CN1915626B - Method for preparing gradient material of strong magnetism and weak magnetism through flow casting molding in pulse magnetism - Google Patents

Method for preparing gradient material of strong magnetism and weak magnetism through flow casting molding in pulse magnetism Download PDF

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CN1915626B
CN1915626B CN2006100532507A CN200610053250A CN1915626B CN 1915626 B CN1915626 B CN 1915626B CN 2006100532507 A CN2006100532507 A CN 2006100532507A CN 200610053250 A CN200610053250 A CN 200610053250A CN 1915626 B CN1915626 B CN 1915626B
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magnetic field
slurry
gradient material
pulsed
weak
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CN1915626A (en
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彭晓领
严密
马天宇
罗伟
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Zhejiang University ZJU
Hengdian Group DMEGC Magnetics Co Ltd
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Zhejiang University ZJU
Hengdian Group DMEGC Magnetics Co Ltd
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Abstract

A doctor blading process for preparing strong magnetic-weak magnetic gradient material in pulse magnetic field includes such steps as proportionally mixing ceramic powder, strong magnetic metal powder, organic solvent and additive, ball grinding, doctor blading to become film, baking, and sintering.

Description

Strong magnetic-weak magnetic gradient material tape casting preparation in the pulsed magnetic field
Technical field
The present invention relates to strong magnetic-weak magnetic gradient material tape casting preparation in a kind of pulsed magnetic field.
Background technology
The tape casting (also claiming the scraper method of forming) is a kind of important forming method for preparing large tracts of land, Boping ceramic material, and technology comprises pulp preparation, ball milling, moulding, drying, peels off processes such as base band.The characteristics of this technology are that equipment is simple, process stabilizing, but continued operation, and the production efficiency height can be realized increasingly automated.Flow casting molding is the thickness of controlling diaphragm easily, helps the membrane material of different components and thickness is designed and structure regulating, to obtain special performances.In recent decades, the application study of The tape casting forming technique has obtained remarkable progress, is applied to many fields such as electronics industry, the energy, comprises the Al of all thickness 2O 3Ic substrate and gasket material, BaTiO 3Capacitor dielectric material, ZrO 2Solid electrolyte fuel cell, oxygen pump and lambda sensor etc.In addition, casting molding processes also can be used for industries such as papermaking, plastics and coating.
Casting technique comprises two kinds of water-based tape casting and non-aqueous tape-castings.Non-aqueous tape-casting technology comparative maturity, the diaphragm structure of preparation is even, the intensity height, pliability is good, uses for many years in industrial production.But the curtain coating process need uses large amount of organic, and the production cost height causes environmental pollution after the discharging.The water-based tape casting cost is low, pollutes for a short time, and Environmental compatibility is good, and still, the influencing factor of this technology is many.Usually, in ceramic powder, to add organic principles such as solvent, dispersant, binding agent, plastic agent, make finely dispersed stable slurry, on casting machine, make certain thickness plain embryophoric membrane again.Plain embryophoric membrane makes the product that burn till that meet desirable characteristics by dry, sintering.
The major advantage of The tape casting moulding process has: (1) for chemistry forming methods such as EVD, CVD, the prices of raw and semifnished materials are cheap and cost of manufacture is low; (2) compare the fine and close and mechanical strength height of prepared material structure with dry pressing; (3) defective of material is few; (4) reduce the hot pressed sintering time, even can cancel hot pressing; (5) can make the laminated composite materials that different component film materials constitute, to satisfy property requirement to material.
The principal character of Functionally Graded Materials is that component structure and physical parameter change continuously, and main preparation methods has that powder compacting, vapour deposition process, self-propagating reaction are synthetic, plasma spraying, electrocasting, galvanoplastic, laser sintered and centrifugal casting etc.These preparation methods require complicated technology or equipment, need change material composition or technological parameter constantly mostly in preparation process.Lacking simple and convenient preparation method, is the major reason that the limitation function functionally gradient material (FGM) further develops.
