CN102211346A - Method for preparing functionally graded material through pressure filtration forming in motional magnetic field - Google Patents
Method for preparing functionally graded material through pressure filtration forming in motional magnetic field Download PDFInfo
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Abstract
The invention discloses a method for preparing a functionally graded material through pressure filtration forming in a motional magnetic field, which comprises the following steps of: 1) preparing a porous mould; 2) mixing powders different in magnetism with de-ionized water in a certain proportion, and stirring all the materials in a ball mill to form evenly dispersed slurry, and carrying out pouring; 3) applying a motional magnetic field having the magnetic field intensity of 0.1 to 10 T to take effect once or multiple times, and performing pressure filtration filtering; and 4) carrying out drying and sintering forming. The method disclosed by the invention has the following advantages that: graded materials different in composition distribution can be obtained by changing the magnetic filed intensity, the speed of motion and the magnetic field acting times; and by employing the mature ceramic pressure filtration forming method, the steps for preparing the functionally graded material are simplified, and the cost is greatly reduced.
Description
Technical field
The present invention relates to a kind of in magnetic field the pressure filtration molding preparation method of motion functionally gradient material (FGM), belong to field of material preparation.
Background technology
The ceramic of powder stock preparation generally includes powder preparation, powder processing, powder compacting, sintering densification several steps.Each step all might be introduced defective.Some will be eliminated the defective of introducing in each step before the sintering in next step technical process, and have some will be retained to last or along with the propelling of technical process changes new defective into.The defective that finally causes material damage originates from the base substrate mostly, that is is formed at forming process.These defectives origin comprises: soft-agglomerated, hard aggregation, organic being mingled with, inorganic being mingled with and big crystal grain.These major defect kinds can be eliminated or reduce mostly by pressure filtration molding.
Filter-pressing process is a kind of forming ceramic parts technology that develops and cause extensive concern in recent years rapidly, its cardinal principle is under the impressed pressure effect, the slurry that is dispersed with the solid phase ceramic particle under certain condition in liquid medium is entered in the model cavity by stock line, and leach the operative liquid medium by the porous filtering layer, thereby closely being arranged, ceramic particle is solidified into ceramic body with definite shape.
Pressure filtration molding is the effective technology that improves the CERAMIC MATERIAL ENGINEERING reliability.Especially for the ceramic of preparation large-size cross section and complicated shape, pressure filtration molding more demonstrates its superiority.Because pressure filtration molding adopts the organic additive of minute quantity, the compact density height, and do not get rid of organic difficulty, and therefore be suitable for moulding heavy in section goods, also can eliminate organic matter and be mingled with the defective that is caused.Pressure filtration molding adopts liquid phase medium to prepare slurry directly-forming, can adopt method such as precipitate and separate to remove aggregate, the bulky grain in the powder and be mingled with body.And avoided the formation of new aggregate, thereby can improve the micro-uniformity of molding blank without the dry run straight forming.When the preparation ceramic matric composite, pressure filtration molding can also avoid destroying fibrous compound phase, and can effectively it be uniformly distributed in the matrix.
FGM (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 harsh environment for use requires material to have excellent heat shock resistance and thermal fatigue property.Traditional pottery, the direct conjugant of metal may be peeled off because of the interface thermal stress and lose efficacy, and forming thermal stress mitigation type functionally gradient material (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.
The FGM main preparation methods has that powder compacting, physical vaporous deposition PVD, chemical vapour deposition technique CVD, self-propagating reaction are synthetic, plasma spraying, 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; The 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.
Above-mentioned preparation method or complicated technology or the equipment of requirement, or need in preparation process, change material composition or technological parameter constantly.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 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.
