CN113773084B - Tungsten carbide target for decorative coating and preparation method thereof - Google Patents
Tungsten carbide target for decorative coating and preparation method thereof Download PDFInfo
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Abstract
The invention provides a tungsten carbide target for decorative coating and a preparation method thereof, wherein the preparation method comprises the following steps: (1) Screening a tungsten carbide raw material with the purity of more than or equal to 99.98 percent to obtain tungsten carbide powder; (2) Carrying out vacuum hot-pressing sintering treatment on the tungsten carbide powder obtained in the step (1) at a sintering temperature of 1800-1900 ℃ and a pressing pressure of 35-45MPa to obtain a tungsten carbide target blank; (3) Machining the tungsten carbide target blank obtained in the step (2) to obtain a tungsten carbide target material; the vacuum hot-pressing sintering treatment in the step (2) comprises heat preservation treatment and heat preservation and pressure maintaining treatment which are sequentially carried out, and the temperature rising process of the heat preservation treatment is divided into at least 3 temperature rising stages. The preparation method provided by the invention simplifies the process flow and improves the quality of the tungsten carbide target material and the coating film.
Description
Technical Field
The invention belongs to the technical field of sputtering targets, relates to a tungsten carbide target, and in particular relates to a tungsten carbide target for decorative coating and a preparation method thereof.
Background
In the production process of automobile parts, in order to improve the wear resistance and the aesthetic property of the surfaces of the parts, technicians often plate a layer of tungsten carbide on the surfaces of the parts to serve as a wear-resistant layer. Most of the current coating adopts physical vapor deposition, which requires a tungsten carbide target with a larger size. However, as the tungsten carbide target material has high forming temperature, large quality, difficult processing and high target material performance requirement, the production process of the tungsten carbide target material is complex and unstable, so that the existing target material cannot meet the high requirement of industry on the target material quality.
CN 103567440a discloses a preparation method of tungsten carbide target material for petroleum exploration drill coating, comprising the following steps: (1) Filling tungsten carbide powder with the purity of 99.999% into a graphite mold, and carrying out cold pressing pre-treatment; (2) Placing a graphite mould filled with pre-cooled and pressed tungsten carbide powder into a discharge plasma furnace, and heating to 1600-2200 ℃ under a protective atmosphere; (3) Carrying out rapid discharge in the discharge plasma furnace to form a short circuit, and instantly sintering the tungsten carbide powder to form a tungsten carbide target blank with fine and uniform grains; (4) And cooling the blank in a furnace, taking out, and carrying out mechanical processing according to requirements to obtain the tungsten carbide target. The tungsten carbide target prepared by the method has uniform and fine grains, can obviously improve the strength and wear resistance of the petroleum exploration drill bit, and prolongs the service life of the petroleum exploration drill bit. However, the rapid discharge in the method is not easy to control and has high risk coefficient, and certain degree of anisotropy exists in the process of preparing the large-size tungsten carbide target, so that a large improvement space is still reserved.
CN 110171975a discloses a large-size high-density non-binding phase tungsten carbide target material and a preparation method thereof, comprising the following steps: s1, proportioning: weighing the raw materials according to the mass fraction ratio for standby; s2, ball milling and screening treatment: ball milling the weighed raw materials in the step S1 to obtain slurry, drying the uniformly mixed slurry, and finally sieving to obtain mixed powder with uniform particle size; s3, sintering treatment: the mixed powder in the step S2 is put into a die and is put into a sintering furnace for sintering treatment, dynamic oscillating pressure is applied at the same time, and a tungsten carbide target blank is obtained after cooling and demoulding; s4, post-treatment: and (3) cutting and surface processing the tungsten carbide target blank obtained in the step (S3) to obtain the tungsten carbide target blank. According to the invention, a certain amount of free carbon is introduced into the pure tungsten carbide powder, so that the hardness of the tungsten carbide film can be reduced to a certain extent, the sintering-assisted condition of high-pressure oscillation is not easy to control, and the production process is complex.
