CN116023142A - Tungsten carbide target material, preparation method thereof and special die - Google Patents
Tungsten carbide target material, preparation method thereof and special die Download PDFInfo
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- CN116023142A CN116023142A CN202211717769.6A CN202211717769A CN116023142A CN 116023142 A CN116023142 A CN 116023142A CN 202211717769 A CN202211717769 A CN 202211717769A CN 116023142 A CN116023142 A CN 116023142A
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- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 239000013077 target material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 45
- 239000000843 powder Substances 0.000 claims abstract description 36
- 238000007731 hot pressing Methods 0.000 claims abstract description 31
- 238000000465 moulding Methods 0.000 claims abstract description 13
- 238000003825 pressing Methods 0.000 claims abstract description 12
- 238000011068 loading method Methods 0.000 claims abstract description 10
- 238000003754 machining Methods 0.000 claims abstract description 9
- 238000004321 preservation Methods 0.000 claims description 26
- 239000000758 substrate Substances 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 18
- 230000000630 rising effect Effects 0.000 claims description 15
- 238000000462 isostatic pressing Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000012545 processing Methods 0.000 abstract description 6
- 239000000047 product Substances 0.000 description 19
- 239000000463 material Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 6
- 238000012216 screening Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
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- 238000005516 engineering process Methods 0.000 description 2
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- 238000002490 spark plasma sintering Methods 0.000 description 2
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 239000010941 cobalt Substances 0.000 description 1
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- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
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- 239000007789 gas Substances 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
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Abstract
The application provides a tungsten carbide target, a preparation method thereof and a special die. The preparation method of the target material comprises the following steps: and (3) mould pressing: molding tungsten carbide powder to obtain a first blank; and (3) charging: loading a plurality of first blanks into a die through superposition or/and regular arrangement; and hot-pressing and sintering: putting the die provided with the first blank into a hot pressing furnace, and performing hot pressing sintering to obtain a second blank; and (3) machining: and machining the second blank to obtain the tungsten carbide target material with the required size. The invention adopts the special hot-pressing die to carry out hot pressing, and the prepared tungsten carbide target material has the advantages of near-net forming, low cost, high density, no air holes, no cracks, good processing performance, uniform tissue and the like.
Description
Technical Field
The invention belongs to the technical field of hard alloy materials, and particularly relates to a tungsten carbide target, a preparation method thereof and a special die.
Background
The pure tungsten carbide material can be applied to the field of surface hard coatings due to higher hardness, good corrosion resistance and excellent high-temperature oxidation resistance. The tungsten carbide target material for the coating is required to have higher compactness and uniform grain size so as to prepare a film layer with compactness and few surface defects.
Because the melting point of the pure tungsten carbide is as high as 2800 ℃, and the solid phase sintering resistance between the pure tungsten carbide powder is very large, under the condition of no binder addition, the high-density material with the density of more than 99% is difficult to obtain. However, the presence of the binder may reduce the properties of the cemented tungsten carbide, such as the presence of cobalt, may reduce the corrosion resistance of the cemented tungsten carbide, while reducing its hardness and wear resistance. Binder-free tungsten carbide alloys are becoming an important development.
In recent years, the hottest research at home and abroad is Spark Plasma Sintering (SPS) technology, and a compact sintered body with the relative density of about 98% can be obtained by adopting the pressure of 30MPa at 1900 ℃ and the heat preservation time of 5 min. However, SPS sintering is limited by the size of the sample, has poor stability, and cannot meet the requirements of large-size and mass industrialized production.
In addition, in order to ensure the compactness of the sintered material, there is a technology of sintering by combining hot pressing and hot isostatic pressing, and the sintering mode is complex, the cost is high, and the material utilization rate is low.
Therefore, in the preparation of high-quality tungsten carbide targets, the reduction of cost, the simplification of process flows and the increase of material utilization rate are all the targets pursued in the industry.
Disclosure of Invention
Aiming at the problems in the prior art, the purpose of the application is to provide a tungsten carbide target material, a preparation method thereof and a special die. The tungsten carbide target prepared by the method has the advantages of near-net forming, low cost, high density, no air holes, no cracks, good processing performance, uniform tissue and the like.
