CN112811908A - Silicon carbide composite target material and preparation method thereof - Google Patents

Silicon carbide composite target material and preparation method thereof Download PDF

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CN112811908A
CN112811908A CN202110287506.5A CN202110287506A CN112811908A CN 112811908 A CN112811908 A CN 112811908A CN 202110287506 A CN202110287506 A CN 202110287506A CN 112811908 A CN112811908 A CN 112811908A
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powder
silicon carbide
ball milling
temperature
spray granulation
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姚力军
潘杰
王巨宝
单长滨
王学泽
王科
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Shanghai Rongchuangkaixun Special Material Co ltd
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Shanghai Rongchuangkaixun Special Material Co ltd
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    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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Abstract

The invention provides a silicon carbide composite target material and a preparation method thereof, wherein the preparation method comprises the following steps: mixing silicon carbide powder, carbon powder, a binder and a solvent, and carrying out wet ball milling to obtain mixed slurry; carrying out spray granulation on the mixed slurry to obtain granulated powder; carrying out cold isostatic pressing on the granulated powder to obtain a target blank; and carrying out hot-pressing sintering on the target blank to obtain the silicon carbide composite target. According to the method, a wet ball milling process is selected according to the characteristics of the raw materials, and then the raw materials are subjected to spray granulation and cold isostatic pressing to obtain a blank with uniformly mixed powder and high density, so that the problems of powder overflow and ejection in the hot-pressing sintering process are avoided; the hot-pressing sintering process is controlled to obtain a target product with stable quality and consistent performance, and the performance requirement of subsequent sputtering use is met; the method has the advantages of simple operation, good consistency, low cost and wide application range.

Description

Silicon carbide composite target material and preparation method thereof
Technical Field
The invention belongs to the technical field of target preparation, and relates to a silicon carbide composite target and a preparation method thereof.
Background
The silicon carbide material has the excellent characteristics of high hardness, high strength, strong high-temperature oxidation resistance, good thermal stability, small thermal expansion coefficient, chemical corrosion resistance and the like, is increasingly widely applied in the fields of semiconductors, mechanical and chemical engineering, energy, environmental protection and the like, and becomes an irreplaceable structural ceramic material in various fields. The silicon carbide target material is an important ceramic target material, and the preparation method generally adopts a powder metallurgy method, takes powder as a raw material, and prepares various structural materials through molding and sintering.
In view of the characteristics of silicon carbide materials, the silicon carbide materials have poor friction performance and high friction coefficient, and therefore, the silicon carbide materials are usually compounded with materials with good lubricating performance to prepare composite materials so as to improve the performance of the composite materials. In the mixing process before powder metallurgy, if the specific gravity difference of different raw material powders is large, powder agglomeration is easily caused by adopting common dry mixing, the mixing is not uniform, and the problem of powder overflow in the sintering process causes the product quality defect.
CN 105541336A discloses a preparation method of a boron carbide/silicon carbide ceramic whole plate, which comprises the following steps: mixing boron carbide powder, silicon carbide powder, carbon powder, a binder, a dispersant and water, and then performing ball milling pulping to obtain slurry; drying and granulating the prepared slurry by a spray granulation drying process to obtain granules; pressing and molding the prepared granulated material by adopting a cold isostatic pressing process to obtain a biscuit; pressureless sintering is carried out on the prepared biscuit, and the ceramic whole plate can be obtained after cooling; when the method is used for preparing the whole ceramic plate, boron carbide and silicon carbide are used as main raw materials, the product is mainly used as a bulletproof plate, the product has different purposes, the requirements on the raw materials and the process method are different, and how to improve the process when the product is used as a target material is not involved.
CN 101551012A discloses a carbon-containing silicon carbide sealing ring and a preparation method thereof, the method uses silicon carbide powder, yttrium aluminum garnet and carbon powder as main raw materials, and comprises the following steps in sequence: adding the main raw materials, the binder and the dispersing agent into deionized water, and preparing into water-based silicon carbide composite slurry after ball milling and mixing; spray drying the water-based silicon carbide composite slurry by adopting a spray granulation process; molding the obtained silicon carbide granulation powder by adopting a two-step mode of dry pressing prepressing and cold isostatic pressing final pressing; and sintering the obtained sealing ring blank in a vacuum pressureless sintering furnace to obtain the carbon-containing silicon carbide sealing ring. In the method, the silicon carbide product is mainly used as a sealing ring, has different performance requirements compared with the silicon carbide product used as a target material, and belongs to different application fields, so that the selection of raw materials and process operation is different.
In summary, for the preparation of the silicon carbide composite target, a proper process needs to be selected according to the performance requirement of the target, so as to obtain a compact and uniform target product, and ensure stable product quality and good uniformity.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a silicon carbide composite target and a preparation method thereof, wherein a wet ball milling process is selected according to the characteristics of raw materials in the preparation method of the composite target, and then a blank with uniformly mixed powder and high density is obtained through spray granulation and cold isostatic pressing, so that the problem of powder ejection in the hot-pressing sintering process is avoided, and then the composite target meeting the requirements of density and strength is obtained through the control of the hot-pressing sintering process, so that the performance guarantee is provided for the subsequent use of the target.
