CN107914007B - 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
CN107914007B
CN107914007B CN201711077726.5A CN201711077726A CN107914007B CN 107914007 B CN107914007 B CN 107914007B CN 201711077726 A CN201711077726 A CN 201711077726A CN 107914007 B CN107914007 B CN 107914007B
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soft magnetic
magnetic materials
powder
molded
antioxidant
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CN107914007A (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 processes, the soft magnetic materials each component is alloy powder 82.5%-87.5% by weight, 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 are as follows: Si:2.9%-3.1%, C≤0.01%, remaining is Fe.Present invention accomplishes currently advanced scientific and technological industries to the requirement such as the high-precision of iron-based soft magnetic part, high labyrinth, high efficiency and large-scale production, expands iron-based soft magnetic part in the application in metal powder 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, in particular to a kind of powder injection-molded soft magnetic materials and its system Standby technique.
Background technique
With the rise of electric power and mechanics of communication since 19th century, the iron based soft magnetic materials based on mild steel are answered extensively 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 cost is relatively low for its own, while the excellent magnetics energy such as coercivity is low, improve the efficiency and reduction of transformer Energy loss, the preferred material being increasingly becoming in power industry soft magnetic materials.Nowadays, with the rapid development of science and technology, The fields such as automobile, radar, television broadcasting, integrated circuit, computer, automatic control propose higher want to iron based soft magnetic materials It asks, traditional processing manufacturing process has been unable to satisfy the requirement of all Element Designs in structure, and in raw material processing, utilization rate It is difficult to get both in terms of quality control, therefore and wastes a large amount of manufacture and material cost.
Summary of the invention
The first purpose of the invention is to provide one kind can meet currently advanced scientific and technological industry to the height of iron-based soft magnetic part The powder injection-molded of requirements 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 alloy by weight 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 are as follows: Si:2.9%- 3.1%, C≤0.01%, remaining is Fe.
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.
A second object of the present invention is to provide the preparation processes how one kind prepares 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, comprising 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 are kneaded 2-3 hours, melting means 400-750g/10min at 190 DEG C, Eventually form feeding;
B, the feeding being kneaded is prepared by fixed particle by pelletizer.
Third object of the present invention is to provide a kind of methods how to make product using above-mentioned soft magnetic materials.
Realizing the technical solution of third purpose of the present invention is: powder injection-molded make of soft magnetic materials produces in the present invention The method of product, comprising 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 are kneaded 2-3 hours, melting means 400-750g/10min at 190 DEG C, Eventually form feeding;
B, the feeding being kneaded is prepared by fixed particle by pelletizer;
C, it by the barrel of fixed particle injection injector, is then injected in mold and is 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, 2-4 hours sinter moldings are kept 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 the effect of positive: (1) present invention accomplishes currently advanced scientific and technological industries to iron-based soft magnetic part In high precision, the requirement such as high labyrinth, high efficiency and large-scale production expands iron-based soft magnetic part in metal powder near-net-shape The application of technical field;
(2) alloy powder used in the present invention is to add Si element 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 The magnetic property with higher under alternating current magnetic field.
In addition, acquisition even tissue, average grain size are big under 1270-1310 DEG C of temperature reduction hydrogen shield, 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).
Specific embodiment
(embodiment 1)
Soft magnetic materials each component is alloy powder 83.8%, polyacetal copolymer 10.6%, second by weight in the present invention 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 are as follows: Si:3%, C: 0.01%, remaining is Fe.
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, comprising 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 are kneaded 2-3 hours, melting means 400-750g/10min at 190 DEG C, Eventually form feeding;
B, the feeding being kneaded is prepared by fixed particle by pelletizer.
The powder injection-molded method with soft magnetic materials production product in the present invention, comprising 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 are kneaded 2.5 hours, melting means 500g/10min at 190 DEG C, finally Form feeding;
B, the feeding being kneaded is prepared by fixed particle by pelletizer;
C, it by the barrel of fixed particle injection injector, is then injected in mold and is 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, 3 hours sinter moldings, sintered density >=7.5g/cm are kept at a temperature of hydrogen atmosphere, 1290 DEG C3, shrinkage ratio It is 1.216 ± 0.003.