Therefore, how to provide a tungsten carbide target material for decorative coating and a preparation method thereof, which can simplify the process flow and improve the quality of the tungsten carbide target material and the coating film, becomes a 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 the tungsten carbide target for decorative coating and the preparation method thereof, which simplify the process flow and improve the quality of the tungsten carbide target and the coating.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a tungsten carbide target for decorative coating, the method comprising the steps of:
(1) Screening a tungsten carbide raw material with the purity of more than or equal to 99.98 percent to obtain tungsten carbide powder;
(2) Carrying out vacuum hot-pressing sintering treatment on the tungsten carbide powder obtained in the step (1) at a sintering temperature of 1800-1900 ℃ and a pressing pressure of 35-45MPa to obtain a tungsten carbide target blank;
(3) Machining the tungsten carbide target blank obtained in the step (2) to obtain a tungsten carbide target material;
the vacuum hot-pressing sintering treatment in the step (2) comprises heat preservation treatment and heat preservation and pressure maintaining treatment which are sequentially carried out, and the temperature rising process of the heat preservation treatment is divided into at least 3 temperature rising stages.
According to the invention, the density of the tungsten carbide target material is increased to more than 99% and the purity is as high as more than 99.98% by reasonably controlling the sintering temperature and the pressing pressure of the vacuum hot-pressing sintering treatment, meanwhile, the heat preservation treatment is carried out firstly, then the heat preservation and pressure maintaining treatment is carried out, the heating process is divided into at least 3 heating stages, the uniformity and the sputtering stability of crystal grains in the target material are further improved, the microstructure is uniform and has no air holes, and the wear resistance of the decorative coating film is obviously improved.
In the present invention, the purity of the tungsten carbide 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) may be 1800 to 1900 ℃, for example, 1800 ℃, 1810 ℃, 1820 ℃, 1830 ℃, 1840 ℃, 1850 ℃, 1860 ℃, 1870 ℃, 1880 ℃, 1890 ℃ or 1900 ℃, but is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value range are equally applicable.
In the present invention, the pressing pressure in the step (2) is 35 to 45MPa, and may be, for example, 35MPa, 36MPa, 37MPa, 38MPa, 39MPa, 40MPa, 41MPa, 42MPa, 43MPa, 44MPa or 45MPa, 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 average particle diameter of the tungsten carbide powder in the step (1) is not more than 5. Mu.m, for example, 1. Mu.m, 1.5. Mu.m, 2. Mu.m, 2.5. Mu.m, 3. Mu.m, 3.5. Mu.m, 4.5. Mu.m, or 5. Mu.m, but not limited to the values recited, and other values not recited in the range are applicable.
Preferably, the vacuum hot-pressing sintering treatment in the step (2) comprises die filling, vacuumizing, heating, heat preservation, pressurization, heat preservation and pressure maintaining treatment, pressure removal and cooling which are sequentially carried out.
Preferably, the die-filling body is: tungsten carbide powder is filled into a graphite mold and compacted to ensure flatness of 0.5mm or less after mold filling, and may be, for example, 0.1mm, 0.15mm, 0.2mm, 0.25mm, 0.3mm, 0.35mm, 0.4mm, 0.45mm or 0.5mm, although not limited to the recited values, other non-recited values within this range are equally applicable.
Preferably, the vacuumizing specifically comprises: the graphite mold is placed in a vacuum sintering furnace, and the furnace is evacuated to an absolute pressure of not more than 100Pa, for example, 10Pa, 20Pa, 30Pa, 40Pa, 50Pa, 60Pa, 70Pa, 80Pa, 90Pa, or 100Pa, but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value range are applicable.
Preferably, the temperature raising process is divided into 3 temperature raising stages, i.e., a first temperature raising stage, a second temperature raising stage, and a third temperature raising stage, which are sequentially performed.
Preferably, the temperature rising rate of the first temperature rising stage is 8-12 ℃/min, for example, 8 ℃/min, 8.5 ℃/min, 9 ℃/min, 9.5 ℃/min, 10 ℃/min, 10.5 ℃/min, 11 ℃/min, 11.5 ℃/min or 12 ℃/min, but the temperature rising rate is not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
The target temperature of the first temperature increasing step is preferably 900 to 1100 ℃, and may be 900 ℃, 920 ℃, 940 ℃, 960 ℃, 980 ℃, 1000 ℃, 1020 ℃, 1040 ℃, 1060 ℃, 1080 ℃, or 1100 ℃, for example, but the target temperature is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value range are equally applicable.
