal to 100Pa;
(D) Heating to 1000-1200deg.C at a rate of 6-8deg.C/min, and maintaining the temperature for 40-80min;
(E) Heating to 1250-1300 ℃ at a speed of 2-4 ℃/min, and preserving heat for 60-100min;
(F) Pressurizing to 20-30MPa at a rate of 0.3-0.5MPa/min, pressurizing to 35-40MPa at a rate of 0.2-0.3MPa/min, and maintaining the temperature and pressure for 100-150min;
(G) Filling nitrogen and/or argon into the vacuum sintering furnace until the absolute pressure in the furnace is 0.02-0.04MPa;
(H) Cooling the mold along with the furnace to a temperature less than or equal to 200 ℃, taking out the mold and airing to room temperature;
(3) And (3) sequentially carrying out grinding, cutting, finishing, surface treatment, cleaning, drying and packaging on the chromium-silicon alloy target blank obtained in the step (2) to obtain the chromium-silicon alloy sputtering target material.
20. A chromium silicon alloy sputtering target prepared by the preparation method according to any one of claims 1 to 19.
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| CN114540692B (en) * | 2022-03-29 | 2022-12-13 | 宁波江丰电子材料股份有限公司 | Vanadium-tungsten alloy target material and preparation method and application thereof |
| CN114799175B (en) * | 2022-04-24 | 2023-09-12 | 宁波江丰电子材料股份有限公司 | Chromium silicon carbon alloy target and preparation method thereof |
| CN115110044B (en) * | 2022-07-25 | 2023-09-12 | 宁波江丰电子材料股份有限公司 | Preparation method of chromium-silicon alloy sputtering target material |
| CN115213411B (en) * | 2022-07-26 | 2024-02-27 | 先导薄膜材料（广东）有限公司 | Low-oxygen uniform chromium silicon target material and preparation method thereof |
| CN115745603B (en) * | 2022-10-17 | 2023-08-29 | 河北东同光电科技有限公司 | Preparation method of large-size high-performance niobium oxide target |
| CN116804267A (en) * | 2023-07-06 | 2023-09-26 | 宁波江丰电子材料股份有限公司 | Chromium silicon target material and preparation method and application thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009197334A (en) * | 2009-05-07 | 2009-09-03 | Toshiba Corp | Method for manufacturing sputtering target, method for forming hard film and hard film coated member using the same |
| CN101638771A (en) * | 2008-07-28 | 2010-02-03 | 中国钢铁股份有限公司 | Metal-base ceramic composite target material containing noble metals and manufacturing method thereof |
| CN102400004A (en) * | 2011-11-25 | 2012-04-04 | 宁波江丰电子材料有限公司 | Manufacturing methods of tungsten-titanium alloy target billet and target material |
| CN103143710A (en) * | 2013-03-27 | 2013-06-12 | 宁夏东方钽业股份有限公司 | Method of producing molybdenum alloy target |
| CN105568237A (en) * | 2014-10-15 | 2016-05-11 | 宁波江丰电子材料股份有限公司 | Chromium-molybdenum alloy target material preparation method |
| CN111996507A (en) * | 2020-08-14 | 2020-11-27 | 宁波江丰电子材料股份有限公司 | Preparation method of chromium-silicon sputtering target material |
| CN112376023A (en) * | 2020-11-04 | 2021-02-19 | 宁波江丰电子材料股份有限公司 | Preparation method of chromium-silicon alloy sputtering target material |
| CN113073299A (en) * | 2021-03-24 | 2021-07-06 | 宁波江丰电子材料股份有限公司 | Preparation method of chromium-silicon alloy sputtering target material |
-
2021
- 2021-09-08 CN CN202111048524.4A patent/CN113770360B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101638771A (en) * | 2008-07-28 | 2010-02-03 | 中国钢铁股份有限公司 | Metal-base ceramic composite target material containing noble metals and manufacturing method thereof |
| JP2009197334A (en) * | 2009-05-07 | 2009-09-03 | Toshiba Corp | Method for manufacturing sputtering target, method for forming hard film and hard film coated member using the same |
| CN102400004A (en) * | 2011-11-25 | 2012-04-04 | 宁波江丰电子材料有限公司 | Manufacturing methods of tungsten-titanium alloy target billet and target material |
| CN103143710A (en) * | 2013-03-27 | 2013-06-12 | 宁夏东方钽业股份有限公司 | Method of producing molybdenum alloy target |
| CN105568237A (en) * | 2014-10-15 | 2016-05-11 | 宁波江丰电子材料股份有限公司 | Chromium-molybdenum alloy target material preparation method |
| CN111996507A (en) * | 2020-08-14 | 2020-11-27 | 宁波江丰电子材料股份有限公司 | Preparation method of chromium-silicon sputtering target material |
| CN112376023A (en) * | 2020-11-04 | 2021-02-19 | 宁波江丰电子材料股份有限公司 | Preparation method of chromium-silicon alloy sputtering target material |
| CN113073299A (en) * | 2021-03-24 | 2021-07-06 | 宁波江丰电子材料股份有限公司 | Preparation method of chromium-silicon alloy sputtering target material |
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