At present,, comprise proving to have good thermal stress slow release effect, testing the ZrO at high temperature difference positions such as being used for rocket chamber inwall, nuclear reactor and engine inlet for many important function functionally gradient material (FGM)s 2/ Ni, ZrO 2/ steel, Al 2O 3/ Ni, SiC/ α phase stainless steel etc., metal constituent element Fe, transition metal such as Ni, Co belong to ferromagnetic substance, and ceramic constituent element Al 2O 3, ZrO 2, SiC, AlN, Si 3N 4Deng being weak magnetic substance.Ferromagnetic substance has ferromagnetism below Curie temperature, and weak magnetic substance is insensitive to magnetic field.Utilize the difference of magnetic property between metal and the ceramic constituent element, our group adopted doctor-blade casting process successfully to prepare functionally gradient material (FGM) in magnetostatic field in 2003.This technology has been authorized patent of invention.
In the past few years, our group updates on original experiment basis, and makes a breakthrough.At present, we have successfully adopted doctor-blade casting process to prepare functionally gradient material (FGM) in pulsed magnetic field.The present invention is with the pottery (Al of ferromagnetic metal (transition metal such as Fe, Ni, Co) with weak magnetic 2O 3, ZrO 2, SiC, AlN, Si 3N 4) slurry formed, in pulsed magnetic field, adopting the fixed shaping of doctor-blade casting process, sintering prepares strong magnetic-weak magnetic gradient material then.Compare with preparation functionally gradient material (FGM) under the magnetostatic field, utilize the easier realization of pulsed magnetic field big magnetic field intensity and magnetic field gradient, and particle is subjected to the reinforcement and lax effect repeatedly, easier strong magnetic-weak magnetic gradient material of preparing various gradients of magnetic force under pulsed magnetic field.
Outstanding advantage of the present invention utilizes ceramic flow casting molding method to produce strong magnetic-weak magnetic gradient material exactly, by adjusting magnetic field intensity, magnetic field gradient, slurry composition, viscosity and other preparation technology parameter, can prepare composition easily and change continuously and controlled functionally gradient material (FGM) in very big thickness range, cost greatly reduces.
Summary of the invention
The purpose of this invention is to provide strong magnetic-weak magnetic gradient material tape casting preparation in a kind of pulsed magnetic field.
Its step is:
1) pulp preparation
With particle size is ferromagnetism nickel powder or the cobalt powder of 0.1~100 μ m, with particle size be 0.1~100
The ZrO of μ m 2, SiC, AlN, Si 3N 4, B 4C, SiO 2, TiC, Al 2O 3In one or more mix by weight ratios of 0.1~10: 1, add organic solvent, dispersant, plastic agent, binding agent, ball milling 5~30h in ball mill; Add plastic agent and binding agent, ball milling 10~40h again in ball mill, ultrasonic dispersion processing 1~15min, vacuum degassing obtains the disperse slurry, and slurry viscosity is 1~100mPas, and the pH value is 5~12;
2) flow casting molding in the pulsed magnetic field
The disperse slurry is injected casting machine, and the height of scraper is 0.4~1.0mm, and control curtain coating motor speed is 0.5~5cm/s, do substrate with refractory ceramics during curtain coating, discontinuity applies pulsed magnetic field at the substrate place, and magnetic field intensity is 0.1~5.0T, and magnetic field gradient is 0.1~50T/m;
3) drying and sintering
20~30 ℃ of baking temperatures, relative humidity is 30~60%, plain flake thickness degree 0.1~0.5mm behind the slurry drying.Carry out sintering after drying is finished, sintering is in graphite or protection of nitrogen gas environment, and control sintering heating rate is 0.2~2 ℃/min; at 150~600 ℃ of insulation 1~5h; be heated to 1200~1400 ℃ again, insulation 1~3h cools to 100~400 ℃ of taking-ups at last with the furnace.
Described pulsed magnetic field is the magnetic field that the pulse current that utilizes capacitor to spark to produce produces by coil.Organic solvent is one or more in ethanol, methylethylketone, butanone or the trichloroethylene.Ethanol and methylethylketone, trichloroethylene and methylethylketone, trichloroethylene and ethanol or butanone and ethanol are by 0.1~10: 1 mixed.Organic solvent volume fraction in the disperse slurry is 20~60% of a slurry.Dispersant is herring oil, phosphate, olein or triethanolamine.Dispersant in the disperse slurry is 0.2~5% of a slurry volume mark.Bonding agent is polyvinyl butyral resin or polyvinyl alcohol.Plastic agent is one or more in glycerine, dioctyl phthalate, polyethylene glycol or the phthalic acid.Bonding agent in the disperse slurry is 10~30% of a stock quality mark; Binding agent/plastic agent weight ratio is 0.5~1.0.
