CN104201279A - Preparation method for magnetostrictive material and magnetostrictive material - Google Patents
Preparation method for magnetostrictive material and magnetostrictive material Download PDFInfo
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- CN104201279A CN104201279A CN201410361622.7A CN201410361622A CN104201279A CN 104201279 A CN104201279 A CN 104201279A CN 201410361622 A CN201410361622 A CN 201410361622A CN 104201279 A CN104201279 A CN 104201279A
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Abstract
The invention discloses a preparation method for magnetostrictive material and the magnetostrictive material. The preparation method for the magnetostrictive material includes that providing raw material nanometer powder slurry; extruding the slurry, accumulating in linear shape to form a pre-designed three-dimensional model to obtain a sample blank; drying and sintering the sample blank to obtain the cured magnetostrictive material. The preparation method for the magnetostrictive material realizes to manufacture the magnetostrictive material through a three-dimensional mold-less slurry direct-write forming technique, the technique is simple and controlled through program, and different slurry and structure models can be prepared according to needs; the preparation method for the magnetostrictive material manufactures the magnetostrictive material with the complex grid structure in one time, and accordingly the production cost is lowered, the agility is improved, and the magnetostrictive characteristic is greatly improved.
Description
Technical field
The present invention relates to magnetic functional material preparing technical field, in particular a kind of preparation method of magnetostrictive material and magnetostrictive material.
Background technology
Pottery three-dimensional is a kind of mould that do not rely on without the straight write forming technology of mould slurry, do not need preparation miniature scale 3 D complex structure function ceramic material that subsequent external processes without the straight write forming method of mould.This technology is to take air pressure raw material to be extruded as power, by computer program, control successively moulding of former and obtain designed structure, it is a kind of method that integrates computer-aided design, precision optical machinery and materialogy, can be used for the processing to high polymer, functional ceramic and some soft materials (as paraffin), especially aspect the preparation of functional ceramic device, have the features such as shaping speed is fast, the manufacturing cycle is short, its path width is from sub-micron to millimeter rank.
Because magnetostrictive material are under magnetic fields, its length changes, can be subjected to displacement and do work or can occur repeatedly to uphold and shorten at action of alternating magnetic field, thereby produce vibration or sound wave, this material can convert electromagnetic energy (or electromagnetic information) to mechanical energy or acoustic energy (or mechanical displacement information or acoustic intelligence), on the contrary also can be by mechanical energy (or mechanical displacement and information).Convert electromagnetic energy (or electromagnetic information) to, it is important energy and information conversion function material.It is in the underwater acoustic transducer technology of sonar, and the high-tech sectors such as electroacoustic transducer technology, marine exploration and development technique, Micro-displacement Driving, vibration damping and vibrationproof, noise abatement and noise control system, intelligent wing, robot, automatic technology, fuel injection technic, valve, pump, fluctuation oil recovery have wide practical use.But in the preparation method of current magnetostrictive material, manufacturing process is all too complicated, and cost is high, product Magnetostriction is poor.
Therefore, prior art has yet to be improved and developed.
Summary of the invention
The technical problem to be solved in the present invention is, above-mentioned defect for prior art, a kind of preparation method and magnetostrictive material of magnetostrictive material are provided, can effectively solve in prior art magnetostrictive material manufacturing process too complicated, and the defect that cost is high, product Magnetostriction is poor.
The technical scheme that technical solution problem of the present invention adopts is as follows:
A preparation method for magnetostrictive material, wherein, described method comprises step:
The slurry of A, the nano powder of supplying raw materials;
B, described slurry is extruded, be linear and be piled into the threedimensional model of design in advance, obtain sample base substrate;
C, described sample idiosome is carried out to drying and sintering processing, obtain curing magnetostrictive material.
The preparation method of described magnetostrictive material, wherein, described steps A Raw nano powder is Fe
2o
3,, Fe
3o
4, Mn-Zn-Fe ferrite, Ni-Zn-Fe ferrite or TbO
0.3dy
0.7fe
1.95.
