CN102766792B - Preparation method of binding rare-earth iron giant magnetostrictive material - Google Patents
Preparation method of binding rare-earth iron giant magnetostrictive material Download PDFInfo
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- CN102766792B CN102766792B CN 201210201667 CN201210201667A CN102766792B CN 102766792 B CN102766792 B CN 102766792B CN 201210201667 CN201210201667 CN 201210201667 CN 201210201667 A CN201210201667 A CN 201210201667A CN 102766792 B CN102766792 B CN 102766792B
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Abstract
The present invention relates to a preparation method of a binding rare-earth iron giant magnetostrictive material. The method comprises the following steps: first mixing metal raw materials according to the above proportion; carrying out arc melting under protection of high-purity argon to obtain an alloy ingot; and then conducting homogenizing annealing at 700-950 DEG C for 45-50 h, and cooling in a furnace to room temperature; then crushing and grinding the alloy ingot into powder with particle size of 50-180 mum; after compaction, conducting a secondary stress annealing under protection of high-purity argon at 300-500 DEG C for 5-8 h; and finally mixing the powder with a binder, adding the mixture into a mold for press molding, and curing the mixture in a magnetic field for 36-48 h after demolding, so as to finally obtain the bonding rare-earth iron giant magnetostrictive material. According to the invention, a bonding method comprising secondary annealing and magnetic field orientation is employed to significantly reduce the stress of alloy powder, and endow the prepared rare-earth giant magnetostrictive material with obviously improved magnetostriction coefficient, dynamic magnetostriction coefficient and magnetic-mechanical coupling coefficient; while the material has high electrical resistivity, and improved high frequency characteristic.
Description
Technical field
The invention belongs to the Materials Science and Engineering field, be specially a kind of preparation method of bonding rare earth iron super magnetostriction material, relate in particular to the remarkable increase of the dynamic magnetostriction coefficient of bonding rare earth iron super magnetostriction material.
Technical background
Rare-earth-iron super magnetostriction material is a kind of new function material that can produce huge dilatation under magnetic field, it has the characteristics such as magnetostriction is large, energy density is high, fast response time, therefore aspect low-frequency high-power underwater acoustic transducer, precise control system, active weakening and sensor, is being used widely.At present, the preparation method of rare-earth-iron super magnetostriction material mainly contains directional solidification method, sintering process and mull technique.Directional solidification method can be prepared Magnetostriction material preferably, but exist complicated process of preparation, cost expensive, be difficult to prepare complicated shape and the problem such as high frequency characteristics is poor.While adopting mull technique to prepare rare earth ultra-magnetostriction material, usually the powdered alloy after melting, grinding is evenly mixed with resin glue, then be pressed into the matrix material of definite shape.Although adding of binding agent descends the magnetic property of material to some extent, mull technique have technique simple, can be made into complicated shape material and the advantage such as with low cost.Some investigators adopt mull technique to prepare the rare-earth-iron giant magnetostrictive material, studied the magnetostriction of material, dynamically magnetostriction coefficient and magnetic mechanical percentage coupling (Hudson etc., J.Appl.Phys., 1998,83(11), 7255; Sandlund etc., J.Appl.Phys., 1994,75(10), 5656; Xie Wei etc., Metallic Functional Materials, 2001,8(4), 29).But the Magnetostriction of the material of preparation, especially dynamic magnetostriction coefficient and magnetic mechanical percentage coupling are on the low side, and (the common dynamic magnetostriction coefficient is 1.8nmA
-1, the magnetic mechanical percentage coupling is 0.28), limited the application of agglutinate rare earth ultra-magnetostriction material.The complicated process of preparation existed in technology for current rare-earth-iron super magnetostriction material, cost be expensive, be difficult to prepare the problems such as the high frequency characteristics of complicated shape material and material is poor, proposes a kind of adhesive method of second annealing, magnetic field orientating that adopts and prepare giant magnetostrictive material.The method have preparation technology simple, can be made into the advantages such as complicated shape material, high frequency characteristics with low cost and material are good, obviously improve the kinetic characteristic of bonding rare earth iron super magnetostriction material.
Summary of the invention
The complicated process of preparation that the objective of the invention is to exist in the technology for current rare-earth-iron super magnetostriction material, cost be expensive, be difficult to prepare the problems such as the high frequency characteristics of complicated shape material and material is poor, proposes a kind of preparation method of bonding rare earth iron super magnetostriction material.The method adopts the adhesive method of second annealing, magnetic field orientating, have preparation technology simple, can be made into the advantages such as complicated shape material, high frequency characteristics with low cost and material are good, can obviously improve the kinetic characteristic of bonding rare earth iron super magnetostriction material.
