CN100548604C - Strong magnetic-weak magnetic gradient material formed by slip casting preparation method in the pulsed magnetic field - Google Patents
Strong magnetic-weak magnetic gradient material formed by slip casting preparation method in the pulsed magnetic field Download PDFInfo
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- CN100548604C CN100548604C CNB2006100532475A CN200610053247A CN100548604C CN 100548604 C CN100548604 C CN 100548604C CN B2006100532475 A CNB2006100532475 A CN B2006100532475A CN 200610053247 A CN200610053247 A CN 200610053247A CN 100548604 C CN100548604 C CN 100548604C
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- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses the preparation method of strong magnetic-weak magnetic gradient material formed by slip casting in a kind of pulsed magnetic field.The steps include: 1) the preparation gypsum mold; 2) ceramic powders and strong magnetic metal powder in certain ratio are mixed with water or nonaqueous solvents, and in ball mill, stir the slurries of making even dispersion; 3) be 0.1～5.0T in magnetic field intensity, magnetic field gradient is a moulding by casting in the pulsed magnetic field of 0.1～50T/m; 4) oven dry, sinter molding.The advantage of the inventive method is: by changing pulsed magnetic field intensity and magnetic field gradient, can prepare the functionally gradient material (FGM) of all thickness in very big composition range, composition changes continuously and is controlled.Utilize the ripe moulding of traditional handicraft ceramic grout, powder metallurgy process to make that the formality of producing function-graded material is greatly simplified, cost reduces greatly.
Description
Technical field
The present invention relates to strong magnetic-weak magnetic gradient material formed by slip casting preparation method in a kind of pulsed magnetic field.
Background technology
Along with the develop rapidly of science and technology, more and more higher to the performance requirement of material, particularly the part of (superhigh temperature, ultralow temperature, super-pressure, supersonic speed and XHV etc.) work has more required special performances under extreme environment.Function-graded material (FGM) is under the condition at high temperature, thermal cycle and big temperature fall, operate as normal and the class new material developed repeatedly, and so harsh environment for use requires material to have excellent heat shock resistance and thermal fatigue property.Traditional pottery, the direct conjugant of metal are very easily peeled off because of the interface thermal stress and were lost efficacy, and forming thermal stress mitigation type FGM is that head it off has been opened up approach.FGM is the ideal material at some high temperature difference positions such as engine inlet of airborne vehicle, space shuttle, and its principal character is that component structure and physical parameter change continuously.
Up to now, the FGM main preparation methods have that powder compacting, physical vaporous deposition (PVD), chemical vapour deposition technique (CVD), self-propagating reaction are synthetic, plasma spraying, electrocasting, galvanoplastic, laser sintered and centrifugal casting etc.Powder metallurgic method is with composition gradient lamination structures such as feed particulate material such as metal, pottery and whiskers, through compacting, sintering and make 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.The PVD method is to make the metal of heating evaporation be deposited on the method for carrying out coating on the substrate, in metal, semimetal, send into reacting gas 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 by electronics or ion, and the metal that sputters out is deposited on the substrate; Ion plating is by the metal vapors ionization, obtains the good and fine and close deposit of caking property.Chemical vapour deposition technique is that halide gas is added thermal 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.From to spread the thermal response method be the element powders that will constitute compound with metal dust by the gradient composition filling, with cold isostatic compaction, put into reaction vessel, at one end light a fire.Because volume changes during reaction, so reaction vessel (hydrostatic pressing or air pressure) pressurization in a certain way, to guarantee the finished product densification.Plasma spraying method with plasma spraying machine blow out have metal, the pottery mixed-powder and plasma jet the test with matrix material on.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.The thickness of electroforming metal or alloy can be 50 microns to tens centimetres.Galvanoplastic are usually said direct current electrode position, are a kind of electrochemical process that obtains metal (or alloy) sedimentary deposit by the method for electrolysis at the surface of solids.Utilizing this process to prepare FGM is to wait the composition that continuously changes coating by changing plating bath composition between each coating bath or bath flow rate and current density, thereby obtains gradient coating.