In order to achieve the above purpose, the present application adopts the following technical scheme:
in a first aspect, the present application provides a method for preparing a tungsten carbide target, including the steps of:
and (3) mould pressing: molding tungsten carbide powder to obtain a first blank;
and (3) charging: loading a plurality of first blanks into a die through superposition or/and regular arrangement;
and hot-pressing and sintering: putting the die provided with the first blank into a hot pressing furnace, and performing hot pressing sintering to obtain a second blank;
and (3) machining: and machining the second blank to obtain the tungsten carbide target material with the required size.
In some embodiments, the tungsten carbide powder has a particle size D50 of 0.5 to 1 μm (e.g., 0.6 μm, 0.7 μm, 0.8 μm, or 0.9 μm). The tungsten carbide powder with the particle size can ensure that the compactness of the tungsten carbide target material obtained by the method reaches more than 99 percent, the particle size of the powder is too large to be beneficial to the densification of the target material, tissue defects, air holes and the like exist, the oxygen content can be increased when the particle size of the powder is too small, the purity of the target material is reduced, and meanwhile, the smaller the particle size of the powder is, the higher the cost is, so that unnecessary waste is caused.
In some embodiments, the molding pressure is 50-70 MPa (e.g., 51, 55, 60, 65, or 68 MPa), and the density of the first billet after molding is 8.0-10 g/cm 3 . The molding pressure is controlled within the range, so that gas and gaps among the powders can be primarily removed, the loose height is reduced, a first blank with a certain density and shape is primarily formed, and subsequent hot press sintering is facilitated.
In some embodiments, the cross-sectional shape of the first blank that is molded is the same as the cross-sectional shape of the finished target, and the cross-sectional dimension of the first blank is equal to or greater than the cross-sectional dimension of the finished target, preferably the difference between the cross-sectional dimension of the first blank and the cross-sectional dimension of the finished target is 0-5mm; the relation between the cross section size of the first blank and the size of the finished target material is controlled, so that the material utilization rate can be improved, and the cost is reduced; further preferably, the cross-sectional shape of the first blank is circular and the difference between the cross-sectional diameter of the first blank and the cross-sectional diameter of the finished target is 0-5mm (e.g. 0.1%, 0.5%, 1%, 2%, 3%, 4% or 4.8%).
In some embodiments, the first blank is cylindrical in shape, which facilitates smooth demolding after molding, in addition to conforming to the shape of the finished target.
It should be noted that, the size and shape of the first blank can be adjusted according to the size requirement of the actually prepared finished target.
In some embodiments, the mold of the charging step is an isostatic mold.
In some embodiments, the mold of the charging step is an isostatic graphite mold.
The graphite mold can resist sintering temperature up to 2200 ℃ so as to avoid deformation or cracking of the mold in the sintering process and influence the sintering quality.
In some embodiments, the isostatic die comprises a female die and a male die cooperating with the female die, the male die cap, when disposed on the female die, defining a plurality of die cavity spaces for receiving a first blank.
Preferably, the male die comprises a second substrate and a plurality of protrusions formed on the surface of the second substrate, and the female die comprises a first substrate and a plurality of grooves formed on the first substrate; the number of the grooves and the protrusions are the same and the arrangement modes of the grooves and the protrusions on the corresponding substrates are the same, and each groove is matched with the corresponding protrusion to form a die cavity space for accommodating a first blank. The cross-sectional shape of each of the grooves and the protrusions is the same as the cross-sectional shape of the first blank. The cross-sectional dimensions of each of the grooves are comparable to the cross-sectional dimensions of the first blank so that the first blank can be snugly received in the groove.
In some embodiments, the plurality of grooves on the first substrate are arranged regularly, preferably in a plurality of rows and columns of grooves, for example, 9 grooves in three rows and three columns, and 9 protrusions are correspondingly arranged on the second substrate.
In order to be able to obtain more targets by hot press sintering at a time, the height of each groove is generally greater than the height of the first blank, preferably the height of the groove is more than 3 times the height of the first blank, more preferably 3-6 times.
The concave die in the isostatic pressing die is provided with a plurality of grooves, a plurality of second blanks can be molded at one time, the production efficiency is high, and the cost is saved.