The preparation method of described magnetostrictive material, wherein, described step B specifically comprises:
B1, described slurry is stored in and can carries out in the syringe of three-dimensional motion;
B2, described syringe, by predefined orbiting motion, promote the piston in syringe by nitrogen simultaneously, and described slurry is extruded from syringe;
B3, described slurry are on the ceramic substrate that is piled up in pedestal of lines, until be piled into the threedimensional model of design in advance, obtain sample base substrate.
The preparation method of described magnetostrictive material, wherein, the described threedimensional model of design is in advance that cross section is the cuboidal yard structure of 10mm * 10mm, and described yard structure has 8 layers, and same layer adjacent lines spacing is 1mm.
The preparation method of described magnetostrictive material, wherein, the speed that described syringe moves is 3-8 mm/s.
The preparation method of described magnetostrictive material, wherein, described step C specifically comprises:
C1, described sample idiosome is put into the environment that is full of argon gas, at the temperature of 300-500 ℃, preheat 0.5-1.5h, obtain pre-warmed sample idiosome;
C2, described pre-warmed sample idiosome is put into the environment that is full of argon gas, and with 4-6 ℃/min heating-up temperature is warming up to 1000-1200 ℃ from 300-500 ℃, be then incubated 1-3h, be finally cooled to 20-30 ℃, obtain curing magnetostrictive material.
Based on said method, the present invention also provides a kind of magnetostrictive material, and wherein, described magnetostrictive material make by the preparation method of described magnetostrictive material.
The preparation method of a kind of magnetostrictive material provided by the present invention and magnetostrictive material, method comprises: the slurry of the nano powder of supplying raw materials; Described slurry is extruded, be linear and be piled into the threedimensional model of design in advance, obtain sample base substrate; Described sample idiosome is carried out to drying and sintering processing, obtain curing magnetostrictive material.The present invention has realized the manufacture of magnetostrictive material without the straight write forming technique of mould slurry by three-dimensional, this technique is simple, program control, can prepare as required different slurries, project organization model, disposable manufacture has the magnetostrictive material of complex mesh structure, thereby reduced production cost, improved flexibility, Magnetostriction is also greatly improved simultaneously.
Accompanying drawing explanation
Fig. 1 is the flow chart of preparation method's preferred embodiment of magnetostrictive material of the present invention.
Fig. 2 is the particular flow sheet of sample idiosome extrusion molding in the preparation method of magnetostrictive material of the present invention.
Fig. 3 a, Fig. 3 b are respectively stereogram, the front views of yard structure of the present invention.
Fig. 4 a, Fig. 4 b are respectively vertical view, the end views of yard structure of the present invention.
Fig. 5 carries out the particular flow sheet of drying and sintering to sample idiosome in the preparation method of magnetostrictive material of the present invention.
Fig. 6 is the careful telescopicing performance test result coordinate diagram of yard structure of the present invention.
Embodiment
For making object of the present invention, technical scheme and advantage clearer, clear and definite, referring to accompanying drawing, developing simultaneously, the present invention is described in more detail for embodiment.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The preparation method of magnetostrictive material
The present invention implements preparation method of the present invention with straight write forming equipment.Straight write forming equipment used in the present invention, for example, can be comprised of the gentle pumping system two parts of formation system that are positioned on three-dimensional motion platform.Wherein, formation system utilizes mould-free forming platform to prepare three-dimensional structure.Slurry is stored in syringe, and syringe can move in three dimensions, and these two parts are controlled by microcomputer.During work, the slurry in syringe promotes piston by high pure nitrogen and is extruded by syringe needle, be linear and be piled up on pedestal, according to the size of syringe needle diameter, can machine-shaping the bar that is different-diameter.Syringe can be in the x-direction and the motion of y direction, completes after one deck two-dimensional structure, and syringe certain height that rises in the z-direction repeats second layer structure in x-y face.So successively moulding successively, can complete final three-dimensional structure.
