CN1490435A - Rareearth supermagnetostrictive material one step preparation and apparatus and products thereof - Google Patents
Rareearth supermagnetostrictive material one step preparation and apparatus and products thereof Download PDFInfo
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- CN1490435A CN1490435A CNA031569269A CN03156926A CN1490435A CN 1490435 A CN1490435 A CN 1490435A CN A031569269 A CNA031569269 A CN A031569269A CN 03156926 A CN03156926 A CN 03156926A CN 1490435 A CN1490435 A CN 1490435A
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- rare earth
- preservation cylinder
- earth ultra
- magnetostriction material
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- 239000000463 material Substances 0.000 title claims abstract description 96
- 229910052761 rare earth metal Inorganic materials 0.000 title claims description 111
- 150000002910 rare earth metals Chemical class 0.000 title claims description 107
- 238000002360 preparation method Methods 0.000 title claims description 27
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 31
- 239000000956 alloy Substances 0.000 claims abstract description 31
- 238000003723 Smelting Methods 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 238000004321 preservation Methods 0.000 claims description 80
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000007669 thermal treatment Methods 0.000 claims description 16
- 238000005516 engineering process Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 238000012856 packing Methods 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 230000006698 induction Effects 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000002826 coolant Substances 0.000 claims description 3
- 238000013461 design Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 238000005273 aeration Methods 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- 239000004020 conductor Substances 0.000 claims 1
- 229910052706 scandium Inorganic materials 0.000 claims 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000009792 diffusion process Methods 0.000 description 57
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 32
- 101100298225 Caenorhabditis elegans pot-2 gene Proteins 0.000 description 17
- 229910052786 argon Inorganic materials 0.000 description 16
- 239000007789 gas Substances 0.000 description 16
- 229910052692 Dysprosium Inorganic materials 0.000 description 9
- 229910052771 Terbium Inorganic materials 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 8
- 239000000498 cooling water Substances 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000004857 zone melting Methods 0.000 description 2
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003280 down draw process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
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Abstract
A one-step process for preparing the super magnetostrictive RE material includes such steps as under the protection of inertial gas or in vacuum state smelting alloy in the crucible contained in the vacuum chamber which also contains insulating cylinder and its separable base connected to a driver for moving it up and down, heating the insulating cylinder to a directional solidifying temp, pouring the molten alloy into the insulating cylinder, pulling the super magnetostrictive RE material out of the insulating cylinder to obtain the directionally solidified rod material, cooling the insulating cylinder to heat treating temp, and raising up the rod material into the insulating cylinder for thermal treating. The resultant material has excellent property.
Description
Technical field
Originally relate to the rare earth ultra-magnetostriction material that invention relates to rare earth ultra-magnetostriction material one-step technology and equipment thereof and adopts this prepared.
Background technology
At present, traditional magnetostriction materials such as Ni, Co, Fe and their alloy have the little shortcoming of magnetostriction coefficient, and Application Areas is restricted.Therefore, people seek the more excellent magnetostriction materials of performance.The surface weapon center A.E.Clark of United States Navy in 1963, people such as R.Bozorth and B.Desavage find heavy rare earth metal in some, as Tb, Dy etc., have bigger 1000 times than Fe, than the big 200 times magnetostriction coefficient of Ni.But middle heavy rare earth metal only shows near the Kelvin's thermodynamic scale zero degree.Therefore, people such as A.E.Clark studies TbFe
2, DyFe
2And SmFe
2Deng the magnetostriction performance of rare earth intermetallic compound, and with the TbFe of magnetocrystalline anisotropy field opposite in sign
2And DyFe
2Form (Tb, Dy) Fe