In order to achieve the purpose, the invention adopts the following technical scheme:
on one hand, the invention provides a preparation method of a silicon carbide composite target material, which comprises the following steps:
(1) mixing silicon carbide powder, carbon powder, a binder and a solvent, and carrying out wet ball milling to obtain mixed slurry;
(2) carrying out spray granulation on the mixed slurry obtained in the step (1) to obtain granulated powder;
(3) carrying out cold isostatic pressing on the granulated powder obtained in the step (2) to obtain a target blank;
(4) and (4) carrying out hot-pressing sintering on the target blank obtained in the step (3) to obtain the silicon carbide composite target.
According to the invention, the composite target material is prepared by powder metallurgy hot-pressing sintering, the mixing uniformity of different raw materials is an important factor influencing the product performance, especially when the specific gravity difference between the raw materials is large, the wet ball milling process is adopted in the invention, and the binder is combined, so that the raw material powder can be effectively uniformly mixed, and then the raw material powder is subjected to spray granulation and cold isostatic pressing to prepare a molding blank with uniform powder mixing, certain strength and density, so that the problems of powder overflow and ejection in the hot-pressing sintering process are solved, and the obtained target material product has stable quality and consistent performance by controlling the hot-pressing sintering process, and meets the performance requirements of subsequent sputtering use; the method has the advantages of simple operation, good consistency, low cost and wide application range.
The following technical solutions are preferred technical solutions of the present invention, but not limited to the technical solutions provided by the present invention, and technical objects and advantageous effects of the present invention can be better achieved and achieved by the following technical solutions.
As a preferable technical scheme of the invention, the carbon powder in the step (1) comprises graphite powder and/or petroleum coke.
Preferably, the mass ratio of the silicon carbide powder to the carbon powder in step (1) is 1:1.3 to 1:2, for example, 1:1.3, 1:1.4, 1:1.5, 1:1.6, 1:1.7, 1:1.8, 1:1.9, or 1:2, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
In the invention, the mass ratio of the silicon carbide to the carbon powder is an important factor influencing the product performance and the application, if the mass ratio of the silicon carbide to the carbon powder is too low, the carbon powder is added in a large amount, the powder is easy to agglomerate during mixing, the mixed material is not uniform, and if the mass ratio of the silicon carbide to the carbon powder is too high, the added amount of the carbon powder is small, the mixing uniformity during ball milling is reduced, the conductivity of the obtained target material is reduced, and the performance of subsequent coating is influenced.
Preferably, the binder of step (1) comprises an organic binder.
Preferably, the organic binder comprises any one or a combination of at least two of polyvinyl alcohol, starch, maltodextrin or epoxy resins, typical but non-limiting examples of which are: combinations of polyvinyl alcohol and starch, combinations of starch and maltodextrin, combinations of polyvinyl alcohol, starch and epoxy resin, starch, maltodextrin and epoxy resin, and the like.
Preferably, the binder of step (1) is added in an amount of 1 to 6 wt%, such as 1 wt%, 2 wt%, 3 wt%, 4 wt%, 5 wt% or 6 wt%, based on the total mass of the silicon carbide powder and the carbon powder, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the solvent of step (1) comprises deionized water and/or ethanol.
Preferably, the solvent is added in the step (1) in an amount of 40 to 80 wt%, such as 40 wt%, 45 wt%, 50 wt%, 55 wt%, 60 wt%, 65 wt%, 70 wt%, 75 wt% or 80 wt%, based on the total mass of the silicon carbide powder and the carbon powder, but not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
As a preferable technical scheme of the invention, the wet ball milling in the step (1) is carried out in a horizontal ball mill.
Preferably, the ball milling medium used for the wet ball milling in the step (1) is silicon carbide balls.
Preferably, the particle size of the ball milling media is 5 to 10mm, such as 5mm, 6mm, 7mm, 8mm, 9mm or 10mm, but not limited to the recited values, and other values not recited within this range are equally applicable.
Preferably, the amount of the ball milling media is: the ratio of the ball-milling medium to the total mass of the silicon carbide powder and the carbon powder is (0.8 to 1.2):1, for example, 0.8:1, 0.9:1, 1:1, 1.1:1 or 1.2:1, but the present invention is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
In the invention, the selection of the ball milling medium is related to the raw materials used by the target material, the material quality of the ball milling medium is selected to influence the purity of the material, other impurities are not required to be introduced, and the type of the raw materials which have enough strength and can meet the requirements of ball milling is selected, so that the silicon carbide is properly selected as the ball milling medium; the usage amount and the particle size of the ball milling medium play an important role in the effect of mixing and ball milling of the raw materials.
Preferably, the rotation speed of the wet ball milling in the step (1) is 10 to 40r/min, such as 10r/min, 15r/min, 20r/min, 25r/min, 30r/min, 35r/min or 40r/min, but not limited to the recited values, and other non-recited values in the range of the values are also applicable.
