CN101503299A - Gel injection moulding preparation for gradient material in rotating magnetic field - Google Patents

Gel injection moulding preparation for gradient material in rotating magnetic field Download PDF

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CN101503299A
CN101503299A CN 200910096061 CN200910096061A CN101503299A CN 101503299 A CN101503299 A CN 101503299A CN 200910096061 CN200910096061 CN 200910096061 CN 200910096061 A CN200910096061 A CN 200910096061A CN 101503299 A CN101503299 A CN 101503299A
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rotatingfield
injection moulding
gradient material
gel injection
magnetic field
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CN101503299B (en
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彭晓领
葛洪良
张朋越
洪波
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China Jiliang University
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China Jiliang University
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Abstract

The invention relates to a method for preparing a gel injection mold of a gradient material in a revolving magnetic field. The existing method is difficult to realize continuous and even variation of material compositions, or difficult to obtain large-thickness materials and the like. The method comprises the following steps: mixing ferromagnetic particles and non-magnetic particles into mixed powder; preparing organic monomer and a cross-linking agent into premixed solution; adding the mixed powder into the premixed solution; adding a dispersing agent into the solution; obtaining a dispersed slurry through ball milling and ultrasonic dispersion treatment; adding an initiator and a catalyst into the dispersed size; pouring the size into a mold after stirring; applying the revolving magnetic field outside the mold; and taking out the mold after gelling, drying, pressing and sintering. The method can prepare gradient materials with various thicknesses in a large ingredient range, has continuous variable and controllable ingredients, simplified process and reduced cost.

Description

The gel injection moulding preparation of gradient material in the rotatingfield
Technical field
The present invention relates to the gel injection moulding preparation of gradient material in a kind of rotatingfield, belong to field of material preparation.
Background technology
Stupalith has been widely used in industrial circles such as electronics, machinery, national defence because of its particular performances.But be difficult to carry out machining behind the stupalith sintering, old friends are seeking the dead size forming method of complicated shape ceramic component always, and this has become the key link that guarantees the ceramic component quality and make the material acquisition practical application of being developed.The forming method of stupalith generally can be divided into dry method and wet method two big classes.Comparatively speaking, wet therapy forming process equipment is simple, the molding blank component is even, defective is few, be easy to advantage such as moulding complicated shape part, and practicality is stronger.But all there are some problems in traditional wet moulding technology, is to absorb water by plaster mould to realize as injection forming, cause to form density gradient distribution and nonaffine deformation in the base substrate, and blank strength is low, is easy to damage.Injection moulding or injection molding need add mass fraction up to 20% wax or organism, cause skimming processes loaded down with trivial details, and the thawing of wedding agent or evaporation reduce the intensity of base substrate, easily form defective even collapse.These problems have improved the production cost of stupalith, have reduced its quality of stability.The beginning of the nineties, U.S.'s Oak Ridge National Laboratory has been invented a kind of brand-new stupalith wet moulding technology---gel casting forming technology, and the main production process is: ceramic raw material mixes → moulding (solidifying) → eliminating medium → drying → sintering with medium.
Gel casting forming is the very strong technology of a kind of practicality, and it has following distinguishing feature: (1) applicable to various stupaliths, the ceramic part of various complicated shapes of moulding and size.(2) because type-approval process and injection molding operation are isolating fully, typing forms the cancellated gelinite of interlinkage by organic monomer in-situ polymerization in the slurry and realizes.So the molding blank component is even, density is even, defective is few.(3) slurry solidifies shaping time than short and controlled.Add-on according to polymerization temperature and catalyzer is different, and it is general controlled at 5~60min to solidify shaping time.(4) this technology mould therefor is no punch die, and mould is not had particular requirement, can be metal, glass or plastics etc.(5) organic content is less in the base substrate, and its mass fraction is generally 3%~5%.But intensity is higher, generally more than 10MPa.Can carry out machining (car, mill, dig, mill, boring, saw etc.) to base substrate, thus cancellation or reduce sintering after processing.(6) this is a kind of dead size forming technique.Because the component and the density of base substrate are even, thereby in dry and sintering process, can not be out of shape the shape and size ratio when sintered compact can keep moulding.(7) used ceramic material is high solid phase (volume parts is not less than 50%), low viscosity (less than 1Pas).The solid load of slurry is density, intensity and the inhomogeneity factor that influences molding blank, and the magnitude relationship of viscosity is to the become quality of base substrate shape and the exhaust effect of slurry.
