CN110369730B - Copper-coated iron powder and preparation method thereof - Google Patents
Copper-coated iron powder and preparation method thereof Download PDFInfo
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- CN110369730B CN110369730B CN201910757218.4A CN201910757218A CN110369730B CN 110369730 B CN110369730 B CN 110369730B CN 201910757218 A CN201910757218 A CN 201910757218A CN 110369730 B CN110369730 B CN 110369730B
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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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
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
Abstract
The invention provides copper-coated iron powder and a preparation method thereof. The preparation method comprises the following steps: uniformly mixing copper oxide powder and iron powder to obtain mixed powder; heating the mixed powder to T in a protective atmosphere consisting of a reducing gas1And maintaining the temperature, and then heating to T2Keeping the temperature, and continuously heating to T3Preserving heat, cooling to below 40 ℃ to obtain a cooled product, wherein T is more than or equal to 2501<600℃,600≤T2<690℃,690≤T3< 820 ℃; and crushing and screening the cooled product to obtain the copper-clad iron powder. The copper-clad iron powder comprises a product prepared by the method. The beneficial effects of the invention include: the preparation method is simple and convenient, and the process has no pollution emission; the copper-clad iron powder has excellent performance indexes, reasonable and easily-controlled particle size distribution, good powder fluidity, strong oxidation resistance and small shrinkage coefficient of sintered products.
Description
Technical Field
The invention relates to the field of preparation of composite metal powder, in particular to composite powder of metal copper coated iron and a preparation method thereof.
Background
The metal powder is the main raw material for manufacturing powder metallurgy mechanical parts and oil-retaining bearings, and the prior art is developed from single-value pure metal powder to coating powder and alloy powder. Copper alloy powder is generally adopted as a raw material for manufacturing small and micro oil-retaining bearings at home and abroad, and oil-retaining bearing manufacturing enterprises have widely started to produce the oil-retaining bearings by using metal copper-coated iron composite powder as a main raw material to replace the copper alloy powder due to the requirements on the performance of the oil-retaining bearings and the reduction of the production cost.
The patent CN1241250A of japan kokukukukukukukuai corporation discloses a composite metal powder for sintered bearings and a method for producing oil-containing sintered bearings. The oil-retaining bearing is prepared by using composite iron powder coated with pure copper accounting for 10-30% of the total weight of the powder, adding 0.1-2% of low-melting-point metal powder such as tin or lead into the pure copper-coated iron powder before forming, uniformly mixing, forming, pressing and sintering to obtain the oil-retaining bearing.
The Japanese patent publication No. 55-38019 proposes to produce an oil-impregnated bearing from 30-60% pure copper-clad iron powder. The patent uses pure copper-clad iron powder to mix and add low-melting-point metal, and presses and sinters to prepare the oil-retaining bearing, and has the disadvantages that when the low-melting-point metal powder is mixed with the copper-clad iron powder, because the respective density difference is large, segregation is easy to occur during mixing, and the mechanical property of an oil-retaining bearing product is influenced, and when the low-melting-point metal is sintered, a liquid phase appears, so that the shrinkage rate and deformation of the oil-retaining bearing product are increased, and the dimensional accuracy of a high-precision fine bearing is difficult to control.
The CN1548261A patent proposes a method for manufacturing a copper-coated iron powder composite powder. The method comprises the steps of rapidly adding iron powder into a copper sulfate solution which is doped with a stabilizer and has a pH value of 0.5-4.8 under a stirring state, continuously stirring for 2-10 minutes, settling for 3-20 minutes, removing supernatant, adding water, cleaning, drying, performing anti-oxidation treatment, and packaging to obtain the product.
The CN200610065023.6 patent proposes a method for producing copper-coated iron powder. Adding iron powder into 10-20 g/L acid copper solution under a stirring state, carrying out displacement reaction at the temperature of 30-50 ℃, depositing copper on the surface of the iron powder, and forming a layer of copper film to coat the surface of the iron powder to obtain the product.