These preparation methods respectively have oneself characteristics and applicable situation, but 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 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.Therefore, if the metal or the ceramic forming material means of maturation can be used for preparing FGM, have great importance undoubtedly and vast potential for future development.And because traditional production technique such as metal castings, forming process of ceramics, preparation all be the basic product uniformly of microstructure and property, the hardening constituent in the composite also is equally distributed usually.Therefore, these are tradition and ripe production technology, can not directly be used for preparing component structure and physical parameter continually varying FGM.
Various metals and ceramic material can be divided into ferromagnetism, ferrimagnetism, paramagnetism, anti-ferromagnetism and diamagnetism etc. according to magnetic performance.Wherein, ferromagnetism and ferrimagnetism belong to ferromagnetism, and (the ferrimagnetism material demand is than high-intensity magnetic field) takes place to attract strongly in magnetic field material.Paramagnetism, anti-ferromagnetism and diamagnetism belong to weak magnetic, and magnetic field that applies and intensity thereof are very little to their influences.Transition metal such as Fe, Ni, Co belong to ferromagnetic material, have ferromagnetism below Curie temperature.Most potteries are as Al
2O
3, ZrO
2, SiC, AlN, Si
3N
4, B
4C, SiO
2, TiC etc., all be weak magnetic substance, magnetic field is not had sensitiveness basically.At present, many important function functionally gradient material (FGM)s comprise proving to have good thermal stress slow release effect, are testing the ZrO at high temperature difference positions such as being used for rocket chamber inwall, nuclear reactor and engine inlet
2/ Ni, ZrO
2/ NiCr, ZrO
2/ Co, ZrO
2/ steel, Al
2O
3/ Ni, MgO/Ni, SiC/ α phase stainless steel, and the gradient film of FeN series etc., the magnetic contrast of group element material is all very big.These characteristics provide important basis for people utilize the different magnetic properties of constituent element to prepare functionally gradient material (FGM).Utilize the difference of magnetic property between metal and the ceramic constituent element, this group adopted the method for injection forming 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 successfully utilize slip casting to prepare functionally gradient material (FGM) in pulsed magnetic field.The present invention is the slurry that the pottery of ferromagnetic metal and weak magnetic is formed, and adopts the fixed shaping of slip casting in pulsed magnetic field, and 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.
The outstanding advantage of this method is exactly to utilize ripe traditional handicraft ceramic grout moulding, powder metallurgy process to produce function-graded material, by adjusting pulsed 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 reduces greatly.
Summary of the invention
The purpose of this invention is to provide strong magnetic-weak magnetic gradient material formed by slip casting preparation method in a kind of pulsed magnetic field.
Its step is:
1) gypsum mold is prepared
α-gypsum and β-gypsum mix with 15～25 ℃ water, stir cast after 3～8 minutes, solidify, harden the gypsum mold that makes after drying by calcium plaster, preserve in the environment of 25～38 ℃ of temperature, relative humidity 20～30%;
2) pulp preparation
With particle size is the stainless iron powder of 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, Y
2O
3, Al
2O
3In one or more mix by weight ratios of 0.1～10: 1, add solvent, dispersant, bonding agent, ball milling 1～10h in ball mill, ultrasonic dispersion processing 1～15min, obtain the disperse slurry, the humidity of slurry is 20%～50%, and temperature is 30～60 ℃, viscosity is 1～100mPas, and regulating the pH value is 5～12;
3) moulding by casting in the pulsed magnetic field
Slurry is charged in the plaster mold, and mould applies pulsed magnetic field outward, and magnetic field intensity is 0.1～5.0T, and magnetic field gradient is 0.1～50T/m, and magnetizing time is 3～30min;
4) sintering
Remove mould after the curing, and 35～60 ℃ of slowly oven dry down, the green compact that obtain sinter molding in graphite or protection of nitrogen gas environment, sintering temperature cool to 100～400 ℃ of taking-ups with the furnace between 800～1800 ℃.