Functionally Graded Materials (FGM) is under the condition at high temperature, thermal cycling and big temperature fall, works better and the class type material developed repeatedly, and so harsh environment for use requires material to have excellent heat shock resistance and thermal fatigue property.At present, the Functionally Graded Materials main preparation methods has powder compacting, physical vaporous deposition (PVD), chemical Vapor deposition process (CVD), plasma spraying, electrocasting, electrochemical plating etc.The powder compacting method is with composition gradient lamination structures such as feed particulate material such as metal, pottery and whiskers, through compacting, sintering and make Functionally Graded Materials.Heat-stable ceramic is used for temperature end, and metallic substance or plastics are used for low-temperature end.Form mutually or raising ceramic phase toughness for reinforced metal, can mix whisker.Chemical Vapor deposition process is that halide gas is carried out thermal degradation, and metal or semi-metal are deposited on the substrate surface, perhaps mixed gass such as the carbide that generates, muriate is sent into reaction tubes, and the compound that heating is generated is deposited on the substrate.Electrocasting is to separate out layer of metal or alloy with metal salt solution through electrodeposition process on the parent form surface. peels off then and obtains and establish the opposite goods of the surperficial convex-concave of type.Physical vaporous deposition is to make the metal deposition of heating evaporation carry out the method for coating on substrate, in metal, semi-metal, send into reactant gasess such as oxygen, nitrogen and hydrocarbon after, potteries such as synthesis oxide, muriate and carbide, and being deposited on the substrate.Physical vaporous deposition has vacuum plating, sputter and ion plating etc.Vacuum plating is that merely heating of metal makes its hydatogenesis; Sputtering method is to hit by electronics or ion, makes the metal deposition that sputters out on substrate; The ion plating is by the metal vapors ionization, obtains the good and fine and close settling of cohesiveness.The thickness of electroforming metal or alloy can be 50 microns to tens centimetres.
But these preparation methods all exist important limitation.Be difficult to realize the material component continuous and even variation as powder compacting; Vapour deposition is difficult to obtain big thickness material; The self-propagating combustion density is lower; Plasma spraying respectively be coated with the interface that there is composition sudden change in interlayer; Or the like.These methods require complicated technology or equipment, lack simple and convenient preparation method, are the major reasons that the limitation function gradient material further develops.Therefore, if sophisticated metal or ceramic forming material means can be used for preparing Functionally Graded Materials, have great importance undoubtedly and vast potential for future development.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, the gel injection moulding preparation of gradient material in a kind of rotatingfield is provided.
Concrete steps of the present invention are:
Step (1) pulp preparation
With particle size is the ferromagnetic particle of 0.1~100 μ m and non-magnetic particle that particle size is 0.1~100 μ m by mass ratio 0.1~10: 1 is mixed into mixed powder; With organic monomer and linking agent by 6~24: 1 weight ratio is dissolved in the deionized water, is made into organism quality mark and is 10~25% premixed liquid; Mixed powder is added in the premixed liquid, add dispersion agent simultaneously, ball milling 1~10h in ball mill, ultrasonic dispersion processing 1~15min, obtain the disperse slurry, adopt 15~38% strong aquas and 15%~40% concentrated hydrochloric acid that the disperse slurry pH value is adjusted to 5~12, solid volume content is 50~70% in the slurry; Dispersant is 0.05%~0.50% of a stock quality.
Described ferromagnetic particle is one or more the mixture in Fe alloy, Co alloy, Ni alloy, rare earth permanent magnet, the ferrite powder.
Described non-magnetic particle is ZrO 2, SiC, AlN, Si 3N 4, B 4C, SiO 2, TiC, Y 2O 3, Al 2O 3In one or more mixture.