Advantage of the present invention is:
1) by applying pulsed magnetic field, changes magnetic field intensity and magnetic field gradient, can in very big composition range, prepare the strong magnetic-weak magnetic gradient material of large tracts of land, Boping.
2) prepare Functionally Graded Materials down with magnetostatic field and compare, particle is subjected to the reinforcement and lax effect repeatedly, easier strong magnetic-weak magnetic gradient material of preparing various gradients of power under the pulsed magnetic field.
3) utilize ripe traditional ceramics technology The tape casting that the formality simplification of production function-graded material, cost are reduced.
Description of drawings
Fig. 1 is that flow casting molding prepares strong magnetic-weak magnetic gradient material technology schematic diagram in the magnetic field, among the figure, and the pulsed magnetic field 7 that casting machine 1, slurry 2, controlled scraper open height 3, curtain coating thin layer 4, refractory ceramics substrate 5, pulsed coil 6, coil produce;
Fig. 2 is a magnetization back curtain coating thin film model schematic diagram, among the figure, and ceramic size 8, ferromagnetism slurry 9 refractory ceramics substrates 10.
Embodiment
Strong magnetic of the present invention-weak magnetic gradient material preparation method is with ferromagnetic metal (in nickel powder, the cobalt powder a kind of) and pottery (ZrO 2, SiC, AlN, Si 3N 4, B 4C, SiO 2, TiC, Al 2O 3In one or more) mixed-powder and organic solvent form slurry, curtain coating is to the refractory ceramics substrate, the substrate place applies magnetic field.Slurry is subjected to the effect of magnetic force, builds up to two ends in mould respectively, forms component gradient, makes strong magnetic-weak magnetic gradient material behind the blank drying of acquisition, the sintering.The strong magnetic of this kind-weak magnetic gradient material has excellent heat shock resistance and thermal fatigue property.
The present invention adopts concrete steps as follows:
1) pulp preparation
Adopting particle size is ferromagnetism nickel powder, the cobalt powder of 0.1~100 μ m, with particle size be the ZrO of 0.1~100 μ m 2, SiC, AlN, Si 3N 4, B 4C, SiO 2, TiC, Al 2O 3In one or more ceramic powders in 0.1~10: 1 ratio is formed mixed-powder, adds a kind of in organic solvent ethanol, methylethylketone, butanone, the trichloroethylene.Organic solvent viscosity is low, boiling point is high, vapour pressure is high, and is more volatile than the water capacity, and drying time is short, is applicable to very much flow casting molding.But consider that from the electrical property aspect organic dielectric constant is low, the lyate ion degree is also lower, and Coulomb repulsion is also less to the stabilization of slurry.In order to obtain more lower boiling solvent, and organic additive there is higher solubility, usually use mixed solvent and azeotropic mixed solvent, mixed solvent commonly used has ethanol/methylethylketone, trichloroethylene/methylethylketone, trichloroethylene/ethanol, butanone/ethanol etc. by 0.1~10: 1 mixed, and add dispersant, plastic agent, binding agent.Dispersant is herring oil, phosphate, olein, triethanolamine etc., plastic agent is glycerine, dioctyl phthalate, polyethylene glycol (PEC), phthalic acid (PHT) etc., and binding agent is polyvinyl butyral resin (PVB), polyvinyl alcohol (PVA).General organic solvent and the dispersant of in powder, adding earlier, in ball mill, stir 5~30h mixing after, add plastic agent and binding agent again, subsequently slurry is stirred 10~40h in ball mill, make the slurries of even dispersion.Mainly be that dispersant is difficult for desorb after being adsorbed on particle surface earlier, thereby makes the slurry dispersion effect good because binding agent and dispersant are to being adsorbed with between competitiveness of powder granule.The solvent volume mark is 20~60% of a slurry in this slurry, and bonding agent is 10~30% of a stock quality mark, and binding agent/plastic agent weight ratio is 0.5~1.2, and dispersant is 0.2~5% of a slurry volume mark.And with ultrasonic wave slurry is carried out disperse processing 1~15min, through vacuum degassing, remove bubble after, slurry promptly can be used for flow casting molding, viscosity is 1~100mPas, the pH value is 5~12, temperature is 30~60 ℃.