Described pulsed magnetic field is the magnetic field that the pulse current that utilizes capacitor to spark to produce produces by coil.Solvent is water, dibasic ester, higher boiling gasoline or long-chain alcohol.Dispersant is one or more in polyvinyl butyral resin, polyvinylpyrrolidone, waterglass, caustic soda, the sodium phosphate trimer.Bonding agent is one or more of polyvinyl butyral resin, trimethyl propane three acrylates, acrylamide or 1,6 ethylene glycol bisthioglycolate ethene hydrochlorate.Dispersant is 0.1%～1.8% of a stock quality mark; Bonding agent is 1～4% of a stock quality mark;
Advantage of the present invention is:
1) by applying pulsed magnetic field, change magnetic field intensity and magnetic field gradient, can prepare the functionally gradient material (FGM) of all thickness in very big composition range, composition changes continuously and is controlled.
2) prepare FGM 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 magnetic force under the pulsed magnetic field.
3) utilize the ripe moulding of traditional handicraft ceramic grout, powder metallurgy process that formality simplification, the cost of producing function-graded material are reduced greatly.
The specific embodiment
Strong magnetic of the present invention-weak magnetic gradient material preparation method is with ferromagnetic metal (in stainless iron, 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 solvent composition slurry, pour into dies cavity and in magnetic field, be shaped.Slurry is subjected to the effect of magnetic force, builds up to two ends in mould respectively, forms component gradient.The blank that obtains is made strong magnetic-weak magnetic gradient material behind curing, sintering.The strong magnetic of this kind-weak magnetic gradient material is super heat proof material, has excellent heat shock resistance and thermal fatigue property.
Concrete steps of the present invention are as follows:
1) preparation of mould
Gypsum is to be formed through calcination process by plaster of paris rock, and the purity of selenolite is high more, and the quality of gypsum is also good more.Gypsum can be divided into α-gypsum and β-gypsum according to the difference of process.α-gypsum intensity height, water imbibition is poor, and β-gypsum good water absorption, intensity difference.The fineness of gypsum is also influential to intensity and water imbibition, and along with the increase of fineness, the intensity of gained mould can increase, but water imbibition can reduce.We had both required used gypsum mold to have stronger water imbibition, required it to have certain intensity again, therefore adopted the preparation of mixed type gypsum.
The temperature of institute's water can influence the setting time of calcium plaster in the mould manufacturing, can influence the expansion of calcium plaster again.Along with the rising of water temperature, will accelerate the setting time of calcium plaster, expand then to reduce.Mineral matter in the water also can be deposited in the mould, influences the performance of mould.Therefore, should adopt pure running water in the production, water temperature is 15～25 ℃.The porosity, intensity and the structure of mould in the scale effect of gypsum and water.Along with the raising of plaster-water ratio, the intensity and the density of mould all increase, and water absorption rate then reduces, and the control plaster-water ratio is 1.3～1.5.Gypsum soaked in water 1～2 minute, to guarantee fully contacting of gypsum and water.The oversize meeting of soak time in water makes the calcium plaster premature hardening, and mould produces the surface of sand shape; Soak time is too short, and then die surface produces pin hole and other defect.About 4 minutes of the mixing time of control gypsum.The back gypsum mold need drying of being solidified, being hardened and make by calcium plaster of cast is discharged the surplus water that has neither part nor lot in hydration reaction.The gypsum mold that is used for slip casting should be fully dry, but can not drying undue (humidity 3～20%).Use dry not good mould will hinder blank to eat slurry fast, and that too dry mould can make blank eat slurry is too fast, causes the delamination of notes part.The baking temperature of mould is at 50～70 ℃.When the temperature in the drier still more than 38 ℃ the time, should not take out mould, otherwise easy to crack.Gypsum mold is deposited in the plane of dustless no dirt, 25～38 ℃ of temperature, relative humidity 20～30%.