2, making it becomes practical rare earth ultra-magnetostriction material, and has applied for U.S. Pat 3,949,351 on April 6th, 1976.After this, rare earth ultra-magnetostriction material becomes one of research focus of rare earth functional materials.Early stage patent, as the US4 of on December 29th, 1981 application, 308,474 and the US4 of application on May 29 nineteen eighty-three, 378,258, mainly concentrate on the theory and the composition Study of rare earth ultra-magnetostriction material, preparation technology is a horizontal zone-melting technique.There are shortcomings such as material easily pollutes, shape misconduct, consistency of performance difference in horizontal zone-melting technique.September in 1986 U.S. on the 2nd patent US4,609,402 have announced that the vertical area process of smelting prepares rare earth ultra-magnetostriction material.The technology that this patent is set forth is that first melting obtains Tb-Dy-Fe prealloy rod, fixes by upper and lower anchor clamps then, adopts high frequency (about 450kHz) ruhmkorff coil to distinguish molten the processing from the bottom to top and obtains the rareearth super magnetostrictive bar.Vertical area process of smelting complicated operation, and adopt the high-frequency induction mode to melt, be difficult to obtain the major diameter rare earth ultra-magnetostriction material.September in 1988 U.S. on the 13rd patent US4,770,704 have announced that a kind of down draw process prepares rare earth ultra-magnetostriction material.April in 1989 U.S. on the 4th patent US4,818,304 have announced rareearth super magnetostrictive bar thermomagnetic treatment technology.Above-mentioned two patents have been set forth the Tb-Dy-Fe alloy and have been formed behind the alloy liquation in aperture by the crucible bottom silica tube below flowing into then by induction melting that directional freeze obtains the rareearth super magnetostrictive bar, carry out 400 ℃ of-600 ℃ of thermomagnetic treatment at last.May in 1992 U.S. on the 19th patent US5,114,467 have announced that a kind of using plasma melting technology prepares rare earth ultra-magnetostriction material.This process using screw thread feed appliance is sent previously prepared master alloy powder into the plasma melting district and is formed the alloy liquation, the alloy liquation flows in the water-cooled mould of bottom, and mould moves downward with certain speed and carries out directional freeze and obtain rare earth ultra-magnetostriction material.Rare earth ultra-magnetostriction material impurity (as oxygen) the content height of this prepared, rare earth element scaling loss are serious, composition is difficult to control, material property is relatively poor and consistence is poor.
Summary of the invention
The purpose of this invention is to provide that a kind of technical process is short, production cost is low, production efficiency is high, be suitable for the one-step preparation process of suitability for industrialized production major diameter high-performance rare-earth giant magnetostrictive material.
Another object of the present invention provides the employed equipment of a kind of rare earth ultra-magnetostriction material one-step preparation process.
A further object of the present invention provides the prepared rare earth ultra-magnetostriction material of one-step technology.
For achieving the above object, the present invention takes following technical scheme:
A kind of one-step preparation process of rare earth ultra-magnetostriction material, this preparation technology comprises the steps:
(1), adopts the vacuum chamber that is provided with smelting pot, heat-preservation cylinder and detachable heat-preservation cylinder base in it, wherein, the heat-preservation cylinder base is a hollow form, and bring water outlet into, the bottom of heat-preservation cylinder connects can make its upper and lower mobile drive unit, and vacuum chamber is under vacuum or the protection of inert gas state, and the proportioning raw materials of the rare earth ultra-magnetostriction material of surface cleaning arrives the target component of material design after treatment again, the smelting pot of packing into then carries out alloy melting;
(2), heat-preservation cylinder is heated to more than the rare earth ultra-magnetostriction material fusing point 100 ℃-250C °, it is the directional freeze temperature, molten alloy is poured in the heat-preservation cylinder, after the cast, by the drop-down rare earth ultra-magnetostriction material of drive unit, up to all pulling out heat-preservation cylinder, obtain the bar of the rare earth ultra-magnetostriction material of directional freeze;
(3), heat-preservation cylinder is cooled to thermal treatment temp after, by drive unit bar is risen in the heat-preservation cylinder and to heat-treat,, obtain high-performance＜110 at last through thermal treatment〉rare earth ultra-magnetostriction material of texture.
In described step (2), the directional freeze temperature is 1300 ℃-1550 ℃.
In described step (2), drop-down speed is 30mm/h-240mm/h.
In described step (3), thermal treatment temp is 800 ℃-1250 ℃, and heat treatment time is 1.0-3.0h.
In described step (1), the type of heating of the alloy melting of smelting pot is selected from a kind of in induction heating, resistive heating, electrical spark heating and the plasma heating.
The employed equipment of the one-step preparation process of rare earth ultra-magnetostriction material of the present invention, this equipment is to be provided with smelting pot, heat-preservation cylinder and detachable heat-preservation cylinder base in vacuum chamber from top to bottom successively, wherein, the heat-preservation cylinder base is a hollow form, and bring water outlet into, and connection water inlet pipe and water outlet pipe, the heat-preservation cylinder base connects can make its upper and lower mobile drive unit, vacuum-chamber wall is provided with inflation valve, outside vacuum chamber, be provided with vacuum extractor, and join by vacuum pipe and the vacuum chamber that is provided with vacuum valve.
