CN111872414B - Preparation method of micro-nano pre-alloyed powder - Google Patents
Preparation method of micro-nano pre-alloyed powder Download PDFInfo
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- CN111872414B CN111872414B CN202010534937.2A CN202010534937A CN111872414B CN 111872414 B CN111872414 B CN 111872414B CN 202010534937 A CN202010534937 A CN 202010534937A CN 111872414 B CN111872414 B CN 111872414B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F9/26—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions using gaseous reductors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0235—Starting from compounds, e.g. oxides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
- C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
Abstract
A preparation method of micro-nano pre-alloyed powder comprises the following steps: taking iron oxalate, cobalt carbonate and copper carbonate as raw materials, and carrying out thermal decomposition in a nitrogen atmosphere; uniformly mixing the powder obtained after pyrolysis with tungsten oxide and graphite, and then filling the mixture into a high-energy ball milling tank to prepare a precursor material through ball milling; sending the precursor material into a reduction furnace, introducing hydrogen, heating and reducing; introducing nitrogen after reduction, cooling to 55-60 ℃, adding paraffin under the protection of nitrogen flow, stirring uniformly, and cooling to room temperature; crushing and screening to obtain the micro-nano Fe-Co-Cu-Wu pre-alloy powder. Compared with the prior art, the invention has the beneficial effects that: the method has the advantages of simple production process, short flow, reduced energy consumption and pollution, and low oxygen content of the alloy powder.
Description
Technical Field
The invention relates to the field of powder metallurgy, in particular to a preparation method of micro-nano pre-alloyed powder.
Background
In order to achieve the use performance of the traditional diamond tool, a certain amount of Co powder needs to be added, but the development of the diamond tool industry is limited due to the high price of pure Co powder. The concept of pre-alloy powder is first proposed by Umicore company in the field of diamond tools in Belgium in the 20 th century, and the pre-alloy powder can be widely applied to diamond tools and powder metallurgy industries at low cost by virtue of uniform chemical components of the pre-alloy powder.
The production method of the pre-alloyed powder mainly comprises a hydrometallurgy method, an atomization method and a mechanical alloying method. Xie Zhigang [1]And injecting the metal chloride salt solution and the oxalic acid solution into the reaction kettle at the same speed under a certain temperature condition, fully stirring, adding an ammonia water solution to adjust the pH value, standing and precipitating for a period of time after complete reaction, and thus obtaining the Fe, co and Cu composite oxalate precipitate. Filtering and separating the composite oxalate precipitate, washing with deionized water, removing water in a drying box, calcining in a pusher calcining furnace, and fully decomposingThe composite oxide powder of Fe, co and Cu can be obtained. The Fe, co and Cu composite oxide powder is put into a push rod reducing furnace and reduced by ammonia decomposition gas to obtain Fe 73 Co 25 Cu 2 Prealloyed powder. The pre-alloyed powder for diamond products prepared by the coprecipitation method has high purity, uniform particles and stable performance, but the powder preparation production period is long, a large amount of waste liquid is generated in the production process, the waste liquid treatment is needed, and a large amount of energy is consumed in the whole production process. Huang Shengkun et al [3-5 ]]The research on the preparation of the pre-alloyed powder by the water atomization method is carried out. The production of pre-alloyed powder by water atomization method is that pure metal is melted by induction furnace according to a certain proportion, the molten metal is broken into fine metal drops by using high-pressure water as medium, and then the fine metal drops are cooled to form powder particles. The pre-alloyed powder prepared by the water atomization method has high alloying degree, good sphericity and good fluidity, but has complex production process, large particles and easy oxidation of powder in the production process, often needs secondary reduction, and increases the production cost. In addition to the above two methods, mechanical alloying is also an important method for producing pre-alloyed powder, wu Zhiying et al, which are obtained by crushing deeply frozen alloy powder in a jaw crusher, zhou Jiang et al [6-7 ] 3242]The related research is carried out on the prealloying powder prepared by the mechanical alloying method. The method is suitable for producing brittle alloys or alloys with brittleness after special treatment, and has certain limitations. The mechanical alloying method has simple production process, the produced pre-alloyed powder has low sintering temperature but low production efficiency, and impurities are easily introduced in the production process, thus having great influence on the powder performance.