2) pulp preparation
Adopt strong magnetic metal powder (in stainless iron, nickel powder, the cobalt powder a kind of, particle size is at 0.1～100 μ m) and ceramic powders (ZrO
2, SiC, AlN, Si
3N
4, B
4C, SiO
2, TiC, Y
2O
3, Al
2O
3In one or more, particle size is at 0.1～100 μ m) in 0.1～10: 1 ratio is formed mixed-powder, this mixed-powder mixes with aqueous solvent, and add one or more dispersants to change the dispersiveness of slurry, dispersant has polyvinyl butyral resin, polyvinylpyrrolidone, waterglass, caustic soda and sodium phosphate trimer, and standard content is 0.1%～1.8% of a stock quality mark.Dispersant or can make surface charging in particle surface absorption is avoided particle agglomeration by Coulomb repulsion, and electrostatic repulsion forces can be by being controlled between the pH value 5～12 of regulating suspension, or be adsorbed on particle surface, avoids particle agglomeration by sterically hindered effect.In ball mill, stir 1～10h, make the slurries of even dispersion.Because fine particle is easy to reunite, and is the slurry of nanometer and sub-micron for granularity, adopt ultrasonic wave to carry out the disperse processing.
The humidity of slurry cast is 20%～50%, and temperature is 30～60 ℃.Ensureing under the good flow implementations, should reduce the humidity of slurry as far as possible.The humidity of slurry is more little, and it is fast more to eat slurry speed, and the air shrinkage factor of annotating part is low more, and the useful life of mould is long more.
3) moulding by casting in the pulsed magnetic field
Moulding by casting is the critical process that injection forming prepares strong magnetic-weak magnetic gradient material in the employing pulsed magnetic field in the pulsed magnetic field.Gypsum mold is on every side that temperature is under 25～28 ℃ of conditions during cast, is to eliminate attachment and differentiation die-face, uses soda solution wiping mould.Slurry is charged in the plaster mold, and mould applies pulsed magnetic field outward.Pulsed magnetic field is produced by solenoid coil by pulse current.
Be subjected to the effect of magnetic force, the metal 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, have formed in the slurry and have arranged orderly " micelle ".Adjust magnetic field intensity at 0.1～5.0T, magnetic field gradient is controlled magnetizing time 3～30min at the OK range of 0.1～50T/m, obtains the sample of required component gradient.
Increase the pressure of slurry in mould, can accelerate to eat slurry speed.Swing die can reduce viscosity in case of necessity, and deaeration improves green strength.The pole sample that part is long, stack rotation in position or alternating magnetic field can make suspension stir and homogenising in mould, thereby on purpose adjust composition or thermograde.These all are ancillary methods of avoiding the semi-finished product defective to form.
4) sintering
Base substrate after the curing goes slowly to dry down at 35～60 ℃ behind the mould.According to the difference of particulate component, green compact can be in the ordinary sinter stove sintering, perhaps be anti-oxidation sintering in the environment of protection.Heating rate is that 100～400 ℃/h makes furnace temperature reach 500～1200 ℃, is heated to 1000～1600 ℃ of insulation 1～3h again, cools to 100～400 ℃ of taking-ups at last with the furnace.
The functionally gradient material (FGM) of all thickness that can prepared composition in very large range changes by the present invention, and composition changes continuously.The finished product internal flaw is few, and structure closely has excellent heat shock resistance and thermal fatigue property.
Embodiment 1:
1) calcium plaster solidified, harden the gypsum mold that makes after drying, the mould inside die cavity is to be the disk of 65mm for 40mm, diameter highly.
2) average particle size particle size is that nickel by powder and the average particle size particle size of 3 μ m are the Al of 0.9 μ m
2O
3Powder is formed mixed-powder in proportion at 1: 1, mix with water, and adding content is 0.2% caustic soda, in ball mill, stir 5h, add the polyvinyl butyral resin bonding agent, continue ball milling 5h, make the slurries of even dispersion, and adopt ultrasonic wave to carry out the disperse processing.The humidity that obtains pouring into a mould slurry is 40%, and temperature is 35 ℃, and viscosity is 46mPas, pH value of slurry 7.8.
3) the mould temperature is 25 ℃ during slip casting, the soda solution wiping mould with 3%.Slurry is charged in the plaster mold, and mould applies pulsed magnetic field outward, and pulsed magnetic field is produced by solenoid coil by pulse current, and magnetic field intensity is 0.4T, and magnetic field gradient is 3T/m, and magnetizing time is 5min.
4) base substrate after the curing is at 40 ℃ of slowly oven dry down, sintering green compact under the powdered graphite protection.Heating rate heating with 200 ℃/h makes furnace temperature reach 500 ℃ of insulation 2h, is heated to 1280 ℃ with 200 ℃/h then, insulation 1h.Cool to 200 ℃ of taking-ups with the furnace.