Preferably, the wet ball milling time in step (1) is 0.5 to 12 hours, such as 0.5 hour, 1 hour, 2 hours, 4 hours, 6 hours, 8 hours, 10 hours or 12 hours, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
In a preferred embodiment of the present invention, the spray granulation in the step (2) is performed in a spray granulation tower.
Preferably, the temperature of the inlet air to the spray granulation tower is 220 to 260 ℃, for example 220 ℃, 230 ℃, 240 ℃, 250 ℃ or 260 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable; the outlet air temperature is 105 to 150 ℃, for example 105 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃ or 150 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
In the invention, before the mixed slurry enters the spray granulation tower, the mixed slurry can be fed into the stirring barrel by using a feeding pump, and then fed into the spray granulation tower by using a metering pump, and the adding amount and the adding speed of the mixed slurry are controlled.
Preferably, the granulated powder obtained by spray granulation in step (2) is sieved.
Preferably, the granulated powder used after sieving has a particle size of 40 to 100. mu.m, for example 40. mu.m, 50. mu.m, 60. mu.m, 70. mu.m, 80. mu.m, 90. mu.m or 100. mu.m, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
In a preferred embodiment of the present invention, the cold isostatic pressing in step (3) is performed in a mold, and the mold is preferably a rubber mold.
Preferably, the pressure of the cold isostatic pressing in step (3) is 150 to 200MPa, such as 150MPa, 160MPa, 170MPa, 180MPa, 190MPa or 200MPa, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the cold isostatic pressing in step (3) has a dwell time of 1 to 3 hours, such as 1 hour, 1.5 hours, 2 hours, 2.5 hours, or 3 hours, but not limited to the recited values, and other values not recited in the range of values are also applicable.
As a preferable technical scheme of the invention, the hot pressing sintering in the step (4) is carried out in a vacuum hot pressing sintering furnace.
Preferably, the target blank is firstly placed into a graphite mold, and then placed into a vacuum hot-pressing sintering furnace together with the graphite mold.
Preferably, the hot press sintering in step (4) is divided into three-stage heating sintering processes, wherein the first stage heating is performed from normal temperature to 1400-1500 ℃, such as 1400 ℃, 1420 ℃, 1450 ℃, 1480 ℃ or 1500 ℃, the second stage heating is performed by continuing to 1750-1850 ℃, such as 1750 ℃, 1780 ℃, 1800 ℃, 1820 ℃ or 1850 ℃, and the third stage heating is performed by continuing to 2000-2050 ℃, such as 2000 ℃, 2010 ℃, 2020 ℃, 2030 ℃, 2040 ℃ or 2050 ℃, but not limited to the recited values, and other non-recited values within the respective value range are also applicable.
Preferably, the temperature increase rate of the one-stage temperature increase is 8 to 12 ℃/min, such as 8 ℃/min, 9 ℃/min, 10 ℃/min, 11 ℃/min or 12 ℃/min, but not limited to the values listed, and other values not listed in the range of the values are also applicable.
Preferably, the temperature rise rate of the second-stage temperature rise is 4 to 6 ℃/min, for example, 4 ℃/min, 4.5 ℃/min, 5 ℃/min, 5.5 ℃/min, or 6 ℃/min, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
Preferably, the temperature rise rate of the three-stage temperature rise is 2-4 ℃/min, such as 2 ℃/min, 2.5 ℃/min, 3 ℃/min, 3.5 ℃/min or 4 ℃/min, but not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
In a preferred embodiment of the present invention, the protective gas is introduced during the temperature raising to maintain the pressure at-0.06 to-0.02 MPa, for example, -0.06MPa, -0.05MPa, -0.04MPa, -0.03MPa or-0.02 MPa, but the pressure is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
Preferably, the pressure is maintained at-0.08 to-0.06 MPa, such as-0.08 MPa, -0.075MPa, -0.07MPa, -0.065MPa or-0.06 MPa, but not limited to the values listed, and other values not listed within this range are equally applicable.
In the invention, before the vacuum hot-pressing sintering furnace starts to heat up, vacuum pumping is firstly carried out, then inert gas is introduced in the heating process, the process maintains a certain vacuum degree range, once the pressure exceeds-0.02 MPa, vacuum pumping is carried out again, the pressure is controlled to be not lower than-0.06 MPa, the pressure is maintained in the range in the heating process, and after the required temperature is reached, the sintering pressure is controlled again, and the hot-pressing sintering of the target blank is carried out.
Preferably, the protective gas comprises an inert gas, such as argon, helium, neon, or the like.
Preferably, the temperature is maintained for 50-75 min after the two-stage temperature rise, for example, 50min, 55min, 60min, 65min, 70min or 75min, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
Preferably, the temperature is maintained for 40-80 min after the three-stage temperature rise, for example, 40min, 50min, 60min, 70min or 80min, but the temperature is not limited to the recited values, and other values not recited in the range of the values are also applicable.
In a preferred embodiment of the present invention, the hot press sintering in step (4) is followed by cooling.