Refer to Fig. 1, Fig. 1 is the flow chart of preparation method's preferred embodiment of magnetostrictive material of the present invention.As shown in Figure 1, the preparation method of described magnetostrictive material, comprises the following steps:
The slurry of step S100, the nano powder of supplying raw materials;
Prepare the basis that high-quality gel slurry is the straight write forming technology of whole slurry.The gel slurry that can construct the three-dimensional periodic structure with span need to meet two conditions below: first, slurry must have good viscoplasticity, this means that slurry can flow out under shear stress from extrusion molding syringe needle, even also can solidify immediately to keep predetermined injection forming shape in the situation that the relevant position of one deck does not have to support below; Secondly, slurry must have high solid content in volume and reduce the contraction being caused by dry as far as possible, that is to say that particle network must can resist the shrinkage stress being caused by capillarity.These standard-requireds are carefully controlled the active force between particle, first obtain highly filled stable dispersion slurry, then by changing pH value, ionic strength or the solvent quality of slurry, make slurry system produce the change of properties from fluid to gel.
For the ease of disperseing and extruding, raw material of the present invention preferably adopts the magnetostrictive material raw material of nano powder form.The magnetostrictive material nano powder using in the present invention comprises magnetostrictive Metal and Alloy, ferrite mangneto telescopic material and rare earth intermetallic compound magnetostrictive material.Concrete, be applicable to raw material nano powder of the present invention and be preferably Fe
2o
3,, Fe
3o
4, Mn-Zn-Fe ferrite, Ni-Zn-Fe ferrite or TbO
0.3dy
0.7fe
1.95.
Above-mentioned slurry is by being scattered in nano powder raw material in solvent and preparing.Described solvent is to pass through solvent dry, that sintering process is removed,, can select as required.Be preferably volatile solvent such as methyl alcohol, ethanol, acetone, water etc., be preferably water, particularly deionized water.Can be single solvent of planting, can be also the mixture of multi-solvents.
For the effect of extruding obtaining, can suitably add therein pH adjusting agent as acetic acid or ammoniacal liquor etc.In order to obtain required fluid property, can also call in the auxiliary materials such as surfactant, binding agent, tension regulator, thickener, wetting agent, filler.For avoiding affecting the Magnetostriction of resulting devices, these adding ingredients are preferably selected the auxiliary material that can remove in dry, sintering process.
In addition, in raw material, can also add for strengthening the supporting material of final products mechanical performance.
In a scheme of the present invention, nano-powder dispersion, in deionized water, and is added to dispersant and binding agent, obtain slurry.
Step S200, described slurry is extruded, be linear and be piled into the threedimensional model of design in advance, obtain sample base substrate.
In embodiments of the invention, by CAD Software for Design, need the Complicated Spatial Structure of the sample of moulding, and the concrete moving line of syringe needle is extruded in design therein.After complete design, convert this design result to code language that machine can be identified, and add speed, acceleration etc. to control parameter, generate compiler language file, deposit controller module in.Under the control of driver, three-dimensional motion platform drives extrusion device to advance according to the path of design, completes the motion process of three-D space structure, construct out design without the straight write forming sample of mould base substrate.
In forming process, syringe translational speed is 0.1-20mm/s, and preferred 3-8 mm/s, with the lines generation deformation that prevents that span is larger.Optimum, described syringe translational speed is 5 mm/s.
According to the difference of technique and actual needs, the lines diameter of extruding can be for tens to hundreds of micron.This can control by extruding the aperture of syringe needle, is generally not more than 1mm, for example, within the scope of 15-1000 μ m, more preferably within the scope of 50-500 μ m.As long as have time enough and raw material, can provide the product of the large-size needing.The number of plies of piling up is generally 5-200 layer, preferably 6-20 layer.
