CN118026688A - CK32 duplex carbide with low oxygen content and low free carbon and preparation method thereof - Google Patents
CK32 duplex carbide with low oxygen content and low free carbon and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 111
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 70
- 239000001301 oxygen Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000000203 mixture Substances 0.000 claims abstract description 53
- 238000001238 wet grinding Methods 0.000 claims abstract description 52
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002245 particle Substances 0.000 claims abstract description 23
- 229910052786 argon Inorganic materials 0.000 claims abstract description 14
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000010937 tungsten Substances 0.000 claims abstract description 14
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 14
- 239000011363 dried mixture Substances 0.000 claims abstract description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000010936 titanium Substances 0.000 claims abstract description 9
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 28
- 238000001354 calcination Methods 0.000 claims description 25
- 239000000463 material Substances 0.000 claims description 20
- 238000001291 vacuum drying Methods 0.000 claims description 19
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 17
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 17
- 239000006229 carbon black Substances 0.000 claims description 12
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 11
- 238000003825 pressing Methods 0.000 claims description 10
- 238000007873 sieving Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 abstract description 8
- 238000004663 powder metallurgy Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 11
- 239000006104 solid solution Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000007580 dry-mixing Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention belongs to the technical field of powder metallurgy, and particularly relates to a CK32 compound carbide with low oxygen content and low free carbon and a preparation method thereof, wherein a tungsten source, a titanium source and a carbon source are taken for wet grinding to obtain a mixture, the mixture obtained by wet grinding is dried, the dried mixture is pressed and molded, then the mixture is calcined in an argon environment, crushed and sieved, and the sieved substance is taken to obtain the CK32 compound carbide with low oxygen content and low free carbon, wherein the Fischer particle size of the CK32 compound carbide with low oxygen content and low free carbon is 2.2-2.7 mu m, the total carbon content is 11.2-11.4 wt%, the content of free carbon C f is less than or equal to 0.03wt%, and the O content is less than or equal to 0.04wt%.
Description
Technical Field
The invention belongs to the technical field of powder metallurgy, and particularly relates to a CK32 duplex carbide with low oxygen content and low free carbon and a preparation method thereof.
Background
The cutting performance of the cutter is improved as much as possible, the abrasion rate of the cutter in the cutting process is slowed down, the service life of the cutter is prolonged, and the cutting tool is an important way for reducing the production and processing cost. The effect of the solid solution properties of tungsten carbide and titanium carbide on the properties of YT cemented carbide is important because the properties of the solid solution directly determine the overall properties of the cemented carbide, including hardness, wear resistance, thermal stability, corrosion resistance, and cutting properties. The high content of free carbon and oxygen in the CK material can influence the change of the carbon content in the process of preparing the alloy, thereby adversely affecting the performance of the alloy.
The free carbon content of the prior CK32 complex carbide is generally above 0.03 weight percent, the oxygen content is generally about 0.1 weight percent, and the relative height is relatively high; tiO 2 has small density, small apparent density, easy agglomeration and difficult full and uniform mixing under the dry mixing condition; and the CK32 compound carbide is mainly dissolved in the hydrogen atmosphere at present, and although part of oxygen can be taken away by the hydrogen to reduce the oxygen content, the hydrogen can react with carbon black, a boat and graphite materials in equipment to generate a small amount of methane and crack the methane into C and H 2, so that the C always exists in the furnace atmosphere, and finally the free carbon content of the CK32 compound carbide is difficult to reduce to a lower state.
Disclosure of Invention
In order to solve the problems in the prior art, the main purpose of the invention is to provide a CK32 duplex carbide with low oxygen content and low free carbon and a preparation method thereof.
In order to solve the technical problems, according to one aspect of the present invention, the following technical solutions are provided:
A preparation method of CK32 duplex carbide with low oxygen content and low free carbon comprises the following steps:
S1, taking 46-46.5wt% of tungsten source, 38-39wt% of titanium source and 15-15.5wt% of carbon source in percentage by mass, and wet-milling to obtain a mixture;
S2, carrying out vacuum drying on the mixture obtained by wet grinding;
and S3, pressing and forming the dried mixture, calcining in an argon environment, crushing and sieving, and taking the undersize to obtain the CK32 duplex carbide with low oxygen content and low free carbon.
