CN113414396A - Preparation method of high-molding FeCu prealloying powder - Google Patents

Preparation method of high-molding FeCu prealloying powder Download PDF

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Publication number
CN113414396A
CN113414396A CN202010673876.8A CN202010673876A CN113414396A CN 113414396 A CN113414396 A CN 113414396A CN 202010673876 A CN202010673876 A CN 202010673876A CN 113414396 A CN113414396 A CN 113414396A
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China
Prior art keywords
powder
temperature
prealloying
fecu
copper
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CN202010673876.8A
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Chinese (zh)
Inventor
朱新娟
何俊超
符立金
王双
张新会
杨建林
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Xixia Taixiang Industrial Co ltd
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Xixia Taixiang Industrial Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B22F9/22Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/16Ferrous alloys, e.g. steel alloys containing copper
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0824Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

According to the preparation method of the high-forming FeCu prealloying powder, the formability of the FeCu prealloying powder is improved by changing the appearance of the water atomized powder, so that the rejection rate of products is reduced, the spherical powder is etched at high temperature through the copper salt, the appearance of the original spherical prealloying powder is changed, the surface element composition of the spherical prealloying powder is improved, the cohesiveness and the strength of the prealloying powder are improved, the stability of the prealloying powder is greatly enhanced, the green strength of the flaky powder is respectively improved by 68% and 45% compared with the prior art, and unexpected technical effects are achieved.

