CN107914007A - A kind of powder injection-molded soft magnetic materials and its preparation process - Google Patents

A kind of powder injection-molded soft magnetic materials and its preparation process Download PDF

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Publication number
CN107914007A
CN107914007A CN201711077726.5A CN201711077726A CN107914007A CN 107914007 A CN107914007 A CN 107914007A CN 201711077726 A CN201711077726 A CN 201711077726A CN 107914007 A CN107914007 A CN 107914007A
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soft magnetic
magnetic materials
powder
alloy powder
molded
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CN107914007B (en
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薛永超
邬均文
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Jiangsu Gian Technology 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
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • 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
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1003Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007Atmosphere
    • 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
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1017Multiple heating or additional steps
    • B22F3/1021Removal of binder or filler
    • B22F3/1025Removal of binder or filler not by heating only
    • 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
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/22Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • B22F3/225Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/02Ferrous alloys, e.g. steel alloys containing silicon
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147Alloys characterised by their composition
    • H01F1/14766Fe-Si based alloys
    • 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
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps
    • 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
    • B22F2999/00Aspects linked to processes or compositions used in powder metallurgy

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Dispersion Chemistry (AREA)
  • Electromagnetism (AREA)
  • Physics & Mathematics (AREA)
  • Power Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Soft Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)
  • Injection Moulding Of Plastics Or The Like (AREA)

Abstract

The present invention relates to a kind of powder injection-molded soft magnetic materials and its preparation process, the soft magnetic materials each component is by weight for alloy powder 82.5% 87.5%, polyacetal copolymer 9.2% 10.6%, ethene/acrylic ester copolymer 1 .0% 3.0%, 1 butylene/propylene copolymer 1.0% 2.0%, lubricant 0.1% 0.5%, antioxidant 0.01% 0.1%;The alloy powder is made of Fe, Si and C;The weight ratio that each component accounts in alloy powder is:Si:2.9% 3.1%, C≤0.01%, remaining is Fe.Present invention accomplishes high-precision, high labyrinth, high efficiency and the large-scale production of currently advanced scientific and technological industry to iron-based soft magnetic part etc. to require, and expands application of the iron-based soft magnetic part in metal dust near-net-shape technology field.