Technical scheme of the present invention is:
A kind of preparation method of bonding rare earth iron super magnetostriction material, this material composition is (R
xdy
1-x) Fe
y, wherein R is Tb or Sm, and the scope of x is between 0.25-0.9, and the scope of y is between 1.5-2.0; Starting material adopt high pure metal Tb, Dy, Sm, Fe, and the weight percentage of purity is 99.9%; Its preparation method comprises the following steps:
At first after raw material metal being mixed according to the above ratio under high-purity argon gas protection arc melting obtain alloy cast ingot, alloy pig carries out 700-950 ℃ under the high-purity argon gas protection, 45-50 hour homogenizing annealing, stove is chilled to room temperature, then under the organic liquid protection, alloy pig is pulverized, grind to form the powder that granularity is 50-180 μ m, carry out 300-500 ℃ after compacting under the high-purity argon gas protection, the secondary of 5-8 hour moves back stress annealing, finally by powder and binding agent powder in mass ratio: binding agent=100:6-8 mixes, put into the mould press molding, solidify 36-48 hour after moving back mould in magnetic field, finally obtain the bonding rare earth iron super magnetostriction material.
Described binding agent can be epoxy adhesive, and model is HY-914;
Described organic liquid can be high purity alcohol, purity >=99.7%.
Described moving back after mould while in magnetic field, solidifying mixing material, solidify field direction perpendicular to sample axially.
Due to the adhesive method that has adopted second annealing, magnetic field orientating, reduced significantly the stress of powdered alloy, the magnetostriction of the rare earth ultra-magnetostriction material of preparation, dynamic magnetostriction coefficient and magnetic mechanical percentage coupling are obviously improved, compare (Hudson etc. with background technology, J.Appl.Phys., 1998,83(11), 7255; Sandlund etc., J.Appl.Phys., 1994,75(10), 5656; Xie Wei etc., Metallic Functional Materials, 2001,8(4), and 29), the magnetostriction of the material of preparation improves 11%, and dynamically magnetostriction coefficient improves 49%, and the magnetic mechanical percentage coupling improves 43%-54%.Simultaneously, material has higher resistivity, and high frequency characteristics is good.Therefore, the method for invention is significant for application and the device exploitation of rare earth ultra-magnetostriction material.
The accompanying drawing explanation
Fig. 1 is the Tb that in embodiment 1 prepared by adhesive method
0.3dy
0.7fe
1.9the magnetostriction of material and the relation curve in magnetic field;
Fig. 2 is the Tb that in embodiment 1 prepared by adhesive method
0.3dy
0.7fe
1.9the dynamic magnetostriction coefficient d of material
33relation curve with magnetic field;
Fig. 3 is the Tb that in embodiment 1 prepared by adhesive method
0.3dy
0.7fe
1.9the magnetic mechanical percentage coupling of material and the relation curve in magnetic field;
Fig. 4 is the Sm that in embodiment 2 prepared by adhesive method
0.88dy
0.12fe
1.9the magnetostriction of material and the relation curve in magnetic field;
Fig. 5 is the Tb that in embodiment 3 prepared by adhesive method
0.25dy
0.75fe
2the magnetostriction of material and the relation curve in magnetic field;
Fig. 6 is the Tb that in embodiment 4 prepared by adhesive method
0.35dy
0.65fe
1.8the magnetostriction of material and the relation curve in magnetic field;
Fig. 7 is the Sm that in embodiment 5 prepared by adhesive method
0.8dy
0.2fe
1.6the dynamic magnetostriction coefficient d of material
33relation curve with magnetic field.
Embodiment
The present invention adopts the adhesive method of second annealing, magnetic field orientating, and the bonding rare earth iron super magnetostriction material of preparation has improved the characteristic of bonding rare earth iron super magnetostriction material, has especially improved the kinetic characteristic of material.Can be prepared into diameter is 5-20mm, the sample that length is 10-40mm.The adhesive method of second annealing of the present invention, magnetic field orientating, the Magnetostriction of prepared material, especially dynamically magnetostriction coefficient and magnetic mechanical percentage coupling obviously improve.
Embodiment 1
(1) by purity, be after 99.9% Tb, Dy and the block raw material of Fe metal mix according to mol ratio Tb:Dy:Fe=0.3:0.7:1.9 in the sweet pot of the electric arc furnace of packing into, electric arc furnace first vacuumizes and reaches 5 * 10
-3more than Pa, with high-purity argon gas, rinse twice, then under the protection of high-purity argon gas, carry out melting, melting electric current 150-180 ampere, the time is 20-30 second, by the alloy pig upset, melting obtains the uniform alloy pig of composition for 3 times afterwards.