Preferably, the temperature rising rate of the second temperature rising stage is 4-6 ℃ per minute, for example, 4 ℃/min, 4.2 ℃/min, 4.4 ℃/min, 4.6 ℃/min, 4.8 ℃/min, 5 ℃/min, 5.2 ℃/min, 5.4 ℃/min, 5.6 ℃/min, 5.8 ℃/min or 6 ℃/min, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
The target temperature of the second temperature increasing step is preferably 1450 to 1550 ℃, and may be 1450, 1460, 1470, 1480, 1490, 1500, 1510, 1520, 1530, 1540 or 1550, for example, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are equally applicable.
Preferably, the temperature rising rate of the third temperature rising stage is 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.
The target temperature in the third temperature increasing step is preferably 1800 to 1900 ℃, and may be 1800 to 1810 ℃, 1820 ℃, 1830 ℃, 1840 ℃, 1850 ℃, 1860 ℃, 1870 ℃, 1880 ℃, 1890 ℃ or 1900 ℃, for example, but is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned range are equally applicable.
Preferably, the time of the incubation is 80-100min, for example, 80min, 82min, 84min, 86min, 88min, 90min, 92min, 94min, 96min, 98min or 100min, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the pressurizing rate is 0.4-0.6MPa/min, for example, but not limited to, the recited values, other non-recited values within the range are equally applicable, and the pressurizing rate is 0.4MPa/min, 0.42MPa/min, 0.44MPa/min, 0.46MPa/min, 0.48MPa/min, 0.5MPa/min, 0.52MPa/min, 0.54MPa/min, 0.56MPa/min, 0.58MPa/min or 0.6 MPa/min.
Preferably, the target pressure of the pressurization is 35 to 45MPa, for example, 35MPa, 36MPa, 37MPa, 38MPa, 39MPa, 40MPa, 41MPa, 42MPa, 43MPa, 44MPa or 45MPa, but the target pressure is not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
Preferably, the time of the heat and pressure maintaining treatment is 80-100min, for example, 80min, 82min, 84min, 86min, 88min, 90min, 92min, 94min, 96min, 98min or 100min, 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.
Preferably, the grinding is performed on a flat grinder, and the grinding wheel of the grinder is 60-100 mesh, for example, 60 mesh, 65 mesh, 70 mesh, 75 mesh, 80 mesh, 85 mesh, 90 mesh, 95 mesh or 100 mesh, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the flatness achieved by the flattening is less than or equal to 0.05mm, and may be, for example, 0.005mm, 0.01mm, 0.015mm, 0.02mm, 0.025mm, 0.03mm, 0.035mm, 0.04mm, 0.045mm or 0.05mm, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the amount of the knife cut per step of the grinding is less than or equal to 0.05mm, for example, 0.005mm, 0.01mm, 0.015mm, 0.02mm, 0.025mm, 0.03mm, 0.035mm, 0.04mm, 0.045mm or 0.05mm, but not limited to the listed values, and other non-listed values in the range of the values are equally applicable.
Preferably, the cutting is performed on a wire cutter.
Preferably, the finishing is performed on a milling machine, and the cylindrical grinding head used is 300-500 mesh, for example, 300 mesh, 320 mesh, 340 mesh, 360 mesh, 380 mesh, 400 mesh, 420 mesh, 440 mesh, 460 mesh, 480 mesh or 500 mesh, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the feeding amount of each step of the finishing is less than or equal to 0.05mm, for example, 0.005mm, 0.01mm, 0.015mm, 0.02mm, 0.025mm, 0.03mm, 0.035mm, 0.04mm, 0.045mm or 0.05mm, but the finishing is not limited to the listed values, and other non-listed values in the range of the values are equally applicable.
Preferably, the surface treatment comprises grinding and polishing performed sequentially.