Transition metal and alloys thereof such as Fe, Ni, Co, ferrite, rare earth permanent magnet compound etc. all belongs to ferromagnetic material, has ferromagnetism below Curie temperature.And most potteries, 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.Utilize the difference of magnetic property between metal and the ceramic constituent element, our group adopted the pressure filtration molding method successfully to prepare functionally gradient material (FGM) in magnetostatic field in 2003.This technology has been authorized patent of invention, patent No. CN03116138.3, patent name " FGM pressure filtration molding preparation method in the magnetostatic field ".Subsequently, this group was improved to pulsed magnetic field in 2006 with magnetostatic field, and successfully prepared functionally gradient material (FGM).This technology has been authorized patent of invention, patent No. CN200610053248.X, patent name " strong magnetic-weak magnetic gradient material pressure filtration molding preparation method in the pulsed magnetic field ".
In the past few years, our group updates on original experiment basis, and makes a breakthrough.On the basis of injection forming, utilize moving magnetic field to replace magnetostatic field and pulsed magnetic field, successfully prepared the continuous functionally gradient material (FGM) of composition.Compare with preparation functionally gradient material (FGM) under the pulsed magnetic field with magnetostatic field, utilize moving magnetic field to prepare functionally gradient material (FGM), can replace gradient magnetic with the magnetic field of a motion, for the bigger system of magnetic contrast, no longer need to obtain high magnetic field gradient with big magnetic field intensity, thereby can obtain big component gradient in less magnetic field, high magnetic field intensity then can make the less system of magnetic contrast form gradient.The method has the advantage of repeated multiple times simultaneously.By adjust magnetic field intensity, movement velocity and magnetic field effect number of times can controlling magnetic field to the restraining force of magnetic constituent element, further control the component distributing in the material.
The present invention is the slurry that two or more materials with different magnetic are formed, adopt the fixed shaping of pressure filtration molding method, with magnetic field the one or many relative motion takes place in the curing molding process, thereby obtain the component gradient along the Movement in Magnetic Field direction, sintering prepares functionally gradient material (FGM) then.
The outstanding advantage of this method is exactly to apply moving magnetic field to prepare functionally gradient material (FGM) on the basis of the ceramic pressure filtration molding technology of maturation, by adjusting technological parameters such as magnetic field intensity, Movement in Magnetic Field speed and magnetic field effect number of times, can utilize less magnetic field to prepare composition easily and change continuously and controlled functionally gradient material (FGM).
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, the pressure filtration molding preparation method of functionally gradient material (FGM) in a kind of moving magnetic field is provided.
Its step of pressure filtration molding preparation method of functionally gradient material (FGM) is as follows in the moving magnetic field:
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 that two or more of 0.1～100 μ m have that the weight ratio by 0.1～10:1 becomes mixed-powder in the metal of different magnetic or the compound, add that to account for the stock quality mark be 10%～80% deionized water and 0.1%～5% organic additive, ball milling 1～10h in ball mill, ultrasonic dispersion processing 1～15min, obtain finely dispersed 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) pressure filtration molding in the moving magnetic field
Slurry is charged in the plaster mold, mould applies moving magnetic field more than 1 time outward, magnetic field intensity is 0.1～10T, Movement in Magnetic Field speed is 0.1～500mm/s, the direction of motion and magnetic direction are 0～180 °, subsequently slurry is exerted pressure, and 10～120min is handled in pressurize under the pressure of 0.1～12Mpa;
4) sintering
Remove mould after the curing; and, place punching block 35～60 ℃ of slowly oven dry down, under the pressure of 0.1～1GPa, suppress; sinter molding in argon gas or protection of nitrogen gas environment is warming up to 500～1200 ℃, and heating rate is 100～400 ℃/h; insulation l～3h; be heated to 1000～1600 ℃ again, insulation l～3h cools to 100～400 ℃ of taking-ups at last with the furnace.