Description

A kind of powder injection-molded soft magnetic materials and its preparation process
Technical field
The present invention relates to metal injection moulding material, more particularly to a kind of powder injection-molded soft magnetic materials and its system Standby technique.
Background technology
With the rise of electric power and mechanics of communication since 19th century, the iron based soft magnetic materials based on mild steel extensively should In magnetic core for motor, transformer, telephone line etc. inductance coil.Into after 20th century, succeeding in developing for silicon steel sheet is replaced Generation mild steel, because its own cost is relatively low, while the excellent magnetic energy such as coercivity is low, improve efficiency and the reduction of transformer Energy loss, the preferred material being increasingly becoming in power industry soft magnetic materials.Nowadays, with science and technology rapid development, Automobile, radar, television broadcasting, integrated circuit, computer, the field such as automatically control and propose higher to iron based soft magnetic materials and want To ask, traditional processing manufacturing process can not meet the requirement of all Element Designs in structure, and in raw material processing, utilization rate It is difficult to get both with terms of quality control, therefore and wastes substantial amounts of manufacture and material cost.
The content of the invention
First purpose of the present invention, which is to provide, a kind of meets height of the currently advanced scientific and technological industry to iron-based soft magnetic part The powder injection-molded of requirement such as precision, high labyrinth, high efficiency and large-scale production use soft magnetic materials.
Realizing the technical solution of first purpose of the invention is:Soft magnetic materials each component is by weight alloy in the present invention Powder 82.5%-87.5%, polyacetal copolymer 9.2%-10.6%, ethene/acrylic ester copolymer 1 .0%-3.0%, 1- Butylene/propylene copolymer 1.0%-2.0%, lubricant 0.1%-0.5%, antioxidant 0.01%-0.1%;
The alloy powder is made of Fe, Si and C;The weight ratio that each component accounts in alloy powder is:Si:2.9%- 3.1%, C≤0.01%, remaining is Fe.
The particle diameter of at least 10% alloy powder is 2.02 μm in above-mentioned alloy powder, the grain of at least 50% alloy powder Footpath is 4.29 μm, and the particle diameter of at least 90% alloyed powder is 8.93 μm.
As optimal, the weight ratio that the weight ratio of Si is 3%, C in above-mentioned alloy powder is 0.01%, remaining is Fe.
Above-mentioned lubricant is lithium stearate (C18H35LiO2).
Above-mentioned antioxidant is B225 antioxidant.
Second object of the present invention is to provide a kind of preparation process for how preparing above-mentioned soft magnetic materials.
Realizing the technical solution of second purpose of the invention is:The powder injection-molded preparation with soft magnetic materials in the present invention Technique, comprises the following steps:
A, by alloy powder, polyacetal copolymer, ethene/acrylic ester copolymer, 1- butylene/propylene copolymer, lubrication Agent and antioxidant are proportionally added into kneading machine, and at 190 DEG C be kneaded 2-3 it is small when, its melting means is 400-750g/10min, Eventually form feeding;
B, the feeding being kneaded is prepared into by fixed particle by comminutor.
Third object of the present invention is to provide a kind of method for how utilizing above-mentioned soft magnetic materials to make product.
Realizing the technical solution of the 3rd purpose of the invention is:Powder injection-molded made of soft magnetic materials is produced in the present invention The method of product, comprises the following steps:
A, by alloy powder, polyacetal copolymer, ethene/acrylic ester copolymer, 1- butylene/propylene copolymer, lubrication Agent and antioxidant are proportionally added into kneading machine, and at 190 DEG C be kneaded 2-3 it is small when, its melting means is 400-750g/10min, Eventually form feeding;
B, the feeding being kneaded is prepared into by fixed particle by comminutor;
C, fixed particle is injected in the barrel of injector, is then injected in mould and shaped by injector, depanning is made Tungsten-nickel hard alloy blank;
D, at a temperature of 110 ± 10 DEG C, using nitric acid catalysis degreasing, degreasing rate >=7.8%;
E, the sinter molding when keeping 2-4 small at a temperature of hydrogen atmosphere, 1290 ± 20 DEG C, sintered density >=7.5g/cm3, Shrinkage ratio is 1.216 ± 0.003.
Concentration >=98% of nitric acid described in above-mentioned steps d.
The present invention has positive effect:(1) present invention accomplishes currently advanced scientific and technological industry to iron-based soft magnetic part High accuracy, high labyrinth, high efficiency and large-scale production etc. require, and expand iron-based soft magnetic part in metal dust near-net-shape The application of technical field;
(2) alloy powder used in the present invention is to add Si elements using Fe as matrix to form FeSi solid solution, improves conjunction Golden resistivity, reduces magnetic loss, increases magnetic conductivity, reduces magnetocrystalline anisotropy constant, reduces the eddy-current loss of material, make the alloy There is higher magnetic property under alternating current magnetic field.
In addition, under 1270-1310 DEG C of temperature reduction hydrogen shield, acquisition even tissue, average grain size are big, cause The high sintering state of density, relative density reach 99.5%, and it is soft to obtain preferable low-coercivity, high saturated magnetic induction etc. Magnetic property (performance such as following table).
Embodiment
(embodiment 1)
Soft magnetic materials each component is by weight being alloy powder 83.8% in the present invention, polyacetal copolymer 10.6%, second Alkene/acrylate copolymer 3.0%, 1- butylene/propylene copolymer 2.0%, lubricant 0.5%, antioxidant 0.1%;
The alloy powder is made of Fe, Si and C;The weight ratio that each component accounts in alloy powder is:Si:3%, C: 0.01%, remaining is Fe.
The particle diameter of at least 10% alloy powder is 2.02 μm in the alloy powder, the grain of at least 50% alloy powder Footpath is 4.29 μm, and the particle diameter of at least 90% alloyed powder is 8.93 μm.
Above-mentioned lubricant is lithium stearate (C18H35LiO2).
Above-mentioned antioxidant is B225 antioxidant.
The powder injection-molded preparation process with soft magnetic materials in the present invention, comprises the following steps:
