阅读说明：本技术 一种碳化钒和碳化铬复合材料的制备方法 (Preparation method of vanadium carbide and chromium carbide composite material ) 是由 王新东 周冰晶 李兰杰 卢明亮 王浩 祁健 杨丽丽 周涛 于 2021-07-06 设计创作，主要内容包括：本发明涉及冶金技术领域,尤其涉及一种碳化钒和碳化铬复合材料的制备方法,包括如下步骤：步骤一,将含钒铬的物料和碳原料混合均匀后加入粘结剂,混合均匀后制成球团；步骤二,将所述球团干燥后放入真空炉中,以350～450℃/h的升温速度匀速升温至900～1200℃,保温2～4h；步骤三,将所述球团在惰性气体的保护下冷却出炉,破碎即得到碳化钒和碳化铬复合材料。本发明提供的碳化钒和碳化铬复合材料的制备方法操作简单,制备得到的碳化钒和碳化铬复合材料粒度细,粒径均匀,组成单一,杂质含量少,可以满足超细硬质合金、金属陶瓷等领域的需求,对于提高碳化钒和碳化铬复合材料品质具有十分重要的意义。(The invention relates to the technical field of metallurgy, in particular to a preparation method of a vanadium carbide and chromium carbide composite material, which comprises the following steps: step one, uniformly mixing a vanadium-chromium-containing material and a carbon raw material, adding a binder, and uniformly mixing to prepare pellets; drying the pellets, then putting the pellets into a vacuum furnace, uniformly heating the pellets to 900-1200 ℃ at a heating speed of 350-450 ℃/h, and keeping the temperature for 2-4 h; and step three, cooling the pellets under the protection of inert gas, discharging the pellets out of the furnace, and crushing the pellets to obtain the vanadium carbide and chromium carbide composite material. The preparation method of the vanadium carbide and chromium carbide composite material provided by the invention is simple to operate, and the prepared vanadium carbide and chromium carbide composite material is fine in granularity, uniform in particle size, single in composition and low in impurity content, can meet the requirements of the fields of superfine hard alloy, metal ceramic and the like, and has very important significance for improving the quality of the vanadium carbide and chromium carbide composite material.)

1. A preparation method of a vanadium carbide and chromium carbide composite material is characterized by comprising the following steps:

step one, uniformly mixing a vanadium-chromium-containing material and a carbon raw material, adding a binder, and uniformly mixing to prepare pellets;

drying the pellets, then putting the pellets into a vacuum furnace, uniformly heating the pellets to 900-1200 ℃ at a heating speed of 350-450 ℃/h, and keeping the temperature for 2-4 h;

and step three, cooling the pellets under the protection of inert gas, discharging the pellets out of the furnace, and crushing the pellets to obtain the vanadium carbide and chromium carbide composite material.

2. The method of preparing a vanadium carbide and chromium carbide composite material according to claim 1, wherein: in the first step, the vanadium content of the vanadium-chromium-containing material is 1-5% by mass, and the chromium content of the vanadium-chromium-containing material is 10-15% by mass.

3. The method of preparing a vanadium carbide and chromium carbide composite material according to claim 1, wherein: in the first step, the carbon raw material is one or more of semi-coke, graphite, carbon black, activated carbon, coke and organic carbon.

4. The method of preparing a vanadium carbide and chromium carbide composite material according to claim 1, wherein: in the first step, the binder is one of polyacrylamide, polyethylene glycol, polyvinyl alcohol or starch glue.

5. The method of preparing a vanadium carbide and chromium carbide composite material according to claim 1, wherein: in the first step, the weight ratio of the vanadium-chromium-containing material to the carbon raw material to the binder is 1: 0.2-0.4: 0.03 to 0.05.

6. The method of preparing a vanadium carbide and chromium carbide composite material according to claim 1, wherein: in the second step, the drying temperature is 80-150 ℃, and the drying time is 1-2 hours.

7. The method of preparing a vanadium carbide and chromium carbide composite material according to claim 1, wherein: in the third step, the inert gas is argon or helium.

8. The method of preparing a vanadium carbide and chromium carbide composite material according to claim 1, wherein: and in the third step, cooling to 130-150 ℃ and discharging.

Technical Field

The invention relates to the technical field of metallurgy, in particular to a preparation method of a vanadium carbide and chromium carbide composite material.

Background

The vanadium carbide and the chromium carbide have higher melting point, hardness and strength, and good electrical conductivity and thermal conductivity under a high-temperature environment. The vanadium carbide and chromium carbide composite material has important function as a grain inhibitor in the fields of superfine hard alloy and metal ceramic.