In above-mentioned equipment, described heat-preservation cylinder is made up of lagging material, and is provided with the heating element by temperature controller control.The heat-preservation cylinder base is to be made by the high material of thermal conductivity (as copper).
In above-mentioned equipment, described drive unit comprises servomotor, reduction box and lifts leading screw, and servomotor connects the lower end that lifts leading screw by reduction box, and the heat-preservation cylinder base connects the upper end that lifts leading screw.Drive unit is made of hydro-cylinder transmission mechanism and the transmission rod that driven thereof.
In above-mentioned equipment, described vacuum extractor is made up of diffusion pump, lobe pump, mechanical pump and vacuum pipe.Lobe pump is connected with mechanical pump.The lobe pump load divides two-way, and one the tunnel connects the preceding step valve of diffusion pump, and another road connects slightly takes out valve and vacuum chamber.The diffusion pump main valve connects vacuum chamber.
The rare earth ultra-magnetostriction material of one-step technology of the present invention preparation be RE (Fe, M)
2-x, RE is rare earth element one or more of totally 17 kinds that comprise Y and Sc, M is Mn, Ni, Al, Co etc., can partly substitute Fe, 0≤x≤0.10.
Described rare earth ultra-magnetostriction material has axial crystalline＜110〉texture.
Advantage of the present invention is:
Long at the rare earth ultra-magnetostriction material technological process of production, production cost is high, be difficult to obtain major diameter and the good shortcomings such as material of consistency of performance, the present invention proposes the rare earth ultra-magnetostriction material one-step preparation process.This technology is that melting, directional freeze and three critical processes of thermal treatment are finished at an equipment, is particularly suitable for preparing rare earth ultra-magnetostriction material.One-step technology has that technical process is short, production cost is low, production efficiency is high, is suitable for suitability for industrialized production major diameter high-performance rare-earth giant magnetostrictive material.Principle of the present invention is: the rareearth super magnetostrictive molten alloy is by directional freeze, can obtain to have＜110〉texture rare earth ultra-magnetostriction material; For reduce the defective that material produces in the directional freeze process, further improving material property heat-treats material, made rare earth ultra-magnetostriction material is a kind of textured material, its＜110〉texture have higher saturation magnetostriction coefficient and a low performance, possess the industrial applications prospect.According to above-mentioned principle, the present invention successfully finishes three critical processes such as melting, directional freeze and thermal treatment of rare earth ultra-magnetostriction material at an equipment.
Description of drawings
Fig. 1 is an one-step technology specific equipment synoptic diagram of the present invention.Label among the figure is: the 1-vacuum chamber; The 2-smelting pot; The 3-molten alloy; The 4-rare earth ultra-magnetostriction material; The 5-heat-preservation cylinder; 6-lifts leading screw; 7-heat-preservation cylinder base; The 8-inflation valve; The 9-servomotor; 10,11, the 14-vacuum valve, promptly diffusion pump main valve 10, slightly take out step valve 14 before the valve 11, diffusion pump; The 12-diffusion pump; 13-lobe pump: 15-mechanical pump.
Fig. 2 is the φ 50mm * magnetostriction performance curve of 300mm rareearth super magnetostrictive bar when prestress is 3.8MPa of the present invention's preparation.
Fig. 3 is the φ 70mm * magnetostriction performance curve of 250mm rareearth super magnetostrictive bar when prestress is 7.7MPa of the present invention's preparation.
Fig. 4 is the x x ray diffration pattern x of the φ 50mm * 300mm rareearth super magnetostrictive bar of the present invention's preparation.
Fig. 5 is the x x ray diffration pattern x of the φ 70mm * 250mm rareearth super magnetostrictive bar of the present invention's preparation.
Fig. 6 is the ODF sciagraph of the φ 50mm * 300mm rareearth super magnetostrictive bar of the present invention's preparation.
Fig. 7 is the ODF stereographic map of the φ 250mm * 300mm rareearth super magnetostrictive bar of the present invention's preparation.