According to the invention, the tungsten carbide target blank is processed into the tungsten carbide target material with smooth surface and no corner collapse burrs through machining with specific flow and parameter requirements, so that the appearance requirements of magnetron sputtering coating on the target material are met.
As a preferred technical solution of the first aspect of the present invention, the preparation method includes the following steps:
(1) Screening the tungsten carbide raw material with the purity of more than or equal to 99.98 percent to obtain tungsten carbide powder with the average grain diameter of less than or equal to 5 mu m;
(2) Carrying out vacuum hot-pressing sintering treatment on the tungsten carbide powder obtained in the step (1) to obtain a tungsten carbide target blank; the vacuum hot-pressing sintering treatment specifically comprises the following steps:
(A) And (5) die filling: filling tungsten carbide powder into a graphite mold and compacting, so as to ensure that the flatness of the molded tungsten carbide powder is less than or equal to 0.5mm;
(B) Vacuumizing: placing the graphite mold into a vacuum sintering furnace, and vacuumizing until the absolute pressure in the furnace is less than or equal to 100Pa;
(C) Heating: firstly, heating to 900-1100 ℃ at the speed of 8-12 ℃/min, then heating to 1450-1550 ℃ at the speed of 4-6 ℃/min, and finally heating to 1800-1900 ℃ at the speed of 2-4 ℃/min;
(D) And (3) heat preservation treatment: preserving heat for 80-100min to fully heat the green body;
(E) Pressurizing: pressurizing to 35-45MPa at a rate of 0.4-0.6 MPa/min;
(F) And (3) heat preservation and pressure maintaining treatment: preserving heat and pressure for 80-100min;
(G) And (3) pressure relief: filling nitrogen and/or argon into the vacuum sintering furnace until the absolute pressure in the furnace is 0.02-0.04MPa;
(H) And (3) cooling: 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) Machining the tungsten carbide target blank obtained in the step (2) to obtain a tungsten carbide target material; the machining comprises sequentially performing grinding, cutting, finish machining, surface treatment, cleaning, drying and packaging; the grinding is carried out on a plane grinding machine, and the adopted grinding wheel of the grinding machine has the specification of 60-100 meshes; the planeness achieved by grinding is less than or equal to 0.05mm, and the cutter feeding amount of each step is less than or equal to 0.05mm; the cutting is performed on a wire cutting machine; the finish machining is carried out on a milling machine, the specification of a cylindrical grinding head is 300-500 meshes, and the feed rate of each step is less than or equal to 0.05mm; the surface treatment comprises grinding and polishing which are sequentially carried out.
In a second aspect, the present invention provides a tungsten carbide 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 density of the tungsten carbide target material is increased to more than 99% and the purity is as high as more than 99.98% by reasonably controlling the sintering temperature and the pressing pressure of the vacuum hot-pressing sintering treatment, meanwhile, the heat preservation treatment is carried out firstly, then the heat preservation and pressure maintaining treatment is carried out, the heating process is divided into at least 3 heating stages, the uniformity and the sputtering stability of crystal grains in the target material are further improved, the microstructure is uniform and has no air holes, and the wear resistance of the decorative coating film is obviously improved.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments.