Described dispersion agent is a kind of among ammonium polyacrylate, SD-38, JA-281, the D3005.
Described organic monomer is a kind of in acrylamide, Methacrylamide, the vinyl pyrrole ketone.
Described linking agent is a methylene-bisacrylamide.
Casting in step (2) rotatingfield
To add initiator and catalyzer in the disperse slurry, stir the back and inject mould, mould applies rotatingfield outward, and magneticstrength is 0.1~2.5T, and the magnetic field rotating speed is 10~300rpm, and magnetizing time is 3~60min; The initiator add-on is 0.3~3% of a stock quality, and the catalyzer add-on is 0.5 of stock quality~5 ‰.
Described initiator is that massfraction is 1~5% the persulfuric acid aqueous solution.
Described catalyzer is a Tetramethyl Ethylene Diamine.
Described mould is steel, iron, glass or mould of plastics.
Described rotatingfield is the magnetic field that is produced by electro-magnet or permanent magnet, utilizes mechanism to make its rotation, and sense of rotation is perpendicular to field direction.
Step (3) gel, drying, compacting, sintering
Slurry is placed baking oven gel 5~60min of 60~80 ℃, then in drying at room temperature.Green compact place punching block, suppress under the pressure of 0.1~1GPa.Take out green compact and put into sintering oven, charge into argon gas or nitrogen is protected, sintering temperature cools to 100~300 ℃ of taking-ups with the furnace between 600~1400 ℃.
The present invention utilizes moving of rotatingfield control magnetic constituent element on the basis of gel injection technology, successfully prepared composition successive gradient material.The present invention is with the slurry of ferromagnetic material and weak magnetic substance composition, adopts the fixed shaping of casting method of condensing in rotatingfield, compacting, and sintering prepares gradient material then.Magnetic particle in the slurry is subjected to the constraint of magnetic force in magnetic field, therefore when magnetic field rotated, magnetic particle also moved along the magnetic field sense of rotation, thereby forms field gradient along sense of rotation.Compare with preparation gradient material under the static magnetic field, utilize rotatingfield, in gradient material, obtain big component gradient easilier the constraint control of magnetic constituent element.Simultaneously, by adjust magneticstrength, magnetic field rotating speed and the action of a magnetic field time can controlling magnetic field to the restraint force of magnetic constituent element, the further composition profiles in the control material.
Advantage of the present invention is:
1) by applying rotatingfield, change magneticstrength, magnetic field rotating speed and the action of a magnetic field time, can prepare the gradient material of all thickness in very big composition range, composition changes continuously and is controlled.
2) magnetic particle is subjected to the constraint of magnetic force in magnetic field, and therefore when magnetic field rotated, magnetic particle also moved along the magnetic field sense of rotation, thereby forms field gradient along sense of rotation.Prepare Functionally Graded Materials down with static magnetic field and compare, rotatingfield is stronger to the restraint force of magnetic particle, and particle is subjected to magnetically confined and lax effect repeatedly, the easier gradient material of preparing various composition profiles simultaneously.
3) utilize sophisticated gel injection technology that operation simplification, the cost of preparation gradient material are reduced.
Embodiment
Embodiment 1:
1) pulp preparation
Average particle size particle size is the BaO6Fe of 0.1 μ m 2O 3Powder and average particle size particle size are the Al of 0.1 μ m 2O 3Powder is formed mixed powder in proportion at 1: 10; Organic monomer acrylamide (AM) and linking agent methylene-bisacrylamide (MBAM) are dissolved in the deionized water by 6: 1 weight ratio, be made into organism quality mark and be 10% premixed liquid; Mixed powder is added in the premixed liquid, adding content simultaneously is the dispersion agent ammonium polyacrylate of stock quality mark 0.05%, ball milling 1h in ball mill, ultrasonic dispersion processing 1min, obtain the disperse slurry, solid volume content is 50% in the slurry, and regulating the pH value with the concentrated hydrochloric acid of 15% strong aqua and 15% then is 5.0.