Preferably, the cooling mode is natural cooling along with the furnace.
Preferably, the cooling rate is 5 to 20 deg.C/min, such as 5 deg.C/min, 8 deg.C/min, 10 deg.C/min, 12 deg.C/min, 15 deg.C/min, 18 deg.C/min, or 20 deg.C/min, but is not limited to the recited values, and other values not recited within the range of values are also applicable.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) mixing silicon carbide powder, carbon powder, an organic binder and a solvent for wet ball milling, wherein the carbon powder comprises graphite powder and/or petroleum coke, the mass ratio of the silicon carbide powder to the carbon powder is 1: 1.3-1: 2, the addition amount of the binder is 1-6 wt% of the total mass of the silicon carbide powder and the carbon powder, the addition amount of the solvent is 40-80 wt% of the total mass of the silicon carbide powder and the carbon powder, a ball milling medium used for the wet ball milling is silicon carbide balls, the particle size of the ball milling medium is 5-10 mm, the ratio of the ball milling medium to the total mass of the silicon carbide powder and the carbon powder is (0.8-1.2): 1, the rotation speed of the wet ball milling is 10-40 r/min, and the time is 0.5-12 h, so as to obtain mixed slurry;
(2) carrying out spray granulation on the mixed slurry obtained in the step (1) in a spray granulation tower, wherein the air inlet temperature of the spray granulation tower is 220-260 ℃, the air outlet temperature of the spray granulation tower is 105-150 ℃, the obtained granulation powder is screened, and the particle size of the granulation powder used after screening is 40-100 mu m;
(3) carrying out cold isostatic pressing on the granulated powder obtained in the step (2), wherein the pressure of the cold isostatic pressing is 150-200 MPa, and the pressure maintaining time is 1-3 h, so as to obtain a target blank;
(4) and (3) carrying out hot-pressing sintering on the target blank obtained in the step (3) in a vacuum hot-pressing sintering furnace, wherein the hot-pressing sintering is divided into three-stage heating sintering processes, the first-stage heating process is carried out at a heating rate of 8-12 ℃/min from the normal temperature to 1400-1500 ℃, the second-stage heating process is carried out at a heating rate of 4-6 ℃/min and is continuously heated to 1750-1850 ℃, the third-stage heating process is carried out at a heating rate of 2-4 ℃/min and is heated to 2000-2050 ℃, protective gas is introduced in the heating process, the pressure is maintained at-0.06-0.02 MPa, the pressure is maintained at-0.08-0.06 MPa after the heating process is completed, the temperature is maintained for 50-75 min after the second-stage heating, the temperature is maintained for 40-80 min after the third-stage heating process, and then cooling is carried out at a cooling.
On the other hand, the invention provides the silicon carbide composite target material prepared by the method.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the method, a wet ball milling process is selected according to the characteristics of the raw materials, and then the raw materials are subjected to spray granulation and cold isostatic pressing to obtain a blank with uniformly mixed powder and high density, so that the problems of powder overflow and ejection in the hot-pressing sintering process are avoided; the hot-pressing sintering process is controlled, so that a target product with high strength and density, stable quality and consistent performance is obtained, and the requirements on the performances such as conductivity and the like during subsequent sputtering use are met;
(2) the method disclosed by the invention is simple to operate, good in continuity, lower in cost and wide in application range.
Drawings
Fig. 1 is a process flow chart of a method for preparing a silicon carbide composite target material provided in embodiment 1 of the present invention.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. However, the following examples are only simple examples of the present invention and do not represent or limit the scope of the present invention, which is defined by the claims.
The specific embodiment of the invention partially provides a preparation method of a silicon carbide composite target material, which comprises the following steps:
(1) mixing silicon carbide powder, carbon powder, a binder and a solvent, and carrying out wet ball milling to obtain mixed slurry;
(2) carrying out spray granulation on the mixed slurry obtained in the step (1) to obtain granulated powder;
(3) carrying out cold isostatic pressing on the granulated powder obtained in the step (2) to obtain a target blank;
(4) and (4) carrying out hot-pressing sintering on the target blank obtained in the step (3) to obtain the silicon carbide composite target.