What is needed in industrial applications is a vanadium carbide and chromium carbide composite material with a single fine grain size and phase composition, such as in the preparation of ultra-fine cemented carbides, that can better inhibit the grain growth of tungsten carbide if a vanadium carbide and chromium carbide composite material with a single fine grain size and phase composition is used as a grain growth inhibitor. If the composite material of vanadium carbide and chromium carbide with coarse particles is used as the grain growth inhibitor, the grain growth of tungsten carbide is difficult to inhibit due to the small specific surface, low surface activation energy and low atom transfer speed of the composite material of vanadium carbide and chromium carbide with coarse particles, so that the performance of the superfine hard alloy is difficult to further improve. Therefore, vanadium carbide and chromium carbide composite materials with fine particle size and single phase composition are urgently needed in the fields of high-performance superfine hard alloys and the like.

Disclosure of Invention

Based on the problems in the prior art, the invention provides a preparation method of a vanadium carbide and chromium carbide composite material, the vanadium carbide and chromium carbide composite material prepared by the preparation method has the advantages of fine particle size, uniform particle size, single phase composition and low impurity content, can meet the requirements of the fields of superfine hard alloy, metal ceramic and the like, and overcomes the defects in the prior art.

In order to achieve the purpose, the invention adopts the following technical scheme:

the embodiment of the invention provides a preparation method of a vanadium carbide and chromium carbide composite material, which comprises the following steps: step one, uniformly mixing a vanadium-chromium-containing material and a carbon raw material, adding a binder, and uniformly mixing to prepare pellets;

drying the pellets, then putting the pellets into a vacuum furnace, uniformly heating the pellets to 900-1200 ℃ at a heating speed of 350-450 ℃/h, and keeping the temperature for 2-4 h;

and step three, cooling the pellets under the protection of inert gas, discharging the pellets out of the furnace, and crushing the pellets to obtain the vanadium carbide and chromium carbide composite material.

According to the preparation method of the vanadium carbide and chromium carbide composite material, the vanadium and chromium containing material and the carbon raw material are uniformly mixed and then added with the binder to prepare the pellet, so that the vanadium and chromium containing material and the carbon raw material can be fully mixed and tightly contacted, and the phenomenon of unstable product quality caused by incomplete reaction is reduced. The preparation method of the vanadium carbide and chromium carbide composite material provided by the invention is favorable for controlling the reaction temperature by controlling the temperature rise speed, and can avoid the phenomena of incomplete carbonization or over-carbonization of vanadium-chromium-containing materials due to large temperature fluctuation in the process of preparing the vanadium carbide and chromium carbide composite material, thereby reducing the generation of impurities and greatly improving the quality of the vanadium carbide and chromium carbide composite material. In addition, the combination of the first step, the second step and the third step in the preparation method of the vanadium carbide and chromium carbide composite material provided by the invention can ensure that the prepared vanadium carbide and chromium carbide composite material has fine granularity, uniform grain size and single phase composition, and can meet the requirements of the fields of superfine hard alloy, metal ceramic and the like.

The material containing vanadium and chromium can adopt vanadium and chromium-containing waste recovered from vanadium precipitation wastewater vanadium and chromium, so that the cost can be reduced, and the resource utilization of the vanadium and chromium-containing waste can be realized.

Preferably, in the step one, the mass percent of vanadium in the vanadium-chromium-containing material is 1-5%, and the mass percent of chromium is 10-15%.

Preferably, in the step one, the carbon raw material is one or more of semi coke, graphite, carbon black, activated carbon, coke and organic carbon.

Preferably, in the first step, the binder is one of polyacrylamide, polyethylene glycol, polyvinyl alcohol or starch glue.

Preferably, in the first step, the weight ratio of the vanadium-chromium-containing material to the carbon raw material to the binder is 1: 0.2-0.4: 0.03 to 0.05.

Preferably, in the second step, the drying temperature is 80-150 ℃, and the drying time is 1-2 hours.

Preferably, in step three, the inert gas is argon or helium.

Preferably, in the third step, the mixture is cooled to 130-150 ℃ and discharged.

The preparation method of the vanadium carbide and chromium carbide composite material provided by the invention is simple to operate, and the prepared vanadium carbide and chromium carbide composite material is fine in granularity, uniform in particle size, single in composition and low in impurity content, can meet the requirements of the fields of superfine hard alloy, metal ceramic and the like, and has very important significance for improving the quality of the vanadium carbide and chromium carbide composite material. The method can select the vanadium-chromium-containing waste recovered from vanadium-precipitation wastewater vanadium and chromium as the raw material, not only can reduce the cost, but also can realize the resource utilization of the vanadium-chromium-containing waste.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

Example 1

The embodiment provides a preparation method of a vanadium carbide and chromium carbide composite material, which comprises the following steps:

(1) 100g of vanadium-chromium-containing waste (the content of vanadium is 5 percent, and the content of chromium is 10 percent) and 20g of semi-coke are mixed uniformly, 3g of polyacrylamide is added, and the mixture is put into a mixer, added with a certain amount of water and mixed uniformly to prepare pellets.