In some embodiments the cross-section of the groove on the female die is circular, the cross-section of the protrusion on the male die is circular, the cross-sectional diameter of the protrusion is less than the cross-sectional inner diameter of the groove, and the difference between the cross-sectional diameter of the protrusion and the cross-sectional inner diameter of the groove is less than 0.5 millimeters.
The cross sections of the grooves on the female die and the protrusions on the male die are set to be round, friction with the die is reduced, and uniform deformation of each part of the blank is facilitated.
The number, the size and the shape of the female die and the male die are not limited, and can be adjusted according to actual preparation requirements.
In some embodiments, the hot press sintering step comprises:
a first temperature rising stage: heating the hot pressing furnace from the furnace temperature to the first heat preservation temperature of 900-1100 ℃ for 60-70 min;
a first heat preservation stage: preserving heat for 50-70 min at 900-1100 ℃;
a second temperature rising stage: heating from the first heat preservation temperature to the second heat preservation temperature of 1500-1700 ℃ for 100-140min;
and a second heat preservation stage: preserving heat at 1500-1700 ℃ for 60-70 min;
and a third temperature rising stage: heating from the second heat preservation temperature to a third heat preservation temperature of 2000-2100 ℃ for 160-200min;
and a third heat preservation stage: and preserving heat for 2.5-4 h at the third heat preservation temperature.
In some embodiments, in the third elevated temperature stage, the pressure applied to the autoclave is gradually increased to 25 to 40MPa.
Through the temperature rising and heat preservation process control of the first stage and the second stage, the temperature and stress of each part of the blank tend to be consistent, and in the third temperature rising stage, the pressure is gradually increased to 25-40 MPa, and the pressure, the temperature and the temperature rising speed are cooperatively controlled so as to obtain the blank with uniform and consistent tissues.
In some embodiments, in the third incubation period, the pressure applied to the autoclave is between 25 and 40Mpa.
In the pressure range, the blank finally obtains higher density, has uniform grain size and has no tissue defect and air hole.
In some embodiments, the hot pressed sintering is performed at a vacuum level of 5x 10 -1 Pa～5*10 -2 Under Pa.
In a second aspect, the present application provides a tungsten carbide target prepared by the above-described preparation method.
In some embodiments, the density of the tungsten carbide target: 15.4-15.7 g/cm 3 Product hardness: 85-95 (HRA), and the average grain size of the product is less than 2 microns.
In a third aspect, the present application provides a mold for preparing the tungsten carbide target described above.
In some embodiments, the mold is an isostatic mold. Preferably, the mould is an isostatic graphite mould.
In some embodiments, the isostatic die comprises a female die and a male die cooperating with the female die, the male die cap, when disposed on the female die, defining a plurality of die cavity spaces for receiving a first blank.
Preferably, the male die comprises a second substrate and a plurality of protrusions formed on the surface of the second substrate, and the female die comprises a first substrate and a plurality of grooves formed on the first substrate; the number of the grooves and the protrusions are the same and the arrangement modes of the grooves and the protrusions on the corresponding substrates are the same, and each groove is matched with the corresponding protrusion to form a die cavity space for accommodating a first blank. The cross-sectional shape of each of the grooves and the protrusions is the same as the cross-sectional shape of the first blank. The cross-sectional dimensions of each of the grooves are comparable to the cross-sectional dimensions of the first blank so that the first blank can be snugly received in the groove.
In some embodiments, the plurality of grooves on the first substrate are arranged regularly, preferably in a plurality of rows and columns of grooves, for example, 9 grooves in three rows and three columns, and 9 protrusions are correspondingly arranged on the second substrate.
In order to be able to obtain more targets by hot press sintering at a time, the height of each groove is generally greater than the height of the first blank, preferably the height of the groove is more than 3 times the height of the first blank, more preferably 3-6 times.
The concave die in the isostatic pressing die is provided with a plurality of grooves, a plurality of second blanks can be molded at one time, the production efficiency is high, and the cost is saved.
In some embodiments the cross-section of the groove on the female die is circular, the cross-section of the protrusion on the male die is circular, the cross-sectional diameter of the protrusion is less than the cross-sectional inner diameter of the groove, and the difference between the cross-sectional diameter of the protrusion and the cross-sectional inner diameter of the groove is less than 0.5 millimeters.