Disclosure of Invention
The invention aims to provide a preparation method of micro-nano pre-alloyed powder, which has the advantages of simple production process, short flow, reduced energy consumption, reduced pollution and low oxygen content of the alloyed powder.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of micro-nano pre-alloyed powder comprises the following steps:
1) Mixing iron oxalate, cobalt carbonate and copper carbonate serving as raw materials by using a mixer, putting the mixed powder into a tubular furnace, introducing nitrogen, and heating for thermal decomposition;
2) Uniformly mixing and stirring the powder obtained after pyrolysis in the step 1) with tungsten oxide and graphite in a mixer, and then filling the uniformly mixed and stirred mixture into a high-energy ball-milling tank to prepare a precursor material through ball milling;
3) Flatly paving the precursor material obtained in the step 2) into a burning boat, placing the burning boat in a heating zone in a tubular reduction furnace, firstly introducing nitrogen to exhaust air in the furnace, and then introducing hydrogen to heat and reduce;
4) After the reduction is finished, introducing nitrogen to exhaust hydrogen in the furnace, cooling to 55-60 ℃ under the condition of nitrogen, loading the powder obtained by reduction into a mixer under the protection of nitrogen airflow, adding micron-sized paraffin powder, stirring for more than 30 minutes at the temperature of 50-55 ℃, uniformly stirring, and cooling to room temperature;
5) Crushing and screening the material obtained in the step 4) to obtain micro-nano Fe-Co-Cu-Wu pre-alloy powder.
The micro-nano pre-alloyed powder is prepared from the following raw materials in parts by weight: 30-40 parts of ferric oxalate, 20-30 parts of cobalt carbonate, 4-7 parts of copper carbonate, 3-7 parts of tungsten oxide and 2-5 parts of graphite.
The thermal decomposition temperature in the step 1) is 400-420 ℃.
The ball milling time in the step 2) is 2-5h.
The reduction temperature in the step 3) is 600-800 ℃, the hydrogen flow is 1-5L/min, and the heat preservation time is 60-120 minutes.
The volume ratio of the addition amount of the paraffin to the powder material in the step 4) is 3-5:18-24.
The micro-nano pre-alloyed powder has the particle size distribution of 0.1-20 mu m and the oxygen content of less than 0.8%.
Compared with the prior art, the invention has the beneficial effects that:
1) The invention has simple production process, short flow and low reduction temperature, can effectively reduce energy consumption and pollution and is suitable for large-scale production.
2) The precursor material prepared by ball milling has the advantages that the alloy powder prepared by reduction has uniform particle size distribution, small particle size and large specific surface area, and the sintering temperature can be effectively reduced; the powder has irregular shape, good formability and easy production and processing.
3) According to the invention, a certain proportion of graphite is added in the reduction process of the metal oxide, so that the reduction speed of the metal oxide can be accelerated during high-temperature reduction, the metal oxide is reduced more thoroughly, the oxygen content of the alloy powder is reduced, and meanwhile, a small amount of residual graphite powder which does not participate in the reaction can also play a role of a low-melting-point binding phase in the alloy powder, so that the wear resistance of the alloy is improved. Meanwhile, micro-nano metal tungsten is added in a mode of ball milling and reduction on tungsten oxide, so that the hardness of the pre-alloy powder is effectively improved.
4) The reduced alloy powder is uniformly mixed with paraffin under the protection of nitrogen, and then is crushed and sieved, so that a layer of paraffin is covered on the surface of the powder, and the powder is prevented from being oxidized again in the processes of storage, transportation or reprocessing. The process of the invention ensures that the powder prepared after reduction does not need passivation, is easy to store and effectively reduces the oxygen content of the powder.
5) The micro-nano pre-alloyed powder has the particle size distribution of 0.1-20 mu m and the oxygen content of less than 0.8 percent.
Drawings
FIG. 1 is an SEM photograph of example 1;
FIG. 2 is an SEM photograph of example 2.
Detailed Description
The present invention will be described in detail below, but the scope of the present invention is not limited to the following embodiments.
