CN101503299B - 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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CN101503299B
CN101503299B CN 200910096061 CN200910096061A CN101503299B CN 101503299 B CN101503299 B CN 101503299B CN 200910096061 CN200910096061 CN 200910096061 CN 200910096061 A CN200910096061 A CN 200910096061A CN 101503299 B CN101503299 B CN 101503299B
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magnetic field
slurry
rotating magnetic
mould
powder
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CN101503299A (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 functionally gradient material (FGM) in the rotating magnetic field
Technical field
The present invention relates to the gel injection moulding preparation of functionally gradient material (FGM) in a kind of rotating magnetic field, belong to field of material preparation.
Background technology
Ceramic material has been widely used in industrial circles such as electronics, machinery, national defence because of its particular performances.But be difficult to carry out machine work behind the ceramic material 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 ceramic material generally can be divided into two big types of dry method and wet methods.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 the traditional wet forming technique, absorbs water by plaster mold like injection forming and realizes, cause to form density gradient distribution and inhomogeneous deformation in the base substrate, and blank strength is low, is easy to damage.Injection moulding or injection moulding need add mass fraction up to 20% wax or organic substance, cause skimming processes loaded down with trivial details, and the thawing of bond or evaporation reduce the intensity of base substrate, are prone to form defective even collapse.These problems have improved the production cost of ceramic material, have reduced its quality of stability.The beginning of the nineties; It is technological that U.S.'s Oak Ridge National Laboratory has been invented a kind of brand-new ceramic material wet moulding---and the gel casting forming technology, 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 ceramic materials, the ceramic part of various complicated shapes of moulding and size.(2) operation separates fully because type-approval process is with injection molding, and 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.Addition according to polymerization temperature and catalyst 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 specific (special) requirements, can be metal, glass or plastics etc.(5) content of organics 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 machine work (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 body 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 concentration 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.
FGM (FGM) is under the condition to high temperature, thermal cycle and big temperature fall, operate as normal and one type of new material developing times without number, and so harsh environment for use requires material to have excellent heat shock resistance and thermal fatigue property.At present, the FGM main preparation methods has powder compacting, physical vaporous deposition (PVD), chemical vapour deposition technique (CVD), plasma spraying, electrocasting, galvanoplastic 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 process FGM.Heat-stable ceramic is used for temperature end, and metal material or plastics are used for low-temperature end.Form mutually or raising ceramic phase toughness for reinforced metal, can mix whisker.Chemical vapour deposition technique is that halide gas is carried out heating and decomposition, and metal or semimetal are deposited on the substrate surface, perhaps mists such as the carbide that generates, chloride is sent into reaction tube, and the compound that heating is generated is deposited on the substrate.Electrocasting is on the parent form surface, to separate out layer of metal or alloy with metal salt solution through electrodeposition process. peels off then and obtains and establish the opposite goods of type surface convex-concave.Physical vaporous deposition is to make the Metal Deposition of heating evaporation on substrate, carry out the method for coating, in metal, semimetal, send into reacting gass such as oxygen, nitrogen and hydrocarbon after, potteries such as synthesis oxide, chloride and carbide, and being deposited on the substrate.Physical vaporous deposition has vacuum coating, sputter and ion plating etc.Vacuum coating is that merely heating of metal makes its hydatogenesis; Sputtering method is to hit through electronics or ion, makes the Metal Deposition that sputters out on substrate; The ion plating is through the metal vapors ionization, obtains the good and fine and close deposit of caking property.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 like 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 functionally gradient material (FGM) further develops.Therefore, if can the metal or the ceramic forming material means of maturation be used for preparing FGM, have great importance undoubtedly and vast potential for future development.
Summary of the invention
The objective of the invention is deficiency, the gel injection moulding preparation of functionally gradient material (FGM) in a kind of rotating magnetic field is provided to prior art.