The cross sections of the grooves on the female die and the protrusions on the male die are set to be round, friction with the die is reduced, and uniform deformation of each part of the blank is facilitated.
It should be noted that the number, shape and size of the grooves and the protrusions of the mold are not limited, and may be determined according to practical requirements, for example, according to the size of the final target.
The mould can lead the prepared tungsten carbide target blank to be equivalent to the final target in size, is formed near the end, basically has no large-size sintering problem, saves the processing cost, saves the materials and effectively improves the utilization rate of the materials.
Compared with the prior art, the invention has the beneficial effects that:
1) The tungsten carbide ceramic target prepared by the technical scheme has the advantages of high density, no air holes, no cracks, good processing performance, uniform structure and the like.
2) The tungsten carbide target blank prepared by the method is equivalent to the final target in size, is formed near the end, basically has no problem of difficult sintering of large size, saves the processing cost, saves the materials, and effectively improves the utilization rate of the materials. The material utilization rate of the tungsten carbide target material prepared by the method can reach 88%, the material utilization rate of the tungsten carbide target material prepared by large-size sintering is 68%, and compared with the large-size sintering, the cost of each tungsten carbide target material is reduced from 1760 yuan to 1005 yuan by taking the tungsten carbide target material with phi 100x12mm as an example, and the cost is greatly reduced.
Drawings
Fig. 1 is a schematic microstructure of a tungsten carbide target prepared according to an embodiment of the present application.
Fig. 2 is a schematic structural diagram of a female die in a mold for preparing a tungsten carbide target according to an embodiment of the present application.
Fig. 3 is a schematic structural diagram of a male die in a die for preparing a tungsten carbide target according to an embodiment of the present application.
Fig. 4 is a schematic structural diagram of an isostatic pressing mold with a female mold and a male mold matched in a mold for preparing a tungsten carbide target according to an embodiment of the present application.
Fig. 5 is a schematic diagram of machining positions of a carbide target blank prepared in comparative example 1 of the present application when a finished target is subsequently prepared.
Wherein, the reference numerals are as follows: 1-isostatic pressing mould, 11-female mould, 111-first matrix, 112-groove, 12-male mould, 121-protrusion, 122-second matrix, 2-large-size hot-pressed sintered blank and 3-finished target machining position.
Detailed Description
The following examples further illustrate the content of the present application in detail, but the scope of the present invention is not limited to the following examples.
One specific embodiment of the preparation method of the tungsten carbide target provided by the application comprises the following steps:
screening powder: the pure tungsten carbide powder with the purity of more than 99.95 percent is taken as raw material powder to be screened, and the tungsten carbide powder with the D50 of 0.5-1 micron is obtained.
And (3) mould pressing: and molding the tungsten carbide powder obtained by screening to obtain a first blank.
And (3) charging: and loading the first blanks obtained after the mould pressing into a hot-pressing mould.
And hot-pressing and sintering: and (3) putting the die provided with the first blank into a hot pressing furnace, and performing hot pressing sintering to obtain a second blank.
And a finished product meeting the requirements of customer size and surface quality can be processed later according to the requirements.
The pure tungsten carbide raw material powder used in the examples is prepared by adopting a conventional preparation method in the field or adopts a commercial product, and the purity of the pure tungsten carbide raw material powder is more than 99.95 percent.
The isostatic pressing die used in the specific embodiment of the present application is made of graphite, and the structure of the isostatic pressing die is shown in fig. 2-4, and includes: comprises a female die 11 and a male die 12 which are matched to form an isobaric die 1, and when the male die 12 is covered on the female die 11, a plurality of die cavity spaces for accommodating a first blank are formed.
Referring to fig. 3, the male die 12 includes a second base 122 and a plurality of protrusions 121 formed on a surface of the second base 122, and referring to fig. 2, the female die 11 includes a first base 111 and a plurality of grooves 112 formed on the first base 111; the number of grooves 112 and protrusions 121 is the same and the arrangement on the respective substrates is the same, each groove 112 and its corresponding protrusion 121 matching to form a cavity space for receiving a first blank. The cross-sectional shape of each groove 112 and protrusion 121 is the same as the cross-sectional shape of the first blank. The cross-sectional dimensions of each groove 112 are comparable to the cross-sectional dimensions of the first blank so that the first blank can be just fit into the groove for near net shape formation.