The CN100595006C patent proposes that an acid is added into an alkaline etching solution of copper to adjust the pH value to 2-4.5, the concentration of copper ions is 10-20 g/L, iron powder is added into the solution to carry out a displacement reaction under the stirring state, and copper is deposited on the surface of the iron powder to obtain copper-coated iron powder.
The patent CN101254542A proposes a method for producing brass-coated iron powder. And (2) performing a displacement reaction on the iron powder in a copper salt solution and a zinc salt solution by adopting a liquid phase deposition method, depositing copper and zinc on the surface of the iron powder to form a copper-zinc coating layer, and performing reduction roasting to obtain the brass-coated iron composite powder.
The defects of the patents are that the copper-coated iron composite powder is prepared by a chemical displacement method, namely, iron powder is added into a copper sulfate solution or other copper salt solutions, and the copper-coated iron composite powder is obtained by a displacement reaction method. The method for obtaining the copper-clad iron composite powder by the replacement reaction has the following defects: (1) the iron powder is added into the copper sulfate solution, and the copper sulfate solution quickly dissolves and consumes fine-grained iron powder in the iron powder during the replacement reaction, so that the distribution of the coated composite powder particles is poor, and the formability of the pressed micro-bearing product is influenced. And (2) the copper layer deposited on the surface of the iron powder through the displacement reaction is sparse and is easy to oxidize, and the size sintering shrinkage of the molded product is large. (3) When one ton of products is generated in the displacement reaction, dozens of tons of industrial wastewater are discharged, and the environment is polluted. (4) Acid radicals are remained in the product, so that the service performance of the product is reduced.
Disclosure of Invention
In view of the deficiencies in the prior art, it is an object of the present invention to address one or more of the problems in the prior art as set forth above. For example, an object of the present invention is to provide a copper-coated iron powder and a method for preparing the same, which can solve the problem of environmental pollution in the prior art and improve the product quality of the copper-coated iron composite powder.
In order to achieve the above object, the present invention provides a preparation method of copper-clad iron powder.
The preparation method of the copper-clad iron powder comprises the following steps: uniformly mixing copper oxide powder and iron powder to obtain mixed powder, placing the mixed powder in a protective atmosphere consisting of reducing gas, and carrying out reduction coating treatment to obtain copper-coated iron powder, wherein the mass ratio of Cu element to Fe element in the mixed powder is 7.5-20.7: 79 to 92 parts; the step of reduction coating treatment comprises: heating the mixed powder to T1Preserving heat for 5-40 min, and then heating to T2Keeping the temperature for 20-50 min, and continuously heating to T3Keeping the temperature for 15-30 min, and finally cooling, wherein T is more than or equal to 2501<600℃,600≤T2<690℃,690≤T3<820℃。
According to one or more exemplary embodiments of the present invention, the mass fraction of CuO in the copper-oxide powder may be above 98%, and the particle size of the copper-oxide powder may be below 74 μm.
According to one or more exemplary embodiments of the present invention, the mass fraction of the Fe element in the iron powder may be above 98%, and the particle size of the iron powder may be below 200 μm.
According to one or more exemplary embodiments of the present invention, the reducing gas may include decomposed ammonia, hydrogen, carbon monoxide, or coal gas.
According to one or more exemplary embodiments of the present invention, the reducing gas may include decomposing at least one of ammonia, hydrogen, carbon monoxide, and coal gas.
According to one or more exemplary embodiments of the present invention, the dew point of the reducing gas may be lower than-60 ℃.
According to one or more exemplary embodiments of the present invention, the pressure of the protective atmosphere may be 20 to 100Pa, for example, 50 ± 10Pa, higher than the external pressure.
According to one or more exemplary embodiments of the present invention, the reduction coating process may be performed in a continuous reduction apparatus, and the movement direction of the mixed powder in the reduction apparatus may be opposite to the flow direction of the reducing gas.