2) casting in the rotatingfield
With adding the concentration that accounts for stock quality 0.3% in the disperse slurry is the persulfuric acid aqueous solution initiator of 1wt.% and the Tetramethyl Ethylene Diamine catalyzer that accounts for stock quality 0.5 ‰, stirs the back and injects mould, and mould applies rotatingfield outward.Rotatingfield is produced by electro-magnet, and sense of rotation vertical magnetic field direction, magneticstrength are 0.1T, and the magnetic field rotating speed is 10rpm, and magnetizing time is 3min.Mould adopts stainless punching block, and the mould inside die cavity is to be the disk of 15mm for 15mm, diameter highly.
3) gel, drying, compacting, sintering
Slurry is placed 60 ℃ baking oven gel 5min, then in drying at room temperature.Green compact are placed punching block, under the pressure of 0.1GPa, suppress.Sintering green compact under the protection environment of argon gas.Temperature rise rate with 200 ℃/h is heated to 500 ℃ of insulation 2h, is heated to 1100 ℃ with 200 ℃/h then, insulation 1h.Cool to 200 ℃ of taking-ups with the furnace.
Example 1 prepared sample is carried out the electronic probe line analysis, find that its composition changes continuously, barium ferrite reduces to 0% of opposite side by 78% of a side, and sample interior does not have macroscopic interface and exists.To the sample thermal shock test that circulates, through 100 circulations crackle does not appear under 800 ℃ of temperature difference, chilling condition.
Embodiment 2:
1) pulp preparation
Average particle size particle size is the SmCo of 0.9 μ m 5Powder and average particle size particle size are the ZrO of 0.6 μ m 2And Y 2O 3Powder is formed mixed powder in proportion at 1: 4; Organic monomer Methacrylamide and linking agent methylene-bisacrylamide (MBAM) are dissolved in the deionized water by 15: 1 weight ratio, be made into organism quality mark and be 20% premixed liquid; Mixed powder is added in the premixed liquid, adding content simultaneously is the dispersion agent SD-38 of stock quality umber 0.2%, ball milling 6h in ball mill, ultrasonic dispersion processing 8min, obtain the disperse slurry, solid volume content is 65% in the slurry, and regulating the pH value with the concentrated hydrochloric acid of 25% strong aqua and 30% then is 8.2.
2) casting in the rotatingfield
With adding the concentration that accounts for stock quality 2% in the disperse slurry is the persulfuric acid aqueous solution initiator of 3wt.% and the Tetramethyl Ethylene Diamine catalyzer that accounts for stock quality 3 ‰, stirs the back and injects mould, and mould applies rotatingfield outward.Rotatingfield is produced by electro-magnet, and sense of rotation vertical magnetic field direction, magneticstrength are 0.4T, and the magnetic field rotating speed is 180rpm, and magnetizing time is 10min.Mould adopts the cast iron mould, and the mould inside die cavity is to be the disk of 15mm for 15mm, diameter highly
3) gel, drying, compacting, sintering
Slurry is placed 70 ℃ baking oven gel 12min, then in drying at room temperature.Green compact are placed punching block, under the pressure of 0.4GPa, suppress.The green compact that obtain are sintering under nitrogen protection.Temperature rise rate with 300 ℃/h is heated to 500 ℃ of insulation 1.5h, is heated to 1200 ℃ with 200 ℃/h then, insulation 2h.Cool to 300 ℃ of taking-ups with the furnace.
Example 2 prepared samples are carried out the electronic probe line analysis, find that its composition changes SmCo continuously 5Is 0% by 86% of a side to opposite side, and no macroscopic interface exists.To the thermal shock test that circulates of the sample of gained, through 150 circulations crackle does not appear under 800 ℃ of temperature difference, chilling condition.
Embodiment 3:
1) pulp preparation
Average particle size particle size is that the nickel by powder of 8 μ m and SiC that average particle size particle size is 3 μ m and TiC powder are formed mixed powder in proportion at 1: 1; Organic monomer vinyl pyrrole ketone and linking agent methylene-bisacrylamide (MBAM) are dissolved in the deionized water by 24: 1 weight ratio, be made into organism quality mark and be 25% premixed liquid; Mixed powder is added in the premixed liquid, adding content simultaneously is the dispersion agent JA-281 of stock quality umber 0.5%, ball milling 10h in ball mill, ultrasonic dispersion processing 15min, obtain the disperse slurry, solid volume content is 70% in the slurry, and regulating the pH value with the concentrated hydrochloric acid of 38% strong aqua and 40% then is 12.