In the embodiment, a plurality of rows and columns of grooves 112, for example, 9 grooves 112 in three rows and three columns are disposed on the surface of the first substrate 111, and 9 protrusions 121 are disposed on the second substrate 122 correspondingly. In order to enable more targets to be obtained by hot press sintering at a time, the height of each groove 112 is equal to the height of a plurality of first blanks, for example, the height of the groove 112 is 3-6 times the height of the first blanks. The concave die 11 in the isostatic pressing die 1 is provided with a plurality of grooves 112, so that a plurality of second blanks can be molded at one time, the production efficiency is high, and the cost is saved. The cross section of the groove 112 is circular, the cross section of the protrusion 121 on the male die 12 is circular, the cross section diameter of the protrusion 121 is slightly smaller than the cross section inner diameter of the groove 112, and the difference between the cross section diameter of the protrusion 121 and the cross section inner diameter of the groove 112 is below 0.5 mm, so that the protrusion 121 can be just seated in the groove, and the effect of pressing down a blank is realized.
The mould can lead the prepared tungsten carbide target blank to be equivalent to the final target in size, is formed near the end, basically has no large-size sintering problem, saves the processing cost, saves the materials and effectively improves the utilization rate of the materials.
The method for preparing the tungsten carbide target by using the die is described in detail below, and the density is measured by using an archimedes drainage method in the following examples, and the hardness of the product is measured by using a hardness tester.
Example 1
The preparation method comprises the following steps:
(1) Screening powder: screening the tungsten carbide powder to obtain tungsten carbide powder with D50 of 1 micron;
(2) And (3) mould pressing: the obtained tungsten carbide powder with D50 of 1 micrometer is molded to obtain a cylindrical first blank, the molding pressure is 60Mpa, the powder loading amount is 1220 g, the size of the first blank is phi 100x19mm, and the density of the first blank after molding is 8.2g/cm 3 ；
(3) And (3) charging: filling a first blank into a die, wherein the die is an isostatic pressing graphite die, 5 first blanks which are molded are placed in layers in each groove of a female die (the number of grooves on the female die is 9 in the embodiment), and the size of each groove is phi 101x110mm; by adopting the die disclosed by the invention, a plurality of blanks can be prepared at one time, so that the production efficiency is improved, and the cost is further saved.
(4) And hot-pressing and sintering: and (3) putting the die provided with the first blank into a hot pressing furnace, and performing hot pressing sintering. After loading, the hot press furnace is vacuumized by a diffusion pump until the vacuum degree is 1x 10 -1 Pa, and this vacuum is maintained during the hot press sintering process.
The pressure applied during the hot press sintering step and the time parameters maintained at each stage are shown in table 1 below:
TABLE 1
| Stage(s) | Temperature (temperature) | Pressure (MPa) | Time |
| A first temperature rising stage | Furnace temperature-1000 DEG C | 0 | 1h |
| First heat preservation stage | 1000℃ | 0 | 1h |
| A second temperature rising stage | 1000℃-1500℃ | 0 | 2h |
| Second heat preservation stage | 1500℃ | 0 | 1h |
| A third temperature rising stage | 1500℃-2000℃ | 0-35MPa | 3h |
| Fourth heat preservation stage | 2000℃ | 35MPa | 2.5h |
The second blank heat pressed into each groove had a size of Φ102×50mm.
Product density prepared in this example: 15.6-15.7 g/cm 3 Product hardness: 89-92 (HRA), microscopic dimensions of the product: the average grain size is < 2 microns.
FIG. 1 is a schematic diagram of the microstructure of a tungsten carbide target prepared by the preparation method of the present application. As can be seen from the microstructure of FIG. 1, defects such as holes are not seen, and the crystal grain is equiaxed in morphology and uniform in size.