2) flow casting molding in the pulsed magnetic field
Flow casting molding is to adopt doctor-blade casting process to prepare the critical process of strong magnetic-weak magnetic gradient material in pulsed magnetic field in the pulsed magnetic field.Slurry is injected in the casting machine, ambient temperature is under 25~28 ℃ of conditions during curtain coating, the height of scraper is controlled at 0.4~1.0mm, it is 0.5~5cm/s that the control casting machine makes its movement velocity, do substrate with refractory ceramics in the curtain coating process, the substrate place applies pulsed magnetic field, and magnetic field intensity is 0.1~5.0T, magnetic field gradient is 0.1~50T/m, and magnetizing time is 1~20min.Pulsed magnetic field is produced by solenoid coil by pulse current.
Be subjected to the effect of magnetic force, the magnetic constituent element is poly-partially to specific direction, forms component gradient.In pulsed magnetic field, the ferromagnetic metal particle is magnetized and Xiang Yiduan attracts, and weak magnetic ceramics particle is then driven to the other end under the barometric gradient effect.Weaken pulsed magnetic field intensity and magnetic field gradient, component gradient reduces.Improve pulsed magnetic field intensity and magnetic field gradient, component gradient then increases, and is 100% metal until an end, and the other end is 100% pottery.Under the effect of pulsed magnetic field, magnetic field intensity and magnetic field gradient are when smaller value increases, and metal and ceramic particle are built up to two ends respectively in mould.Adjust magnetic field intensity at 0.1~5.0T, magnetic field gradient is controlled magnetizing time 1~20min in the OK range of 0.1~50T/m, obtains the sample of required component gradient.
3) dry, sintering
The slurry drying temperature is 20~30 ℃, and envionmental humidity is 30~60%, and it is 0.1~0.5mm that slurry is done the plain flake thickness degree in back, and the control heating rate is 0.2~2 ℃/min, and at 150~600 ℃ of insulation 1~5h, all sloughs to guarantee organic additive.Continue to be heated to 1200~1400 ℃ subsequently, insulation 1~3h cools to 100~400 ℃ of taking-ups with the furnace.Be anti-oxidation, sintering in protective atmosphere.
The large tracts of land that can prepared composition in very large range changes by the present invention, the strong magnetic-weak magnetic gradient material of Boping.The finished product internal flaw is few, and structure closely has excellent heat shock resistance and thermal fatigue property.
Embodiment 1:
1) average particle size particle size is that nickel by powder and the average particle size particle size of 20 μ m are the Al of 9 μ m 2O 3Powder is formed mixed-powder in proportion at 1: 2, adds mixed solvent, and mixed solvent is that trichloroethylene and ethanol mixed by 1: 1, and adding dispersant olein, with above raw material mixing and ball milling 30h, add binding agent PVB then, plastic agent glycerine and dioctyl phthalate.Bonding agent is 30% of a stock quality mark, and binding agent/plastic agent weight ratio is 0.6.Ball milling slurry 36h again with ultrasonic dispersion 5min, through vacuum degassing, removes the slurry of making even dispersion behind the bubble.The solvent volume mark is 50% of a slurry in this slurry, and dispersant is 3% of a slurry volume mark, and slurry viscosity is 60mPas, and the pH value is 5.7, and temperature is 32 ℃.
2) ambient temperature is 28 ℃ during curtain coating, the curtain coating speed that adopts is 1.0cm/s, the height of scraper is controlled at 0.5mm, do substrate with refractory ceramics in the curtain coating process, the substrate place applies pulsed magnetic field, pulsed magnetic field is produced by solenoid coil by pulse current, and magnetic field intensity is 0.5T, and magnetic field gradient is 4T/m.
3) the slurry drying temperature is 24 ℃, and relative humidity is 40%, and it is 0.2mm that slurry is done the plain flake thickness degree in back.Sintering green compact under nitrogen protection, the control heating rate is 0.5 ℃/min, and at 400 ℃ of insulation 3h, is heated to 1200 ℃ with 100 ℃/h subsequently, insulation 1h cools to 200 ℃ of taking-ups with the furnace.