A preparation method of micro-nano pre-alloyed powder comprises the following steps:
1) Mixing iron oxalate, cobalt carbonate and copper carbonate serving as raw materials by using a mixer, putting the mixed powder into a tubular furnace, introducing nitrogen, and heating for thermal decomposition; the metallic oxides of iron, cobalt and copper are obtained after thermal decomposition, and the metallic oxides of iron, cobalt and copper obtained by the method have low impurity content and high purity.
2) Uniformly mixing and stirring the powder obtained after pyrolysis in the step 1) with tungsten oxide and graphite in a mixer, and then filling the uniformly mixed and stirred mixture into a high-energy ball-milling tank to prepare a precursor material through ball milling;
3) Flatly paving the precursor material obtained in the step 2) into a burning boat, placing the burning boat in a heating zone in a tubular reduction furnace, firstly introducing nitrogen to exhaust air in the furnace, and then introducing hydrogen to heat and reduce;
4) After the reduction is finished, introducing nitrogen to exhaust hydrogen in the furnace, cooling to 55-60 ℃ under the condition of nitrogen, loading the powder obtained by reduction into a mixer under the protection of nitrogen airflow, adding micron-sized paraffin powder, stirring for more than 30 minutes at the temperature of 50-55 ℃, uniformly stirring, and cooling to room temperature;
5) Crushing and screening the material obtained in the step 4) to obtain micro-nano Fe-Co-Cu-Wu pre-alloy powder.
The micro-nano pre-alloyed powder is prepared from the following raw materials in parts by weight: 30-40 parts of ferric oxalate, 20-30 parts of cobalt carbonate, 4-7 parts of copper carbonate, 3-7 parts of tungsten oxide and 2-5 parts of graphite.
The thermal decomposition temperature in the step 1) is 400-420 ℃.
The ball milling time in the step 2) is 2-5h.
The reduction temperature in the step 3) is 600-800 ℃, the hydrogen flow is 1-5L/min, and the heat preservation time is 60-120 minutes.
The volume ratio of the addition amount of the paraffin to the powder material in the step 4) is 3-5:18-24.
Example 1:
1) 332g of iron oxalate, 248g of cobalt oxalate and 46g of copper oxalate were weighed in this order and mixed for 30min using a mixer. And (3) placing the mixed powder into a tubular furnace, introducing nitrogen gas for thermal decomposition, and setting the decomposition temperature to be 400 ℃ and the time to be 60min.
2) Uniformly mixing the powder obtained after pyrolysis in the step 1), 40g of tungsten oxide and 30g of graphite in a mixer, adding the uniformly mixed material and 3000g of grinding balls into a ball milling tank, and setting the ball milling time to be 2h to obtain precursor powder. The high-energy ball milling can effectively reduce the granularity of initial powder and can greatly reduce the reduction temperature of precursor powder.
3) And putting the precursor powder into a burning boat, pushing the burning boat into a heating zone of a reduction furnace, setting the reduction temperature to be 600 ℃, setting the hydrogen flow to be 1.5L/min, stopping heating when the reduction temperature reaches a preset temperature, and keeping the temperature for 60 minutes.
4) And after the heat preservation is finished, furnace cooling is carried out to 55-60 ℃ in the nitrogen atmosphere, the powder obtained by reduction is loaded into a mixer under the protection of nitrogen airflow, micron-sized paraffin powder is added, stirring is carried out for more than 30 minutes at the temperature of 50-55 ℃, and cooling is carried out to the room temperature after uniform stirring. The volume ratio of the addition amount of the paraffin to the powder material is 3-5:18-24.
5) Crushing and screening the material obtained in the step 4), and detecting the material, wherein the pre-alloyed powder has uniform particles and good dispersibility as shown in a pre-alloyed powder SEM picture 1; measuring the particle size distribution of the powder by a laser particle size analyzer to be 0.1-1 mu m; the oxygen content was 0.59% by weight.
Example 2:
1) 300g of iron oxalate, 240g of cobalt oxalate and 45g of copper oxalate were weighed in this order and mixed for 30min using a mixer. And (3) placing the mixed powder into a tubular furnace, introducing nitrogen gas for thermal decomposition, and setting the decomposition temperature to be 400 ℃ and the time to be 90min.