2) casting in the rotatingfield
With adding the concentration that accounts for stock quality 3% in the disperse slurry is the persulfuric acid aqueous solution initiator of 5wt.% and the Tetramethyl Ethylene Diamine catalyzer that accounts for stock quality 5 ‰, stirs the back and injects mould, and mould applies rotatingfield outward.Rotatingfield is produced by the magnetic circuit that a pair of NdFeB permanent magnet constitutes, and sense of rotation vertical magnetic field direction, magneticstrength are 0.5T, and the magnetic field rotating speed is 300rpm, and magnetizing time is 60min.Mould adopts glass mold, and the mould inside die cavity is to be the disk of 15mm for 15mm, diameter highly.
3) gel, drying, compacting, sintering
Slurry is placed 80 ℃ baking oven gel 60min, then in drying at room temperature.Green compact are placed punching block, under the pressure of 1GPa, suppress.The green compact that obtain are sintering under nitrogen protection.Temperature rise rate with 200 ℃/h is heated to 500 ℃ of insulation 2h, is heated to 1400 ℃ with 200 ℃/h then, insulation 1h.Cool to 300 ℃ of taking-ups with the furnace.
Example 3 prepared samples are carried out the electronic probe line analysis, find that its composition changes continuously, the Ni powder is 0% by 89% of a side to opposite side, and no macroscopic interface exists.To the thermal shock test that circulates of the sample of gained, through 100 circulations crackle does not appear under 800 ℃ of temperature difference, chilling condition.
Embodiment 4:
1) pulp preparation
Average particle size particle size is that the equal particle size of stainless iron powder peace of 12.4 μ m is AlN and the Si of 10.6 μ m 3N 4Powder is formed mixed powder in proportion at 4: 1; Organic monomer Methacrylamide and linking agent methylene-bisacrylamide (MBAM) are dissolved in the deionized water by 16: 1 weight ratio, be made into organism quality mark and be 15% premixed liquid; Mixed powder is added in the premixed liquid, adding content simultaneously is the dispersion agent D3005 of stock quality umber 0.3%, ball milling 6h in ball mill, ultrasonic dispersion processing 8min, obtain the disperse slurry, solid volume content is 60% in the slurry, and regulating the pH value with the concentrated hydrochloric acid of 38% strong aqua and 15% then is 10.
2) casting in the rotatingfield
With adding the concentration that accounts for stock quality 2% in the disperse slurry is the persulfuric acid aqueous solution initiator of 2wt.% and the Tetramethyl Ethylene Diamine catalyzer that accounts for stock quality 2 ‰, stirs the back and injects mould, and mould applies rotatingfield outward.Rotatingfield is produced by the magnetic circuit that a pair of NdFeB permanent magnet constitutes, and sense of rotation vertical magnetic field direction, magneticstrength are 0.5T, and the magnetic field rotating speed is 120rpm, and magnetizing time is 15min.Mould adopts stainless steel mould, and the mould inside die cavity is to be the disk of 15mm for 15mm, diameter highly.
3) gel, drying, compacting, sintering
Slurry is placed 75 ℃ baking oven gel 15min, then in drying at room temperature.Green compact are placed punching block, under the pressure of 0.2GPa, suppress.The green compact that obtain are sintering under nitrogen protection.Temperature rise rate with 200 ℃/h is heated to 500 ℃ of insulation 2h, is heated to 1000 ℃ with 200 ℃/h then, insulation 2h.Cool to 200 ℃ of taking-ups with the furnace.
Example 4 prepared samples are carried out the electronic probe line analysis, find that it is 0% by 88% of a side to opposite side that its composition changes continuously stainless iron powder, no macroscopic interface existence.To the thermal shock test that circulates of the sample of gained, through 80 circulations crackle does not appear under 800 ℃ of temperature difference, chilling condition.