(2) the alloy pig surface treatment after melting is clean, with the molybdenum foil parcel, be sealed in the silica tube that vacuumizes, is filled with high-purity argon gas, wherein vacuum reaches 5 * 10
-3pa.Homogenizing annealing in tube type resistance furnace, 950 ℃ of annealing temperatures, annealing time are 50 hours, then the alloy pig stove are chilled to 20 ℃ of room temperatures.
(3) the alloy pig removing surface after annealing is clean; applying pressure is made granularity by alloy pig and is less than the 0.5mm particle; then the alloy of pulverizing is soaked as in purity >=99.7% spirituous solution, under the protection of spirituous solution, the alloy after annealing is ground to form to the powder that granularity is 50-180 μ m in the sweet pot of agate.
(4) by granularity, be the compacting of pressurizeing of packing in mould of the powder of 50-180 μ m, pressure is 20MPa, and the sample moved back after mould tightly wraps up with molybdenum foil, is packaged in the silica tube that vacuumizes, is filled with high-purity argon gas, and vacuum reaches 5 * 10
-3pa.Carry out second annealing in tube type resistance furnace, annealing temperature is that 400 ℃, annealing time are 6 hours.
(5) sample after second annealing is put into to sweet pot and pulverized, make sample revert to the powder that granularity is 50-180 μ m.
(6) by granularity, be the powder of 50-180 μ m and model be petrel board HY-914 epoxy adhesive in mass ratio, powder: binding agent=100:6 is placed in sweet pot and mixes, mechanical stirring is even, then the matrix material mixed is put into to the pressure forming that mould adds 80-100MPa, move back mould and obtain the certain size matrix material.
(7) matrix material is solidified in magnetic field, curing magnetic field is 500kA/m, and field direction is axial perpendicular to sample, and be 48 hours set time, after solidifying, obtains the certain size composite sample.
Can find out bonding Tb from accompanying drawing 1
0.3dy
0.7fe
1.9alloy sample has higher magnetostriction numerical value under downfield, and when magnetic field is 100kA/m, magnetostriction can reach 465 * 10
-6.
Can find out bonding Tb from accompanying drawing 2
0.3dy
0.7fe
1.9the dynamic magnetostriction coefficient d of alloy sample
33obtain maximum value under 60kA/m magnetic field, 2.69nmA
-1, dynamically magnetostriction coefficient is than the raising of bibliographical information 49%.
Can find out bonding Tb from accompanying drawing 3
0.3dy
0.7fe
1.9alloy sample has very high magnetic mechanical percentage coupling in the 90-150kA/m magnetic field range, and maximum value is 0.4, the raising 43%-54% of magnetic mechanical coupling coefficient ratio bibliographical information.
(1) by purity, be after 99.9% Sm, Dy and the block raw material of Fe metal mix according to mol ratio Sm:Dy:Fe=0.88:0.12:1.9 in the sweet pot of the electric arc furnace of packing into, electric arc furnace first vacuumizes and reaches 5 * 10
-3more than Pa, with high-purity argon gas, rinse twice, then under the protection of high-purity argon gas, carry out melting, 120-150 amperes, melting electric current, the time is 20-30 second, then, by the alloy pig upset, melting obtains the uniform alloy pig of composition for 3 times.
(2) the alloy pig surface treatment after melting is clean, with the molybdenum foil parcel, be sealed in the silica tube that vacuumizes, is filled with high-purity argon gas, wherein vacuum reaches 5 * 10
-3pa.Homogenizing annealing in tube type resistance furnace, 750 ℃ of annealing temperatures, annealing time are 48 hours, then the alloy pig stove are chilled to 20 ℃ of room temperatures.
(3) the alloy pig removing surface after annealing is clean, and applying pressure is pulverized alloy pig, then the alloy of pulverizing is soaked as in purity >=99.7% spirituous solution, under the protection of spirituous solution, the alloy after annealing is ground to form to the powder that granularity is 50-180 μ m.
(4) by granularity, be the compacting of pressurizeing of packing in mould of the powder of 50-180 μ m, pressure is 20MPa, with molybdenum foil, tightly wraps up, and is packaged in the silica tube that vacuumizes, is filled with high-purity argon gas, and vacuum reaches 5 * 10
-3pa.Carry out second annealing in tube type resistance furnace, annealing temperature is that 350 ℃, annealing time are 5 hours.
(5) sample after second annealing is put into to sweet pot and pulverized, make sample revert to the powder that granularity is 50-180 μ m.
(6) by granularity, be the powder of 50-180 μ m and model be petrel board HY-914 epoxy adhesive in mass ratio, powder: binding agent=100:8 is placed in sweet pot and mixes, mechanical stirring is even, then the matrix material mixed is put into to the pressure forming that mould adds 100MPa, move back mould and obtain the certain size matrix material.