As a preferable scheme of the preparation method of the CK32 duplex carbide with low oxygen content and low free carbon, the invention comprises the following steps: in the step S1, the tungsten source is WC or a mixture of nano tungsten oxide and WC with the mass ratio of (3-5) (95-97).
As a preferable scheme of the preparation method of the CK32 duplex carbide with low oxygen content and low free carbon, the invention comprises the following steps: in the step S1, the titanium source is TiO 2, and the carbon source is carbon black.
As a preferable scheme of the preparation method of the CK32 duplex carbide with low oxygen content and low free carbon, the invention comprises the following steps: in the step S1, the granularity of WC is 2.0-2.5 μm.
As a preferable scheme of the preparation method of the CK32 duplex carbide with low oxygen content and low free carbon, the invention comprises the following steps: in the step S1, the specific surface area of the nano tungsten oxide is 7-13 m 2/g.
As a preferable scheme of the preparation method of the CK32 duplex carbide with low oxygen content and low free carbon, the invention comprises the following steps: in the step S1, wet grinding is performed in a planetary ball grinder, and the wet grinding process parameters are as follows: the ball-material ratio is 4-6:1, the wet milling time is 4-8 h, and the adding amount of alcohol just exceeds the solid surface.
As a preferable scheme of the preparation method of the CK32 duplex carbide with low oxygen content and low free carbon, the invention comprises the following steps: in the step S2, the vacuum drying process parameters are as follows: the vacuum degree is-0.055 to-0.1 MPa, and the temperature is 80-100 ℃.
As a preferable scheme of the preparation method of the CK32 duplex carbide with low oxygen content and low free carbon, the invention comprises the following steps: in the step S3, the calcination temperature is 2250-2350 ℃ and the calcination time is 0.5-2 h.
In order to solve the above technical problems, according to another aspect of the present invention, the following technical solutions are provided:
The CK32 double carbide with low oxygen content and low free carbon is prepared by the preparation method of the CK32 double carbide with low oxygen content and low free carbon.
As a preferred embodiment of the CK32 duplex carbide with low oxygen content and low free carbon, the invention is characterized in that: the Fischer particle size of the CK32 duplex carbide with low oxygen content and low free carbon is 2.2-2.7 mu m, the total carbon content is 11.2-11.4wt%, the free carbon C f content is less than or equal to 0.03wt% and the O content is less than or equal to 0.04wt%.
The beneficial effects of the invention are as follows:
The invention provides a CK32 compound carbide with low oxygen content and low free carbon and a preparation method thereof, wherein a tungsten source, a titanium source and a carbon source are taken for wet grinding to obtain a mixture, the mixture obtained by wet grinding is dried, the dried mixture is pressed and molded, then the mixture is calcined in an argon environment, crushed and sieved, the sieved material is taken out, the CK32 compound carbide with low oxygen content and low free carbon is obtained, the Fischer-Tropsch particle size of the CK32 compound carbide with low oxygen content and low free carbon is 2.2-2.7 mu m, the total carbon content is 11.2-11.4wt%, the free carbon C f content is less than or equal to 0.03wt%, and the O content is less than or equal to 0.04wt%.
Detailed Description
The following description will be made clearly and fully with reference to the technical solutions in the embodiments, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
According to one aspect of the invention, the invention provides the following technical scheme:
A preparation method of CK32 duplex carbide with low oxygen content and low free carbon comprises the following steps:
S1, taking 46-46.5wt% of tungsten source, 38-39wt% of titanium source and 15-15.5wt% of carbon source in percentage by mass, and wet-milling to obtain a mixture;
S2, carrying out vacuum drying on the mixture obtained by wet grinding;
and S3, pressing and forming the dried mixture, calcining in an argon environment, crushing and sieving, and taking the undersize to obtain the CK32 duplex carbide with low oxygen content and low free carbon.