Described metal or compound with different magnetic is Fe, Co, Ni alloy, ferrite or rare earth permanent-magnet powder.Described metal or compound with different magnetic is Al, Cu, Mg or Sb alloy.Described metal or compound with different magnetic is ZrO
2, SiC, AlN, Si
3N
4, B
4C, SiO
2, TiC, Y
2O
3Or Al
2O
3Described moving magnetic field is the magnetic field that is produced by electromagnet, permanent magnet or superconducting magnet.The organic additive of described adding is poly-ethylene fluoride, melmac or phenolic resins.Applied pressure was 0.1～10Mpa during described pressurize was handled, and the dwell time is 10～100min.
The beneficial effect that the present invention and prior art have mutually:
1) by applying moving magnetic field, change magnetic field intensity, movement velocity and magnetic field effect number of times, can in very big composition range, prepare the functionally gradient material (FGM) of all thickness, composition changes continuously and is controlled;
2) compare with preparation functionally gradient material (FGM) under the pulsed magnetic field with magnetostatic field, utilize moving magnetic field to prepare functionally gradient material (FGM), can replace gradient magnetic with the magnetic field of a motion, for the bigger system of magnetic contrast, no longer need to obtain high magnetic field gradient with big magnetic field intensity, thereby can obtain big component gradient in less magnetic field, high magnetic field intensity then can make the less system of magnetic contrast form gradient.The method has the advantage of repeated multiple times simultaneously;
3) utilize ripe traditional pressure filtration molding technology that operation simplification, the cost of preparation function-graded material are reduced greatly.
Description of drawings
Model schematic diagram when Fig. 1 has just injected for slurry;
Fig. 2 is a moving magnetic field effect disposed slurry model schematic diagram;
Among the figure: electromagnet, permanent magnet or superconducting magnet 1, the magnetic field 2 that produces, mould 3, more weak magnetic particle 4, than ferromagnetism particle 5, Movement in Magnetic Field direction 6.
The specific embodiment
Functionally gradient material (FGM) preparation method of the present invention be just two or more have the metal of different magnetic or compound (as Fe, Co, Ni alloy, ferrite and rare earth permanent-magnet powder, Al, Cu, Mg, Sb alloy, ZrO
2, SiC, AlN, Si
3N
4, B
4C, SiO
2, TiC, Y
2O
3, Al
2O
3Deng) form slurry with deionized water, pour into dies cavity, in moving magnetic field, be shaped, pressure filtration molding is carried out in pressurization subsequently.The strong constituent element of magnetic is subjected to the one or many effect of moving magnetic field in the slurry, moves along the Movement in Magnetic Field direction, thereby forms component gradient.The blank that obtains is made functionally gradient material (FGM) behind curing, sintering.
Its step of pressure filtration molding preparation method of functionally gradient material (FGM) is as follows in the moving magnetic field:
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%.Press filtration is owing to being by porous mold the operative liquid medium to be leached and moulding, so porous mold is very important.The press filtration mould should satisfy the requirement of filter-pressing process to porous filter material, satisfies the requirement to mould structure again.Press filtration will have desirable strainability on the one hand with porous material, promptly have enough little pore, narrow air vent aperture distribution, the porosity and the transmission coefficient of appropriateness, on the other hand, for guaranteeing the size and dimension of formed body, these porous materials must have enough rigidity and intensity, easily controlling dimension and shape.In addition, porous material should have enough durabilitys or can carry out model modification neatly.These materials comprise that gypsum is material modified, porous metals, porous organic material and composite porous.This law adopts gypsum material modified, is exactly to add the later materials of organic additive modification such as poly-ethylene fluoride, melmac, phenolic resins in gypsum, and mechanical strength and durability are higher.Can adjust the porosity and water filtering performance by the ratio that changes organic additive and 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.Add poly-ethylene fluoride, its content is 5～25% of gypsum quality.The mixing time of control gypsum 3～8 minutes.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%).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
With particle size is that two or more of 0.1～100 μ m have that the weight ratio by 0.1～10:1 becomes mixed-powder in the metal of different magnetic or the compound, add that to account for the stock quality mark be 10%～80% deionized water and 0.1%～5% organic additive, ball milling 1～10h in ball mill, because fine particle is easy to reunite, for granularity is the slurry of nanometer and sub-micron, adopt ultrasonic wave to carry out disperse processing 1～15min, obtain finely dispersed slurry, the humidity of slurry is 20%～50%, temperature is 30～60 ℃, viscosity is 1～100mPas, and regulating the pH value is 5～12.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 foundry goods is low more, and the useful life of mould is long more.