Example 1
The embodiment provides a tungsten carbide target for decorative coating and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Screening a tungsten carbide raw material with the purity of more than or equal to 99.99 percent to obtain tungsten carbide powder with the average particle size of 3 mu m;
(2) Carrying out vacuum hot-pressing sintering treatment on the tungsten carbide powder obtained in the step (1) to obtain a tungsten carbide target blank; the vacuum hot-pressing sintering treatment specifically comprises the following steps:
(A) And (5) die filling: filling tungsten carbide powder into a graphite mold and compacting, so as to ensure that the flatness after mold filling is 0.3+/-0.1 mm;
(B) Vacuumizing: placing the graphite mold into a vacuum sintering furnace, and vacuumizing until the absolute pressure in the furnace is 80Pa;
(C) Heating: firstly, heating to 1000 ℃ at the speed of 10 ℃/min, then heating to 1500 ℃ at the speed of 5 ℃/min, and finally heating to 1850 ℃ at the speed of 3 ℃/min;
(D) And (3) heat preservation treatment: preserving heat for 90min to fully heat the green body;
(E) Pressurizing: pressurizing to 40MPa at a rate of 0.5 MPa/min;
(F) And (3) heat preservation and pressure maintaining treatment: preserving heat and pressure for 90min;
(G) And (3) pressure relief: argon is filled into the vacuum sintering furnace until the absolute pressure in the furnace is 0.03MPa;
(H) And (3) cooling: cooling the mold to 150 ℃ along with the furnace, taking out the mold and airing to room temperature;
(3) Machining the tungsten carbide target blank obtained in the step (2) to obtain a tungsten carbide target material; the machining comprises sequentially performing grinding, cutting, finish machining, surface treatment, cleaning, drying and packaging; the grinding is carried out on a plane grinding machine, and the adopted grinding wheel of the grinding machine has the specification of 80 meshes; the planeness achieved by grinding is 0.03+/-0.01 mm, and the cutter feeding amount of each step is 0.03mm; the cutting is performed on a wire cutting machine; the finish machining is carried out on a milling machine, the specification of a cylindrical grinding head is 400 meshes, and the amount of each stepping cutter is 0.03mm; the surface treatment comprises grinding and polishing which are sequentially carried out.
Example 2
The embodiment provides a tungsten carbide target for decorative coating and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Screening a tungsten carbide raw material with the purity of more than or equal to 99.98 percent to obtain tungsten carbide powder with the average particle size of 4 mu m;
(2) Carrying out vacuum hot-pressing sintering treatment on the tungsten carbide powder obtained in the step (1) to obtain a tungsten carbide target blank; the vacuum hot-pressing sintering treatment specifically comprises the following steps:
(A) And (5) die filling: filling tungsten carbide powder into a graphite mold and compacting, so as to ensure that the flatness after mold filling is 0.4+/-0.1 mm;
(B) Vacuumizing: placing the graphite mold into a vacuum sintering furnace, and vacuumizing until the absolute pressure in the furnace is 90Pa;
(C) Heating: firstly, heating to 900 ℃ at the speed of 8 ℃/min, then heating to 1450 ℃ at the speed of 4 ℃/min, and finally heating to 1800 ℃ at the speed of 2 ℃/min;
(D) And (3) heat preservation treatment: preserving heat for 80min to fully heat the green body;
(E) Pressurizing: pressurizing to 35MPa at a rate of 0.4 MPa/min;
(F) And (3) heat preservation and pressure maintaining treatment: preserving heat and pressure for 80min;
(G) And (3) pressure relief: charging nitrogen into the vacuum sintering furnace until the absolute pressure in the furnace is 0.02MPa;
(H) And (3) cooling: cooling the mold to 100 ℃ along with the furnace, taking out the mold and airing to room temperature;
(3) Machining the tungsten carbide target blank obtained in the step (2) to obtain a tungsten carbide target material; the machining comprises sequentially performing grinding, cutting, finish machining, surface treatment, cleaning, drying and packaging; the grinding is carried out on a plane grinding machine, and the adopted grinding wheel of the grinding machine has the specification of 60 meshes; the planeness achieved by grinding is 0.04 plus or minus 0.01mm, and the cutter feeding amount of each step is 0.04mm; the cutting is performed on a wire cutting machine; the finish machining is carried out on a milling machine, the specification of a cylindrical grinding head is 300 meshes, and the amount of each stepping cutter is 0.04mm; the surface treatment comprises grinding and polishing which are sequentially carried out.