Cost analysis:
by adopting the mould pressing and novel sintering process, the blank with the thickness of 50mm can be pressed because the groove size is phi 101mm, and the second blank size is phi 101x50mm. 4 phi 100x12mm finished tungsten carbide targets can be processed by 50mm phi 101x, and 36 tungsten carbide targets can be processed by each furnace. The material utilization rate (calculated by the total mass of the finished tungsten carbide target material/the total mass of tungsten carbide powder) is 88 percent, the sintering cost is calculated by 300 yuan per kilogram of tungsten carbide powder and 20000 yuan per furnace, the powder loading amount per furnace is 6 kg x9, and the tungsten carbide cost per phi 100x12mm is 1005 yuan.
Example 2
This example the process was the same as in example 1 except that the tungsten carbide powder particle size and the hot press sintering step parameters were different. The tungsten carbide powder particle size D50 for the molding of this example was 0.5 microns and the parameters of the hot press sintering step are shown in table 2.
TABLE 2
| Stage(s) | Temperature (temperature) | Pressure (MPa) | Time |
| A first temperature rising stage | Furnace temperature-1100 DEG C | 0 | 65min |
| First heat preservation stage | 1100℃ | 0 | 55min |
| A second temperature rising stage | 1100℃-1700℃ | 0 | 140min |
| Second heat preservation stage | 1700℃ | 0 | 1h |
| A third temperature rising stage | 1700℃-2100℃ | 0-30MPa | 3h |
| Fourth heat preservation stage | 2100℃ | 30MPa | 2.5h |
Product density prepared in this example: 15.4-15.6 g/cm 3 Product hardness: 89-94 (HRA), microscopic dimensions of the product: the average grain size is < 2 microns.
From the microstructure, defects such as holes are not seen, and the crystal grain is equiaxed and uniform in size.
Comparative example 1
The preparation method comprises the following steps:
(1) Screening powder: screening the tungsten carbide powder to obtain tungsten carbide powder with D50 of 1 micron;
(2) And (3) mould pressing: the obtained tungsten carbide powder with the D50 of 1 micrometer is molded to obtain a square blank with the length of 315x315x (45-50) mm (length x width x thickness), and the density of the blank after molding is 7-9 g/cm 3 ；
(3) And (3) charging: loading the blank obtained after the mould pressing into a hot-pressing mould for hot-pressing sintering, wherein the cavity of the hot-pressing mould is in a square shape of 315x315 mm;
(4) And hot-pressing and sintering: placing the loaded mould into a hot pressing furnace for hot pressing sintering, and after loading, vacuumizing the hot pressing furnace by adopting a diffusion pump until the vacuum degree is 1x 10 -1 Pa, and this vacuum is maintained during the hot press sintering process.
The process parameters of the hot press sintering step are as in table 1 above.
The size of the blank sintered by hot pressing is 315x315x25mm, referring to fig. 5, 9 finished target machining positions 3 are arranged on the large-size hot pressed sintered blank 2, and two phi 100x12mm finished targets can be cut at each position.
The density of the product prepared in this example is 15.6-15.7 g/cm 3 Product hardness: 89-93 (HRA), microscopic dimensions of the product: the average grain size is < 2 microns.
Cost analysis:
with the preparation method of comparative example 1, a square blank of 315x315mm size was pressed and sintered, and then rounded (shown in fig. 5). Because the blank size is large, sintering is difficult, the sintering thickness is limited, only 315x315x25mm blanks can be sintered, at most 18 phi 100x12mm finished products can be processed at one time, and the material utilization rate is about 68%. The sintering cost of the tungsten carbide powder is 20000 yuan per furnace per kilogram of 300 yuan, the powder loading amount per furnace is 39 kilograms, and the cost of the tungsten carbide powder with the diameter of D100x12mm per block is 1760 yuan.
Comparative example 2
This comparative example was conducted in the same manner as in example 1 except that the molding was conducted using tungsten carbide powder having a particle size D50 of 4. Mu.m.
The density of the product prepared in this comparative example: 13.5 to 13.7g/cm 3 The relative density is only about 86%, the product hardness: 75-80 (HRA), microscopic dimensions of the product: the average grain size is < 5 microns.
From the microstructure, many pores exist in the product, and the sintering difficulty is increased due to the large particle size, so that the product cannot be sintered to a proper density.