In practical operation, the lines of extruding, the mode so that continuous or centre can be interrupted all the time, is piled up on the ceramic substrate of pedestal.As long as formed three-dimensional structure shape can self-supporting, unrestricted.By regulating ratio and the composition of slurry, can keep lines to endure with all one's will, maintain this three-dimensional structure and not cave in.In the process of successively piling up, for stablizing of structure, adjacent layer line orientations is preferably orthogonal.Three-dimensional structure can be for example that outward appearance shown in Fig. 3 a is roughly cuboidal yard structure, also can be even elliposoidal etc. of triangular pyramidal, frustoconical, I-shaped, hemisphere.Interval between lines can equate also can be each other not etc.For example, this interval can first increase rear minimizing with certain rule at grade, even obtains hollow three-dimensional structure.For example, but in order to economize in raw materials, alleviate product weight, the interval between each lines is not exclusively preferably 0, preferably at least 50 μ m, more preferably 0.1-2mm, 1mm.
As further embodiment, as shown in Figure 2, in described step S200, sample idiosome extrusion molding idiographic flow comprises:
Step S201, described slurry is stored in and can carries out in the syringe of three-dimensional motion;
Step S202, described syringe, by predefined orbiting motion, promote the piston in syringe by nitrogen simultaneously, and described slurry is extruded from syringe;
Step S203, described slurry are on the ceramic substrate that is piled up in pedestal of lines, until be piled into the threedimensional model of design in advance, obtain sample base substrate.
When needs are prepared different magnetoconstriction material, only need to change slurry, this expressing technique is influenced hardly, can adopt same operating procedure and process conditions.
Step S300, described sample idiosome is carried out to drying and sintering processing, obtain curing magnetostrictive material.
For the sample base substrate after moulding with complex three-dimensional structure, owing to still containing more moisture and organic additive, therefore need research material feature in dry and sintering process under thering is 3 D complex structure situation, by intense adjustment be dried and sintering shrinkage process in various parameters reduce and even prevent from various the disadvantageous situation of final molding sample maintenance shape being occurred.
Temperature Distribution and other conditions such as pressure, atmosphere dry and sintering are determined according to the concrete composition of slurry.As required, also can before sintering, be provided with presintering step.
Further as shown in Figure 5, the idiographic flow that in described step S300, sample idiosome is carried out to drying and sintering comprises:
Step S301, described sample idiosome is put into the environment that is full of argon gas, at the temperature of 300-500 ℃, preheat 0.5-1.5h, obtain pre-warmed sample idiosome.
Step S302, described pre-warmed sample idiosome is put into the environment that is full of argon gas, and with 4-6 ℃/min, heating-up temperature is warming up to 1000-1200 ℃ from 300-500 ℃, then be incubated 1-3h, be finally cooled to 20-30 ℃, obtain curing magnetostrictive material.
Obviously; shape in dry run keeps; need to accurately control temperature, humidity and the change procedure thereof in dry run by environmental test chamber; find best dry relevant parameter, by the temperature in reasonable control dry run, humidity, change and select suitable protection solvent can make dry rear sample well keep shape.Also need the sintering shrinkage process of different materials system labyrinth to study respectively, as find the temperature range of the binder removal (eliminating organic substance) of every individual system the best; For the smaller sample of characteristic cross-section size, also need to adopt two-part sintering method different and ordinary sinter method, can obtain like this three-D space structure material still with nanometer-size die feature after sintering, this little grainiess can prevent that crystal grain from too growing up and destroying original three-D space structure, to the maintenance of net shape, is very favourable.
Magnetostrictive material
Different from the block magnetostrictive material that existing method is manufactured, the magnetostrictive material that the present invention is prepared without the straight write forming technique of mould slurry by three-dimensional typically have yard structure.Particularly, by lines continuous and/or that be interrupted, pile up and form.The number of plies of piling up is generally 5-200 layer, preferably 6-20 layer.Adjacent layer line orientations is preferably orthogonal.Lines diameter can, for tens to hundreds of micron, generally be not more than 1mm, for example, within the scope of 15-1000 μ m, more preferably within the scope of 50-500 μ m.
Three-dimensional structure can be for example that outward appearance shown in Fig. 3 a is roughly cuboidal yard structure, also can be even elliposoidal etc. of triangular pyramidal, frustoconical, I-shaped, hemisphere.
Interval between each lines is not exclusively preferably 0, preferably at least 50 μ m, more preferably 0.1-2mm, for example 1mm.