Example 3
The embodiment provides a tungsten carbide target for decorative coating and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Screening a tungsten carbide raw material with the purity of more than or equal to 99.98 percent to obtain tungsten carbide powder with the average particle size of 5 mu m;
(2) Carrying out vacuum hot-pressing sintering treatment on the tungsten carbide powder obtained in the step (1) to obtain a tungsten carbide target blank; the vacuum hot-pressing sintering treatment specifically comprises the following steps:
(A) And (5) die filling: filling tungsten carbide powder into a graphite mold and compacting, so as to ensure that the flatness after mold filling is 0.4+/-0.1 mm;
(B) Vacuumizing: placing the graphite mold into a vacuum sintering furnace, and vacuumizing until the absolute pressure in the furnace is 100Pa;
(C) Heating: firstly, heating to 1100 ℃ at a speed of 12 ℃/min, then heating to 1550 ℃ at a speed of 6 ℃/min, and finally heating to 1900 ℃ at a speed of 4 ℃/min;
(D) And (3) heat preservation treatment: preserving heat for 100min to fully heat the green body;
(E) Pressurizing: pressurizing to 45MPa at a rate of 0.6 MPa/min;
(F) And (3) heat preservation and pressure maintaining treatment: preserving heat and pressure for 100min;
(G) And (3) pressure relief: argon is filled into the vacuum sintering furnace until the absolute pressure in the furnace is 0.04MPa;
(H) And (3) cooling: cooling the mold to 200 ℃ along with the furnace, taking out the mold and airing to room temperature;
(3) Machining the tungsten carbide target blank obtained in the step (2) to obtain a tungsten carbide target material; the machining comprises sequentially performing grinding, cutting, finish machining, surface treatment, cleaning, drying and packaging; the grinding is carried out on a plane grinding machine, and the specification of a grinding wheel of the adopted grinding machine is 100 meshes; the planeness achieved by grinding is 0.04 plus or minus 0.01mm, and the cutter feeding amount of each step is 0.05mm; the cutting is performed on a wire cutting machine; the finish machining is carried out on a milling machine, the specification of a cylindrical grinding head is 500 meshes, and the feed rate of each step is 0.05mm; the surface treatment comprises grinding and polishing which are sequentially carried out.
Example 4
The present embodiment provides a tungsten carbide target for decorative coating and a preparation method thereof, and the preparation method is the same as embodiment 1 except that the time of heat preservation in step (2) is changed to 70min, so that no description is given here.
Example 5
The embodiment provides a tungsten carbide target for decorative coating and a preparation method thereof, and the preparation method is the same as embodiment 1 except that the treatment time of Wen Baoya in step (2) is changed to 70min, so that no description is given here.
Comparative example 1
The comparative example provides a tungsten carbide target for decorative coating and a preparation method thereof, and the preparation method is the same as that of example 1 except that the final target temperature for heating in step (2) is changed to 1750 ℃, so that the description thereof is omitted.
Comparative example 2
The comparative example provides a tungsten carbide target for decorative coating and a preparation method thereof, and the preparation method is the same as that of example 1 except that the final target temperature for heating in step (2) is changed to 1950 ℃, so that no description is given here.
Comparative example 3
The comparative example provides a tungsten carbide target for decorative coating 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 pressurizing in the step (2) is changed to 30MPa, so that no description is given here.
Comparative example 4
The comparative example provides a tungsten carbide target for decorative coating 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 pressurizing in the step (2) is changed to 50MPa, so that no description is given here.
Comparative example 5
The comparative example provides a tungsten carbide target for decorative coating and a preparation method thereof, wherein the preparation method changes the heating process in the step (2) into: the temperature was raised to 1500℃at a rate of 12℃per minute and then to 1850℃at a rate of 5℃per minute, and the other conditions were the same as in example 1, so that no description is given here.
