CN113086984A - Preparation method of chromium carbide powder - Google Patents
Preparation method of chromium carbide powder Download PDFInfo
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Abstract
The invention discloses a preparation method of chromium carbide powder. The preparation method comprises the following steps: s1, sequentially carrying out first ball milling, first carbonization and second ball milling on the mixed powder of the chromium powder and the carbon black to obtain a precursor; and S2, sequentially carrying out secondary carbonization and tertiary ball milling on the mixed powder of the precursor and the carbon black to obtain the chromium carbide powder. The preparation method is simple, low in production cost and suitable for industrial production; the prepared chromium carbide powder has submicron-level granularity, high powder purity and very uniform secondary particle size.
Description
Technical Field
The invention belongs to the technical field of powder metallurgy, and particularly relates to a preparation method of chromium carbide powder.
Background
Chromium carbide (Cr)3C2) As the transition metal carbide, the alloy has higher melting point, hardness, high-temperature strength and good electrical conductivity and thermal conductivity, and the excellent properties ensure the alloy to be applied to metallurgy, electronics,The catalyst and the high-temperature coating material are widely applied. Wherein, the chromium carbide is widely applied in the fields of hard alloy grain growth inhibitors, special steel additives, nickel-chromium carbide high-temperature coatings and the like.
The current common method for preparing chromium carbide is as follows:
(1) carbothermic reduction: i.e. reduction of chromium oxides by solid carbon. The method has simple process, good repeatability and high industrial application value; however, the method has high carbonization temperature (not less than 1400 ℃), long reaction time (not less than 4h), obvious crystal grain growth at high temperature, and thick granularity (30-300 μm) of the prepared chromium carbide powder, and is difficult to meet the requirement of modern industry on superfine submicron (less than 1.0 μm) chromium carbide powder.
(2) Gas-phase reduction method: carbon-containing gas is used as a reducing agent, and when chromium carbide is prepared, a carbon source is provided by cracking of gaseous hydrogen compound molecules, so that the carbonization temperature can be reduced (less than or equal to 1200 ℃), and the reaction time is shortened (less than or equal to 4 hours); however, the method using the mixed gas as the reducing gas has relatively high economic cost, poor controllability of carbon content in the product, and difficulty in ensuring single-phase Cr3C2(ii) a And the prepared powder has large secondary particle size and wide particle size distribution, and cannot meet the requirement of the modern industry on the uniformity of the submicron chromium carbide powder.
(3) A precursor method: the precursor method is that various raw materials are fully contacted in a solution mixing mode, then the solution is sprayed, dried or heated and evaporated to obtain solid phase precursor powder containing a chromium source and a carbon source, and then the solid phase precursor powder is further subjected to heat treatment to prepare the chromium carbide powder. The precursor method is not easy to control the carbon content in the mixture, is difficult to ensure the purity of the product, is not simple enough in process and higher in cost compared with the traditional carbonization-reduction reaction, and is not easy to apply in industrial large-scale production.
As can be seen, the existing method for preparing chromium carbide has complex process and high cost, and the prepared chromium carbide powder has the defects of coarse granularity, poor purity and poor secondary particle size uniformity.
Disclosure of Invention
The invention provides a preparation method of chromium carbide powder, aiming at solving the defects that the preparation method of chromium carbide powder in the prior art is complex in process and high in cost, and the prepared chromium carbide powder is thick in granularity, poor in purity and poor in secondary particle size uniformity. The preparation method is simple, low in production cost and suitable for industrial production; the prepared chromium carbide powder has superfine submicron level granularity, high powder purity and very uniform secondary particle size.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of chromium carbide powder, which comprises the following steps:
s1, sequentially carrying out first ball milling, first carbonization and second ball milling on the mixed powder of the chromium powder and the carbon black to obtain a precursor; wherein in the mixed powder of the chromium powder and the carbon black, the mass ratio of the chromium powder to the carbon black is (8-12):1, and the temperature of the first carbonization is 1350-;
s2, sequentially carrying out second carbonization and third ball milling on the mixed powder of the precursor and the carbon black to obtain chromium carbide powder; wherein, in the mixed powder of the precursor and the carbon black, the mass ratio of the precursor to the carbon black is (15-25) to 1; the temperature of the second carbonization is 1000-1500 ℃.