3) pressure filtration molding in the moving magnetic field
Slurry is charged in the plaster mold, mould applies moving magnetic field more than 1 time outward, magnetic field intensity is 0.1～10T, Movement in Magnetic Field speed is 0.1～500mm/s, the direction of motion and magnetic direction are 0～180 °, subsequently slurry is exerted pressure, and 10～120min is handled in pressurize under the pressure of 0.1～12Mpa.Moving magnetic field is produced by electromagnet, permanent magnet or superconducting magnet.In moving magnetic field, the effect that is subjected to magnetic force than the ferromagnetism particle will form component gradient along the migration of Movement in Magnetic Field direction greater than more weak magnetic-particle.Reduce magnetic field intensity, magnetic field reduces the restraining force than the ferromagnetism constituent element, and component gradient reduces; Improve magnetic field intensity, improve the restraining force than the ferromagnetism constituent element in magnetic field, and component gradient then increases.When Movement in Magnetic Field speed was too big, magnetic field reduced the action time than the ferromagnetism constituent element, and component gradient reduces; Along with the reduction of movement velocity, improved the action time than the ferromagnetism constituent element in magnetic field, and component gradient increases.The adjustment magnetic field intensity is 0.1～10T, and movement velocity obtains the sample of required component gradient at the OK range of 0.1～500mm/s.
4) sintering
Remove mould after the curing; and, place punching block 35～60 ℃ of slowly oven dry down, under the pressure of 0.1～1GPa, suppress; sinter molding in argon gas or protection of nitrogen gas environment is warming up to 500～1200 ℃, and heating rate is 100～400 ℃/h; insulation l～3h; be heated to 1000～1600 ℃ again, insulation l～3h cools to 100～400 ℃ of taking-ups at last with the furnace.Base substrate plasticity is lower in the drying course, and the outer surface of complicated base substrate is different with inner rate of drying, can produce very high shrinkage stress and ftractures.In this case, must be held in the high humility of the dry environment of parison soma, with the evaporation rate of control billet surface layer moisture.Perhaps adopt microwave action, to the whole heating of base substrate, quickening the base substrate internal moisture spreads to the outside, the inside and outside temperature of base substrate is reached unanimity, cooperate again with the high water vapor pressure of external environment condition, then the moisture of base substrate can slowly be got rid of equably, and base substrate shrinks consistent, thereby eliminates or the minimizing drying stress.
Described metal or compound with different magnetic is Fe, Co, Ni alloy, ferrite or rare earth permanent-magnet powder.Described metal or compound with different magnetic is Al, Cu, Mg or Sb alloy.Described metal or compound with different magnetic is ZrO
2, SiC, AlN, Si
3N
4, B
4C, SiO
2, TiC, Y
2O
3Or Al
2O
3Described moving magnetic field is the magnetic field that is produced by electromagnet, permanent magnet or superconducting magnet.The organic additive of described adding is poly-ethylene fluoride, melmac or phenolic resins.Applied pressure was 0.1～10Mpa during described pressurize was handled, and the dwell time is 10～100min.
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, and the finished product internal flaw is few, and structure is tight.