(7) matrix material is solidified in magnetic field, curing magnetic field is 500kA/m, and field direction is axial perpendicular to sample, and be 48 hours set time, after solidifying, obtains the certain size composite sample.
Can find out bonding Sm from accompanying drawing 4
0.88dy
0.12fe
1.9alloy sample has higher magnetostriction numerical value under downfield, and when magnetic field is 100kA/m, magnetostriction can reach 265 * 10
-6, than the high 43%(J.Alloys Compd. of bibliographical information, 2011,509,4954) and the magnetostriction hysteresis of alloy of preparation less, material is adapted at applying in device.
Embodiment 3
Other step of the present embodiment is with embodiment 1, and difference is: the mol ratio of the metal that step (1) is used is changed to Tb:Dy:Fe=0.25:0.75:2; Annealing temperature in step (2) is 900 ℃, and the time is 50 hours; Second annealing temperature in step (4) is 300 ℃, and the time is 8 hours.
Can find out bonding Tb from accompanying drawing 5
0.25dy
0.75fe
2material (400-500kA/m) under upfield has higher magnetostriction, but (0-150kA/m) is starkly lower than bonding Tb under downfield
0.3dy
0.7fe
1.9the magnetostriction of material.
Embodiment 4
Other step of the present embodiment is with embodiment 1, and difference is: the mol ratio of the metal that step (1) is used is changed to Tb:Dy:Fe=0.35:0.65:1.8; Annealing temperature in step (2) is 900 ℃, and the time is 50 hours; Second annealing temperature in step (4) is 450 ℃, and the time is 5 hours.
Can find out bonding Tb from accompanying drawing 6
0.35dy
0.65fe
1.8the magnetostriction of material is lower than bonding Tb
0.3dy
0.7fe
1.9and Tb
0.25dy
0.75fe
2the magnetostriction of material.
Embodiment 5
Other step of the present embodiment is with embodiment 2, and difference is: the mol ratio of the metal that step (1) is used is changed to Sm:Dy:Fe=0.8:0.2:1.6; Annealing temperature in step (2) is 700 ℃, and the time is 45 hours; Second annealing temperature in step (4) is 300 ℃, and the time is 6 hours.
Can find out bonding Sm from accompanying drawing 7
0.8dy
0.2fe
1.6material has higher dynamic magnetostriction coefficient d in the 90-150kA/m magnetic field range
33.
Claims (1)
1. the preparation method of a bonding rare earth iron super magnetostriction material, it is characterized by this material composition is (R
xdy
1-x) Fe
y, wherein R is Tb or Sm, and the scope of x is between 0.25-0.9, and the scope of y is between 1.5-2.0; Starting material adopt high pure metal Tb, Dy, Sm, Fe, and the weight percentage of purity is 99.9%; Its preparation method comprises the following steps:
At first after raw material metal being mixed according to the above ratio under high-purity argon gas protection arc melting obtain alloy cast ingot, alloy pig carries out 700-950 ℃ under the high-purity argon gas protection, 45-50 hour homogenizing annealing, stove is chilled to room temperature, then under the organic liquid protection, alloy pig is pulverized, grind to form the powder that granularity is 50-180 μ m, carry out 300-500 ℃ after compacting under the high-purity argon gas protection, the secondary of 5-8 hour moves back stress annealing, finally by powder and binding agent powder in mass ratio: binding agent=100:6-8 mixes, put into the mould press molding, solidify 36-48 hour after moving back mould in magnetic field, finally obtain the bonding rare earth iron super magnetostriction material,
Described binding agent is epoxy adhesive;
Described organic liquid is high purity alcohol, purity >=99.7%;
Described moving back after mould while in magnetic field, solidifying mixing material, solidify field direction perpendicular to sample axially.
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| CN106098929A (en) * | 2016-07-24 | 2016-11-09 | 泉州海岸线新材料科技有限公司 | The formula of a kind of high-performance bonding rare earth magnetostriction materials and preparation technology |
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| CN1772937A (en) * | 2005-11-16 | 2006-05-17 | 北京科技大学 | Super magnetostrictive material with super wide work temperature range |
| CN101220437A (en) * | 2008-01-26 | 2008-07-16 | 桂林电子科技大学 | High-performance ring shaped agglutinate rare earth ultra-magnetostriction material, manufacturing method and device thereof |
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| CN1772937A (en) * | 2005-11-16 | 2006-05-17 | 北京科技大学 | Super magnetostrictive material with super wide work temperature range |
| CN101220437A (en) * | 2008-01-26 | 2008-07-16 | 桂林电子科技大学 | High-performance ring shaped agglutinate rare earth ultra-magnetostriction material, manufacturing method and device thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016183761A1 (en) * | 2015-05-18 | 2016-11-24 | 北京大学 | Method for testing local mechanics-magnetic coupling coefficient of magnetic material |
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