(2) Drying the pellets, then putting the pellets into a vacuum furnace, drying at 80 ℃ for 2h, uniformly heating from 200 ℃ to 900 ℃, heating at a speed of 400 ℃/h, and keeping the temperature for 2 h.

(3) And cooling the pellets to 150 ℃ under the protection of helium, discharging the pellets out of the furnace, and crushing the pellets to obtain the vanadium carbide and chromium carbide composite material. The particle size of the obtained vanadium carbide and chromium carbide composite material is 200-500 nm, and through detection, the content of chromium in the product is 82.64%, the content of vanadium is 5.67%, and the content of carbon is 11.59%.

Example 2

The embodiment provides a preparation method of a vanadium carbide and chromium carbide composite material, which comprises the following steps:

(1) 100g of vanadium-chromium-containing waste (the vanadium content is 4 percent, and the chromium content is 11 percent) and 30g of semi-coke are mixed uniformly, 5g of polyacrylamide is added, and the mixture is put into a mixer, added with a certain amount of water and mixed uniformly to prepare pellets.

(2) Drying the pellets, then putting the pellets into a vacuum furnace, drying at 90 ℃ for 1h, uniformly heating the pellets from 150 ℃ to 950 ℃, heating at the speed of 350 ℃/h, and keeping the temperature for 3 h.

(3) And cooling the pellets to 140 ℃ under the protection of helium, discharging the pellets out of the furnace, and crushing the pellets to obtain the vanadium carbide and chromium carbide composite material. The particle size of the obtained vanadium carbide and chromium carbide composite material is 200-500 nm, and through detection, the chromium content in the product is 83.12%, the vanadium content is 4.82%, and the carbon content is 11.93%.

Example 3

The embodiment provides a preparation method of a vanadium carbide and chromium carbide composite material, which comprises the following steps:

(1) 100g of vanadium-chromium-containing waste (the content of vanadium is 3 percent, and the content of chromium is 12 percent) and 40g of semi-coke are mixed uniformly, then 3g of polyacrylamide is added, and the mixture is put into a mixer, added with a certain amount of water and mixed uniformly to prepare pellets.

(2) Drying the pellets, then putting the pellets into a vacuum furnace, drying at 100 ℃ for 1h, uniformly heating from 250 ℃ to 1200 ℃, heating at a speed of 450 ℃/h, and keeping the temperature for 4 h.

(3) And cooling the pellets to 130 ℃ under the protection of helium, discharging the pellets out of the furnace, and crushing the pellets to obtain the vanadium carbide and chromium carbide composite material. The particle size of the obtained vanadium carbide and chromium carbide composite material is 200-500 nm, and through detection, the chromium content in the product is 84.06%, the vanadium content is 3.99%, and the carbon content is 11.83%.

Example 4

The embodiment provides a preparation method of a vanadium carbide and chromium carbide composite material, which comprises the following steps:

(1) 100g of vanadium-chromium-containing waste (the vanadium content is 2 percent, and the chromium content is 13 percent) and 25g of semi-coke are uniformly mixed, 4g of polyacrylamide is added, and the mixture is put into a mixer, added with a certain amount of water and uniformly mixed to prepare pellets.

(2) Drying the pellets, then putting the pellets into a vacuum furnace, drying at 130 ℃ for 2h, uniformly heating from 180 ℃ to 1000 ℃, heating at a speed of 380 ℃/h, and keeping the temperature for 3 h.

(3) And cooling the pellets to 140 ℃ under the protection of helium, discharging the pellets out of the furnace, and crushing the pellets to obtain the vanadium carbide and chromium carbide composite material. The particle size of the obtained vanadium carbide and chromium carbide composite material is 200-500 nm, and through detection, the content of chromium in the product is 84.36%, the content of vanadium is 3.04%, and the content of carbon is 12.45%.

Example 5

The embodiment provides a preparation method of a vanadium carbide and chromium carbide composite material, which comprises the following steps:

(1) 100g of vanadium-chromium-containing waste (the vanadium content is 1 percent, and the chromium content is 15 percent) and 35g of semi-coke are uniformly mixed, 5g of polyacrylamide is added, and the mixture is put into a mixer, added with a certain amount of water and uniformly mixed to prepare pellets.

(2) Drying the pellets, then putting the pellets into a vacuum furnace, drying at 150 ℃ for 1h, uniformly heating from 230 ℃ to 1100 ℃, heating at a speed of 420 ℃/h, and keeping the temperature for 4 h.

(3) And cooling the pellets to 150 ℃ under the protection of helium, discharging the pellets out of the furnace, and crushing the pellets to obtain the vanadium carbide and chromium carbide composite material. The particle size of the obtained vanadium carbide and chromium carbide composite material is 200-500 nm, and through detection, the content of chromium in the product is 84.75%, the content of vanadium is 2.58%, and the content of carbon is 12.51%.

The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.