The wet grinding mixing mode can effectively avoid the problems that TiO 2 is difficult to fully and uniformly mix under the dry mixing condition due to small density, small loose density and easy agglomeration, and realizes uniform mixing of materials; the vacuum drying can effectively avoid oxygen absorption in the drying process after wet grinding, and reduce the oxygen content of the mixture; the high-activity carbon generated after methane cracking caused by the reaction of hydrogen and graphite can be effectively avoided by sintering under the argon environment, the free carbon of CK32 duplex carbide can be obviously reduced, and the existence of the free carbon is further reduced by solid solution under the high-temperature condition.
Preferably, in the step S1, the tungsten source is WC or a mixture of nano tungsten oxide and WC with a mass ratio of (3-5): (95-97). The nano tungsten oxide is beneficial to reducing the total reaction time and improving the preparation efficiency. The nano tungsten oxide is fully ground and mixed after wet grinding, and reacts with carbon black in the sintering process to produce nano tungsten carbide, so that the surface activity is high, the solid solution reaction is promoted, the rate of WC entering TiC particles is increased, the reaction time is shortened, and the product quality is not affected by a small amount of addition. The excessive addition of nano tungsten oxide influences the solid solution effect of CK materials, so that free carbon and oxygen are higher; the effect of reducing the solid solution time cannot be achieved if the addition amount of the nano tungsten oxide is too small.
Preferably, in the step S1, the titanium source is TiO 2 and the carbon source is carbon black.
As a preferable scheme of the preparation method of the CK32 duplex carbide with low oxygen content and low free carbon, the invention comprises the following steps: in the step S1, the granularity of WC is 2.0-2.5 μm. The WC has too fine granularity and high oxygen content, which is not beneficial to preparing CK32 duplex carbide with low oxygen content; if the granularity of WC is too coarse, the granularity of the prepared CK32 duplex carbide is too coarse, and the technical requirements of products cannot be met.
Preferably, in the step S1, the specific surface area of the nano tungsten oxide is 7-13 m 2/g. The preparation is difficult if the specific surface area of the nano tungsten oxide is too high, and the surface activity of the particles is high, so that the particles are easy to agglomerate and are not favorable for full mixing; when the specific surface area is too small, microscopic nanotopography (better inter-particle dispersibility) cannot be formed, and the particles cannot be fully mixed in a shorter grinding time, so that the reduction of free carbon and oxygen content of the CK material is not facilitated.
Preferably, in the step S1, wet milling is performed in a planetary ball mill, and the wet milling process parameters are as follows: the ball-material ratio is 4-6:1, the wet milling time is 4-8 h, and the adding amount of alcohol just exceeds the solid surface. The probability of introducing other impurities is high when the ball material ratio is too large and the ball milling time is long, so that the preparation of the subsequent alloy is not facilitated; the ball material ratio is too small, the ball milling time is short, and the mixture is difficult to uniformly mix, which is unfavorable for complete solid solution and free carbon reduction.
Preferably, in the step S2, the vacuum drying process parameters are as follows: the vacuum degree is-0.055 to-0.1 MPa, and the temperature is 80-100 ℃. The slurry is easily pumped out due to high vacuum degree, so that the material loss is caused, and meanwhile, the requirement on equipment is high; too low vacuum is unfavorable for oxygen removal, and the oxygen content of the mixture is high. The material is easy to boil when the temperature is high, so that the material is splashed, the material loss is caused, and the energy consumption is high; the drying effect is poor when the temperature is low, the time is long, the efficiency is low, and the removal of oxygen is not facilitated.
Preferably, in the step S3, the calcination temperature is 2250-2350 ℃ and the calcination time is 0.5-2 h. The temperature is too low, the calcination time is short, the solid solution is easy to be incomplete, and the content of free carbon and oxygen is higher; the temperature is too high, the calcination time is long, the requirements on equipment are high, and the energy consumption is high;
according to another aspect of the invention, the invention provides the following technical scheme:
The CK32 double carbide with low oxygen content and low free carbon is prepared by the preparation method of the CK32 double carbide with low oxygen content and low free carbon.
Preferably, the Fischer particle size of the CK32 duplex carbide with low oxygen content and low free carbon is 2.2-2.7 mu m, the total carbon content is 11.2-11.4 wt%, the free carbon C f content is less than or equal to 0.03wt% and the O content is less than or equal to 0.04wt%.