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 crosslinking agent by 6~24: 1 weight ratio is dissolved in the deionized water, is made into organic substance quality mark and is 10~25% premixed liquid; Mixed-powder is added in the premixed liquid; Add dispersant simultaneously; Ball milling 1~10h in ball mill, ultrasonic dispersion processing 1~15min obtains the disperse slurry; Adopt 15~38% concentrated ammonia liquors 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 dispersant 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 crosslinking agent is a methylene-bisacrylamide.
Moulding by casting in step (2) rotating magnetic field
With adding initator and catalyst in the disperse slurry, stir the back and inject mould, mould applies rotating magnetic field outward, and magnetic field intensity is 0.1~2.5T, and the magnetic field rotating speed is 10~300rpm, and magnetizing time is 3~60min; The initator addition is 0.3~3% of a stock quality, and the catalyst addition is 0.5 of stock quality~5 ‰.
Described initator is that mass fraction is 1~5% the persulfuric acid aqueous solution.
Described catalyst is a tetramethylethylenediamine.
Described mould is steel, iron, glass or mould of plastics.
Described rotating magnetic field is the magnetic field that is produced by electromagnet or permanent magnet, utilizes mechanical device to make its rotation, and direction of rotation is perpendicular to magnetic 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, in the pressure pressed of 0.1~1GPa.Take out green compact and put into sintering furnace, 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 rotating magnetic field control magnetic constituent element on the basis of gel injection-moulding technology, successfully prepared the continuous functionally gradient material (FGM) of composition.The present invention is with the slurry of ferromagnetic substance and weak magnetic substance composition, in rotating magnetic field, adopts the fixed shaping of casting method of condensing, compacting, and sintering prepares functionally gradient material (FGM) then.Magnetic particle in the slurry receives the constraint of magnetic force in magnetic field, therefore when magnetic field rotated, also direction of rotation moved magnetic particle along magnetic field, thereby forms magnetic field gradient along direction of rotation.Compare with preparation functionally gradient material (FGM) under the magnetostatic field, utilize rotating magnetic field, in functionally gradient material (FGM), obtain big component gradient more easily magnetic constituent element constraint control.Simultaneously, through adjustment magnetic field intensity, magnetic field rotating speed and the action of a magnetic field time can controlling magnetic field to the restraining force of magnetic constituent element, the further component distributing in the control material.
Advantage of the present invention is:
1) through applying rotating magnetic field, change magnetic field intensity, magnetic field rotating speed and the action of a magnetic field time, can in very big composition range, prepare the functionally gradient material (FGM) of all thickness, composition changes continuously and is controlled.
2) magnetic particle receives the constraint of magnetic force in magnetic field, and therefore when magnetic field rotated, also direction of rotation moved magnetic particle along magnetic field, thereby forms magnetic field gradient along direction of rotation.Prepare FGM down with magnetostatic field and compare, rotating magnetic field is stronger to the restraining force of magnetic particle, and particle receives magnetically confined and lax effect repeatedly simultaneously, prepares the functionally gradient material (FGM) of various component distributing more easily.
3) utilize ripe gel injection-moulding technology that the simplified working procedures of preparation functionally gradient material (FGM), cost 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 crosslinking agent methylene-bisacrylamide (MBAM) are dissolved in the deionized water by 6: 1 weight ratio, be made into organic substance quality mark and be 10% premixed liquid; Mixed-powder is added in the premixed liquid; Adding content simultaneously is the dispersant ammonium polyacrylate of stock quality mark 0.05%; Ball milling 1h in ball mill, ultrasonic dispersion processing 1min obtains the disperse slurry; Solid volume content is 50% in the slurry, and using the concentrated hydrochloric acid of 15% concentrated ammonia liquor and 15% to regulate the pH value then is 5.0.
2) casting in the rotating magnetic field
With adding the persulfuric acid aqueous solution initator and the tetramethylethylenediamine catalyst that accounts for stock quality 0.5 ‰ that the concentration that accounts for stock quality 0.3% is 1wt.% in the disperse slurry, stir the back and inject mould, mould applies rotating magnetic field outward.Rotating magnetic field is produced by electromagnet, and direction of rotation vertical magnetic field direction, magnetic field intensity 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, in the pressure pressed of 0.1GPa.Sintering green compact under the protection environment of argon gas.Heating 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.