Embodiment
The employed equipment of the one-step preparation process of rare earth ultra-magnetostriction material of the present invention as shown in Figure 1, this equipment is to be provided with smelting pot 2, heat-preservation cylinder 5 and detachable heat-preservation cylinder base 7 in vacuum chamber 1 from top to bottom successively, wherein, heat-preservation cylinder base 7 is a hollow form, and bring water outlet into, and the connection water inlet pipe and water outlet pipe is furnished with control valve on water inlet pipe and water outlet pipe, with the trip switch water coolant.Heat-preservation cylinder base 7 connects the upper end that lifts leading screw 6, and the lower end that lifts leading screw 6 is connected with servomotor 9 by reduction box.Servomotor 9 connects the lower end that lifts leading screw 6 by reduction box, lifts leading screw 6 with drive and moves up and down, and is routine techniques, so no longer describe in detail.Vacuum-chamber wall is provided with aeration aperture, and is furnished with inflation valve 8, is provided with vacuum extractor outside vacuum chamber 1, and vacuum extractor is made up of diffusion pump 12, lobe pump 13, mechanical pump 15.Lobe pump 13 is connected with mechanical pump 15.Lobe pump 13 loads divide two-way, and one the tunnel connects the preceding step valve 14 of diffusion pump, and another road connection is slightly taken out valve 11 and is communicated with vacuum chamber 1.Diffusion pump main valve 10 connects vacuum chamber 1.
In conjunction with Fig. 1 the one-step preparation process of rare earth ultra-magnetostriction material of the present invention is described in detail.
With the proportioning raw materials of the surface cleaning after treatment target component to the material design, the smelting pot 2 of packing into is then built bell, starts mechanical pump 15, opens and slightly take out 11 pairs of vacuum chambers 1 of valve and vacuumize.When vacuum tightness reaches 5Pa-10Pa, close and slightly take out valve 11, start lobe pump 13 and diffusion pump 12, successively open preceding step valve 14 of diffusion pump and diffusion pump main valve 10 and continue vacuum chamber 1 is vacuumized.When vacuum tightness reaches 10
-2Pa-10
-3Behind the pa, close diffusion pump main valve 10, open inflation valve 8 and clean to the argon gas that vacuum chamber 1 charges into about 0.1atm.Close inflation valve 8, open and slightly take out 11 pairs of vacuum chambers 1 of valve and be evacuated down to 5Pa-10Pa.Close and slightly take out valve 11, open 10 pairs of vacuum chambers 1 of diffusion pump main valve and vacuumize.When vacuum tightness reaches 10
-2Pa-10
-3Behind the Pa, close diffusion pump main valve 10, charge into the 0.5atm argon gas to vacuum chamber 1.Start power supply and carry out heating raw and fusing formation molten alloy 3 to smelting pot 2; Open water coolant simultaneously and heat to 100 ℃-250C ° (being generally 1300 ℃-1550 ℃) more than the rare earth ultra-magnetostriction material fusing point to 7 water flowings of heat-preservation cylinder base and to heat-preservation cylinder 5.Molten alloy 3 is poured in the heat-preservation cylinder 5, starts servomotor 9 and all pull out heat-preservation cylinder 5 with certain velocity pull-down up to rare earth ultra-magnetostriction material 4, finally obtain the rare earth ultra-magnetostriction material 4 of directional freeze by lifting leading screw 6.The temperature that reduces heat-preservation cylinder 5 is to thermal treatment temp (being generally 800 ℃-1250 ℃), start servomotor 9 and promote rare earth ultra-magnetostriction material 4 with certain speed and heat-treat 1.0h-3.0h up to all entering heat-preservation cylinder 5 by lifting leading screw 6, obtain high-performance＜110 at last the rare earth ultra-magnetostriction material of texture.