The technical scheme of the invention is further described below by combining specific embodiments.
Example 1
A preparation method of CK32 duplex carbide with low oxygen content and low free carbon comprises the following steps:
s1, taking 46.5 weight percent of WC, 38 weight percent of TiO 2 and 15.5 weight percent of carbon black for wet grinding to obtain a mixture; the granularity of WC is 2.0 mu m, wet milling is carried out in a planetary ball mill, and the wet milling process parameters are as follows: the ball-material ratio is 4:1, the wet milling time is 8 hours, and the adding amount of alcohol just drops over the solid surface;
S2, carrying out vacuum drying on the mixture obtained by wet grinding; the vacuum drying process parameters are as follows: vacuum degree is-0.055 MPa, and temperature is 80 ℃;
And S3, pressing and forming the dried mixture, calcining the mixture in an argon environment at 2250 ℃ for 2 hours, crushing and sieving the mixture, and taking the undersize to obtain the CK32 duplex carbide with low oxygen content and low free carbon.
The CK32 complex carbide prepared in this example had a fisher particle size of 2.24 μm, a total carbon content of 11.4wt%, a free carbon C f content of 0.03wt% and an O content of 0.04wt%.
Example 2
A preparation method of CK32 duplex carbide with low oxygen content and low free carbon comprises the following steps:
S1, taking 46wt% of WC, 39wt% of TiO 2 and 15wt% of carbon black for wet grinding to obtain a mixture; the granularity of WC is 2.5 mu m, wet milling is carried out in a planetary ball mill, and the wet milling process parameters are as follows: the ball-material ratio is 6:1, the wet milling time is 4 hours, and the adding amount of alcohol just drops over the solid surface;
s2, carrying out vacuum drying on the mixture obtained by wet grinding; the vacuum drying process parameters are as follows: vacuum degree is-0.1 MPa, and temperature is 100 ℃;
And S3, pressing and forming the dried mixture, calcining the mixture in an argon environment at the calcining temperature of 2350 ℃ for 1h, crushing and sieving the mixture, and taking the undersize to obtain the CK32 duplex carbide with low oxygen content and low free carbon.
The CK32 complex carbide prepared in this example has a fisher particle size of 2.68 μm, a total carbon content of 11.3wt%, a free carbon C f content of 0.01wt% and an O content of 0.03wt%.
Example 3
A preparation method of CK32 duplex carbide with low oxygen content and low free carbon comprises the following steps:
S1, taking 46wt% of WC, 39wt% of TiO 2 and 15wt% of carbon black for wet grinding to obtain a mixture; the granularity of WC is 2.24 mu m, wet milling is carried out in a planetary ball mill, and the wet milling process parameters are as follows: the ball-material ratio is 5:1, the wet milling time is 6 hours, and the adding amount of alcohol just drops over the solid surface;
s2, carrying out vacuum drying on the mixture obtained by wet grinding; the vacuum drying process parameters are as follows: vacuum degree is-0.07 MPa, and temperature is 90 ℃;
and S3, pressing and forming the dried mixture, calcining the mixture in an argon environment at the calcining temperature of 2300 ℃ for 1.5 hours, crushing and sieving the mixture, and taking the undersize to obtain the CK32 duplex carbide with low oxygen content and low free carbon.
The CK32 complex carbide prepared in this example has a fisher particle size of 2.38 μm, a total carbon content of 11.35wt%, a free carbon C f content of 0.02wt% and an O content of 0.034wt%.
Example 4
A preparation method of CK32 duplex carbide with low oxygen content and low free carbon comprises the following steps:
S1, taking 46wt% of WC, 39wt% of TiO 2 and 15wt% of carbon black for wet grinding to obtain a mixture; the granularity of WC is 2.5 mu m, wet milling is carried out in a planetary ball mill, and the wet milling process parameters are as follows: the ball-material ratio is 5:1, the wet milling time is 5h, and the adding amount of alcohol just drops over the solid surface;
s2, carrying out vacuum drying on the mixture obtained by wet grinding; the vacuum drying process parameters are as follows: vacuum degree is-0.1 MPa, and temperature is 85 ℃;
And S3, pressing and forming the dried mixture, calcining the mixture in an argon environment at the calcining temperature of 2350 ℃ for 1h, crushing and sieving the mixture, and taking the undersize to obtain the CK32 duplex carbide with low oxygen content and low free carbon.