A, by alloy powder, polyacetal copolymer, ethene/acrylic ester copolymer, 1- butylene/propylene copolymer, lubrication Agent and antioxidant are proportionally added into kneading machine, and at 190 DEG C be kneaded 2-3 it is small when, its melting means is 400-750g/10min, Eventually form feeding;
B, the feeding being kneaded is prepared into by fixed particle by comminutor.
The powder injection-molded method that product is made of soft magnetic materials, comprises the following steps in the present invention:
A, by alloy powder, polyacetal copolymer, ethene/acrylic ester copolymer, 1- butylene/propylene copolymer, lubrication Agent and antioxidant are proportionally added into kneading machine, and at 190 DEG C be kneaded 2.5 it is small when, its melting means is 500g/10min, finally Form feeding;
B, the feeding being kneaded is prepared into by fixed particle by comminutor;
C, fixed particle is injected in the barrel of injector, is then injected in mould and shaped by injector, depanning is made Tungsten-nickel hard alloy blank;
D, at a temperature of 110 ± 10 DEG C, using the nitric acid catalysis degreasing of concentration >=98%, degreasing rate >=7.8%;
E, sinter molding, sintered density >=7.5g/cm when holding 3 is small at a temperature of hydrogen atmosphere, 1290 DEG C3, shrinkage ratio For 1.216 ± 0.003.
The key technical indexes of soft magnetic materials is:
Technical indicator Parameter value
Density p ≥7.5g/cm3
Hardness Hv 140-170HV1
Yield strength σ s ≥280MPa
Coercivity H 45-50A/m
Residual magnetic flux density Br ≤1.3T
Maximum permeability μm ax ≥8000
The attainable technical parameter value of soft magnetic materials institute is in the present invention:
Technical indicator Parameter value
Feeding melting means MFI 495g/10min
Sintered density ρ 7.62g/cm3
Hardness Hv 162HV1
Yield strength σs 291.3MPa
Coercivity H 46.88A/m
Residual magnetic flux density Br 1.24T
Maximum permeability μmax 8403
(embodiment 2)
Soft magnetic materials each component is by weight being alloy powder 87.5% in the present invention, polyacetal copolymer 9.2%, second Alkene/acrylate copolymer 1%, 1- butylene/propylene copolymer 2.0%, lubricant 0.2%, antioxidant 0.1%;
The alloy powder is made of Fe, Si and C;The weight ratio that each component accounts in alloy powder is:Si:3%, C: 0.01%, remaining is Fe.
The particle diameter of at least 10% alloy powder is 2.02 μm in the alloy powder, the grain of at least 50% alloy powder Footpath is 4.29 μm, and the particle diameter of at least 90% alloyed powder is 8.93 μm.
Above-mentioned lubricant is lithium stearate (C18H35LiO2).
Above-mentioned antioxidant is B225 antioxidant.
The powder injection-molded preparation process with soft magnetic materials in the present invention, comprises the following steps:
A, by alloy powder, polyacetal copolymer, ethene/acrylic ester copolymer, 1- butylene/propylene copolymer, lubrication Agent and antioxidant are proportionally added into kneading machine, and be kneaded at 190 DEG C 2 it is small when, its melting means is 750g/10min, last shape Into feeding;
B, the feeding being kneaded is prepared into by fixed particle by comminutor.
The powder injection-molded method that product is made of soft magnetic materials, comprises the following steps in the present invention:
A, by alloy powder, polyacetal copolymer, ethene/acrylic ester copolymer, 1- butylene/propylene copolymer, lubrication Agent and antioxidant are proportionally added into kneading machine, and at 190 DEG C be kneaded 2.5 it is small when, its melting means is 500g/10min, finally Form feeding;
B, the feeding being kneaded is prepared into by fixed particle by comminutor;
C, fixed particle is injected in the barrel of injector, is then injected in mould and shaped by injector, depanning is made Tungsten-nickel hard alloy blank;
D, at a temperature of 115 DEG C, using the nitric acid catalysis degreasing of concentration >=98%, degreasing rate >=7.8%;
E, sinter molding, sintered density >=7.5g/cm when holding 3 is small at a temperature of hydrogen atmosphere, 1310 DEG C3, shrinkage ratio For 1.216 ± 0.003.
(embodiment 3)
Soft magnetic materials each component is by weight being alloy powder 84.89% in the present invention, polyacetal copolymer 10.6%, second Alkene/acrylate copolymer 2.0%, 1- butylene/propylene copolymer 2.0%, lubricant 0.5%, antioxidant 0.01%;
The alloy powder is made of Fe, Si and C;The weight ratio that each component accounts in alloy powder is:Si:3%, C: 0.01%, remaining is Fe.
The particle diameter of at least 10% alloy powder is 2.02 μm in the alloy powder, the grain of at least 50% alloy powder Footpath is 4.29 μm, and the particle diameter of at least 90% alloyed powder is 8.93 μm.
Above-mentioned lubricant is lithium stearate (C18H35LiO2).
Above-mentioned antioxidant is B225 antioxidant.
The powder injection-molded preparation process with soft magnetic materials in the present invention, comprises the following steps:
A, by alloy powder, polyacetal copolymer, ethene/acrylic ester copolymer, 1- butylene/propylene copolymer, lubrication Agent and antioxidant are proportionally added into kneading machine, and be kneaded at 190 DEG C 3 it is small when, its melting means is 400g/10min, last shape Into feeding;
B, the feeding being kneaded is prepared into by fixed particle by comminutor.
The powder injection-molded method that product is made of soft magnetic materials, comprises the following steps in the present invention:
A, by alloy powder, polyacetal copolymer, ethene/acrylic ester copolymer, 1- butylene/propylene copolymer, lubrication Agent and antioxidant are proportionally added into kneading machine, and at 190 DEG C be kneaded 2.5 it is small when, its melting means is 500g/10min, finally Form feeding;
B, the feeding being kneaded is prepared into by fixed particle by comminutor;
C, fixed particle is injected in the barrel of injector, is then injected in mould and shaped by injector, depanning is made Tungsten-nickel hard alloy blank;
D, at a temperature of 100 DEG C, using the nitric acid catalysis degreasing of concentration >=98%, degreasing rate >=7.8%;
E, sinter molding, sintered density >=7.5g/cm when holding 3 is small at a temperature of hydrogen atmosphere, 1270 DEG C3, shrinkage ratio For 1.216 ± 0.003.
Particular embodiments described above, has carried out the purpose of the present invention, technical solution and beneficial effect further in detail Describe in detail it is bright, it should be understood that the foregoing is merely the present invention specific embodiment, be not intended to limit the invention, it is all Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done, should be included in the guarantor of the present invention Within the scope of shield.