Example 1 prepared sample is carried out the electron probe line analysis, find that its composition changes continuously, Ni reduces to 0% of opposite side by 94% of a side.Sample interior does not have macroscopic interface and exists, and does not have pore substantially.To the sample thermal shock test that circulates, the thermal shock cracking does not take place under 800 ℃ of temperature difference, chilling condition.Under 600 ℃ of temperature difference, slow cooling condition through 80 circulations crackle does not appear.
Embodiment 2:
1) calcium plaster solidified, harden the gypsum mold that makes after drying, the mould inside die cavity is to be the disk of 65mm for 40mm, diameter highly.
2) choosing average particle size particle size is that more ferromagnetic cobalt dust of having of 4 μ m and average particle size particle size are the ZrO of 2.2 μ m
2Powder is formed mixed-powder in proportion at 1: 2, and it mixes with ethanol, and adding content is 0.4% polyvinyl butyral resin dispersant, in ball mill, stir 10h, add trimethyl propane three acrylates bonding agents, continue ball milling 6h, make the slurries of even dispersion.Regulate the pH value 8.3 of suspension, and adopt ultrasonic wave to carry out the disperse processing.The humidity that obtains pouring into a mould slurry is 35%, and temperature is 40 ℃, and viscosity is 38mPas.
3) the mould temperature is 27 ℃ during slip casting, die-face, the soda solution wiping mould with 3%.The functionally gradient material (FGM) sample of preparation is that thickness is that 40mm, diameter are the disk of 65mm, and pulsed magnetic field is produced by solenoid coil by pulse current, and magnetic field intensity is 1.0T, and magnetic field gradient is 8T/m, and magnetizing time is 8min.
4) base substrate after the curing is 40 ℃ of slowly oven dry down, and the sintering of green compact carries out under the powdered graphite protection, and heating rate is that 200 ℃/h makes furnace temperature reach 500 ℃, and constant temperature 1.5h makes furnace temperature reach 1500 ℃ with 200 ℃/h then, constant temperature 2h.Then cool to 300 ℃ of taking-ups with the furnace.
Example 2 prepared samples are carried out the electron probe line analysis, find that its composition changes continuously, cobalt powder is 0% by 96% of a side to opposite side, and no macroscopic interface exists, and only there is a small amount of pore inside.To the thermal shock test that circulates of the sample of gained, the thermal shock cracking does not take place under 800 ℃ of temperature difference, chilling condition, under 600 ℃ of temperature difference, slow cooling condition through 100 circulations crackle does not appear.
Embodiment 3:
1) calcium plaster solidified, harden the gypsum mold that makes after drying, the mould inside die cavity is to be the disk of 65mm for 40mm, diameter highly.
2) average particle size particle size is that the nickel by powder of 3 μ m and TiC powder that average particle size particle size is 0.9 μ m are formed mixed-powder in proportion at 1: 3, mix with higher boiling gasoline, and adding content is 0.4% polyvinylpyrrolidone dispersant, in ball mill, stir 8h, add the acrylamide bonding agent, continue ball milling 8h, make the slurries of even dispersion.Regulate the pH value 9 of suspension, and adopt ultrasonic wave to carry out the disperse processing.The humidity that obtains pouring into a mould slurry is 40%, and temperature is 35 ℃, and viscosity is 40mPas.
3) the mould temperature is 25 ℃ during slip casting, the soda solution wiping mould with 3%.Slurry is charged in the plaster mold, and mould applies pulsed magnetic field outward.Pulsed magnetic field is produced by solenoid coil by pulse current, and magnetic field intensity is 0.9T, and magnetic field gradient is 7T/m, and magnetizing time is 15min.
4) base substrate after the curing is 35 ℃ of slowly oven dry down, and the sintering of green compact carries out under nitrogen protection, and heating rate is that 200 ℃/h makes furnace temperature reach 500 ℃, and constant temperature 2h makes furnace temperature reach 1250 ℃ with 200 ℃/h then, constant temperature 2h.Then cool to 200 ℃ of taking-ups with the furnace.