Description

Preparation method of high-molding FeCu prealloying powder
Technical Field
The invention relates to the technical field of preparation of pre-alloyed powder for diamond products, in particular to a preparation technology of high-forming FeCu pre-alloyed powder.
Background
In the diamond tool industry, because diamond is fine particles, a matrix material is generally used to make the diamond into a product with a certain shape and certain mechanical properties. Three common carcass materials are metal, resin and ceramic, with metal carcasses being most widely used with good mechanical properties.
The general method of the matrix material is to mechanically mix a plurality of single element metal powders (such as iron powder, copper powder, cobalt powder and the like) to obtain the matrix material, the mixed powder has thicker particles, the powder surface is easy to oxidize, the sintering activity is poor, the sintering temperature is required to be high, the components of the diamond tool matrix obtained by the method are not uniform, and complete alloying can not be achieved, in order to overcome the defects, the performance of the diamond tool matrix is improved, a raw material powder manufacturer starts to research the prealloying powder, the prealloying powder has more uniform element distribution than the mechanically mixed powder, the component segregation is fundamentally avoided, the matrix structure is uniform, the performance tends to be consistent, meanwhile, the prealloying greatly reduces the activation energy required by the diffusion of metal atoms in the sintering process, the sintering performance is good, the sintering temperature is low, the sintering time is shortened, for example, the Chinese patent CN107385346A adopts a water mist method to add rare earth alloy powder with the conventional content in the prealloying powder, and nickel and cobalt are matched for use, so that the hardness of the diamond cutter head subjected to hot-pressing sintering is not reduced, the bending strength is high, the use of the staggered-tooth cutter head can be ensured, the diamond edge height is greatly increased, the cutting efficiency is improved, the service life is also ensured, and the requirements of both efficiency and service life are met. However, the prealloyed powder prepared by the traditional water mist method is spherical.
The spherical pre-alloyed powder produced by the atomization method has high apparent density and large forming pressure, so that the powder has poor formability, and under the condition that the thickness of a diamond tool is less than 3mm, the green strength of the traditional spherical matrix powder is generally low in the production process, so that the smoothness of the processed surface is poor, the edge damage of parts in the processing process is caused, even the pressed finished products are damaged in the carrying process, and the rejection rate of the products is high.
In order to improve the formability of the press matrix powder and reduce the rejection rate of pressed finished products, manufacturers for producing diamond tools adopt a granulating technology to treat prealloy obtained by a high-pressure water mist production process so as to improve the formability of the powder, and adopt a granulating agent to treat the prealloy and granulate the prealloy by using the existing granulating machine, but the granulating main material of the method is acetone, isopropanol and other volatile chemical solvents which are used as the granulating agent, so that the environment is polluted in the production process, and the granulating cost is high.
Therefore, the research and development of powder for improving the formability of FeCu prealloyed powder by changing the morphology of water atomized powder is urgently needed, which is a great problem that people are urgently required to solve.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing powder to improve the formability of FeCu prealloyed powder.
The invention relates to a preparation method of high-shaping FeCu prealloying powder, which comprises the following steps:
1) melting pure iron and electrolytic copper in an intermediate frequency furnace according to a certain material proportion, and then preparing the spherical iron-copper prealloy powder by using a conventional high-pressure water atomization production process.
2) Drying and screening the prealloying powder prepared in the step 1) to obtain prealloying powder with required mesh number.
3) Mixing the pre-alloyed powder sieved in the step 2) with copper salt in a mixer for a certain time, wherein the mass ratio of the added copper salt is 2-12%.
4) Adding the mixed powder obtained in the step 3) into a rotary electric furnace at the temperature of 450-650 ℃, frying for 1-3 hours, then naturally cooling to room temperature, and gradually changing the powder from a spherical shape to a flaky shape in the frying process.
5) And (3) reducing the powder fried in the step 4) in a hydrogen reduction furnace for a certain time to produce the required flaky FeCu prealloy powder.
Preferably, the material proportion in the step 1) is 70-85% of pure iron and 15-30% of electrolytic copper by mass ratio.
Preferably, step 2) is performed by filtering and screening with a 500-mesh sieve.
Preferably, the adding mass ratio of the copper salt in the step 3) is 10%, and the mixing time is 2-3 hours.
Preferably, the copper salt in step 3) is CuOH or Cu3(PO4)2Or Cu (NO)3)2
Preferably, the frying time in the step 3) is 2 hours.
Preferably, the reduction time in step 5) is 1 to 4 hours.
Preferably, the frying step in the step 4) is as follows: the temperature of the frying furnace is programmed according to a temperature rise curve set at 10 ℃ for 1 minute, after the temperature of four temperature zones of the furnace reaches 450 ℃, the temperature of the first temperature zone and the second temperature zone is continuously raised to 550 ℃, the temperature of the third temperature zone and the fourth temperature zone reaches 650 ℃, the mixed material is placed into a roller to convey the material to the heating zone, and the roller rotates at a certain rotating speed in the frying process to ensure that the mixed material fully reacts in the frying process.