Embodiment 1
Purity is not less than 99.5%Tb, 99.5%Dy and high-purity Fe proportioning Tb
0.3Dy
0.7Fe
2(atomic ratio) 5.41kg smelting pot 2 of packing into is built bell.Start mechanical pump 15, open and slightly take out 11 pairs of vacuum chambers 1 of valve and vacuumize.When vacuum tightness reaches 5Pa-10Pa, close and slightly take out valve 11, start lobe pump 13 and diffusion pump 12, successively open preceding step valve 14 of diffusion pump and diffusion pump main valve 10 and continue vacuum chamber 1 is vacuumized.When vacuum tightness reaches 10
-2Pa-10
-3Behind the Pa, close diffusion pump main valve 10, open inflation valve 8 and clean to the argon gas that vacuum chamber 1 charges into about 0.1atm.Close inflation valve 8, open and slightly take out 11 pairs of vacuum chambers 1 of valve and be evacuated down to 5Pa-10Pa.Close and slightly take out valve 11, open 10 pairs of vacuum chambers 1 of diffusion pump main valve and vacuumize.When vacuum tightness reaches 10
-2Pa-10
-3Behind the Pa, close diffusion pump main valve 10, charge into the 0.5atm argon gas to vacuum chamber 1.Start power supply and carry out heating raw and fusing formation molten alloy 3 to smelting pot 2; Open cooling water intakeoutfall 7 water flowings simultaneously and heat-preservation cylinder 5 is heated to 1300 ℃.Molten alloy 3 is poured in the heat-preservation cylinder 5, starts servomotor 9 and all pull out heat-preservation cylinder 5 so that 60mm/h is drop-down up to rare earth ultra-magnetostriction material 4, finally obtain the rare earth ultra-magnetostriction material 4 of directional freeze by lifting leading screw 6.The temperature that reduces heat-preservation cylinder 5 is to 800 ℃ of thermal treatment temps, start servomotor 9 and heat-treat 2.5h with 400mm/h lifting rare earth ultra-magnetostriction material 4 up to all entering heat-preservation cylinder 5, obtain φ 50mm * 300mm rareearth super magnetostrictive bar at last by lifting leading screw 6.Fig. 2, Fig. 4, Fig. 6 and Fig. 7 are respectively magnetostriction performance curve, x x ray diffration pattern x, ODF sciagraph and the ODF stereographic map of present embodiment φ 50mm * 300mm rareearth super magnetostrictive bar.Accompanying drawing 2 shows that present embodiment prepares φ 50mm * 300mm rareearth super magnetostrictive bar and has good magnetostriction telescopicing performance, and saturation magnetostriction coefficient lambda s reaches 1791.95ppm.Fig. 4, Fig. 6 and Fig. 7 show that present embodiment prepares φ 50mm * 300mm rareearth super magnetostrictive bar and has good＜110〉texture.
Embodiment 2
Purity is not less than 99.5%Tb, 99.5%Dy and high-purity Fe proportioning Tb
0.28Dy
0.72Fe
1.90(atomic ratio) 8.85kg smelting pot 2 of packing into is built bell.Start mechanical pump 15, open and slightly take out 11 pairs of vacuum chambers 1 of valve and vacuumize.When vacuum tightness reaches 5Pa-10Pa, close and slightly take out valve 11, start lobe pump 13 and diffusion pump 12, successively open preceding step valve 14 of diffusion pump and diffusion pump main valve 10 and continue vacuum chamber 1 is vacuumized.When vacuum tightness reaches 10
-2Pa-10
-3Behind the Pa, close diffusion pump main valve 10, open inflation valve 8 and clean to the argon gas that vacuum chamber 1 charges into about 0.1atm.Close inflation valve 8, open and slightly take out 11 pairs of vacuum chambers 1 of valve and be evacuated down to 5Pa-10Pa.Close and slightly take out valve 11, open 10 pairs of vacuum chambers 1 of diffusion pump main valve and vacuumize.When vacuum tightness reaches 10
-2Pa-10
-3Behind the Pa, close diffusion pump main valve 10, charge into the 0.5atm argon gas to vacuum chamber 1.Start power supply and carry out heating raw and fusing formation molten alloy 3 to smelting pot 2; Open cooling water intakeoutfall 7 water flowings simultaneously and heat-preservation cylinder 5 is heated to 1550 ℃.Molten alloy 3 is poured in the heat-preservation cylinder 5, starts servomotor 9 and all pull out heat-preservation cylinder 5 so that 30mm/h is drop-down up to rare earth ultra-magnetostriction material 4, finally obtain the rare earth ultra-magnetostriction material 4 of directional freeze by lifting leading screw 6.The temperature that reduces heat-preservation cylinder 5 is to 1250 ℃ of thermal treatment temps, start servomotor 9 and heat-treat 3h with 400mm/h lifting rare earth ultra-magnetostriction material 4 up to all entering heat-preservation cylinder 5, obtain φ 70mm * 250mm rareearth super magnetostrictive bar at last by lifting leading screw 6.Accompanying drawing 3 and accompanying drawing 5 are respectively the magnetostriction performance curve and the x x ray diffration pattern x of present embodiment φ 70mm * 250mm rareearth super magnetostrictive bar.Fig. 3 shows that present embodiment prepares φ 70mm * 250mm rareearth super magnetostrictive bar and has good magnetostriction telescopicing performance, and saturation magnetostriction coefficient lambda s reaches 1701.4ppm.Fig. 5 shows that present embodiment prepares φ 70mm * 250mm rareearth super magnetostrictive bar and has good＜110〉texture.