In step S1, the chromium powder may be elemental metal chromium powder as is conventional in the art, and the particle size of the chromium powder is preferably not more than 100 μm.
In steps S1 and S2, the carbon black may be a carbon black conventional in the art, and the particle size of the carbon black is preferably not more than 20 μm.
In step S1, in the mixed powder of the chromium powder and the carbon black, the mass ratio of the chromium powder to the carbon black is preferably 10: 1. When the mass ratio of the chromium powder to the carbon black is 10:1, corresponding to the theoretical carbon mixing amount, Cr is generated7C3The stoichiometric ratio of (a).
In step S1, the mixed powder of chromium powder and carbon black may be prepared by a method conventional in the art, and the chromium powder and the carbon black may be mixed. The mixing may occur in the first ball milling.
In steps S1 and S2, the first ball milling, the second ball milling, and the third ball milling may be performed using a ball mill conventional in the art, such as a general planetary ball mill.
In steps S1 and S2, the ball milling media for the first ball milling, the second ball milling and the third ball milling may be conventional in the art, and preferably ethanol. When the ball milling medium is ethanol, the dosage of the ethanol is preferably 20-60%, and the percentage is the mass percentage of the ethanol in the powder. During the ball milling process, the ball milling medium and the powder form a slurry with certain fluidity.
In steps S1 and S2, the ball-to-material ratio of the first ball milling, the second ball milling and the third ball milling may be the conventional ball-to-material ratio capable of dispersing powder in the art, and is generally (5-20):1, for example 5:1, 10:1 or 20: 1. Wherein the ball-material ratio is the mass ratio of the steel balls and the powder of the ball mill.
In steps S1 and S2, after the first ball milling, the second ball milling, or the third ball milling, optionally further comprising a step of drying. Wherein, the drying temperature can be determined according to the ball milling medium. For example, when the milling media is ethanol, the temperature of the oven drying may be 60-100 ℃.
In step S1, the rotation speed of the first ball milling is preferably 100-300 r/min; the time of the first ball milling is preferably 2 to 6 hours.
In step S1, the rotation speed of the second ball milling is preferably 200-; the time of the second ball milling is preferably 5 to 15 hours.
In step S2, the rotation speed of the third ball milling is preferably 200-; the time of the third ball milling is preferably 20 to 60 hours.
In steps S1 and S2, the first carbonization and the second carbonization may be performed in a carbonization apparatus conventional in the art, such as a high-temperature tube furnace. Wherein, the powder can be put into a high-purity graphite burning boat and then put into a high-temperature tube furnace.
In steps S1 and S2, the first carbonization and the second carbonization may be performed under an inert atmosphere. Wherein the inert atmosphere may be an argon atmosphere.
In step S1, the time for the first carbonization is preferably 1 to 5 hours.
In step S1, the precursor is single Cr7C3And (4) phase(s). The carbon content of the precursor is preferably 9-10%, for example 9.3%, 9.5% or 9.6%.
In step S2, in the mixed powder of the precursor and the carbon black, the mass ratio of the precursor to the carbon black is preferably (18 to 22): 1, e.g. 20: 1. When the mass ratio of the precursor to the carbon black is 20:1, Cr is generated corresponding to the theoretical carbon mixing amount3C2The stoichiometric ratio of (a).
In step S2, the mixed powder of the precursor and the carbon black may be prepared by a method conventional in the art, and the precursor and the carbon black may be mixed uniformly.
In step S2, the temperature of the second carbonization is preferably 1000 to 1400 ℃, for example 1100 ℃, 1200 ℃ or 1300 ℃. The time of the second carbonization is preferably 2 to 8 hours. The powder obtained after the second carbonization has a micro-weak bonding phenomenon.
In step S2, the chromium carbide powder is single Cr3C2And (4) phase(s). The carbon content of the chromium carbide powder is preferably 13-14%, for example 13.2%, 13.5% or 13.8%. The particle size D50 of the chromium carbide powder is not more than 1 μm, for example 0.71 μm, 0.75 μm or 0.83 μm.