Embodiment 1:
1) mixes with α-gypsum and β-gypsum pure running water with 20 ℃, and adding phenolic resins, its content is 10% of gypsum quality, stirs cast after 4 minutes, calcium plaster is solidified, hardens the gypsum mold that makes after drying, the cuboid of mould inside die cavity 30mm * 10mm * 5mm;
2) choosing average particle size particle size is the more ferromagnetic SmCo of having of 4 μ m
5Powder and average particle size particle size are the ZrO of 2.2 μ m
2Powder 1:10 is in proportion formed mixed-powder, mixed-powder is constantly joined in the deionization aqueous solvent, and to add hydrochloric acid is 5 to regulate pH value, reaches 45vol% to solid concentration, stir 4h in ball mill, and the employing ultrasonic wave carries out the disperse processing.The humidity that obtains pouring into a mould slurry is 35%, and temperature is 40 ℃, and viscosity is 68mPas;
3) the mould temperature is 28 ℃ during slip casting, slurry is charged in the plaster mold, with 3% soda solution wiping mould, mould applies moving magnetic field outward, and moving magnetic field is produced by the magnetic circuit that a pair of NdFeB magnet constitutes, magnetic field intensity is 0.1T, Movement in Magnetic Field speed is 0.5mm/s, direction of motion vertical magnetic field direction, and the effect number of times is 10 times, 0.1Mpa and pressurize 120min subsequently exert pressure;
4) base substrate after the curing is 40 ℃ of slowly oven dry down.Green compact are placed punching block, under the pressure of 0.1GPa, suppress.Sintering green compact under argon shield.Heating rate with 300 ℃/h is heated to 800 ℃ of insulation 2h, is heated to l500 ℃ with 200 ℃/h then, insulation 2h.Cool to 300 ℃ of taking-ups with the furnace.
Example 1 prepared sample is carried out the electron probe line analysis, find that its composition changes SmCo continuously
5Is 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, 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 2:
1) mix with pure running water with α-gypsum and β-gypsum, and add poly-ethylene fluoride, its content is 10% of gypsum quality, stirs cast after 4 minutes.Calcium plaster solidifies, harden the gypsum mold that makes after drying, and the mould inside die cavity is the cuboid of 30mm * 10mm * 5mm;
2) aluminium powder and the average particle size particle size of choosing 50 μ m is the Al of 2.2 μ m
2O
3Powder 1:1 is in proportion formed mixed-powder, mixed-powder is constantly joined in the deionization aqueous solvent, and with salt acid for adjusting pH value to 3.8, reaches 45vol% to solid concentration, stirs 6h in ball mill, and adopts 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 30mPas;
3) the mould temperature is 27 ℃ during slip casting, and the soda solution wiping mould with 3% charges into slurry in the gypsum mold, and mould applies moving magnetic field outward.Moving magnetic field is produced by superconducting magnet, and magnetic field intensity is 10T, and Movement in Magnetic Field speed is 500mm/s, direction of motion vertical magnetic field direction, and the effect number of times is 5 times, the 10Mpa that exerts pressure subsequently, and pressurize 10min;
4) base substrate after the curing is 40 ℃ of slowly oven dry down.Green compact are placed punching block, under the pressure of 1GPa, suppress.Sintering green compact under nitrogen protection.Heating rate with 300 ℃/h is heated to 800 ℃ of insulation 2h, is heated to l400 ℃ with 200 ℃/h then, insulation 2h.Cool to 200 ℃ of taking-ups with the furnace.