Surprisingly, in the situation that material is identical, compare with existing block magnetostrictive material, magnetostrictive material of the present invention can obtain the equal Magnetostriction even improving.For example, the magnetostriction coefficient obtaining under magnetic field can improve more than 5%, preferably more than 10%, more preferably more than 20%, or more than 40%, even more preferably more than 50%.
Embodiment
The preparation of magnetostrictive material
In illustrative embodiment, the air supporting three-dimensional motion platform that the mould-free forming platform Shi You U.S. Aerotech company of use produces.Itself mechanical movement precision can reach 400nm, required precision that can capable of meeting requirements on three-dimensional motion.
Air pump system adopts air pump EFD U1traTM 2400 that A Nordson Company manufactures to promote the power of piston, its output pressure scope: 0 ~ 689.5kPa so that moulding to be provided.The syringe capacity using in the present embodiment is 30ml, φ 22.5mm; Syringe needle internal diameter is 0.5mm, and corresponding operating air pressure is controlled between 480 ~ 580kPa, and air pump system is controlled slurry in syringe and is extruded on the ceramic substrate being positioned on pedestal with certain speed.
The threedimensional model of described design is in advance by Fe
3o
4the yard structure of 10mm * 10mm that slurry forms, described yard structure has 8 layers, and same layer adjacent lines spacing is 1mm, and concrete structure refers to Fig. 3 a, Fig. 3 b, Fig. 4 a and Fig. 4 b, it is respectively the stereogram of yard structure of the present invention, front view, vertical view and end view.
It is 5 mm/s that syringe translational speed is set, and from described needle tubing, extrudes Fe
3o
4slurry, arranges lines with 1mm spacing in x, y direction, and superposes in z direction, forms three-dimensional structure.
By described sample idiosome pre-burning 1h in ar gas environment at 400 ℃, make structure preliminarily dried.Pre-warmed sample idiosome carries out sintering processes in high temperature furnace (Nabertherm).First, under argon gas atmosphere, with the programming rate of 5 ℃/min, be warming up to 1100 ℃, be then incubated two hours, be finally reduced to room temperature, obtain curing magnetostrictive material.
The performance evaluation of magnetostrictive material
Use JEOL JSM-7001F field emission scanning electron microscope to observe curing magnetostrictive material.
From Fig. 3 a, Fig. 3 b, Fig. 4 a and Fig. 4 b, after sintering, sample overall structure keeps complete, and upper and lower surface is parallel, without warpage; Lines diameter after sintering is about 400 μ m; Lines (center) spacing is about 900 μ m.From the cross section of sample, lower floor's lines are not because of the deformation that bends of the Action of Gravity Field of upper strata lines.
And then, utilize strain gauge method to test the Magnetostriction of sample.
Fig. 6 has provided the careful telescopicing performance test result of yard structure of the present invention.As shown in Figure 6, the magnetostriction coefficient of the long-pending structure sample of yard is greater than the magnetostrictive material of traditional structure, and magnetostriction coefficient can reach 60ppm.With same kind material (Fe
3o
4) magnetostrictive material (about 30ppm) of the block structure that obtains by conventional method compare, Magnetostriction improves about 1 times (100%), has obtained excellent effect.
Compared with the conventional method, the slurry preparation method of this technique is simple, and the selection of paste composition has very much higher sample.By simple extrusion molding, can design complicated stack architecture, be applied to various fields.
Should be understood that, application of the present invention is not limited to above-mentioned giving an example, and for those of ordinary skills, can be improved according to the above description or convert, and all these improvement and conversion all should belong to the protection range of claims of the present invention.
Claims (7)
1. a preparation method for magnetostrictive material, is characterized in that, described method comprises step:
The slurry of A, the nano powder of supplying raw materials;
B, described slurry is extruded, be linear and be piled into the threedimensional model of design in advance, obtain sample base substrate;
C, described sample idiosome is carried out to drying and sintering processing, obtain curing magnetostrictive material.