Embodiment 5:
1) pulp preparation
Average particle size particle size is that cobalt powder and the average particle size particle size of 100 μ m is the B of 100 μ m 4The C powder is formed mixed powder in proportion at 10: 1; Organic monomer acrylamide (AM) and linking agent methylene-bisacrylamide (MBAM) are dissolved in the deionized water by 15: 1 weight ratio, be made into organism quality mark and be 20% premixed liquid; Mixed powder is added in the premixed liquid, adding content simultaneously is the dispersion agent D3005 of stock quality umber 0.5%, ball milling 5h in ball mill, ultrasonic dispersion processing 15min, obtain the disperse slurry, solid volume content is 65% in the slurry, and regulating the pH value with the concentrated hydrochloric acid of 20% strong aqua and 30% then is 9.5.
2) casting in the rotatingfield
With adding the concentration that accounts for stock quality 2% in the disperse slurry is the persulfuric acid aqueous solution initiator of 2wt.% and the Tetramethyl Ethylene Diamine catalyzer that accounts for stock quality 4 ‰, stirs back injected plastic mould, and mould applies rotatingfield outward.Rotatingfield is produced by electro-magnet, and sense of rotation vertical magnetic field direction, magneticstrength are 2.5T, and the magnetic field rotating speed is 70rpm, and magnetizing time is 5min.Mould adopts mould of plastics, and the mould inside die cavity is to be the disk of 15mm for 15mm, diameter highly.
3) gel, drying, compacting, sintering
Slurry is placed 70 ℃ baking oven gel 15min, then in drying at room temperature.Green compact are placed punching block, under the pressure of 0.4GPa, suppress.The green compact that obtain are sintering under argon shield.Temperature rise rate with 200 ℃/h is heated to 500 ℃ of insulation 2h, is heated to 1300 ℃ with 200 ℃/h then, insulation 2h.Cool to 300 ℃ of taking-ups with the furnace.
Example 5 prepared samples are carried out the electronic probe line analysis, find that its composition changes continuously, Co is 0% by 96% of a side to opposite side, and no macroscopic interface exists.To the thermal shock test that circulates of the sample of gained, through 120 circulations crackle does not appear under 800 ℃ of temperature difference, chilling condition.
Embodiment 6:
1) pulp preparation
Average particle size particle size is that rare earth permanent magnet and the average particle size particle size of 45 μ m is the SiO of 32 μ m 2Powder is formed mixed powder in proportion at 6: 1; Organic monomer acrylamide (AM) and linking agent methylene-bisacrylamide (MBAM) are dissolved in the deionized water by 10: 1 weight ratio, be made into organism quality mark and be 20% premixed liquid; Mixed powder is added in the premixed liquid, adding content simultaneously is the dispersion agent D3005 of stock quality umber 0.5%, ball milling 5h in ball mill, ultrasonic dispersion processing 15min, obtain the disperse slurry, solid volume content is 65% in the slurry, and regulating the pH value with the concentrated hydrochloric acid of 20% strong aqua and 30% then is 6.
2) casting in the rotatingfield
With adding the concentration that accounts for stock quality 2% in the disperse slurry is the persulfuric acid aqueous solution initiator of 2wt.% and the Tetramethyl Ethylene Diamine catalyzer that accounts for stock quality 4 ‰, stirs the back and injects mould, and mould applies rotatingfield outward.Rotatingfield is produced by electro-magnet, and sense of rotation vertical magnetic field direction, magneticstrength are 1.6T, and the magnetic field rotating speed is 100rpm, and magnetizing time is 10min.Mould adopts mould of plastics, and the mould inside die cavity is to be the disk of 15mm for 15mm, diameter highly.
3) gel, drying, compacting, sintering
Slurry is placed 70 ℃ baking oven gel 15min, then in drying at room temperature.Green compact are placed punching block, under the pressure of 0.2GPa, suppress.The green compact that obtain are sintering under argon shield.Temperature rise rate with 200 ℃/h is heated to 500 ℃ of insulation 2h, is heated to 1250 ℃ with 200 ℃/h then, insulation 2h.Cool to 300 ℃ of taking-ups with the furnace.