Embodiment 3
Purity is not less than 99.5%Tb, 99.5%Dy, high-purity Fe and 99.99%Al proportioning Tb
0.3Dy
0.7Fe
1.83A
10.12(atomic ratio) 6.52kg smelting pot 2 of packing into is built bell.Start mechanical pump 15, open and slightly take out 11 pairs of vacuum chambers 1 of valve and vacuumize.When vacuum tightness reaches 5Pa-10Pa, close and slightly take out valve 11, start lobe pump 13 and diffusion pump 12, successively open preceding step valve 14 of diffusion pump and diffusion pump main valve 10 and continue vacuum chamber 1 is vacuumized.When vacuum tightness reaches 10
-2Pa-10
-3Behind the Pa, close diffusion pump main valve 10, open inflation valve 8 and clean to the argon gas that vacuum chamber 1 charges into about 0.1atm.Close inflation valve 8, open and slightly take out 11 pairs of vacuum chambers 1 of valve and be evacuated down to 5Pa-10Pa.Close and slightly take out valve 11, open 10 pairs of vacuum chambers 1 of diffusion pump main valve and vacuumize.When vacuum tightness reaches 10
-2Pa-10
-3Behind the Pa, close diffusion pump main valve 10, charge into the 0.5atm argon gas to vacuum chamber 1.Start power supply and carry out heating raw and fusing formation molten alloy 3 to smelting pot 2; Open cooling water intakeoutfall 7 water flowings simultaneously and heat-preservation cylinder 5 is heated to 1400 ℃.Molten alloy 3 is poured in the heat-preservation cylinder 5, starts servomotor 9 and all pull out heat-preservation cylinder 5 so that 120mm/h is drop-down up to rare earth ultra-magnetostriction material 4, finally obtain the rare earth ultra-magnetostriction material 4 of directional freeze by lifting leading screw 6.The temperature that reduces heat-preservation cylinder 5 is to 950 ℃ of thermal treatment temps, start servomotor 9 and heat-treat 2h with 400mm/h lifting rare earth ultra-magnetostriction material 4 up to all entering heat-preservation cylinder 5, obtain φ 60mm * 250mm rareearth super magnetostrictive bar at last by lifting leading screw 6.Analytical test shows: present embodiment prepares φ 60mm * 250mm rareearth super magnetostrictive bar and has good＜110〉texture, saturation magnetostriction coefficient lambda s reaches 1750.8ppm under 10Mpa prestress.