Example 3 prepared samples are carried out the electron probe line analysis, find that its composition changes continuously, the Ni powder by a side 90% to other～side is 0%, no macroscopic interface exists, only there is a small amount of pore inside.To the thermal shock test that circulates of the sample of gained, the thermal shock cracking does not take place under 800 ℃ of temperature difference, chilling condition, under 600 ℃ of temperature difference, slow cooling condition through 150 circulations crackle does not appear.
Embodiment 4:
1) calcium plaster solidified, harden the gypsum mold that makes after drying, the mould inside die cavity is to be the disk of 65mm for 40mm, diameter highly.
2) average particle size particle size is that the equal particle size of stainless iron powder peace of 2.8 μ m is that the SiC powder of 1.2 μ m is formed mixed-powder in proportion at 1: 5, mix with dibasic ester, and adding content is 0.8% waterglass dispersant, in ball mill, stir 6h, add 1,6 ethylene glycol bisthioglycolate ethene hydrochlorate bonding agents continue ball milling 10h, make the slurries of even dispersion.Regulate the pH value 8 of suspension, and adopt ultrasonic wave to carry out the disperse processing.The humidity that obtains pouring into a mould slurry is 35%, and temperature is 38 ℃, and viscosity is 45mPas.
3) the mould temperature is 25 ℃ during slip casting, the soda solution wiping mould with 3%.Slurry is charged in the plaster mold, and mould applies pulsed magnetic field outward.Pulsed magnetic field is produced by solenoid coil by pulse current, and magnetic field intensity is 1.0T, and magnetic field gradient is 8T/m, and magnetizing time is 15min.
4) base substrate after the curing is 35 ℃ of slowly oven dry down, and the sintering of green compact carries out under nitrogen protection, and heating rate is that 200 ℃/h makes furnace temperature reach 500 ℃, and constant temperature 2h makes furnace temperature reach 1300 ℃ with 200 ℃/h then, constant temperature 2h.Then cool to 200 ℃ of taking-ups with the furnace.
Example 4 prepared samples are carried out the electron probe line analysis, find that its composition changes continuously, the Fe powder is 0% by 96% of a side to opposite side, and no macroscopic interface exists, and only there is a small amount of pore inside.To the thermal shock test that circulates of the sample of gained, the thermal shock cracking does not take place under 800 ℃ of temperature difference, chilling condition, under 600 ℃ of temperature difference, slow cooling condition through 150 circulations crackle does not appear.
Embodiment 5:
1) calcium plaster solidified, harden the gypsum mold that makes after drying, the mould inside die cavity is to be the disk of 65mm for 40mm, diameter highly.
2) average particle size particle size is that the equal particle size of stainless iron powder peace of 4.2 μ m is the Si of 2.4 μ m
3N
4Powder is formed mixed-powder in proportion at 1: 4, mixes with long-chain alcohol, and to add content is 0.6% sodium phosphate trimer dispersant, stirs 6h in ball mill, adds the acrylamide bonding agent, and continuation ball milling 6h makes the slurries of even dispersion.Regulate the pH value 9.6 of suspension, and adopt ultrasonic wave to carry out the disperse processing.The humidity that obtains pouring into a mould slurry is 35%, and temperature is 35 ℃, and viscosity is 80mPas.
3) the mould temperature is 25 ℃ during slip casting, the soda solution wiping mould with 3%.Slurry is charged in the plaster mold, and mould applies pulsed magnetic field outward.Pulsed magnetic field is produced by solenoid coil by pulse current, and magnetic field intensity is 0.6T, and magnetic field gradient is 5T/m, and magnetizing time is 15min.
4) base substrate after the curing is 35 ℃ of slowly oven dry down, and the sintering of green compact carries out under nitrogen protection, and heating rate is that 200 ℃/h makes furnace temperature reach 500 ℃, and constant temperature 2h makes furnace temperature reach 1300 ℃ with 200 ℃/h then, constant temperature 2h.Then cool to 200 ℃ of taking-ups with the furnace.