Comparative example 6
The comparative example provides a tungsten carbide target for decorative coating and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Screening a tungsten carbide raw material with the purity of more than or equal to 99.99 percent to obtain tungsten carbide powder with the average particle size of 3 mu m;
(2) Carrying out vacuum hot-pressing sintering treatment on the tungsten carbide powder obtained in the step (1) to obtain a tungsten carbide target blank; the vacuum hot-pressing sintering treatment specifically comprises the following steps:
(A) And (5) die filling: filling tungsten carbide powder into a graphite mold and compacting, so as to ensure that the flatness after mold filling is 0.3+/-0.1 mm;
(B) Vacuumizing: placing the graphite mold into a vacuum sintering furnace, and vacuumizing until the absolute pressure in the furnace is 80Pa;
(C) Heating and pressurizing: firstly, heating to 1000 ℃ at the speed of 10 ℃/min, then heating to 1500 ℃ at the speed of 5 ℃/min, and finally heating to 1850 ℃ at the speed of 3 ℃/min; simultaneously pressurizing to 40MPa at a rate of 0.5 MPa/min;
(D) And (3) heat preservation and pressure maintaining treatment: preserving heat and pressure for 180min;
(E) And (3) pressure relief: argon is filled into the vacuum sintering furnace until the absolute pressure in the furnace is 0.03MPa;
(F) And (3) cooling: cooling the mold to 150 ℃ along with the furnace, taking out the mold and airing to room temperature;
(3) Machining the tungsten carbide target blank obtained in the step (2) to obtain a tungsten carbide target material; the machining comprises sequentially performing grinding, cutting, finish machining, surface treatment, cleaning, drying and packaging; the grinding is carried out on a plane grinding machine, and the adopted grinding wheel of the grinding machine has the specification of 80 meshes; the planeness achieved by grinding is 0.03+/-0.01 mm, and the cutter feeding amount of each step is 0.03mm; the cutting is performed on a wire cutting machine; the finish machining is carried out on a milling machine, the specification of a cylindrical grinding head is 400 meshes, and the amount of each stepping cutter is 0.03mm; the surface treatment comprises grinding and polishing which are sequentially carried out.
The results of performance testing of the tungsten carbide targets obtained in examples 1 to 5 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 tungsten carbide target material obtained in the examples 1-5 has excellent performance, the density is more than or equal to 99 percent, and the purity is more than or equal to 99.98 percent; 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 temperature rising process was changed to 2 temperature rising stages 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 are performed simultaneously on the basis of example 1, namely, a separate heat preservation process is eliminated, and the comprehensive performance of the target material is reduced, which is not beneficial to the improvement of the coating quality.
Therefore, the density of the tungsten carbide target material is increased to more than 99 percent and the purity is up to more than 99.98 percent by reasonably controlling the sintering temperature and the pressing pressure of the vacuum hot-pressing sintering treatment, meanwhile, the heat preservation treatment is firstly carried out, then the heat preservation and pressure maintaining treatment is carried out, the heating process is divided into at least 3 heating stages, the uniformity and the sputtering stability of crystal grains in the target material are further improved, the microstructure is uniform and has no air holes, and the wear resistance of the decorative coating film is obviously improved.
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 (16)
1. The preparation method of the tungsten carbide target for decorative coating is characterized by comprising the following steps of:
(1) Screening a tungsten carbide raw material with the purity of more than or equal to 99.98 percent to obtain tungsten carbide powder;
(2) Carrying out vacuum hot-pressing sintering treatment on the tungsten carbide powder obtained in the step (1) at a sintering temperature of 1800-1900 ℃ and a pressing pressure of 35-45MPa to obtain a tungsten carbide target blank;
(3) Machining the tungsten carbide target blank obtained in the step (2) to obtain a tungsten carbide target material;
the vacuum hot-pressing sintering treatment in the step (2) comprises die filling, vacuumizing, heating, heat preservation, pressurizing, heat preservation and pressure maintaining treatment, pressure removing and cooling which are sequentially carried out, wherein the heating process of the heat preservation is divided into 3 heating stages, namely a first heating stage, a second heating stage and a third heating stage which are sequentially carried out;
the temperature rising rate of the first temperature rising stage is 8-12 ℃/min, and the target temperature is 900-1100 ℃; the temperature rising rate of the second temperature rising stage is 4-6 ℃/min, and the target temperature is 1450-1550 ℃; the temperature rising rate of the third temperature rising stage is 2-4 ℃/min, and the target temperature is 1800-1900 ℃; the heat preservation treatment time is 80-100min;
the pressurizing speed is 0.4-0.6MPa/min, and the target pressure is 35-45MPa; the heat preservation and pressure maintaining treatment time is 80-100min.
2. The method according to claim 1, wherein the tungsten carbide powder in the step (1) has an average particle diameter of 5 μm or less.
3. The method according to claim 1, wherein the die-filling body is: and (3) filling tungsten carbide powder into a graphite die, compacting, and ensuring flatness less than or equal to 0.5mm after die filling.