The following are typical but non-limiting examples of the invention:
example 1:
the embodiment provides a preparation method of a silicon carbide composite target, wherein a process flow chart of the preparation method is shown in fig. 1, and the preparation method comprises the following steps:
(1) mixing silicon carbide powder, graphite powder, polyvinyl alcohol and water for wet ball milling, wherein the mass ratio of the silicon carbide to the graphite is 1:1.6, the addition amount of the polyvinyl alcohol is 3 wt% of the total mass of the silicon carbide and the graphite, the addition amount of the water is 60 wt% of the total mass of the silicon carbide and the graphite, a ball milling medium used for the wet ball milling is silicon carbide balls, the particle size of the ball milling medium is 8mm, the ratio of the ball milling medium to the total mass of the silicon carbide and the graphite is 1:1, the rotating speed of the wet ball milling is 25r/min, and the time is 6 hours, so that mixed slurry is obtained;
(2) carrying out spray granulation on the mixed slurry obtained in the step (1) in a spray granulation tower, wherein the air inlet temperature of the spray granulation tower is 240 ℃, the air outlet temperature of the spray granulation tower is 120 ℃, and the obtained granulation powder is screened, and the average particle size of the granulation powder used after screening is 60 microns;
(3) performing cold isostatic pressing on the granulated powder obtained in the step (2) in a rubber mould, wherein the pressure of the cold isostatic pressing is 180MPa, and the pressure maintaining time is 2h to obtain a target blank;
(4) and (3) placing the target blank obtained in the step (3) into a graphite die, and carrying out hot-pressing sintering in a vacuum hot-pressing sintering furnace, wherein the hot-pressing sintering is divided into three sections of heating sintering processes, wherein the first section of heating process is carried out at a heating rate of 10 ℃/min from normal temperature to 1450 ℃, the second section of heating process is carried out at a heating rate of 5 ℃/min and is continuously carried out at 1800 ℃, the third section of heating process is carried out at a heating rate of 3 ℃/min and is carried out at 2000 ℃, argon is introduced in the heating process, the pressure is maintained at-0.05 MPa, the pressure is maintained at-0.07 MPa after the heating process is completed, the temperature is maintained for 60min after the second section of heating process, the temperature is maintained for 60min after the third section of heating process.
In this embodiment, the powder overflows and is ejected during the sintering process of the composite target, the strength of the composite target reaches 23MPa, and the density is 2.5g/m3And the performance requirement of subsequent sputtering use is met.
Example 2:
the embodiment provides a preparation method of a silicon carbide composite target, which comprises the following steps:
(1) mixing silicon carbide powder, graphite powder, corn starch and water for wet ball milling, wherein the mass ratio of the silicon carbide to the graphite is 1:1.3, the adding amount of the corn starch is 6 wt% of the total mass of the silicon carbide and the graphite, the adding amount of the water is 80 wt% of the total mass of the silicon carbide and the graphite, a ball milling medium used for the wet ball milling is silicon carbide balls, the particle size of the ball milling medium is 5mm, the ratio of the ball milling medium to the total mass of the silicon carbide and the graphite is 1.2:1, the rotating speed of the wet ball milling is 40r/min, and the time is 1h, so that mixed slurry is obtained;
(2) carrying out spray granulation on the mixed slurry obtained in the step (1) in a spray granulation tower, wherein the air inlet temperature of the spray granulation tower is 220 ℃, the air outlet temperature of the spray granulation tower is 105 ℃, and the obtained granulation powder is screened, and the average particle size of the granulation powder used after screening is 75 microns;
(3) carrying out cold isostatic pressing on the granulated powder obtained in the step (2) in a rubber mould, wherein the pressure of the cold isostatic pressing is 150MPa, and the pressure maintaining time is 3h, so as to obtain a target blank;
(4) and (3) placing the target blank obtained in the step (3) into a graphite die, and carrying out hot-press sintering in a vacuum hot-press sintering furnace, wherein the hot-press sintering is divided into three sections of heating and sintering processes, wherein the first section of heating is carried out at a heating rate of 12 ℃/min from normal temperature to 1500 ℃, the second section of heating is carried out at a heating rate of 6 ℃/min and is continuously heated to 1850 ℃, the third section of heating is carried out at a heating rate of 2 ℃/min and is heated to 2050 ℃, argon is introduced in the heating process, the pressure is maintained at-0.04 MPa, the pressure is maintained at-0.06 MPa after the heating process is completed, the temperature is maintained for 50min after the second section of heating, the temperature is maintained for 40min after the third section of heating, and then the temperature is.
In this embodiment, the powder overflows and is ejected during the sintering process of the composite target material, the strength of the composite target material reaches 21MPa, and the composite target material is denseThe degree is 2.3g/cm3And the performance requirement of subsequent sputtering use is met.
Example 3:
the embodiment provides a preparation method of a silicon carbide composite target, which comprises the following steps:
(1) mixing silicon carbide powder, graphite powder, maltodextrin and water for wet ball milling, wherein the mass ratio of the silicon carbide to the graphite is 1:2, the addition amount of the maltodextrin is 1 wt% of the total mass of the silicon carbide and the graphite, the addition amount of the water is 40 wt% of the total mass of the silicon carbide and the graphite, ball milling media used for the wet ball milling are silicon carbide balls, the particle size of the ball milling media is 10mm, the ratio of the ball milling media to the total mass of the silicon carbide and the graphite is 0.8:1, the rotating speed of the wet ball milling is 10r/min, and the time is 12 hours, so as to obtain mixed slurry;
(2) carrying out spray granulation on the mixed slurry obtained in the step (1) in a spray granulation tower, wherein the air inlet temperature of the spray granulation tower is 260 ℃, the air outlet temperature of the spray granulation tower is 150 ℃, and the obtained granulation powder is screened, and the average particle size of the granulation powder used after screening is 40 mu m;
(3) performing cold isostatic pressing on the granulated powder obtained in the step (2) in a rubber mould, wherein the pressure of the cold isostatic pressing is 200MPa, and the pressure maintaining time is 1h, so as to obtain a target blank;
(4) and (3) placing the target blank obtained in the step (3) into a graphite die, and carrying out hot-pressing sintering in a vacuum hot-pressing sintering furnace, wherein the hot-pressing sintering is divided into three sections of heating sintering processes, wherein the first section of heating is carried out at a heating rate of 8 ℃/min from normal temperature to 1400 ℃, the second section of heating is carried out at a heating rate of 4 ℃/min and is continuously heated to 1750 ℃, the third section of heating is carried out at a heating rate of 4 ℃/min and is heated to 2020 ℃, neon gas is introduced in the heating process, the pressure is maintained at-0.03 MPa, the pressure is maintained at-0.08 MPa after the heating process is completed, the temperature is maintained for 75min after the second section of heating, the temperature is maintained for 80min after the third section of heating, and then the cooling is carried.