Prepared sample tissue densification, porosity is low, and the surface ratio of film is more smooth.Example 1 prepared sample is carried out the electron microprobe line analysis, and composition changes continuously, and no macroscopic interface exists, and Ni content reduces to 0% of opposite side by 94% of a side.Carry out thermal shock resistance experiment circulation 50 times between room temperature and 1000K, sample does not have breakage.
Embodiment 2:
1) choosing Co powder and the average particle size particle size that average particle size particle size is 14 μ m is the ZrO of 12.2 μ m 2Powder is formed mixed-powder in proportion at 1: 2, adds mixed solvent.Mixed solvent is methylethylketone and ethanol, mixes by 1: 1, and adds the dispersant triethanolamine, will add binding agent PVB, plastic agent polyethylene glycol (PEC) and phthalic acid (PHT) behind the above raw material mixing and ball milling 30h.Bonding agent is 30% of a stock quality mark, and binding agent/plastic agent weight ratio is 0.8.Ball milling 36h disperses 3min with ultrasonic wave again, through vacuum degassing, removes the slurry of making even dispersion behind the bubble.The solvent volume mark is 60% of a slurry in this slurry, and dispersant is 2% of a slurry volume mark, and slurry viscosity is 40mPas, and the pH value is 6.2, and temperature is 30 ℃.
2) ambient temperature is 28 ℃ during curtain coating, and the curtain coating speed of employing is 1.0cm/s, and the height of scraper is controlled at 0.8mm.Do substrate with refractory ceramics in the curtain coating process, the substrate place applies pulsed magnetic field, and pulsed magnetic field is produced by solenoid coil by pulse current, and magnetic field intensity is 0.7T, and magnetic field gradient is 6T/m.
3) the slurry drying temperature is 24 ℃, and relative humidity is 40%, and it is 0.3mm that slurry is done the plain flake thickness degree in back.Sintering green compact under nitrogen protection, the control heating rate is 0.3 ℃/min, and at 500 ℃ of insulation 2h.Be heated to 1200 ℃ with 100 ℃/h, insulation 2h cools to 200 ℃ of taking-ups with the furnace.
Prepared sample tissue densification, porosity is low, the surfacing of film.Example 2 prepared samples are carried out the electron microprobe line analysis, and composition changes continuously, and it is 0% that the Co powder reduces to opposite side by 96% of a side, and no macroscopic interface exists.Carry out thermal shock resistance experiment circulation 50 times between room temperature and 1000K, sample does not have breakage.
Embodiment 3:
1) choosing average particle size particle size is that the Co powder average particle size particle size of 16 μ m is the TiC powder of 28 μ m, forms mixed-powder in proportion at 1: 1, adds mixed solvent.Mixed solvent is that trichloroethylene and methylethylketone were mixed by 1: 1, and adds dispersant herring oil.With above raw material mixing and ball milling 30h, add binding agent PVB then, plastic agent glycerine.Bonding agent is 20% of a stock quality mark, and binding agent/plastic agent weight ratio is 0.8, ball milling 30h again.With ultrasonic dispersion 5min.Through vacuum degassing, remove bubble after, make the slurry of even dispersion.The solvent volume mark is 50% of a slurry in this slurry, and dispersant is 2% of a slurry volume mark, and slurry viscosity is 80mPas, and the pH value is 7, and temperature is 30 ℃.
2) ambient temperature is 23 ℃ during curtain coating, the curtain coating speed that adopts is 0.8cm/s, the height of scraper is controlled at 0.8mm, do substrate with refractory ceramics in the curtain coating process, the substrate place applies pulsed magnetic field, pulsed magnetic field is produced by solenoid coil by pulse current, and magnetic field intensity is 0.5T, and magnetic field gradient is 4T/m.
3) the slurry drying temperature is 24 ℃, and relative humidity is 30%, and it is 0.3mm that slurry is done the plain flake thickness degree in back.Sintering green compact under the powdered graphite protection, the control heating rate is 0.5 ℃/min, and at 400 ℃ of insulation 2h, is heated to 1300 ℃ with 100 ℃/h, insulation 2h.Cool to 200 ℃ of taking-ups with the furnace.