Example 5 prepared samples are carried out the electronic probe line analysis, find that its composition changes continuously, Co is 0% by 92% of a side to opposite side, and no macroscopic interface exists.To the thermal shock test that circulates of the sample of gained, through 120 circulations crackle does not appear under 800 ℃ of temperature difference, chilling condition.

Claims (9)

1, the gel injection moulding preparation of gradient material in the rotatingfield is characterized in that this method may further comprise the steps:
Step (1) pulp preparation
With particle size is that the ferromagnetic particle of 0.1~100 μ m and non-magnetic particle that particle size is 0.1~100 μ m are mixed into mixed powder by mass ratio 0.1~10:1; Organic monomer and linking agent are dissolved in the deionized water by the weight ratio of 6~24:1, be made into organism quality mark and be 10~25% premixed liquid; Mixed powder is added in the premixed liquid, add dispersion agent simultaneously, ball milling 1~10h in ball mill, ultrasonic dispersion processing 1~15min, obtain the disperse slurry, adopt 15~38% strong aquas and 15%~40% concentrated hydrochloric acid that the disperse slurry pH value is adjusted to 5~12, solid volume content is 50~70% in the slurry; Dispersant is 0.05%~0.50% of a stock quality;
Casting in step (2) rotatingfield
To add initiator and catalyzer in the disperse slurry, stir the back and inject mould, mould applies rotatingfield outward, and magneticstrength is 0.1~2.5T, and the magnetic field rotating speed is 10~300rpm, and magnetizing time is 3~60min; The initiator add-on is 0.3~3% of a stock quality, and the catalyzer add-on is 0.5 of stock quality~5 ‰;
Step (3) gel, drying, compacting, sintering
Slurry is placed baking oven gel 5~60min of 60~80 ℃, then in drying at room temperature; Green compact place punching block, suppress under the pressure of 0.1~1GPa; Take out green compact and put into sintering oven, charge into argon gas or nitrogen is protected, sintering temperature cools to 100~300 ℃ of taking-ups with the furnace between 600~1400 ℃.
2, the gel injection moulding preparation of gradient material in the rotatingfield as claimed in claim 1 is characterized in that: described ferromagnetic particle is one or more the mixture in Fe alloy, Co alloy, Ni alloy, rare earth permanent magnet, the ferrite powder.
3, the gel injection moulding preparation of gradient material in the rotatingfield as claimed in claim 1, it is characterized in that: described non-magnetic particle is ZrO 2, SiC, AlN, Si 3N 4, B 4C, SiO 2, TiC, Y 2O 3, Al 2O 3In one or more mixture.
4, the gel injection moulding preparation of gradient material in the rotatingfield as claimed in claim 1 is characterized in that: described dispersion agent is a kind of among ammonium polyacrylate, SD-38, JA-281, the D3005.
5, the gel injection moulding preparation of gradient material in the rotatingfield as claimed in claim 1 is characterized in that: described organic monomer is a kind of in acrylamide, Methacrylamide, the vinyl pyrrole ketone.
6, the gel injection moulding preparation of gradient material in the rotatingfield as claimed in claim 1, it is characterized in that: described linking agent is a methylene-bisacrylamide.
7, the gel injection moulding preparation of gradient material in the rotatingfield as claimed in claim 1 is characterized in that: described initiator is that massfraction is 1~5% the persulfuric acid aqueous solution, and described catalyzer is a Tetramethyl Ethylene Diamine.
8, the gel injection moulding preparation of gradient material in the rotatingfield as claimed in claim 1, it is characterized in that: described mould is steel, iron, glass or mould of plastics.
9, the gel injection moulding preparation of gradient material in the rotatingfield as claimed in claim 1 is characterized in that: described rotatingfield is the magnetic field that is produced by electro-magnet or permanent magnet, utilizes mechanism to make its rotation, and sense of rotation is perpendicular to field direction.
CN 200910096061 2009-02-06 2009-02-06 Gel injection moulding preparation for gradient material in rotating magnetic field Expired - Fee Related CN101503299B (en)

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