Claims (8)

1. one kind is powder injection-molded to use soft magnetic materials;It is characterized in that:The soft magnetic materials each component is by weight alloyed powder Last 82.5%-87.5%, polyacetal copolymer 9.2%-10.6%, ethene/acrylic ester copolymer 1 .0%-3.0%, 1- fourth Alkene/propylene copolymer 1.0%-2.0%, lubricant 0.1%-0.5%, antioxidant 0.01%-0.1%;
The alloy powder is made of Fe, Si and C;The weight ratio that each component accounts in alloy powder is:Si:2.9%-3.1%, C ≤ 0.01%, remaining is Fe.
2. one kind according to claim 1 is powder injection-molded to use soft magnetic materials, it is characterised in that:In the alloy powder The particle diameter of at least 10% alloy powder is 2.02 μm, and the particle diameter of at least 50% alloy powder is 4.29 μm, at least 90% The particle diameter of alloyed powder is 8.93 μm.
3. one kind according to claim 1 or 2 is powder injection-molded to use soft magnetic materials, it is characterised in that:The alloyed powder The weight ratio that the weight ratio of Si is 3%, C in end is 0.01%, remaining is Fe.
4. one kind according to claim 3 is powder injection-molded to use soft magnetic materials, it is characterised in that:The lubricant is hard Resin acid lithium.
5. one kind according to claim 4 is powder injection-molded to use soft magnetic materials, it is characterised in that:The antioxidant is B225 antioxidant.
A kind of 6. powder injection-molded preparation process with soft magnetic materials as claimed in claim 1 or 2, it is characterised in that including Following steps:
A, by alloy powder, polyacetal copolymer, ethene/acrylic ester copolymer, 1- butylene/propylene copolymer, lubricant and Antioxidant is proportionally added into kneading machine, and at 190 DEG C be kneaded 2-3 it is small when, its melting means is 400-750g/10min, finally Form feeding;
B, the feeding being kneaded is prepared into by fixed particle by comminutor.
7. a kind of powder injection-molded method that product is made of soft magnetic materials using described in claim 1 or 2, its feature exists In comprising the following steps:
A, by alloy powder, polyacetal copolymer, ethene/acrylic ester copolymer, 1- butylene/propylene copolymer, lubricant and Antioxidant is proportionally added into kneading machine, and at 190 DEG C be kneaded 2-3 it is small when, its melting means is 400-750g/10min, finally Form feeding;
B, the feeding being kneaded is prepared into by fixed particle by comminutor;
C, fixed particle is injected in the barrel of injector, is then injected in mould and shaped by injector, tungsten nickel is made in depanning Hard alloy blank part;
D, at a temperature of 110 ± 10 DEG C, using nitric acid catalysis degreasing, degreasing rate >=7.8%;
E, the sinter molding when keeping 2-4 small at a temperature of hydrogen atmosphere, 1290 ± 20 DEG C, sintered density >=7.5g/cm3, shrinks Than for 1.216 ± 0.003.
8. the powder injection-molded method that product is made of soft magnetic materials according to claim 7, it is characterised in that:It is described Concentration >=98% of nitric acid described in step d.
CN201711077726.5A 2017-11-06 2017-11-06 A kind of powder injection-molded soft magnetic materials and its preparation process Active CN107914007B (en)

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CN109986075A (en) * 2019-04-02 2019-07-09 合肥核舟电子科技有限公司 A kind of metal powder injection molding magnetism feeding and preparation method thereof
CN110459398A (en) * 2019-08-27 2019-11-15 江苏精研科技股份有限公司 A kind of MIM- iron nickel magnetic property of soft magnetic material treatment process

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CN109180183A (en) * 2018-11-08 2019-01-11 江苏精研科技股份有限公司 A kind of polyformaldehyde system formulation and a kind of powder injection molding process
CN109986075A (en) * 2019-04-02 2019-07-09 合肥核舟电子科技有限公司 A kind of metal powder injection molding magnetism feeding and preparation method thereof
CN110459398A (en) * 2019-08-27 2019-11-15 江苏精研科技股份有限公司 A kind of MIM- iron nickel magnetic property of soft magnetic material treatment process

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