The CK32 complex carbide prepared in this example has a fisher particle size of 2.64 μm, a total carbon content of 11.3wt%, a free carbon C f content of 0.01wt% and an O content of 0.025wt%.
Example 5
A preparation method of CK32 duplex carbide with low oxygen content and low free carbon comprises the following steps:
S1, wet milling 46wt% of tungsten source, 39wt% of TiO 2 and 15wt% of carbon black to obtain a mixture; the tungsten source is a mixture of nano tungsten oxide and WC with the mass ratio of 3:97, the granularity of WC is 2.5 mu m, the specific surface area of the nano tungsten oxide is 13m 2/g, wet milling is carried out in a planetary ball mill, and the wet milling process parameters are as follows: the ball-material ratio is 5:1, the wet milling time is 5h, and the adding amount of alcohol just drops over the solid surface;
s2, carrying out vacuum drying on the mixture obtained by wet grinding; the vacuum drying process parameters are as follows: vacuum degree is-0.1 MPa, and temperature is 85 ℃;
And S3, pressing and forming the dried mixture, calcining the mixture in an argon environment at the calcining temperature of 2350 ℃ for 50min, crushing and sieving the mixture, and taking the undersize to obtain the CK32 duplex carbide with low oxygen content and low free carbon.
The CK32 complex carbide prepared in this example had a fisher particle size of 2.58 μm, a total carbon content of 11.29wt%, a free carbon C f content of 0.01wt% and an O content of 0.027wt%.
Example 6
A preparation method of CK32 duplex carbide with low oxygen content and low free carbon comprises the following steps:
S1, wet milling 46wt% of tungsten source, 39wt% of TiO 2 and 15wt% of carbon black to obtain a mixture; the tungsten source is a mixture of nano tungsten oxide and WC with the mass ratio of 5:95, the granularity of WC is 2.5 mu m, the specific surface area of the nano tungsten oxide is 7m 2/g, wet milling is carried out in a planetary ball mill, and the wet milling process parameters are as follows: the ball-material ratio is 5:1, the wet milling time is 5h, and the adding amount of alcohol just drops over the solid surface;
s2, carrying out vacuum drying on the mixture obtained by wet grinding; the vacuum drying process parameters are as follows: vacuum degree is-0.1 MPa, and temperature is 85 ℃;
And S3, pressing and forming the dried mixture, calcining the mixture in an argon environment at the calcining temperature of 2350 ℃ for 40min, crushing and sieving the mixture, and taking the undersize to obtain the CK32 duplex carbide with low oxygen content and low free carbon.
The CK32 complex carbide prepared in this example had a fisher particle size of 2.66 μm, a total carbon content of 11.32wt%, a free carbon C f content of 0.01wt% and an O content of 0.029wt%.
Comparative example 1
A preparation method of CK32 duplex carbide comprises the following steps:
S1, taking 46wt% of WC, 39wt% of TiO 2 and 15wt% of carbon black for dry mixing according to mass percentage to obtain a mixture;
and S2, pressing and forming the mixture, calcining the mixture in an argon environment at the calcining temperature of 2350 ℃ for 1h, crushing and sieving the mixture, and taking the undersize to obtain the CK32 duplex carbide.
The CK32 complex carbide prepared in this comparative example had a fisher particle size of 2.6 μm, a total carbon content of 11.3wt%, a free carbon C f content of 0.08wt% and an O content of 0.07wt%.
Comparative example 2
The difference from example 4 is that calcination is performed under hydrogen atmosphere in step S3.
The CK32 complex carbide prepared in this comparative example had a fisher particle size of 2.64 μm, a total carbon content of 11.3wt%, a free carbon C f content of 0.06wt% and an O content of 0.025wt%.
Comparative example 3
The difference from example 4 is that drying is performed at normal pressure in step S2.
The CK32 complex carbide prepared in this comparative example had a fisher particle size of 2.64 μm, a total carbon content of 11.3wt%, a free carbon C f content of 0.01wt% and an O content of 0.11wt%.