2. the preparation method of magnetostrictive material according to claim 1, is characterized in that, described steps A Raw nano powder is Fe
2o
3,, Fe
3o
4, Mn-Zn-Fe ferrite, Ni-Zn-Fe ferrite or TbO
0.3dy
0.7fe
1.95.
3. the preparation method of magnetostrictive material according to claim 1, is characterized in that, described step B specifically comprises:
B1, described slurry is stored in and can carries out in the syringe of three-dimensional motion;
B2, described syringe, by predefined orbiting motion, promote the piston in syringe by nitrogen simultaneously, and described slurry is extruded from syringe;
B3, described slurry are on the ceramic substrate that is piled up in pedestal of lines, until be piled into the threedimensional model of design in advance, obtain sample base substrate.
4. the preparation method of magnetostrictive material according to claim 3, is characterized in that, the described threedimensional model of design is in advance that cross section is the cuboidal yard structure of 10mm * 10mm, and described yard structure has 8 layers, and same layer adjacent lines spacing is 1mm.
5. the preparation method of magnetostrictive material according to claim 3, is characterized in that, the speed that described syringe moves is 3-8 mm/s.
6. the preparation method of magnetostrictive material according to claim 1, is characterized in that, described step C specifically comprises:
C1, described sample idiosome is put into the environment that is full of argon gas, at the temperature of 300-500 ℃, preheat 0.5-1.5h, obtain pre-warmed sample idiosome;
C2, described pre-warmed sample idiosome is put into the environment that is full of argon gas, and with 4-6 ℃/min heating-up temperature is warming up to 1000-1200 ℃ from 300-500 ℃, be then incubated 1-3h, be finally cooled to 20-30 ℃, obtain curing magnetostrictive material.
7. magnetostrictive material, is characterized in that, described magnetostrictive material make by the preparation method of magnetostrictive material as described in claim 1-6 any one.
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| CN106825542A (en) * | 2017-01-19 | 2017-06-13 | 吉林大学 | Negative poisson's ratio high-magnetostriction material and its increasing material manufacturing method |
| CN107555983A (en) * | 2017-09-11 | 2018-01-09 | 横店集团东磁股份有限公司 | A kind of soft magnetism magnetostrictive ferrite material and preparation method thereof |
| CN109550930A (en) * | 2017-09-26 | 2019-04-02 | 中国科学院金属研究所 | A kind of application of magnetoelastic material in 4D printing |
| CN113444898A (en) * | 2021-06-11 | 2021-09-28 | 北京奥特美克科技股份有限公司 | Preparation method of micro displacement sensor sensitive element waveguide wire |
| WO2023176869A1 (en) * | 2022-03-18 | 2023-09-21 | 国立大学法人東北大学 | Magnetostrictive material, energy conversion member, method for manufacturing same, and vibration power generator |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106825542A (en) * | 2017-01-19 | 2017-06-13 | 吉林大学 | Negative poisson's ratio high-magnetostriction material and its increasing material manufacturing method |
| CN106825542B (en) * | 2017-01-19 | 2019-03-22 | 吉林大学 | Negative poisson's ratio high-magnetostriction material and its increasing material manufacturing method |
| CN107555983A (en) * | 2017-09-11 | 2018-01-09 | 横店集团东磁股份有限公司 | A kind of soft magnetism magnetostrictive ferrite material and preparation method thereof |
| CN107555983B (en) * | 2017-09-11 | 2020-09-01 | 横店集团东磁股份有限公司 | Soft magnetic magnetostrictive ferrite material and preparation method thereof |
| CN109550930A (en) * | 2017-09-26 | 2019-04-02 | 中国科学院金属研究所 | A kind of application of magnetoelastic material in 4D printing |
| CN113444898A (en) * | 2021-06-11 | 2021-09-28 | 北京奥特美克科技股份有限公司 | Preparation method of micro displacement sensor sensitive element waveguide wire |
| WO2023176869A1 (en) * | 2022-03-18 | 2023-09-21 | 国立大学法人東北大学 | Magnetostrictive material, energy conversion member, method for manufacturing same, and vibration power generator |
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Application publication date: 20141210 |