In a preferred embodiment of the present invention, the method for preparing the chromium carbide powder comprises the steps of:
(1) ball milling for the first time: accurately weighing chromium powder and carbon black according to the mass ratio of 10:1, pouring the chromium powder and the carbon black into a ball milling tank of a common planetary ball mill, wherein the ball-material ratio is (5-20):1, adding ethanol which is 20-60% of the mass of the powder as a ball milling medium, performing ball milling for 2-6h at the rotating speed of 100-300r/min, and then drying at the temperature of 60-100 ℃;
(2) first carbonization: putting the dried mixed powder into a high-purity graphite burning boat, putting the high-purity graphite burning boat into a high-temperature tube furnace, and preserving heat for 1-5 hours at 1400 ℃ under the protection of argon atmosphere;
(3) ball milling for the second time: putting the first carbonization product into a ball milling tank of a common planetary ball mill, wherein the ball-material ratio is 10:1, adding ethanol with the mass of 20-60% of that of the powder as a ball milling medium, and carrying out ball milling for 5-15h under the condition of the rotation speed of 200-;
(4) and (3) second carbonization: accurately weighing the precursor and the carbon black according to the mass ratio of 20:1, uniformly mixing, loading into a high-purity graphite burning boat, and placing into a high-temperature tube furnace, and preserving heat for 2-8h at the temperature of 1000-1500 ℃ under the protection of argon atmosphere;
(5) ball milling for the third time: and (3) putting the secondary carbonized product into a ball milling tank of a common planetary ball mill, wherein the ball-material ratio is 10:1, adding ethanol with the mass of 20-60% of that of the powder as a ball milling medium, and carrying out ball milling for 20-60h under the condition that the rotating speed is 200-.
In the present invention, the words "first", "second" and "third" have no special meaning, but only indicate the sequence of operations.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows: the chromium carbide powder prepared by the method has the advantages of superfine submicron (less than or equal to 1 mu m) granularity, high powder purity and single Cr tissue3C2Phase, secondary particle size is very uniform; in addition, the preparation method of the invention has low production cost and can be used for industrial production.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
Example 1
A method of preparing chromium carbide powder comprising the steps of:
(1) ball milling for the first time: accurately weighing chromium powder and carbon black according to the mass ratio of 10:1, pouring the chromium powder and the carbon black into a ball milling tank of a common planetary ball mill, wherein the ball-material ratio is 5:1, adding 20% of ethanol of the mass of the powder serving as a ball milling medium into the ball milling tank, forming slurry with certain fluidity by the ball milling medium and the powder, performing ball milling for 2 hours at the rotating speed of 100r/min, and then drying at the temperature of 60 ℃;
(2) first carbonization: putting the dried mixed powder into a high-purity graphite burning boat, putting the high-purity graphite burning boat into a high-temperature tube furnace, and preserving heat for 1h at 1400 ℃ under the protection of argon atmosphere to obtain a first carbonized product;
(3) ball milling for the second time: filling the first carbonization product into a ball milling tank of a common planetary ball mill, wherein the ball-material ratio is 10:1, adding ethanol with the mass of 20% of the powder as a ball milling medium, and performing ball milling for 5 hours at the rotation speed of 200r/min to obtain a precursor;
(4) and (3) second carbonization: accurately weighing the precursor and the carbon black according to the mass ratio of 20:1, uniformly mixing, loading into a high-purity graphite burning boat, and placing into a high-temperature tube furnace, and preserving heat for 2 hours at 1000 ℃ under the protection of argon atmosphere to obtain a secondary carbonized product, wherein the product has a weak bonding phenomenon on microcosmic scale;
(5) ball milling for the third time: and (3) putting the secondary carbonized product into a ball milling tank of a common planetary ball mill, wherein the ball-material ratio is 5:1, adding ethanol with the mass of 20% of that of the powder as a ball milling medium, and carrying out ball milling for 20 hours at the rotating speed of 200r/min to obtain the chromium carbide powder.