Comparative example 4
The difference from example 6 is that the tungsten source in step S1 is a mixture of nano tungsten oxide and WC in a mass ratio of 10:90.
The CK32 double carbide prepared in this comparative example had a fisher particle size of 2.66 μm, a total carbon content of 11.32wt%, a free carbon C f content of 0.19wt% and an O content of 0.085wt%.
Comparative example 5
The difference from example 6 is that the specific surface area of the nano tungsten oxide in step S1 is 5.3m 2/g.
The CK32 complex carbide prepared in this comparative example had a fisher particle size of 2.63 μm, a total carbon content of 11.25wt%, a free carbon C f content of 0.16wt% and an O content of 0.09wt%.
As can be seen from the above examples and comparative examples, according to the invention, a tungsten source, a titanium source and a carbon source are wet-milled to obtain a mixture, the wet-milled mixture is dried, the dried mixture is pressed and molded, and then calcined in an argon environment, crushed and sieved, and the sieved product is taken out to obtain the CK32 complex carbide with low oxygen content and low free carbon, wherein the Fischer particle size of the CK32 complex carbide with low oxygen content and low free carbon is 2.2-2.7 mu m, the total carbon content is 11.2-11.4 wt%, the free carbon C f content is less than or equal to 0.03wt% and the O content is less than or equal to 0.04wt%.
The foregoing description is only of the preferred embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent structural changes made by the content of the present invention or direct/indirect application in other related technical fields are included in the scope of the present invention.
Claims (10)
1. A method for preparing CK32 duplex carbide with low oxygen content and low free carbon, which is characterized by comprising the following steps:
S1, taking 46-46.5wt% of tungsten source, 38-39wt% of titanium source and 15-15.5wt% of carbon source in percentage by mass, and wet-milling to obtain a mixture;
S2, carrying out vacuum drying on the mixture obtained by wet grinding;
and S3, pressing and forming the dried mixture, calcining in an argon environment, crushing and sieving, and taking the undersize to obtain the CK32 duplex carbide with low oxygen content and low free carbon.
2. The method for preparing the CK32 duplex carbide with low oxygen content and low free carbon according to claim 1, wherein in the step S1, the tungsten source is WC or a mixture of nano tungsten oxide and WC with the mass ratio of (3-5): 95-97.
3. The method for preparing CK32 multiple carbide with low oxygen content and low free carbon according to claim 1, wherein in the step S1, the titanium source is TiO 2 and the carbon source is carbon black.
4. The method for preparing CK32 duplex carbide with low oxygen content and low free carbon according to claim 2, wherein in step S1, WC has a particle size of 2.0-2.5 μm.
5. The method for preparing CK32 multiple carbide with low oxygen content and low free carbon according to claim 2, wherein in the step S1, the specific surface area of nano tungsten oxide is 7-13 m 2/g.
6. The method for preparing CK32 multiple carbide with low oxygen content and low free carbon according to claim 1, wherein in step S1, wet milling is performed in a planetary ball mill, and the wet milling process parameters are as follows: the ball-material ratio is 4-6:1, the wet milling time is 4-8 h, and the adding amount of alcohol just exceeds the solid surface.
7. The method for preparing CK32 multiple carbide with low oxygen content and low free carbon according to claim 1, wherein in the step S2, the vacuum drying process parameters are as follows: the vacuum degree is-0.055 to-0.1 MPa, and the temperature is 80-100 ℃.
8. The method for preparing CK32 multiple carbide with low oxygen content and low free carbon according to claim 1, wherein in the step S3, the calcination temperature is 2250-2350 ℃ and the calcination time is 0.5-2 h.
9. A CK32 multiple carbide with low oxygen content and low free carbon, which is prepared by the preparation method of the CK32 multiple carbide with low oxygen content and low free carbon according to any one of claims 1-8.
10. The low oxygen content low free carbon CK32 multiple carbide as claimed in claim 9, wherein the low oxygen content low free carbon CK32 multiple carbide has a fischer particle size of 2.2-2.7 μm, a total carbon content of 11.2-11.4 wt%, a free carbon C f content of 0.03wt% or less, and an O content of 0.04wt% or less.
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