The copper salt is in friction contact with the screened FeCu prealloy in a rotary electric furnace at high temperature, the spherical surface of the FeCu prealloy is etched, the prealloy gradually changes from spherical to flaky shape, the copper salt is reduced after the prealloy is attached and etched, the surface copper content of flaky alloy powder is higher than that of spherical alloy powder, and the copper is less prone to being oxidized relative to iron in the air because the oxidation-reduction potential of the copper is higher than that of the iron.
The invention has the beneficial effects that: according to the invention, the formability of FeCu prealloying powder is improved by changing the appearance of water atomized powder, so that the rejection rate of products is reduced, the spherical powder is etched at high temperature through copper salt, the appearance of the original spherical prealloying powder is changed, the surface element composition of the spherical prealloying powder is improved, the cohesiveness and strength of the prealloying powder are improved, the stability of the prealloying powder is greatly enhanced, the green strength of flake powder is respectively improved by 68% and 45% compared with the prior art, and unexpected technical effects are achieved.
Drawings
FIG. 1 is an SEM image of a flaky FeCu prealloyed powder prepared in example 1;
FIG. 2 is an SEM image of a spherical FeCu prealloyed powder prepared in comparative example 1.
Detailed Description
The following detailed description is made with reference to the accompanying drawings.
Example 1
A preparation method of high-shaping FeCu prealloying powder comprises the following steps:
1) melting 80% of pure iron and 20% of electrolytic copper in an intermediate frequency furnace according to the material ratio, and then preparing spherical iron-copper prealloy powder by using a conventional high-pressure water atomization production process;
2) drying the prealloying powder prepared in the step 1), sieving the powder by a 500-mesh sieve, and screening to obtain prealloying powder with a required mesh number;
3) mixing the pre-alloyed powder sieved in the step 2) with copper nitrate in a mixer for 2 hours, wherein the mass ratio of the added copper nitrate is 5%;
4) adding the mixed powder obtained in the step 3) into a rotary electric furnace at 550 ℃, frying for 2 hours, naturally cooling to room temperature, and gradually changing the powder from a spherical shape to a flaky shape in the frying process; the frying process comprises the following steps: setting a temperature-rise curve for raising the temperature of the frying and heating furnace according to 10 ℃ for 1 minute, raising the temperature of the first and second temperature regions to 550 ℃ after the temperature of the four temperature regions of the furnace reaches 450 ℃, raising the temperature of the third and fourth temperature regions to 650 ℃, putting the mixed material into a roller, conveying the material to the heating region, ensuring that the actual temperature and the set temperature of each temperature region are kept within a range of +/-5 ℃ in the heating process, and rotating the roller at a certain rotating speed in the frying process;
5) and (3) carrying out hydrogen reduction on the powder fried in the step 4) in a hydrogen reduction furnace for 3 hours to produce the required high-molding flaky FeCu prealloy powder.
Comparative example 1
A method for preparing FeCu prealloyed powder, comprising the steps of:
1) melting 80% of pure iron and 20% of electrolytic copper in an intermediate frequency furnace according to the material ratio, and then preparing spherical iron-copper prealloy powder by using a conventional high-pressure water atomization production process;
2) drying the prealloying powder prepared in the step 1), sieving with a 500-mesh sieve, and screening to obtain the prealloying powder with the required mesh number (as shown in figure 2).
Comparative example 2
A method for preparing FeCu prealloyed powder, comprising the steps of:
1) melting 80% of pure iron and 20% of electrolytic copper in an intermediate frequency furnace according to the material ratio, and then preparing spherical iron-copper prealloy powder by using a conventional high-pressure water atomization production process;
2) drying the prealloying powder prepared in the step 1), sieving with a 500-mesh sieve, and screening to obtain the prealloying powder with the required mesh number.
3) Treating the prealloyed powder in the step 2) by using isopropanol, and then granulating by using a granulating agent.
Performance testing
Green strength tests were performed on the powders and the results showed: the green strength of the powder of example 1 was 32MPa, the green strength of the powder of comparative example 2 was 22MPa, and the green strength of the prealloyed powder of comparative example 1 was 19 MPa. The green strength of iron-based powders is generally low, typically not exceeding 20MPa, since metallurgical powder strength depends mainly on the mechanical packing density of the powder particles and the metal composition of the surface atoms, the green compact obtained by forming the spherical powder in the comparative example 1 has a large amount of void defects inside, so that the strength is lower, the green compact density of the flaky powder in the example 1 is obviously improved, the green compact strength is improved by 68 percent compared with the comparative example 1, the copper content on the surface of the powder in the example 1 is higher, the oxidation resistance is higher, the heat dissipation performance is better when cutting, compared with the comparative example 2, the embodiment 1 not only reduces the environmental pollution of the organic solvent, compared with 5 yuan/kg powder of the comparative document 2, the example 1 has the advantages that the production cost is obviously reduced, the green strength of the powder of the example 1 is improved by 45 percent compared with that of the comparative document 2, and the unexpected technical effect is achieved.