Prepared sample tissue densification, porosity is low, the surfacing of film.Example 3 prepared samples are carried out the electron microprobe line analysis, and porosity is low, and composition changes continuously.The Co powder reduces to 0% of opposite side by 16% of a side, and no macroscopic interface exists.Carry out thermal shock resistance experiment circulation 50 times between room temperature and 1000K, sample does not have breakage.
Embodiment 4:
1) choosing nickel by powder and the average particle size particle size that average particle size particle size is 20 μ m is the ZrO of 12.2 μ m 2Powder is formed mixed-powder in proportion at 1: 1, adds mixed solvent.Mixed solvent is mixing by 1: 1 of butanone and ethanol, and adds the dispersant phosphate, with above raw material mixing and ball milling 30h, adds binding agent PVB then, plastic agent polyethylene glycol (PEC) and phthalic acid (PHT).Bonding agent is 30% of a stock quality mark, and binding agent/plastic agent weight ratio is 0.8.Ball milling 36h again, slurry be with ultrasonic dispersion 3min, through vacuum degassing, removes the slurry of making even dispersion behind the bubble.The solvent volume mark is 60% of a slurry in this slurry, and dispersant is 2% of a slurry volume mark, and slurry viscosity is 30mPas, and the pH value is 6.2, and temperature is 30 ℃.
2) ambient temperature is 28 ℃ during curtain coating, and the curtain coating speed of employing is 1.0cm/s, and the height of scraper is controlled at 1mm, does substrate with refractory ceramics in the curtain coating process.The substrate place applies pulsed magnetic field, and pulsed magnetic field is produced by solenoid coil by pulse current, and magnetic field intensity is 0.8T, and magnetic field gradient is 7T/m.
3) the slurry drying temperature is 24 ℃, and relative humidity is 40%, and it is 0.4mm that slurry is done the plain flake thickness degree in back.Sintering green compact under the powdered graphite protection, the control heating rate is 0.5 ℃/min, and at 500 ℃ of insulation 2h.Be heated to 1300 ℃ with 100 ℃/h again, insulation 2h.Cool to 200 ℃ of taking-ups with the furnace.
Prepared sample tissue densification, porosity is low, the surfacing of film.Example 4 prepared samples are carried out the electron microprobe line analysis, and porosity is low, and composition changes continuously.The Ni powder reduces to 0% of opposite side by 94% of a side, and no macroscopic interface exists.Carry out thermal shock resistance experiment circulation 50 times between room temperature and 1000K, sample does not have breakage.
Embodiment 5:
1) choosing average particle size particle size is that the equal particle size of Co powder peace of 16 μ m is the Si of 9 μ m 3N 4Powder is formed mixed-powder in proportion at 1: 1, adds mixed solvent.Mixed solvent is methylethylketone and ethanol, mixes by 1: 1, and adds the dispersant triethanolamine.With above raw material mixing and ball milling 30h, add binding agent PVB then, plastic agent polyethylene glycol (PEC) and phthalic acid (PHT).Bonding agent is 30% of a stock quality mark, and binding agent/plastic agent weight ratio is 0.8, and ball milling 36h again, slurry be with ultrasonic dispersion 3min, through vacuum degassing, removes the slurry of making even dispersion behind the bubble.The solvent volume mark is 60% of a slurry in this slurry, and dispersant is 2% of a slurry volume mark, and slurry viscosity is 30mPas, and the pH value is 6.2, and temperature is 30 ℃.
2) ambient temperature is 28 ℃ during curtain coating, and the curtain coating speed of employing is 1.0cm/s, and the height of scraper is controlled at 1mm, does substrate with refractory ceramics in the curtain coating process, and the substrate place applies pulsed magnetic field.Pulsed magnetic field is produced by solenoid coil by pulse current, and magnetic field intensity is 0.8T, and magnetic field gradient is 7T/m.
3) the slurry drying temperature is 24 ℃, and relative humidity is that plain flake thickness degree was 0.4mm after 30% material was done.Sintering green compact under nitrogen protection, the control heating rate is 0.6 ℃/min, and at 400 ℃ of insulation 2h.Be heated to 1300 ℃ with 100 ℃/h subsequently, insulation 2h.Cool to 200 ℃ of taking-ups with the furnace.