Instance 1 prepared sample is carried out the electron microprobe 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 crosslinking agent methylene-bisacrylamide (MBAM) are dissolved in the deionized water by 15: 1 weight ratio, be made into organic substance quality mark and be 20% premixed liquid; Mixed-powder is added in the premixed liquid; Adding content simultaneously is the dispersant SD-38 of stock quality umber 0.2%; Ball milling 6h in ball mill, ultrasonic dispersion processing 8min obtains the disperse slurry; Solid volume content is 65% in the slurry, and using the concentrated hydrochloric acid of 25% concentrated ammonia liquor and 30% to regulate the pH value then is 8.2.
2) casting in the rotating magnetic field
With adding the persulfuric acid aqueous solution initator and the tetramethylethylenediamine catalyst that accounts for stock quality 3 ‰ that the concentration that accounts for stock quality 2% is 3wt.% in the disperse slurry, stir the back and inject mould, mould applies rotating magnetic field outward.Rotating magnetic field is produced by electromagnet, and direction of rotation vertical magnetic field direction, magnetic field intensity 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, in the pressure pressed of 0.4GPa.The green compact that obtain are sintering under nitrogen protection.Heating 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.
Instance 2 prepared samples are carried out the electron microprobe 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 crosslinking agent methylene-bisacrylamide (MBAM) are dissolved in the deionized water by 24: 1 weight ratio, be made into organic substance quality mark and be 25% premixed liquid; Mixed-powder is added in the premixed liquid; Adding content simultaneously is the dispersant JA-281 of stock quality umber 0.5%; Ball milling 10h in ball mill, ultrasonic dispersion processing 15min obtains the disperse slurry; Solid volume content is 70% in the slurry, and using the concentrated hydrochloric acid of 38% concentrated ammonia liquor and 40% to regulate the pH value then is 12.
2) casting in the rotating magnetic field
With adding the persulfuric acid aqueous solution initator and the tetramethylethylenediamine catalyst that accounts for stock quality 5 ‰ that the concentration that accounts for stock quality 3% is 5wt.% in the disperse slurry, stir the back and inject mould, mould applies rotating magnetic field outward.Rotating magnetic field is produced by the magnetic circuit that a pair of NdFeB permanent magnet constitutes, and direction of rotation vertical magnetic field direction, magnetic field intensity 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, in the pressure pressed of 1GPa.The green compact that obtain are sintering under nitrogen protection.Heating 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.
Instance 3 prepared samples are carried out the electron microprobe 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 crosslinking agent methylene-bisacrylamide (MBAM) are dissolved in the deionized water by 16: 1 weight ratio, be made into organic substance quality mark and be 15% premixed liquid; Mixed-powder is added in the premixed liquid; Adding content simultaneously is the dispersant D3005 of stock quality umber 0.3%; Ball milling 6h in ball mill, ultrasonic dispersion processing 8min obtains the disperse slurry; Solid volume content is 60% in the slurry, and using the concentrated hydrochloric acid of 38% concentrated ammonia liquor and 15% to regulate the pH value then is 10.
2) casting in the rotating magnetic field
With adding the persulfuric acid aqueous solution initator and the tetramethylethylenediamine catalyst that accounts for stock quality 2 ‰ that the concentration that accounts for stock quality 2% is 2wt.% in the disperse slurry, stir the back and inject mould, mould applies rotating magnetic field outward.Rotating magnetic field is produced by the magnetic circuit that a pair of NdFeB permanent magnet constitutes, and direction of rotation vertical magnetic field direction, magnetic field intensity 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, in the pressure pressed of 0.2GPa.The green compact that obtain are sintering under nitrogen protection.Heating 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.
Instance 4 prepared samples are carried out the electron microprobe 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 crosslinking agent methylene-bisacrylamide (MBAM) are dissolved in the deionized water by 15: 1 weight ratio, be made into organic substance quality mark and be 20% premixed liquid; Mixed-powder is added in the premixed liquid; Adding content simultaneously is the dispersant D3005 of stock quality umber 0.5%; Ball milling 5h in ball mill, ultrasonic dispersion processing 15min obtains the disperse slurry; Solid volume content is 65% in the slurry, and using the concentrated hydrochloric acid of 20% concentrated ammonia liquor and 30% to regulate the pH value then is 9.5.