Embodiment 4
Purity is not less than 99.5%Tb, 99.5%Dy, high-purity Fe and 99.9%Mn proportioning Tb
0.3Dy
0.7Fe
1.75Mn
0.20(atomic ratio) 2.00kg smelting pot 2 of packing into is built bell.Start mechanical pump 15, open and slightly take out 11 pairs of vacuum chambers 1 of valve and vacuumize.When vacuum tightness reaches 5Pa-10Pa, close and slightly take out valve 11, start lobe pump 13 and diffusion pump 12, successively open preceding step valve 14 of diffusion pump and diffusion pump main valve 10 and continue vacuum chamber 1 is vacuumized.When vacuum tightness reaches 10
-2Pa-10
-3Behind the pa, close diffusion pump main valve 10, open inflation valve 8 and clean to the argon gas that vacuum chamber 1 charges into about 0.1atm.Close inflation valve 8, open and slightly take out 11 pairs of vacuum chambers 1 of valve and be evacuated down to 5Pa-10Pa.Close and slightly take out valve 11, open 10 pairs of vacuum chambers 1 of diffusion pump main valve and vacuumize.When vacuum tightness reaches 10
-2Pa-10
-3Behind the pa, close diffusion pump main valve 10, charge into the 0.5atm argon gas to vacuum chamber 1.Start power supply and carry out heating raw and fusing formation molten alloy 3 to smelting pot 2; Open cooling water intakeoutfall 7 water flowings simultaneously and heat-preservation cylinder 5 is heated to 1450 ℃.Molten alloy 3 is poured in the heat-preservation cylinder 5, starts servomotor 9 and all pull out heat-preservation cylinder 5 so that 180mm/h is drop-down up to rare earth ultra-magnetostriction material 4, finally obtain the rare earth ultra-magnetostriction material 4 of directional freeze by lifting leading screw 6.The temperature that reduces heat-preservation cylinder 5 is to 1000 ℃ of thermal treatment temps, start servomotor 9 and heat-treat 1h with 400mm/h lifting rare earth ultra-magnetostriction material 4 up to all entering heat-preservation cylinder 5, obtain φ 30mm * 300mm rareearth super magnetostrictive bar at last by lifting leading screw 6.Analytical test shows: present embodiment prepares φ 30mm * 300mm rareearth super magnetostrictive bar and has good＜110〉texture, saturation magnetostriction coefficient lambda s reaches 1680ppm under 8Mpa prestress.
Embodiment 5
Purity is not less than 99.5%Tb, 99.5%Dy, high-purity Fe, 99.99%Al and 99.9%Mn proportioning Tb
0.3Dy
0.7Fe
1.70Mn
0.15Al
0.10(atomic ratio) 3.47kg smelting pot 2 of packing into is built bell.Start mechanical pump 15, open and slightly take out 11 pairs of vacuum chambers 1 of valve and vacuumize.When vacuum tightness reaches 5Pa-10Pa, close and slightly take out valve 11, start lobe pump 13 and diffusion pump 12, successively open preceding step valve 14 of diffusion pump and diffusion pump main valve 10 and continue vacuum chamber 1 is vacuumized.When vacuum tightness reaches 10
-2Pa-10
-3Behind the pa, close diffusion pump main valve 10, open inflation valve 8 and clean to the argon gas that vacuum chamber 1 charges into about 0.1atm.Close inflation valve 8, open and slightly take out 11 pairs of vacuum chambers 1 of valve and be evacuated down to 5Pa-10Pa.Close and slightly take out valve 11, open 10 pairs of vacuum chambers 1 of diffusion pump main valve and vacuumize.When vacuum tightness reaches 10
-2Pa-10
-3Behind the pa, close diffusion pump main valve 10, charge into the 0.5atm argon gas to vacuum chamber 1.Start power supply and carry out heating raw and fusing formation molten alloy 3 to smelting pot 2; Open cooling water intakeoutfall 7 water flowings simultaneously and heat-preservation cylinder 5 is heated to 1350 ℃.Molten alloy 3 is poured in the heat-preservation cylinder 5, starts servomotor 9 and all pull out heat-preservation cylinder 5 so that 150mm/h is drop-down up to rare earth ultra-magnetostriction material 4, finally obtain the rare earth ultra-magnetostriction material 4 of directional freeze by lifting leading screw 6.The temperature that reduces heat-preservation cylinder 5 is to 900 ℃ of thermal treatment temps, start servomotor 9 and heat-treat 1.5h with 400mm/h lifting rare earth ultra-magnetostriction material 4 up to all entering heat-preservation cylinder 5, obtain φ 40mm * 300mm rareearth super magnetostrictive bar at last by lifting leading screw 6.Analytical test shows: present embodiment prepares φ 40mm * 300mm rareearth super magnetostrictive bar and has good＜110〉texture, saturation magnetostriction coefficient lambda s reaches 1750ppm under 7Mpa prestress.