4. The preparation method according to claim 1, wherein the vacuum pumping is specifically: and (3) placing the graphite mould into a vacuum sintering furnace, and vacuumizing until the absolute pressure in the furnace is less than or equal to 100Pa.
5. The method according to claim 1, 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.
6. The method according to claim 1, 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.
7. The method of claim 1, wherein the machining in step (3) comprises sequentially performing grinding, cutting, finishing, surface treatment, cleaning, drying, and packaging.
8. The method according to claim 7, wherein the grinding is performed on a flat grinder, and the grinding wheel size of the grinder is 60-100 mesh.
9. The method of claim 7, wherein the flatness achieved by the grinding is less than or equal to 0.05mm.
10. The method according to claim 7, wherein the amount of the knife cut per step of the grinding is less than or equal to 0.05mm.
11. The method of claim 7, wherein the cutting is performed on a wire cutter.
12. The method according to claim 7, wherein the finishing is performed on a milling machine, and the cylindrical grinding head is 300-500 mesh in size.
13. The method of claim 7, wherein the amount of feed per step of finishing is less than or equal to 0.05mm.
14. The method of claim 7, wherein the surface treatment comprises grinding and polishing performed sequentially.
15. The preparation method according to any one of claims 1 to 14, characterized in that the preparation method comprises the steps of:
(1) Screening the tungsten carbide raw material with the purity of more than or equal to 99.98 percent to obtain tungsten carbide powder with the average grain diameter of less than or equal to 5 mu m;
(2) Carrying out vacuum hot-pressing sintering treatment on the tungsten carbide powder obtained in the step (1) to obtain a tungsten carbide target blank; the vacuum hot-pressing sintering treatment specifically comprises the following steps:
(A) And (5) die filling: filling tungsten carbide powder into a graphite mold and compacting, so as to ensure that the flatness of the molded tungsten carbide powder is less than or equal to 0.5mm;
(B) Vacuumizing: placing the graphite mold into a vacuum sintering furnace, and vacuumizing until the absolute pressure in the furnace is less than or equal to 100Pa;
(C) Heating: firstly, heating to 900-1100 ℃ at the speed of 8-12 ℃/min, then heating to 1450-1550 ℃ at the speed of 4-6 ℃/min, and finally heating to 1800-1900 ℃ at the speed of 2-4 ℃/min;
(D) And (3) heat preservation treatment: preserving heat for 80-100min to fully heat the green body;
(E) Pressurizing: pressurizing to 35-45MPa at a rate of 0.4-0.6 MPa/min;
(F) And (3) heat preservation and pressure maintaining treatment: preserving heat and pressure for 80-100min;
(G) And (3) pressure relief: filling nitrogen and/or argon into the vacuum sintering furnace until the absolute pressure in the furnace is 0.02-0.04MPa;
(H) And (3) cooling: 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) Machining the tungsten carbide target blank obtained in the step (2) to obtain a tungsten carbide target material; the machining comprises sequentially performing grinding, cutting, finish machining, surface treatment, cleaning, drying and packaging; the grinding is carried out on a plane grinding machine, and the adopted grinding wheel of the grinding machine has the specification of 60-100 meshes; the planeness achieved by grinding is less than or equal to 0.05mm, and the cutter feeding amount of each step is less than or equal to 0.05mm; the cutting is performed on a wire cutting machine; the finish machining is carried out on a milling machine, the specification of a cylindrical grinding head is 300-500 meshes, and the feed rate of each step is less than or equal to 0.05mm; the surface treatment comprises grinding and polishing which are sequentially carried out.
16. A tungsten carbide target prepared by the method of any one of claims 1-15.
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| CN114918576B (en) * | 2022-06-23 | 2023-08-18 | 北京安泰六九新材料科技有限公司 | Tungsten carbide binding target and preparation method thereof |
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| KR20160084434A (en) * | 2014-03-26 | 2016-07-13 | 제이엑스금속주식회사 | Sputtering target comprising tungsten carbide or titanium carbide |
| CN105693252B (en) * | 2016-01-22 | 2018-06-19 | 基迈克材料科技（苏州）有限公司 | Heat pressing process prepares boride sputtering target material |
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