According to one or more exemplary embodiments of the present invention, the cooling may include: cooling to below 40 ℃ at a cooling rate of 8-24 ℃/min. For example, the step of cooling comprises: cooling to room temperature at a cooling rate of 15 + -5 deg.C/min.
According to one or more exemplary embodiments of the present invention, the preparation method may further include the steps of: and crushing and screening the copper-clad iron powder obtained after the reduction coating treatment.
According to another aspect of the present invention, there is provided a copper-clad iron powder, which may include a product prepared by the above method, wherein the particle size of the copper-clad iron powder may be below 200 μm, for example, 120 μm.
Compared with the prior art, the beneficial effects of the invention can include: the preparation process has no pollution discharge, the prepared copper-clad iron powder has excellent performance indexes, reasonable and easily-controlled particle size distribution, good powder flowability, strong oxidation resistance and small shrinkage coefficient of sintered products.
Drawings
The above and other objects and features of the present invention will become more apparent from the following description taken in conjunction with the accompanying drawings, in which:
FIG. 1 shows a schematic diagram comparing the preparation method of copper-clad iron powder of the invention with the prior reduction method;
fig. 2 shows a metallographic picture of copper-clad iron powder according to the invention.
Detailed Description
Hereinafter, the copper-clad iron powder (also referred to as copper-clad iron composite powder) and the preparation method thereof according to the present invention will be described in detail with reference to the accompanying drawings and exemplary embodiments.
The invention provides a preparation method of copper-clad iron powder.
FIG. 1 is a schematic diagram showing a comparison between the preparation method of copper-clad iron powder of the present invention and the prior reduction method, wherein (a) is a schematic diagram showing the preparation of copper-clad iron powder by the conventional reduction method, and the product prepared by the method has the problem that the copper powder can not completely coat the iron particles; (b) the figure shows a schematic diagram of the reduction method for preparing copper-clad iron powder, the metal copper of the invention can be completely coated on the surface of iron powder particles, and the coating layer formed by the metal copper is uniform and compact.
According to an exemplary embodiment of the present invention, the preparation method of the copper-clad iron powder may include the steps of:
and uniformly mixing the copper oxide powder and the iron powder to obtain mixed powder. Wherein the mass ratio of the Cu element to the Fe element in the mixed powder can be 7.5-20.7: 79 to 92, for example 8 to 18: 79-92, 10: 89. 18: 80, etc. The copper oxide powder may have a mass fraction of CuO of 98% or more, for example 99%, and a particle size of 74 μm or less, for example 60 ± 10 μm. The mass fraction of the Fe element in the iron powder may be 98% or more, for example, 98.5%, and the particle size of the iron powder may be 200 μm or less, further, 149 μm or less, for example, 100 ± 10 μm. Wherein, the mixed powder selects Cu: fe is 7.5-20.7: 79-92 aims to enable the prepared oil-retaining bearing product to obtain the best wear resistance and noise reduction performance.
Heating the mixed powder to T in a protective atmosphere consisting of a reducing gas1And preserving the heat for 5-40 min, for example, preserving the heat for 25 +/-10 ℃; then the temperature is raised to T2And preserving the heat for 20-50 min, for example, preserving the heat for 35 +/-10 ℃; continue to useHeating to T3And preserving the heat for 15-30 min, for example, preserving the heat for 25 +/-5 ℃; finally cooling to below 40 ℃. Wherein T is more than or equal to 2501< 600 ℃, e.g., 400 ± 100 ℃; t is more than or equal to 6002< 690 ℃, e.g. 650. + -.30 ℃; 690 is less than or equal to T3< 820 deg.C, for example 750. + -. 50 deg.C. Wherein heating to T1The temperature rise rate can be 16-38 ℃/min, and the temperature is heated to T2The temperature rise rate can be 6-22 ℃/min, and the temperature is heated to T3The temperature rise rate can be 8-15 ℃/min. The cooling rate can be 8-24 ℃/min, and the cooling mode can comprise inert gas cooling and furnace tube outer wall water cooling.