The key technical indexes of soft magnetic materials are as follows:
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 in the present invention are as follows:
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 alloy powder 87.5%, polyacetal copolymer 9.2%, second by weight in the present invention 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 are as follows: Si:3%, C: 0.01%, remaining is Fe.
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, comprising 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 are kneaded at 190 DEG C 2 hours, melting means 750g/10min, last shape At feeding;
B, the feeding being kneaded is prepared by fixed particle by pelletizer.
The powder injection-molded method with soft magnetic materials production product in the present invention, comprising 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 are kneaded 2.5 hours, melting means 500g/10min at 190 DEG C, finally Form feeding;
B, the feeding being kneaded is prepared by fixed particle by pelletizer;
C, it by the barrel of fixed particle injection injector, is then injected in mold and is 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, 3 hours sinter moldings, sintered density >=7.5g/cm are kept at a temperature of hydrogen atmosphere, 1310 DEG C3, shrinkage ratio It is 1.216 ± 0.003.
(embodiment 3)
Soft magnetic materials each component is alloy powder 84.89%, polyacetal copolymer 10.6%, second by weight in the present invention 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 are as follows: Si:3%, C: 0.01%, remaining is Fe.
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, comprising 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 are kneaded at 190 DEG C 3 hours, melting means 400g/10min, last shape At feeding;
B, the feeding being kneaded is prepared by fixed particle by pelletizer.
The powder injection-molded method with soft magnetic materials production product in the present invention, comprising 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 are kneaded 2.5 hours, melting means 500g/10min at 190 DEG C, finally Form feeding;
B, the feeding being kneaded is prepared by fixed particle by pelletizer;
C, it by the barrel of fixed particle injection injector, is then injected in mold and is 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, 3 hours sinter moldings, sintered density >=7.5g/cm are kept at a temperature of hydrogen atmosphere, 1270 DEG C3, shrinkage ratio It is 1.216 ± 0.003.
Particular embodiments described above has carried out further in detail the purpose of the present invention, technical scheme and beneficial effects It describes in detail bright, it should be understood that the above is only a specific embodiment of the present invention, is not intended to restrict 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 guarantor of the invention Within the scope of shield.

Claims (7)

1. one kind is powder injection-molded to use soft magnetic materials;It is characterized by: the soft magnetic materials each component is alloyed powder by weight 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 are as follows: 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 weight ratio that the weight ratio of Si is 3%, C is 0.01%, remaining is Fe.
3. one kind according to claim 2 is powder injection-molded to use soft magnetic materials, it is characterised in that: the lubricant is hard Resin acid lithium.
4. one kind according to claim 3 is powder injection-molded to use soft magnetic materials, it is characterised in that: the antioxidant is B225 antioxidant.
5. a kind of 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 is kneaded 2-3 hours, melting means 400-750g/10min at 190 DEG C, finally Form feeding;
B, the feeding being kneaded is prepared by fixed particle by pelletizer.
6. a kind of utilize the powder injection-molded method with soft magnetic materials production product described in claim 1, it is characterised in that The following steps are included:
A, by alloy powder, polyacetal copolymer, ethene/acrylic ester copolymer, 1- butylene/propylene copolymer, lubricant and Antioxidant is proportionally added into kneading machine, and is kneaded 2-3 hours, melting means 400-750g/10min at 190 DEG C, finally Form feeding;
B, the feeding being kneaded is prepared by fixed particle by pelletizer;
C, it by the barrel of fixed particle injection injector, is then injected in mold and is 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, 2-4 hours sinter moldings, sintered density >=7.5g/cm are kept at a temperature of hydrogen atmosphere, 1290 ± 20 DEG C3, shrinkage ratio It is 1.216 ± 0.003.
7. the powder injection-molded method with soft magnetic materials production product according to claim 6, it is characterised in that: described Concentration >=98% of nitric acid described in step d.
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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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