Example 2 prepared samples are carried out the electron probe line analysis, find that its composition changes continuously, Al 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, 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 3:
1) mix with pure running water with α-gypsum and β-gypsum, and add poly-ethylene fluoride, its content is 10% of gypsum quality, stirs cast after 4 minutes.Calcium plaster solidifies, harden the gypsum mold that makes after drying, and the mould inside die cavity is the cuboid of 30mm * 10mm * 5mm;
2) average particle size particle size is the BaO6Fe of 3 μ m
2O
3Powder and average particle size particle size are the Al of 0.9 μ m
2O
3Powder is formed mixed-powder in proportion at 1: 2, mixed-powder is constantly joined in the deionization aqueous solvent, and constantly to add hydrochloric acid is 3 to regulate the pH value, reaches 40vol% to solid concentration.Stir 4h in ball mill, adopt ultrasonic wave to carry out the disperse processing and make slurry, the humidity of slurry is 30%, and temperature is 35 ℃, and viscosity is 40mPas;
3) the mould temperature is 25 ℃ during slip casting, and the soda solution wiping mould with 3% charges into slurry in the plaster mold.Mould applies moving magnetic field outward, and moving magnetic field is produced by electromagnet, and magnetic field intensity is 2T, and Movement in Magnetic Field speed is 5mm/s, direction of motion vertical magnetic field direction, and the effect number of times is 15 times, the 0.6Mpa that exerts pressure subsequently, and pressurize 80min;
4) base substrate after the curing is 40 ℃ of slowly oven dry down.Green compact are placed punching block, under the pressure of 0.5GPa, suppress.Sintering green compact under nitrogen protection.Heating rate with 300 ℃/h is heated to 800 ℃ of insulation 2h, is heated to l400 ℃ with 200 ℃/h then, insulation 1h.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, barium ferrite reduces to 0% of opposite side by 94% of a side.Sample interior does not have macroscopic interface and exists.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 100 circulations crackle does not appear.
Embodiment 3:
1) mixes with α-gypsum and β-gypsum pure running water with 20 ℃, and adding melmac, its content is 10% of gypsum quality, stir cast after 4 minutes, calcium plaster is solidified, hardens the gypsum mold that makes after drying, and the mould inside die cavity is the cuboid of 30mm * 10mm * 5mm;
2) choose average particle size particle size be more ferromagnetic stainless iron powder of having of 10 μ m and average particle size particle size be 5.2 μ m the SiC powder in proportion 5:1 form mixed-powder, mixed-powder is constantly joined in the deionization aqueous solvent, and be 4.5 with the salt acid for adjusting pH value, reach 40vol% to solid concentration, in ball mill, stir 5h, and adopt ultrasonic wave to carry out the disperse processing.The humidity that obtains pouring into a mould slurry is 30%, and temperature is 35 ℃, and viscosity is 60mPas;
3) the mould temperature is 27 ℃ during slip casting, soda solution wiping mould with 3%, slurry is charged in the plaster mold, and mould applies moving magnetic field outward, and moving magnetic field is produced by electromagnet, magnetic field intensity is 3.0T, Movement in Magnetic Field speed is 100mm/s, direction of motion vertical magnetic field direction, and the effect number of times is 10 times, 0.3Mpa and pressurize 60min subsequently exert pressure;
4) base substrate after the curing is 40 ℃ of slowly oven dry down.Green compact are placed punching block, under the pressure of 0.6GPa, suppress.Sintering green compact under nitrogen protection.Heating rate with 200 ℃/h is heated to 700 ℃ of insulation 2h, is heated to l250 ℃ with 200 ℃/h then, insulation 2h.Cool to 300 ℃ of taking-ups with the furnace.