Example 2
A method of preparing chromium carbide powder comprising the steps of:
(1) ball milling for the first time: accurately weighing chromium powder and carbon black according to the mass ratio of 10:1, pouring the chromium powder and the carbon black into a ball milling tank of a common planetary ball mill, wherein the ball-material ratio is 10:1, adding ethanol accounting for 40% of the mass of the powder as a ball milling medium, forming slurry with certain fluidity by the ball milling medium and the powder, performing ball milling for 4 hours at the rotating speed of 200r/min, and then drying at 80 ℃;
(2) first carbonization: putting the dried mixed powder into a high-purity graphite burning boat, putting the high-purity graphite burning boat into a high-temperature tube furnace, and preserving heat for 3 hours at 1400 ℃ under the protection of argon atmosphere to obtain a first carbonized product;
(3) ball milling for the second time: filling the first carbonization product into a ball milling tank of a common planetary ball mill, wherein the ball-material ratio is 10:1, adding ethanol with the mass of 40% of the powder as a ball milling medium, and performing ball milling for 10 hours at the rotation speed of 400r/min to obtain a precursor;
(4) and (3) second carbonization: accurately weighing the precursor and the carbon black according to the mass ratio of 20:1, uniformly mixing, loading into a high-purity graphite burning boat, and placing into a high-temperature tube furnace, and preserving heat for 4 hours at 1100 ℃ under the protection of argon atmosphere to obtain a secondary carbonized product, wherein the product has a weak bonding phenomenon on a microscopic scale;
(5) ball milling for the third time: and (3) putting the secondary carbonized product into a ball milling tank of a common planetary ball mill, wherein the ball-material ratio is 10:1, adding ethanol with the mass of 40% of that of the powder as a ball milling medium, and carrying out ball milling for 40 hours at the rotating speed of 400r/min to obtain the chromium carbide powder.
Example 3
A method of preparing chromium carbide powder comprising the steps of:
(1) ball milling for the first time: accurately weighing chromium powder and carbon black according to the mass ratio of 10:1, pouring the chromium powder and the carbon black into a ball milling tank of a common planetary ball mill, wherein the ball-material ratio is 20:1, adding 60% of ethanol of the mass of the powder serving as a ball milling medium into the ball milling tank, forming slurry with certain fluidity by the ball milling medium and the powder, performing ball milling for 6 hours at the rotating speed of 300r/min, and drying at the temperature of 100 ℃;
(2) first carbonization: putting the dried mixed powder into a high-purity graphite burning boat, putting the high-purity graphite burning boat into a high-temperature tube furnace, and preserving heat for 5 hours at 1400 ℃ under the protection of argon atmosphere to obtain a first carbonized product;
(3) ball milling for the second time: filling the first carbonization product into a ball milling tank of a common planetary ball mill, wherein the ball-material ratio is 20:1, adding ethanol with the powder mass of 60% as a ball milling medium, and performing ball milling for 15 hours at the rotating speed of 600r/min to obtain a precursor;
(4) and (3) second carbonization: accurately weighing the precursor and the carbon black according to the mass ratio of 20:1, uniformly mixing, loading into a high-purity graphite burning boat, and placing into a high-temperature tube furnace, and preserving heat for 8 hours at 1200 ℃ under the protection of argon atmosphere to obtain a secondary carbonized product, wherein the product has a weak bonding phenomenon on a microscopic scale;
(5) ball milling for the third time: and (3) putting the secondary carbonized product into a ball milling tank of a common planetary ball mill, wherein the ball-material ratio is 20:1, adding ethanol with the powder mass of 60% as a ball milling medium, and carrying out ball milling for 60 hours at the rotating speed of 600r/min to obtain the chromium carbide powder.
Effects of the embodiment
The precursors prepared in examples 1 to 3 and chromium carbide powder were taken,
(1) the carbon content in the precursor and the chromium carbide powder was measured by an infrared combustion method using a high-frequency infrared carbon-sulfur analyzer, and the results are shown in table 1.
(2) The particle diameter D50 of the chromium carbide powder was measured by a laser light scattering method using a laser particle size distribution meter, and the results are shown in table 1.
TABLE 1
As is clear from Table 1, the chromium carbide powder produced by the present invention had a particle size D50 of not more than 1 μm and was in the ultrafine and submicron range. According to the content of carbon in the precursor and the chromium carbide powder, the precursor is single Cr7C3Phase, and the final chromium carbide powder is single Cr3C2And the purity of the powder is high. In addition, the secondary particle size of the chromium carbide powder prepared by the invention is very uniform.
Claims (10)
1. A method of preparing chromium carbide powder comprising the steps of:
s1, sequentially carrying out first ball milling, first carbonization and second ball milling on the mixed powder of the chromium powder and the carbon black to obtain a precursor; wherein in the mixed powder of the chromium powder and the carbon black, the mass ratio of the chromium powder to the carbon black is (8-12):1, and the temperature of the first carbonization is 1350-;
s2, sequentially carrying out second carbonization and third ball milling on the mixed powder of the precursor and the carbon black to obtain chromium carbide powder; wherein, in the mixed powder of the precursor and the carbon black, the mass ratio of the precursor to the carbon black is (15-25) to 1; the temperature of the second carbonization is 1000-1500 ℃.