Claims (10)
1. The preparation method of the tungsten carbide target is characterized by comprising the following steps of:
and (3) mould pressing: molding tungsten carbide powder to obtain a first blank;
and (3) charging: loading a plurality of first blanks into a die through superposition or/and regular arrangement;
and hot-pressing and sintering: putting the die provided with the first blank into a hot pressing furnace, and performing hot pressing sintering to obtain a second blank;
and (3) machining: and machining the second blank to obtain the tungsten carbide target material with the required size.
2. The method according to claim 1, wherein the tungsten carbide powder has a particle size D50 of 0.5 to 1 μm.
3. The method according to claim 1, wherein,
the pressure of the mould pressing is 50-70 Mpa, and the density of the first blank after the mould pressing is 8.0-10 g/cm 3 ；
And/or the cross-sectional shape of the first blank extruded is the same as the cross-sectional shape of the finished target, and the cross-sectional dimension of the first blank is equal to or larger than the cross-sectional dimension of the finished target, preferably, the difference between the cross-sectional dimension of the first blank and the cross-sectional dimension of the finished target is 0-5mm.
4. A method of manufacture according to any one of claims 1 to 3, wherein the mould of the charging step is an isostatic mould;
the isostatic pressing die comprises a female die and a male die matched with the female die, and when the male die cover is arranged on the female die, a plurality of die cavity spaces for accommodating a first blank are formed.
5. The method of manufacturing according to claim 4, wherein the male die comprises a second base and a plurality of projections formed on a surface of the second base, and the female die comprises a first base and a plurality of grooves formed on the first base; the number of the grooves and the protrusions are the same, and the arrangement modes of the grooves and the protrusions on the corresponding substrates are the same, and each groove is matched with the corresponding protrusion to form a die cavity space for accommodating a first blank;
preferably, the height of each groove is greater than the height of the first blank, more preferably the height of the groove is more than 3 times the height of the first blank.
6. The method of manufacturing according to claim 5, wherein the hot press sintering step comprises:
a first temperature rising stage: heating the hot pressing furnace from the furnace temperature to the first heat preservation temperature of 900-1100 ℃ for 60-70 min;
a first heat preservation stage: preserving heat for 50-70 min at 900-1100 ℃;
a second temperature rising stage: heating from the first heat preservation temperature to the second heat preservation temperature of 1500-1700 ℃ for 100-140min;
and a second heat preservation stage: preserving heat at 1500-1700 ℃ for 60-70 min;
and a third temperature rising stage: heating from the second heat preservation temperature to a third heat preservation temperature of 2000-2100 ℃ for 160-200min;
and a third heat preservation stage: preserving heat for 2.5-4 h at the third preserving temperature;
in the third heating stage, the pressure applied to the hot pressing furnace gradually increases to 25-40 MPa;
in the third heat preservation stage, the pressure applied to the hot pressing furnace is 25-40 Mpa;
the hot pressed sintering is carried out at a vacuum degree of 5x 10 -1 Pa～5*10 -2 Under Pa.
7. A tungsten carbide target prepared by the method of any one of claims 1-6, the tungsten carbide target having a density of: 15.4-15.7 g/cm 3 Product hardness: 85-95 HRA, and the average grain size of the product is less than 2 microns.
8. The die is characterized by being an isostatic pressing die, and comprises a female die and a male die matched with the female die, wherein when the male die cover is arranged on the female die, a plurality of die cavity spaces for accommodating a first blank are formed.
9. The die of claim 8, wherein the male die comprises a second substrate and a plurality of protrusions formed on a surface of the second substrate, and the female die comprises a first substrate and a plurality of grooves formed on the first substrate; the number of the grooves and the protrusions are the same, and the arrangement modes of the grooves and the protrusions on the corresponding substrates are the same, and each groove is matched with the corresponding protrusion to form a die cavity space for accommodating a first blank; the cross-sectional shape of each of the grooves and the protrusions is the same as the cross-sectional shape of the first blank, and the cross-sectional size of each of the grooves is equivalent to the cross-sectional size of the first blank so that the first blank can be just fitted into the groove.
10. A mould according to claim 9, wherein the height of each recess is greater than the height of the first blank, preferably the height of the recess is more than 3 times the height of the first blank.
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