2) And (2) uniformly mixing the powder obtained after pyrolysis in the step 1), 50g of tungsten oxide and 40g of graphite in a mixer, adding the uniformly mixed material, 2800g of grinding balls and 100ml of alcohol into a ball milling tank, and performing ball milling for 3 hours to obtain precursor powder after drying. The added alcohol is used as a ball milling medium to prevent the powder from being bonded on a ball milling tank in the ball milling process, so that the components and the granularity of the precursor powder are not uniform.
3) And putting the precursor powder into a burning boat, pushing the burning boat into a heating zone of a reduction furnace, setting the reduction temperature to be 800 ℃, setting the hydrogen flow to be 1L/min, stopping heating when the reduction temperature reaches a preset temperature, and keeping the temperature for 90 minutes.
4) And after heat preservation is finished, furnace cooling is carried out to 55-60 ℃ in a nitrogen atmosphere, the powder obtained by reduction is loaded into a mixer under the protection of nitrogen airflow, micron-sized paraffin powder is added, stirring is carried out for more than 30 minutes at the temperature of 50-55 ℃, and the mixture is cooled to room temperature after being uniformly stirred. The volume ratio of the addition amount of the paraffin to the powder material is 3-5:18-24.
5) Crushing and screening the material obtained in the step 4), detecting the material, and measuring the particle size distribution of the material in 10-20 microns by using a laser particle size analyzer according to the SEM (scanning electron microscope) diagram of the pre-alloyed powder shown in FIG. 2; the oxygen content was 0.37wt%.
Claims (6)
1. A preparation method of micro-nano pre-alloy powder is characterized by comprising the following steps:
1) Mixing iron oxalate, cobalt carbonate and copper carbonate serving as raw materials by using a mixer, putting the mixed powder into a tubular furnace, introducing nitrogen, and heating for thermal decomposition;
2) Uniformly mixing and stirring the powder obtained after pyrolysis in the step 1) with tungsten oxide and graphite in a mixer, and then filling the uniformly mixed and stirred mixture into a high-energy ball-milling tank to prepare a precursor material through ball milling;
3) Flatly paving the precursor material obtained in the step 2) into a burning boat, placing the burning boat in a heating zone in a tubular reduction furnace, firstly introducing nitrogen to exhaust air in the furnace, and then introducing hydrogen to heat and reduce;
4) After the reduction is finished, introducing nitrogen to exhaust hydrogen in the furnace, cooling to 55-60 ℃ under the condition of nitrogen, loading the powder obtained by reduction into a mixer under the protection of nitrogen airflow, adding micron-sized paraffin powder, stirring for more than 30 minutes at the temperature of 50-55 ℃, uniformly stirring, and cooling to room temperature;
5) Crushing and screening the material obtained in the step 4) to obtain micro-nano Fe-Co-Cu-W pre-alloy powder;
the volume ratio of the addition amount of the paraffin to the powder material in the step 4) is 3-5:18-24.
2. The preparation method of the micro-nano pre-alloyed powder according to claim 1, wherein the micro-nano pre-alloyed powder is prepared from the following raw materials in parts by weight: 30-40 parts of ferric oxalate, 20-30 parts of cobalt carbonate, 4-7 parts of copper carbonate, 3-7 parts of tungsten oxide and 2-5 parts of graphite.
3. The method for preparing micro-nano pre-alloyed powder according to claim 1, wherein the thermal decomposition temperature in the step 1) is 400-420 ℃.
4. The preparation method of the micro-nano pre-alloyed powder according to claim 1, wherein the ball milling time in the step 2) is 2-5h.
5. The preparation method of the micro-nano pre-alloy powder according to claim 1, wherein the reduction temperature in the step 3) is 600-800 ℃, the hydrogen flow is 1-5L/min, and the heat preservation time is 60-120 minutes.
6. The method for preparing micro-nano pre-alloyed powder according to claim 1, wherein the micro-nano pre-alloyed powder has a particle size distribution of 0.1-20 μm and an oxygen content of less than 0.8%.
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