2) casting in the rotating magnetic field
With adding the persulfuric acid aqueous solution initator and the tetramethylethylenediamine catalyst that accounts for stock quality 4 ‰ that the concentration that accounts for stock quality 2% is 2wt.% in the disperse slurry, stir back injected plastic mould, mould applies rotating magnetic field outward.Rotating magnetic field is produced by electromagnet, and direction of rotation vertical magnetic field direction, magnetic field intensity 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, in the pressure pressed of 0.4GPa.The green compact that obtain are sintering under argon shield.Heating 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.
Instance 5 prepared samples are carried out the electron microprobe 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 crosslinking agent methylene-bisacrylamide (MBAM) are dissolved in the deionized water by 10: 1 weight ratio, be made into organic substance quality mark and be 20% premixed liquid; Mixed-powder is added in the premixed liquid; Adding content simultaneously is the dispersant D3005 of stock quality umber 0.5%; Ball milling 5h in ball mill, ultrasonic dispersion processing 15min obtains the disperse slurry; Solid volume content is 65% in the slurry, and using the concentrated hydrochloric acid of 20% concentrated ammonia liquor and 30% to regulate the pH value then is 6.
2) casting in the rotating magnetic field
With adding the persulfuric acid aqueous solution initator and the tetramethylethylenediamine catalyst that accounts for stock quality 4 ‰ that the concentration that accounts for stock quality 2% is 2wt.% in the disperse slurry, stir the back and inject mould, mould applies rotating magnetic field outward.Rotating magnetic field is produced by electromagnet, and direction of rotation vertical magnetic field direction, magnetic field intensity 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, in the pressure pressed of 0.2GPa.The green compact that obtain are sintering under argon shield.Heating 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.
Instance 5 prepared samples are carried out the electron microprobe 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 (2)

1. the gel injection moulding preparation of functionally gradient material (FGM) in the rotating magnetic field is characterized in that this method may further comprise the steps:
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 crosslinking agent by 6~24: 1 weight ratio is dissolved in the deionized water, is made into organic substance quality mark and is 10~25% premixed liquid; Mixed-powder is added in the premixed liquid; Add dispersant simultaneously; Ball milling 1~10h in ball mill, ultrasonic dispersion processing 1~15min obtains the disperse slurry; Adopt 15~38% concentrated ammonia liquors 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;
Moulding by casting in step (2) rotating magnetic field
With adding initator and catalyst in the disperse slurry, stir the back and inject mould, mould applies rotating magnetic field outward, and magnetic field intensity is 0.1~2.5T, and the magnetic field rotating speed is 10~300rpm, and magnetizing time is 3~60min; The initator addition is 0.3~3% of a stock quality, and the catalyst addition is 0.5 of stock quality~5 ‰;
Described rotating magnetic field is the magnetic field that is produced by electromagnet or permanent magnet, utilizes mechanical device to make its rotation, and direction of rotation is perpendicular to magnetic 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, in the pressure pressed of 0.1~1GPa; Take out green compact and put into sintering furnace, charge into argon gas or nitrogen is protected, sintering temperature cools to 100~300 ℃ of taking-ups with the furnace between 600~1400 ℃;
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 dispersant is a kind of among ammonium polyacrylate, JA-281, the D3005;
Described organic monomer is a kind of in acrylamide, Methacrylamide, the vinyl pyrrole ketone;
Described crosslinking agent is a methylene-bisacrylamide;
Described initator is that mass fraction is 1~5% the persulfuric acid aqueous solution;
Described catalyst is a tetramethylethylenediamine.
2. the gel injection moulding preparation of functionally gradient material (FGM) in the rotating magnetic field as claimed in claim 1 is characterized in that: described mould is steel, iron, glass or mould of plastics.
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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