Claims (8)

1. A preparation method of high-shaping FeCu prealloying powder comprises the following steps:
1) melting pure iron and electrolytic copper in an intermediate frequency furnace according to a certain material proportion, and then preparing iron-copper prealloy powder with a spherical shape by using a conventional high-pressure water atomization production process;
2) drying and screening the prealloying powder prepared in the step 1) to prepare prealloying powder with required mesh number;
3) mixing the pre-alloyed powder sieved in the step 2) with copper salt in a mixer for a certain time, wherein the mass ratio of the added copper salt is 2-12%;
4) adding the mixed powder obtained in the step 3) into a rotary electric furnace at the temperature of 450-650 ℃, frying for 1-3 hours, then naturally cooling to room temperature, and gradually changing the powder from a spherical shape to a sheet shape in the frying process;
5) and (3) reducing the powder fried in the step 4) in a hydrogen reduction furnace for a certain time to produce the required flaky FeCu prealloy powder.
2. The method as claimed in claim 1, wherein the material ratio in step 1) is 70-85% pure iron and 15-30% electrolytic copper by mass ratio.
3. The method of claims 1-2, wherein step 2) is performed by using a 500 mesh sieve for filtering and screening.
4. The method according to claim 1 to 3, wherein the copper salt is added in the step 3) in a mass ratio of 10% and the mixing time is 2 to 3 hours.
5. The method of claims 1-4, wherein the copper salt in step 3) is CuOH or Cu3(PO4)2Or Cu (NO)3)2
6. The method of claims 1-5, wherein the parching time in step 3) is 2 hours.
7. The method of claims 1-6, wherein the reduction time in step 5) is 1-4 hours.
8. The method of claims 1-7, wherein the parching step in step 4) is: the temperature of the frying furnace is programmed according to a temperature rise curve set at 10 ℃ for 1 minute, after the temperature of four temperature zones of the furnace reaches 450 ℃, the temperature of the first temperature zone and the second temperature zone is continuously raised to 550 ℃, the temperature of the third temperature zone and the fourth temperature zone reaches 650 ℃, the mixed material is placed into a roller to convey the material to the heating zone, and the roller rotates at a certain rotating speed in the frying process to ensure that the mixed material fully reacts in the frying process.
CN202010673876.8A 2020-07-14 2020-07-14 Preparation method of high-molding FeCu prealloying powder Pending CN113414396A (en)

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Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60125305A (en) * 1983-12-12 1985-07-04 Kagakuhin Kensa Kyokai Manufacture of copper powder
CN1868637A (en) * 2005-05-25 2006-11-29 成都市同心元新材料有限公司 Copper alloy coated composite powder and its preparation method
CN101146616A (en) * 2005-03-25 2008-03-19 同和环保再生事业有限公司 Organohalogen compound decomposing agents
JP2009215569A (en) * 2008-03-07 2009-09-24 Doshisha Method for producing alloy powder using molten salt reaction bath
CN101818246A (en) * 2010-05-11 2010-09-01 南通新玮镍钴科技发展有限公司 Technology for leaching cobalt-copper white alloy
CN102554216A (en) * 2012-02-07 2012-07-11 建德市易通金属粉材有限公司 Water atomization ferrum-copper alloy powder and manufacturing method
CN102699322A (en) * 2012-06-12 2012-10-03 夏德虎 Production method of copper coated iron powder
US20160165766A1 (en) * 2014-12-03 2016-06-09 National Chung Shan Institute Of Science And Technology Method for making electromagnetic wave shielding material
CN106670454A (en) * 2017-01-24 2017-05-17 昆山德泰新材料科技有限公司 Iron-copper alloy powder and preparation method thereof
CN106716573A (en) * 2015-02-27 2017-05-24 日立金属株式会社 Method for manufacturing R-T-B based sintered magnet

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60125305A (en) * 1983-12-12 1985-07-04 Kagakuhin Kensa Kyokai Manufacture of copper powder
CN101146616A (en) * 2005-03-25 2008-03-19 同和环保再生事业有限公司 Organohalogen compound decomposing agents
CN1868637A (en) * 2005-05-25 2006-11-29 成都市同心元新材料有限公司 Copper alloy coated composite powder and its preparation method
JP2009215569A (en) * 2008-03-07 2009-09-24 Doshisha Method for producing alloy powder using molten salt reaction bath
CN101818246A (en) * 2010-05-11 2010-09-01 南通新玮镍钴科技发展有限公司 Technology for leaching cobalt-copper white alloy
CN102554216A (en) * 2012-02-07 2012-07-11 建德市易通金属粉材有限公司 Water atomization ferrum-copper alloy powder and manufacturing method
CN102699322A (en) * 2012-06-12 2012-10-03 夏德虎 Production method of copper coated iron powder
US20160165766A1 (en) * 2014-12-03 2016-06-09 National Chung Shan Institute Of Science And Technology Method for making electromagnetic wave shielding material
CN106716573A (en) * 2015-02-27 2017-05-24 日立金属株式会社 Method for manufacturing R-T-B based sintered magnet
CN106670454A (en) * 2017-01-24 2017-05-17 昆山德泰新材料科技有限公司 Iron-copper alloy powder and preparation method thereof

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Application publication date: 20210921