In this embodiment, the powder overflows and is ejected during the sintering process of the composite target material, and the strength of the composite target materialUp to 20MPa, and the density is 2.4g/cm3And the performance requirement of subsequent sputtering use is met.
Example 4:
the embodiment provides a preparation method of a silicon carbide composite target, which comprises the following steps:
(1) mixing silicon carbide powder, petroleum coke, epoxy resin and ethanol, and carrying out wet ball milling, wherein the mass ratio of the silicon carbide to the petroleum coke is 1:1.5, the addition amount of the epoxy resin is 4.5 wt% of the total mass of the silicon carbide and the petroleum coke, the addition amount of the ethanol is 50 wt% of the total mass of the silicon carbide and the petroleum coke, a ball milling medium used in the wet ball milling is silicon carbide balls, the particle size of the ball milling medium is 6mm, the ratio of the ball milling medium to the total mass of the silicon carbide and the petroleum coke is 0.9:1, the rotating speed of the wet ball milling is 20r/min, and the time is 8 hours, so as to obtain mixed slurry;
(2) carrying out spray granulation on the mixed slurry obtained in the step (1) in a spray granulation tower, wherein the air inlet temperature of the spray granulation tower is 230 ℃, the air outlet temperature of the spray granulation tower is 110 ℃, and granulation powder is obtained, and the average particle size of the granulation powder is 50 microns;
(3) performing cold isostatic pressing on the granulated powder obtained in the step (2) in a rubber mould, wherein the pressure of the cold isostatic pressing is 160MPa, and the pressure maintaining time is 2.5h, so as to obtain a target blank;
(4) and (3) placing the target blank obtained in the step (3) into a graphite die, and carrying out hot-pressing sintering in a vacuum hot-pressing sintering furnace, wherein the hot-pressing sintering is divided into three sections of heating sintering processes, wherein the first section of heating process is carried out at a heating rate of 9 ℃/min from normal temperature to 1480 ℃, the second section of heating process is carried out at a heating rate of 4.5 ℃/min and is continuously heated to 1780 ℃, the third section of heating process is carried out at a heating rate of 3.5 ℃/min and is carried out at 2040 ℃, nitrogen is introduced in the heating process, the pressure is maintained at-0.045 MPa, the pressure is maintained at-0.065 MPa after the heating process is finished, the temperature is maintained for 70min after the second section of heating process, the temperature is maintained for 50min after the third section of heating process.
In this embodiment, the powder overflows and is ejected during the sintering process of the composite target material, and the composite target materialThe strength of the material reaches 22MPa, and the density is 2.36g/cm3And the performance requirement of subsequent sputtering use is met.
Example 5:
the embodiment provides a preparation method of a silicon carbide composite target, which comprises the following steps:
(1) mixing silicon carbide powder, petroleum coke, polyvinyl alcohol and water for wet ball milling, wherein the mass ratio of the silicon carbide to the petroleum coke is 1:1.8, the addition amount of the polyvinyl alcohol is 2 wt% of the total mass of the silicon carbide and the petroleum coke, the addition amount of the water is 70 wt% of the total mass of the silicon carbide and the petroleum coke, a ball milling medium used for the wet ball milling is silicon carbide balls, the particle size of the ball milling medium is 8mm, the ratio of the ball milling medium to the total mass of the silicon carbide and the petroleum coke is 1.1:1, the rotating speed of the wet ball milling is 30r/min, and the time is 4 hours, so as to obtain mixed slurry;
(2) carrying out spray granulation on the mixed slurry obtained in the step (1) in a spray granulation tower, wherein the air inlet temperature of the spray granulation tower is 250 ℃, the air outlet temperature of the spray granulation tower is 135 ℃, and the obtained granulation powder is screened, and the average particle size of the granulation powder used after screening is 70 mu m;
(3) performing cold isostatic pressing on the granulated powder obtained in the step (2) in a rubber mould, wherein the pressure of the cold isostatic pressing is 190MPa, and the pressure maintaining time is 1.5h, so as to obtain a target blank;
(4) and (3) placing the target blank obtained in the step (3) into a graphite die, and carrying out hot-pressing sintering in a vacuum hot-pressing sintering furnace, wherein the hot-pressing sintering is divided into three sections of heating sintering processes, wherein the first section of heating process is carried out at a heating rate of 11 ℃/min from normal temperature to 1420 ℃, the second section of heating process is carried out at a heating rate of 5.5 ℃/min and is continuously carried out at 1820 ℃, the third section of heating process is carried out at a heating rate of 2.5 ℃/min and is carried out at 2000 ℃, argon is introduced in the heating process, the pressure is maintained at-0.025 MPa, the pressure is maintained at-0.075 MPa after the heating process is completed, the second section of heating process is carried out at 55min, the third section of heating process is carried out at 70min, and then the.