The temperature rise process is divided into the three temperature sections to control the reaction speed of the reducing atmosphere and the copper oxide, so that the copper atoms generated after reduction are microscopically migrated, the copper atoms are firstly uniformly adsorbed and covered on the surface of the iron powder particles, and then the copper atoms are metallurgically bonded with the iron atoms on the surface of the iron powder particles to form a surface full-coating effect (as shown in a (b) diagram in fig. 1), thereby achieving the technical purpose of the invention. The copper powder particles formed substantially in situ after the reduction of the copper oxide particles in the prior art adhere to the surface of the iron powder particles, and as shown in fig. 1 (a), complete coverage of the surface of the iron powder particles cannot be achieved.
In this embodiment, the reducing gas comprises decomposing one or more of ammonia, hydrogen, carbon monoxide and coal gas.
The dew point of the reducing gas can be lower than-60 ℃, such as-65 ℃, 70 ℃ and the like, and if the dew point of the reducing gas is high, the hydrogen loss index of the product can be influenced.
In this embodiment, the reduction coating treatment may be performed in a reduction apparatus capable of passing a protective atmosphere, such as a reduction furnace, a carbon tube furnace, a bell jar furnace, or the like.
The reduction equipment can be a continuous furnace, and the movement direction of the material powder and the flow movement direction of the protective gas can be opposite, so that the efficiency can be improved, and the product quality can be ensured.
The pressure in the reduction equipment (namely the position in the furnace cavity and the reduction reaction) is higher than that outside the furnace by delta P which is 20-100 Pa, thus ensuring good and safe reaction effect in the furnace and proper gas consumption. If the delta P is too low and is less than 20Pa, the product quality is influenced, explosion is possibly caused by air entering the furnace, and safety risk exists; if Δ P is too high and exceeds 100Pa, the reaction effect is impaired and the amount of gas used is increased.
In this embodiment, the method may further include the steps of: and crushing the cooled copper-clad iron powder to obtain a product with the required granularity.
According to another exemplary embodiment of the invention, the preparation method of the copper-clad iron powder comprises the following steps:
(1) weighing copper oxide powder and iron powder according to the weight percentage of copper to be coated in the copper-coated iron composite powder, and pouring the copper oxide powder and the iron powder into mixing equipment together for mixing for 5 to 25 minutes.
(2) Fully and uniformly mixing the mixed powder, and filling the mixed powder into a reduction furnace for reduction coating treatment. Under the protection of reducing atmosphere, reducing copper oxide in a reducing furnace and simultaneously carrying out coating reaction on the mixed powder, wherein the temperature of the reduction coating treatment is divided into three sections: the temperature of the first section is 250-600 ℃, the temperature of the second section is 600-690 ℃, the temperature of the third section is 690-820 ℃, the heat preservation time is 30-120 minutes, the pressure in the furnace is higher than that outside the furnace by 20-100 Pa, and then the furnace is cooled to below 40 ℃ under the protective atmosphere and taken out of the furnace.
(3) And crushing and sieving the discharged material blocks, and packaging to obtain the product.
The reduction coating treatment equipment may be a reduction furnace, a carbon tube furnace, a bell jar furnace, etc. which are widely used in industry and can be filled with protective atmosphere. The material powder moving direction of the continuous furnace is opposite to the flow moving direction of the protective gas, the reducing gas can be used for decomposing ammonia, hydrogen, carbon monoxide, coal gas and the like, and the atmosphere dew point is lower than minus 60 ℃.
The components and contents (in percentage by mass) of the copper-clad iron powder prepared according to the two exemplary embodiments can be as follows: 7.5 to 20.7% of copper, 79 to 92% of iron and 0.2 to 1.5% of others. For example, 20.4 percent of copper and 79.3 percent of iron, and the balance of impurities allowed by industrial raw materials, and the oil-retaining bearing product prepared from the copper-clad iron powder with the components has excellent wear resistance and noise reduction performance.
The particle size of the copper-clad iron powder can be below 200 μm, and further below 180 μm, such as 140 ± 20 μm. The coating of the powder may be above 90%, for example 95. + -. 2%.