Prepared sample tissue densification, porosity is low, the surfacing of film.Example 4 prepared samples are carried out the electron microprobe line analysis, and porosity is low, and composition changes continuously.The Co powder reduces to 0% of opposite side by 96% of a side, and no macroscopic interface exists.Carry out thermal shock resistance experiment circulation 50 times between room temperature and 1000K, sample does not have breakage.

Claims (10)

1. strong magnetic-weak magnetic gradient material tape casting preparation in the pulsed magnetic field is characterized in that its step is:
1) pulp preparation
With particle size is ferromagnetism nickel powder or the cobalt powder of 0.1~100 μ m, with particle size be the ZrO of 0.1~100 μ m 2, SiC, AlN, Si 3N 4, B 4C, SiO 2, TiC, Al 2O 3In one or more mix by weight ratios of 0.1~10: 1, add organic solvent, dispersant, plastic agent, binding agent, ball milling 5~30h in ball mill; Add plastic agent and binding agent, ball milling 10~40h again in ball mill, ultrasonic dispersion processing 1~15min, vacuum degassing obtains the disperse slurry, and slurry viscosity is 1~100mPas, and the pH value is 5~12;
2) flow casting molding in the pulsed magnetic field
The disperse slurry is injected casting machine, and the height of scraper is 0.4~1.0mm, and control curtain coating motor speed is 0.5~5cm/s, do substrate with refractory ceramics during curtain coating, discontinuity applies pulsed magnetic field at the substrate place, and magnetic field intensity is 0.1~5.0T, and magnetic field gradient is 0.1~50T/m;
3) drying and sintering
20~30 ℃ of baking temperatures, relative humidity is 30~60%, plain flake thickness degree 0.1~0.5mm behind the slurry drying.Carry out sintering after drying is finished, sintering is in graphite or protection of nitrogen gas environment, and control sintering heating rate is 0.2~2 ℃/min; at 150~600 ℃ of insulation 1~5h; be heated to 1200~1400 ℃ again, insulation 1~3h cools to 100~400 ℃ of taking-ups at last with the furnace.
2. strong magnetic-weak magnetic gradient material tape casting preparation in a kind of pulsed magnetic field according to claim 1 is characterized in that described pulsed magnetic field is the magnetic field that the pulse current that utilizes capacitor to spark to produce produces by coil.
3. strong magnetic-weak magnetic gradient material tape casting preparation is characterized in that described organic solvent is one or more in ethanol, methylethylketone, butanone or the trichloroethylene in a kind of pulsed magnetic field according to claim 1.
4. strong magnetic-weak magnetic gradient material tape casting preparation is characterized in that described ethanol and methylethylketone, trichloroethylene and methylethylketone, trichloroethylene and ethanol or butanone and ethanol are by 0.1~10: 1 mixed in a kind of pulsed magnetic field according to claim 4.
5. strong magnetic-weak magnetic gradient material tape casting preparation is characterized in that the organic solvent volume fraction in the described disperse slurry is 20~60% of a slurry in a kind of pulsed magnetic field according to claim 1.
6. strong magnetic-weak magnetic gradient material tape casting preparation is characterized in that described dispersant is herring oil, phosphate, olein or triethanolamine in a kind of pulsed magnetic field according to claim 1.
7. strong magnetic-weak magnetic gradient material tape casting preparation is characterized in that the dispersant in the described disperse slurry is 0.2~5% of a slurry volume mark in a kind of pulsed magnetic field according to claim 1.
8. strong magnetic-weak magnetic gradient material tape casting preparation is characterized in that described bonding agent is polyvinyl butyral resin or polyvinyl alcohol in a kind of pulsed magnetic field according to claim 1.
9. strong magnetic-weak magnetic gradient material tape casting preparation is characterized in that described plastic agent is one or more in glycerine, dioctyl phthalate, polyethylene glycol or the phthalic acid in a kind of pulsed magnetic field according to claim 1.
10. strong magnetic-weak magnetic gradient material tape casting preparation is characterized in that the bonding agent in the described disperse slurry is 10~30% of a stock quality mark in a kind of pulsed magnetic field according to claim 1; Binding agent/plastic agent weight ratio is 0.5~1.0.
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