In this embodiment, the composite target material is sinteredThe powder overflows and is sprayed out, the strength of the composite target material reaches 21.5MPa, and the density is 2.45g/cm3And the performance requirement of subsequent sputtering use is met.
Example 6:
the present embodiment provides a method for preparing a silicon carbide composite target, which is as described in embodiment 1, except that: in the step (1), the mass ratio of the silicon carbide to the graphite is 1: 1.2.
In this embodiment, since the mass ratio of the silicon carbide to the graphite is relatively high, that is, the addition amount of the graphite is relatively small, the mixing uniformity during ball milling is reduced, the uniformity of the target product is reduced, and the electrical conductivity of the target is reduced, which affects the subsequent sputtering film formation of the target.
Example 7:
the present embodiment provides a method for preparing a silicon carbide composite target, which is as described in embodiment 1, except that: in the step (1), the mass ratio of the silicon carbide to the graphite is 1: 2.2.
In this embodiment, because the mass ratio of silicon carbide to graphite is relatively low, that is, the addition amount of graphite is relatively large, powder is easily agglomerated during ball milling, the mixing uniformity is not good, the uniformity of the target product is reduced, and meanwhile, the wear resistance of the target is reduced, which easily causes wear.
Comparative example 1:
this comparative example provides a method of preparing a silicon carbide composite target material, with reference to the method of example 1, except that: and (3) dry ball milling is adopted in the step (1), polyvinyl alcohol and water are not added, and spray granulation in the step (2) is not needed.
In the comparative example, because the silicon carbide and the graphite are directly mixed by dry ball milling, the specific gravity difference between the silicon carbide and the graphite is large, the mixing uniformity is poor, the particles are easy to agglomerate, and the powder overflows in the sintering process, so that the target material product has low density which is only 1.8g/cm3The product quality and uniformity are poor.
It can be seen from the above examples and comparative examples that the method of the present invention selects a wet ball milling process according to the characteristics of the raw materials, and then performs spray granulation and cold isostatic pressing to obtain a blank with uniform powder mixing and high density, thereby avoiding the problems of powder overflow and ejection in the hot-pressing sintering process; the hot-pressing sintering process is controlled to obtain a target product with stable quality and consistent performance, and the performance requirement of subsequent sputtering use is met; the method has the advantages of simple operation, good consistency, low cost and wide application range.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It will be apparent to those skilled in the art that any modifications to the present invention, equivalents of the method of the present invention and additions of ancillary steps, selection of specific means, etc., are within the scope and disclosure of the present invention.

Claims (10)

1. The preparation method of the silicon carbide composite target is characterized by comprising the following steps:
(1) mixing silicon carbide powder, carbon powder, a binder and a solvent, and carrying out wet ball milling to obtain mixed slurry;
(2) carrying out spray granulation on the mixed slurry obtained in the step (1) to obtain granulated powder;
(3) carrying out cold isostatic pressing on the granulated powder obtained in the step (2) to obtain a target blank;
(4) and (4) carrying out hot-pressing sintering on the target blank obtained in the step (3) to obtain the silicon carbide composite target.
2. The method according to claim 1, wherein the carbon powder of step (1) comprises graphite powder and/or petroleum coke;
preferably, the mass ratio of the silicon carbide powder to the carbon powder in the step (1) is 1: 1.3-1: 2;
preferably, the binder of step (1) comprises an organic binder;
preferably, the organic binder comprises any one or a combination of at least two of polyvinyl alcohol, starch, maltodextrin or epoxy resin;
preferably, the addition amount of the binder in the step (1) is 1-6 wt% of the total mass of the silicon carbide powder and the carbon powder;
preferably, the solvent of step (1) comprises deionized water and/or ethanol;
preferably, the adding amount of the solvent in the step (1) is 40-80 wt% of the total mass of the silicon carbide powder and the carbon powder.
3. The production method according to claim 1 or 2, wherein the wet ball milling of step (1) is carried out in a horizontal ball mill;
preferably, the ball milling medium used in the wet ball milling in the step (1) is silicon carbide balls;
preferably, the particle size of the ball milling medium is 5-10 mm;
preferably, the amount of the ball milling media is: the proportion of the total mass of the ball-milling medium, the silicon carbide powder and the carbon powder is (0.8-1.2): 1;
preferably, the rotation speed of the wet ball milling in the step (1) is 10-40 r/min;
preferably, the time of the wet ball milling in the step (1) is 0.5-12 h.