Example 5 prepared samples are carried out the electron probe line analysis, find that its composition changes continuously, the Fe powder is 0% by 92% of a side to opposite side, and no macroscopic interface exists, and only there is a small amount of pore inside.To the thermal shock test that circulates of the sample of gained, the thermal shock cracking does not take place under 800 ℃ of temperature difference, chilling condition, under 600 ℃ of temperature difference, slow cooling condition through 150 circulations crackle does not appear.
Claims (6)
1. strong magnetic-weak magnetic gradient material formed by slip casting preparation method in the pulsed magnetic field is characterized in that its step is:
1) gypsum mold is prepared
α-gypsum and β-gypsum mix with 15～25 ℃ water, stir cast after 3～8 minutes, solidify, harden the gypsum mold that makes after drying by calcium plaster, preserve in the environment of 25～38 ℃ of temperature, relative humidity 20～30%;
2) pulp preparation
With particle size is the stainless iron powder of 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, Y
2O
3, Al
2O
3In one or more mix by weight ratios of 0.1～10: 1, add solvent, dispersant, bonding agent, ball milling 1～10h in ball mill, ultrasonic dispersion processing 1～15min, obtain the disperse slurry, the humidity of slurry is 20%～50%, and temperature is 30～60 ℃, viscosity is 1～100mPas, and regulating the pH value is 5～12;
3) moulding by casting in the pulsed magnetic field
Slurry is charged in the plaster mold, and mould applies pulsed magnetic field outward, and magnetic field intensity is 0.1～5.0T, and magnetic field gradient is 0.1～50T/m, and magnetizing time is 3～30min;
4) sintering
Remove mould after the curing, and 35～60 ℃ of slowly oven dry down, the green compact that obtain sinter molding in graphite or protection of nitrogen gas environment, sintering temperature cool to 100～400 ℃ of taking-ups with the furnace between 800～1800 ℃.
2. strong magnetic-weak magnetic gradient material formed by slip casting preparation method 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 formed by slip casting preparation method is characterized in that described solvent is water, dibasic ester, higher boiling gasoline or long-chain alcohol in a kind of pulsed magnetic field according to claim 1.
4. strong magnetic-weak magnetic gradient material formed by slip casting preparation method is characterized in that described dispersant is one or more in polyvinyl butyral resin, polyvinylpyrrolidone, waterglass, caustic soda, the sodium phosphate trimer in a kind of pulsed magnetic field according to claim 1.
5. strong magnetic-weak magnetic gradient material formed by slip casting preparation method in a kind of pulsed magnetic field according to claim 1, it is characterized in that described bonding agent is one or more of polyvinyl butyral resin, trimethyl propane three acrylates, acrylamide or 1,6 ethylene glycol bisthioglycolate ethene hydrochlorate.
6. strong magnetic-weak magnetic gradient material formed by slip casting preparation method is characterized in that described dispersant is 0.1%～1.8% of a stock quality mark in a kind of pulsed magnetic field according to claim 1; Bonding agent is 1～4% of a stock quality mark.
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| CN102225466A (en) * | 2011-06-08 | 2011-10-26 | 浙江大学 | Slip casting preparation method for gradient materials in movement magnetic field |
| CN102930974B (en) * | 2012-10-11 | 2015-06-24 | 厦门钨业股份有限公司 | Humidity adjustment-based manufacturing method for sintered Nd-Fe-B magnets |
| CN102997322B (en) * | 2012-10-31 | 2015-04-22 | 赵宏祥 | Low-voltage direct-current heating plate and manufacturing technique thereof |
| CN105039830B (en) * | 2015-06-28 | 2017-03-01 | 佛山市顺德区昇煌节能材料有限公司 | The tape casting preparation of metal and ceramic gradient material in alternating magnetic field |
| CN104972131B (en) * | 2015-06-28 | 2018-05-11 | 中国计量大学 | The injection forming preparation method of metal and ceramic gradient material in alternating magnetic field |
| CN104975199B (en) * | 2015-06-28 | 2017-03-29 | 中国计量学院 | The preparation method by extrusion molding thereof of metal/reinforcement composite material in alternating magnetic field |
| CN114414438B (en) * | 2022-01-24 | 2024-01-26 | 中国矿业大学 | Identification method for detecting grouting diffusion range based on proton magnetometer |
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