The invention also provides copper-clad iron powder. The copper-clad iron powder can comprise a product prepared by the method.
Fig. 2 shows a metallographic photograph of the copper-clad iron powder prepared by the present invention, from which it can be seen that the particle size surface of the copper-clad iron powder is fully covered by copper, the distribution is uniform, and the equivalent cladding effect of chemical copper-clad (i.e. chemical displacement method) is achieved. During chemical copper-cladding, acid radical materials can remain in the spongy iron powder particles to influence the quality of product parts, and the copper covering layer also shields the spongy iron powder gaps to influence the oil content of the product.
In order that the above-described exemplary embodiments of the invention may be better understood, further description thereof with reference to specific examples is provided below.
The preparation method of the copper-clad iron powder comprises the following steps:
(1) weighing 255 g of industrial-grade copper oxide powder; the chemical composition of the copper oxide powder is shown in table 1.
TABLE 1
Name (R) | Content (mass fraction%) |
Copper oxide (CuO) | 98.46 |
Hydrochloric acid insoluble substance | 0.15 |
Chloride (Cl) | 0.013 |
Sulfur compounds (in SO)4Meter) | 0.12 |
Iron (Fe) | 0.09 |
Total nitrogen (N) | —— |
Water soluble substance | 0.92 |
The particle size of the copper oxide powder is below 74 μm.
(2) 800 g of reduced iron powder is weighed. The chemical composition of the iron powder is shown in table 2, and the physical properties of the iron powder are shown in table 3.
TABLE 2
Composition (I) | Total Fe | Mn | Si | C | S | P | Hydrochloric acid insoluble substance | Loss of hydrogen |
Mass fraction% | 98.37 | 0.43 | 0.11 | 0.07 | 0.03 | 0.02 | 0.32 | 0.39 |
TABLE 3
(3) The weighed copper oxide and iron powder were mixed in a V-blender for 15 minutes.
(4) After being mixed evenly, the mixture is taken out and loaded into a tube type reducing furnace which is filled with decomposed ammonia gas for reduction and coating treatment. Wherein the dew point of the decomposed ammonia gas is-65 ℃, and the pressure in the furnace is higher than the pressure outside the furnace by 20-100 Pa. The temperature schedule of the reduction and coating treatment is divided into three sections: the first section is 350 ℃, the second section is 640 ℃, the third section is 780 ℃ and the treatment time is 110 minutes. And cooling the treated material to room temperature under the protection of hydrogen and discharging.
(5) And crushing and sieving the discharged materials to obtain the product.
The chemical components and physical properties of the prepared copper-clad iron composite powder are shown in table 4 and table 5.
TABLE 4 (mass%)
Cu | Fe | Mn | Si | C | S | P | Hydrochloric acid insoluble substance | Loss of hydrogen |
19.56 | 79.13 | 0.45 | 0.10 | 0.03 | 0.01 | 0.01 | 0.21 | 0.25 |
TABLE 5
In summary, the copper-clad iron powder and the preparation method thereof have the advantages that:
(1) the copper-clad iron composite powder is prepared by using copper oxide and reduced iron powder as raw materials and performing reduction cladding treatment, so that the sewage discharge of copper cladding by a chemical displacement method is avoided, the harmful sewage discharge is reduced by more than 20 tons for one ton of products, and the pollution-free discharge is realized.
(2) The prepared copper-clad iron composite powder has excellent technological performance indexes, does not contain acid radicals, has good fluidity during pressing, and has small unit weight deviation of pressed parts. In the pressing process of producing the oil-retaining bearing, the copper cladding layer on the surface is soft, so that the porosity of the product is easily reduced by rheology, and finally the oil-retaining rate of the bearing is difficult to improve.