4. The production method according to any one of claims 1 to 3, wherein the spray granulation of step (2) is performed in a spray granulation tower;
preferably, the air inlet temperature of the spray granulation tower is 220-260 ℃, and the air outlet temperature is 105-150 ℃;
preferably, sieving is carried out on the granulated powder obtained by the spray granulation in the step (2);
preferably, the granulated powder used after the sieving has a particle size of 40 to 100 μm.
5. The production method according to any one of claims 1 to 4, wherein the cold isostatic pressing in step (3) is performed in a rubber mold;
preferably, the pressure of the cold isostatic pressing in the step (3) is 150-200 MPa;
preferably, the pressure maintaining time of the cold isostatic pressing in the step (3) is 1-3 h.
6. The production method according to any one of claims 1 to 5, wherein the hot press sintering of step (4) is performed in a vacuum hot press sintering furnace;
preferably, the target blank is firstly placed into a graphite mold, and then is placed into a vacuum hot-pressing sintering furnace together with the graphite mold;
preferably, the hot-pressing sintering in the step (4) is divided into three-stage heating sintering processes, wherein the first-stage heating process is carried out from the normal temperature to 1400-1500 ℃, the second-stage heating process is carried out from the normal temperature to 1750-1850 ℃, and the third-stage heating process is carried out from 2000-2050 ℃;
preferably, the temperature rise rate of the first-stage temperature rise is 8-12 ℃/min;
preferably, the temperature rise rate of the second-stage temperature rise is 4-6 ℃/min;
preferably, the temperature rise rate of the three-stage temperature rise is 2-4 ℃/min.
7. The preparation method according to claim 6, characterized in that protective gas is introduced during the temperature rise process, and the pressure is maintained at-0.06 MPa to-0.02 MPa;
preferably, after the temperature rise process is finished, the pressure is maintained to be-0.08 to-0.06 MPa;
preferably, the protective gas comprises an inert gas;
preferably, the temperature of the second section is kept for 50-75 min after temperature rise;
preferably, the temperature of the three sections is kept for 40-80 min after temperature rise.
8. The production method according to any one of claims 1 to 7, wherein the hot press sintering in step (4) is followed by cooling;
preferably, the cooling mode is natural cooling along with the furnace;
preferably, the cooling rate is 5-20 ℃/min.
9. The method of any one of claims 1 to 8, comprising the steps of:
(1) mixing silicon carbide powder, carbon powder, an organic binder and a solvent for wet ball milling, wherein the carbon powder comprises graphite powder and/or petroleum coke, the mass ratio of the silicon carbide powder to the carbon powder is 1: 1.3-1: 2, the addition amount of the binder is 1-6 wt% of the total mass of the silicon carbide powder and the carbon powder, the addition amount of the solvent is 40-80 wt% of the total mass of the silicon carbide powder and the carbon powder, a ball milling medium used for the wet ball milling is silicon carbide balls, the particle size of the ball milling medium is 5-10 mm, the ratio of the ball milling medium to the total mass of the silicon carbide powder and the carbon powder is (0.8-1.2): 1, the rotation speed of the wet ball milling is 10-40 r/min, and the time is 0.5-12 h, so as to obtain mixed slurry;
(2) carrying out spray granulation on the mixed slurry obtained in the step (1) in a spray granulation tower, wherein the air inlet temperature of the spray granulation tower is 220-260 ℃, the air outlet temperature of the spray granulation tower is 105-150 ℃, the obtained granulation powder is screened, and the particle size of the granulation powder used after screening is 40-100 mu m;
(3) carrying out cold isostatic pressing on the granulated powder obtained in the step (2), wherein the pressure of the cold isostatic pressing is 150-200 MPa, and the pressure maintaining time is 1-3 h, so as to obtain a target blank;
(4) and (3) carrying out hot-pressing sintering on the target blank obtained in the step (3) in a vacuum hot-pressing sintering furnace, wherein the hot-pressing sintering is divided into three-stage heating sintering processes, the first-stage heating process is carried out at a heating rate of 8-12 ℃/min from the normal temperature to 1400-1500 ℃, the second-stage heating process is carried out at a heating rate of 4-6 ℃/min and is continuously heated to 1750-1850 ℃, the third-stage heating process is carried out at a heating rate of 2-4 ℃/min and is heated to 2000-2050 ℃, protective gas is introduced in the heating process, the pressure is maintained at-0.06-0.02 MPa, the pressure is maintained at-0.08-0.06 MPa after the heating process is completed, the temperature is maintained for 50-75 min after the second-stage heating, the temperature is maintained for 40-80 min after the third-stage heating process, and then cooling is carried out at a cooling.
10. A silicon carbide composite target material obtained by the preparation method according to any one of claims 1 to 9.
CN202110287506.5A 2021-03-17 2021-03-17 Silicon carbide composite target material and preparation method thereof Pending CN112811908A (en)

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