Example 4 prepared samples are carried out the electron probe line analysis, find that its composition changes continuously, Fe is 0% by 98% of a side to opposite side, and no macroscopic interface exists.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) mix with pure running water with α-gypsum and β-gypsum, and add melmac, its content is 10% of gypsum quality, stirs cast after 4 minutes.Calcium plaster solidifies, harden the gypsum mold that makes after drying, and the mould inside die cavity is the cuboid of 30mm * 10mm * 5mm;
2) choosing average particle size particle size is that more ferromagnetic cobalt powder of having of 3 μ m and average particle size particle size are the Si of 0.9 μ m
3N
4Powder 1:5 is in proportion formed mixed-powder, and mixed-powder is constantly joined in the deionization aqueous solvent, adds ammoniacal liquor and regulates pH value to 9.5, and solid concentration reaches 40vol%, stirs 3h in ball mill, and adopts 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 55mPas;
3) the mould temperature is 27 ℃ during slip casting, and the soda solution wiping mould with 3% charges into slurry in the gypsum mold, and mould applies moving magnetic field outward.Moving magnetic field is produced by electromagnet, and magnetic field intensity is 0.8T, and Movement in Magnetic Field speed is 10mm/s, direction of motion parallel magnetic field direction, and the effect number of times is 15 times, the 2Mpa that exerts pressure subsequently, and pressurize 20min;
4) base substrate after the curing is 40 ℃ of slowly oven dry down.Green compact are placed punching block, under the pressure of 0.6GPa, suppress.Sintering green compact under nitrogen protection.Heating rate with 200 ℃/h is heated to 800 ℃ of insulation 2h, is heated to l250 ℃ with 200 ℃/h then, insulation 2h.Cool to 200 ℃ of taking-ups with the furnace.
Example 5 prepared samples are carried out the electron probe line analysis, find that it is 0% by 90% of a side to opposite side that its composition changes Co continuously, no macroscopic interface exists.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 200 circulations crackle does not appear.
Claims (7)
1. the pressure filtration molding preparation method of functionally gradient material (FGM) in the moving magnetic field is characterized in that its step is as follows:
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 that two or more of 0.1～100 μ m have that the weight ratio by 0.1～10:1 becomes mixed-powder in the metal of different magnetic or the compound, add that to account for the stock quality mark be 10%～80% deionized water and 0.1%～5% organic additive, ball milling 1～10h in ball mill, ultrasonic dispersion processing 1～15min, obtain finely dispersed 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) pressure filtration molding in the moving magnetic field
Slurry is charged in the plaster mold, mould applies moving magnetic field more than 1 time outward, magnetic field intensity is 0.1～10T, Movement in Magnetic Field speed is 0.1～500mm/s, the direction of motion and magnetic direction are 0～180 °, subsequently slurry is exerted pressure, and 10～120min is handled in pressurize under the pressure of 0.1～12Mpa;
4) sintering
Remove mould after the curing; and, place punching block 35～60 ℃ of slowly oven dry down, under the pressure of 0.1～1GPa, suppress; sinter molding in argon gas or protection of nitrogen gas environment is warming up to 500～1200 ℃, and heating rate is 100～400 ℃/h; insulation l～3h; be heated to 1000～1600 ℃ again, insulation l～3h cools to 100～400 ℃ of taking-ups at last with the furnace.
2. the gel injection moulding preparation of functionally gradient material (FGM) in a kind of moving magnetic field according to claim 1 is characterized in that described metal or compound with different magnetic is Fe, Co, Ni alloy, ferrite or rare earth permanent-magnet powder.
3. the gel injection moulding preparation of functionally gradient material (FGM) in a kind of moving magnetic field according to claim 1 is characterized in that described metal or compound with different magnetic is Al, Cu, Mg or Sb alloy.
4. the gel injection moulding preparation of functionally gradient material (FGM) in a kind of moving magnetic field according to claim 1 is characterized in that described metal or compound with different magnetic is ZrO
2, SiC, AlN, Si
3N
4, B
4C, SiO
2, TiC, Y
2O
3Or Al
2O
3
5. the pressure filtration molding preparation method of functionally gradient material (FGM) in a kind of moving magnetic field according to claim 1 is characterized in that described moving magnetic field is the magnetic field that is produced by electromagnet, permanent magnet or superconducting magnet.
6. the pressure filtration molding preparation method of functionally gradient material (FGM) in a kind of moving magnetic field according to claim 1 is characterized in that the organic additive of described adding is poly-ethylene fluoride, melmac or phenolic resins.
7. the pressure filtration molding preparation method of functionally gradient material (FGM) in a kind of moving magnetic field according to claim 1 is characterized in that described applied pressure is 0.1～10Mpa, and the dwell time is 10～100min.
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