(3) Because the coated metal copper is uniformly and compactly coated on the surface of iron powder particles, the binding force is strong, no acid radical residue exists, the particle size distribution of the coated powder is reasonable and easy to control, the fluidity of the powder body is good, the oxidation resistance is strong, the shrinkage coefficient of a sintered product is small, the part precision of the oil-containing bearing is easy to control, the oil content of the product (namely the oil-containing bearing) can be improved by 3-15%, the service life can be prolonged by 5-20%, and the motor noise can be reduced by 3-10%.
Although the present invention has been described above in connection with exemplary embodiments, it will be apparent to those skilled in the art that various modifications and changes may be made to the exemplary embodiments of the present invention without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (9)
1. A preparation method of copper-clad iron powder is characterized by comprising the following steps:
uniformly mixing copper oxide powder and iron powder to obtain mixed powder, placing the mixed powder in protective atmosphere formed by reducing gas, making reduction coating treatment to obtain copper-clad iron powder,
the mass ratio of the Cu element to the Fe element in the mixed powder is 7.5-20.7: 79 to 92 parts;
the step of reduction coating treatment comprises: heating the mixed powder to T1Preserving heat for 5-40 min, and then heating to T2Keeping the temperature for 20-50 min, and continuously heating toT3Keeping the temperature for 15-30 min, and finally cooling, wherein T is more than or equal to 2501<600℃,600≤T2<690℃,690≤T3<820℃;
Heating to T1The temperature rise speed is 16-38 ℃/min, and the heating is carried out until the temperature is T2The temperature rise speed is 6-22 ℃/min, and the heating is carried out until the temperature is T3The temperature rise speed is 8-15 ℃/min;
the dew point of the reducing gas is below-60 ℃.
2. The preparation method of copper-clad iron powder as claimed in claim 1, wherein the mass fraction of CuO in the copper-oxide powder is above 98%, and the particle size of the copper-oxide powder is below 74 μm.
3. The preparation method of copper-clad iron powder as claimed in claim 1, wherein the mass fraction of Fe element in the iron powder is above 98%, and the particle size of the iron powder is below 200 μm.
4. The method for preparing copper-clad iron powder according to claim 1, wherein the reducing gas comprises at least one of decomposed ammonia gas, hydrogen gas, carbon monoxide and coal gas.
5. The preparation method of copper-clad iron powder according to claim 1, wherein the pressure of the protective atmosphere is 20-100 Pa higher than the external pressure.
6. The preparation method of copper-clad iron powder as claimed in claim 1, wherein the reduction coating treatment is carried out in a continuous reduction apparatus, and the movement direction of the mixed powder in the reduction apparatus is opposite to the flow direction of the reducing gas.
7. The preparation method of copper-clad iron powder according to claim 1, wherein the cooling step comprises: cooling to below 40 ℃ at a cooling rate of 8-24 ℃/min.
8. The preparation method of copper-clad iron powder according to claim 1, characterized in that the preparation method further comprises the steps of:
and crushing and screening the copper-clad iron powder obtained after the reduction coating treatment.
9. A copper-clad iron powder, characterized in that the copper-clad iron powder comprises a product prepared by the preparation method of the copper-clad iron powder of any one of claims 1 to 8, wherein the particle size of the copper-clad iron powder is below 200 μm.
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CN110523972B (en) * | 2019-09-20 | 2022-05-27 | 四川容克斯科技有限公司 | Production system of copper-clad iron powder |
CN111451519B (en) * | 2020-04-03 | 2022-10-14 | 龙门金南磁性材料有限公司 | Preparation method of brass-coated iron powder |
CN113481405B (en) * | 2021-06-29 | 2022-05-20 | 宁波金田铜业(集团)股份有限公司 | Preparation method of copper-iron alloy |
CN114309594A (en) * | 2021-12-31 | 2022-04-12 | 北京有研粉末新材料研究院有限公司 | Copper-iron composite powder and preparation method thereof |
CN115026294A (en) * | 2022-06-09 | 2022-09-09 | 重庆有研重冶新材料有限公司 | Low-apparent-density dry-method copper-clad iron powder preparation method, copper-clad iron powder and application thereof |
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