2. The method for producing a chromium carbide powder according to claim 1, wherein the particle size of the chromium powder is not more than 100 μm;
and/or the particle size of the carbon black does not exceed 20 μm;
and/or in the mixed powder of the chromium powder and the carbon black, the mass ratio of the chromium powder to the carbon black is 10: 1.
3. The method for preparing chromium carbide powder according to claim 1, wherein the first ball milling, the second ball milling and the third ball milling are performed using a general planetary ball mill;
and/or the ball milling media of the first ball milling, the second ball milling and the third ball milling are ethanol;
and/or the ball-to-material ratio of the first ball milling, the second ball milling and the third ball milling is (5-20): 1;
and/or the rotating speed of the first ball milling is 100-300 r/min; the time of the first ball milling is 2-6 h;
and/or the rotation speed of the second ball milling is 200-600 r/min; the time of the second ball milling is 5-15 h;
and/or the rotating speed of the third ball milling is 200-600 r/min; the time of the third ball milling is 20-60 h;
and/or drying after the first ball milling, the second ball milling or the third ball milling.
4. The method for preparing chromium carbide powder according to claim 3, wherein the ball milling medium is ethanol, the amount of ethanol is 20-60%, and the percentage is that the ethanol accounts for the mass percentage of the powder;
and/or the ball milling medium is ethanol, and the drying temperature is 60-100 ℃.
5. The method for producing a chromium carbide powder according to claim 1, wherein the first carbonization and the second carbonization are performed in a high-temperature tube furnace;
and/or the first carbonization and the second carbonization are carried out under the protection of inert atmosphere.
6. The method of producing a chromium carbide powder according to claim 5, wherein the inert atmosphere is an argon atmosphere.
7. The method for preparing chromium carbide powder according to claim 1, wherein the time for the first carbonization is 1 to 5 hours.
8. The method for producing a chromium carbide powder according to claim 1, wherein the mixed powder of the precursor and the carbon black has a mass ratio of (18 to 22): 1;
and/or the temperature of the second carbonization is 1000-1400 ℃;
and/or the time of the second carbonization is 2-8 h.
9. The method of claim 1, wherein the precursor is single Cr7C3Phase (1);
and/or the carbon content of the precursor is 9-10%;
and/or the chromium carbide powder is single Cr3C2Phase (1);
and/or the carbon content of the chromium carbide powder is 13-14%;
and/or the particle size D50 of the chromium carbide powder is not more than 1 μm.
10. The method for preparing a chromium carbide powder according to claim 1, comprising the steps of:
(1) ball milling for the first time: accurately weighing chromium powder and carbon black according to the mass ratio of 10:1, pouring the chromium powder and the carbon black into a ball milling tank of a common planetary ball mill, wherein the ball-material ratio is (5-20):1, adding ethanol which is 20-60% of the mass of the powder as a ball milling medium, performing ball milling for 2-6h at the rotating speed of 100-300r/min, and then drying at the temperature of 60-100 ℃;
(2) first carbonization: putting the dried mixed powder into a high-purity graphite burning boat, putting the high-purity graphite burning boat into a high-temperature tube furnace, and preserving heat for 1-5 hours at 1400 ℃ under the protection of argon atmosphere;
(3) ball milling for the second time: putting the first carbonization product into a ball milling tank of a common planetary ball mill, wherein the ball-material ratio is 10:1, adding ethanol with the mass of 20-60% of that of the powder as a ball milling medium, and carrying out ball milling for 5-15h under the condition of the rotation speed of 200-;
(4) and (3) second carbonization: accurately weighing the precursor and the carbon black according to the mass ratio of 20:1, uniformly mixing, loading into a high-purity graphite burning boat, and placing into a high-temperature tube furnace, and preserving heat for 2-8h at the temperature of 1000-1500 ℃ under the protection of argon atmosphere;
(5) ball milling for the third time: and (3) putting the secondary carbonized product into a ball milling tank of a common planetary ball mill, wherein the ball-material ratio is 10:1, adding ethanol with the mass of 20-60% of that of the powder as a ball milling medium, and carrying out ball milling for 20-60h under the condition that the rotating speed is 200-.
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