Embodiment 6
Purity is not less than 99.5%Tb, 99.5%Dy, high-purity Fe and 99.8%Co proportioning Tb
0.3Dy
0.7Fe
1.80Co
0.15(atomic ratio) 4.38kg smelting pot 2 of packing into is built bell.Start mechanical pump 15, open and slightly take out 11 pairs of vacuum chambers 1 of valve and vacuumize.When vacuum tightness reaches 5Pa-10Pa, close and slightly take out valve 11, start lobe pump 13 and diffusion pump 12, successively open preceding step valve 14 of diffusion pump and diffusion pump main valve 10 and continue vacuum chamber 1 is vacuumized.When vacuum tightness reaches 10
-2Pa-10
-3Behind the Pa, close diffusion pump main valve 10, open inflation valve 8 and clean to the argon gas that vacuum chamber 1 charges into about 0.1atm.Close inflation valve 8, open and slightly take out 11 pairs of vacuum chambers 1 of valve and be evacuated down to 5Pa-10Pa.Close and slightly take out valve 11, open 10 pairs of vacuum chambers 1 of diffusion pump main valve and vacuumize.When vacuum tightness reaches 10
-2Pa-10
-3Behind the Pa, close diffusion pump main valve 10, charge into the 0.5atm argon gas to vacuum chamber 1.Start power supply and carry out heating raw and fusing formation molten alloy 3 to smelting pot 2; Open cooling water intakeoutfall 7 water flowings simultaneously and heat-preservation cylinder 5 is heated to 1350 ℃.Molten alloy 3 is poured in the heat-preservation cylinder 5, starts servomotor 9 and all pull out heat-preservation cylinder 5 so that 150mm/h is drop-down up to rare earth ultra-magnetostriction material 4, finally obtain the rare earth ultra-magnetostriction material 4 of directional freeze by lifting leading screw 6.The temperature that reduces heat-preservation cylinder 5 is to 900 ℃ of thermal treatment temps, start servomotor 9 and heat-treat 1.5h with 400mm/h lifting rare earth ultra-magnetostriction material 4 up to all entering heat-preservation cylinder 5, obtain φ 45mm * 300mm rareearth super magnetostrictive bar at last by lifting leading screw 6.Analytical test shows: present embodiment prepares φ 45mm * 300mm rareearth super magnetostrictive bar and has good＜110〉texture, saturation magnetostriction coefficient lambda s reaches 1680ppm under 9.8Mpa prestress.
Embodiment 7
Purity is not less than 99.5%Tb, 99.5%Dy, high-purity Fe, 99.8%Co and 99.8%Ni proportioning Tb
0.3Dy
0.7Fe
1.70Mn
0.15Al
0.10(atomic ratio) 6.55kg smelting pot 2 of packing into is built bell.Start mechanical pump 15, open and slightly take out 11 pairs of vacuum chambers 1 of valve and vacuumize.When vacuum tightness reaches 5Pa-10Pa, close and slightly take out valve 11, start lobe pump 13 and diffusion pump 12, successively open preceding step valve 14 of diffusion pump and diffusion pump main valve 10 and continue vacuum chamber 1 is vacuumized.When vacuum tightness reaches 10
-2Pa-10
-3Behind the Pa, close diffusion pump main valve 10, open inflation valve 8 and clean to the argon gas that vacuum chamber 1 charges into about 0.1atm.Close inflation valve 8, open and slightly take out 11 pairs of vacuum chambers 1 of valve and be evacuated down to 5Pa-10Pa.Close and slightly take out valve 11, open 10 pairs of vacuum chambers 1 of diffusion pump main valve and vacuumize.When vacuum tightness reaches 10
-2Pa-10
-3Behind the Pa, close diffusion pump main valve 10, charge into the 0.5atm argon gas to vacuum chamber 1.Start power supply and carry out heating raw and fusing formation molten alloy 3 to smelting pot 2; Open cooling water intakeoutfall 7 water flowings simultaneously and heat-preservation cylinder 5 is heated to 1350 ℃.Molten alloy 3 is poured in the heat-preservation cylinder 5, starts servomotor 9 and all pull out heat-preservation cylinder 5 so that 150mm/h is drop-down up to rare earth ultra-magnetostriction material 4, finally obtain the rare earth ultra-magnetostriction material 4 of directional freeze by lifting leading screw 6.The temperature that reduces heat-preservation cylinder 5 is to 900 ℃ of thermal treatment temps, start servomotor 9 and heat-treat 1.5h with 400mm/h lifting rare earth ultra-magnetostriction material 4 up to all entering heat-preservation cylinder 5, obtain φ 55mm * 300mm rareearth super magnetostrictive bar at last by lifting leading screw 6.Analytical test shows: present embodiment prepares φ 55mm * 300mm rareearth super magnetostrictive bar and has good＜110〉texture, saturation magnetostriction coefficient lambda s reaches 1710ppm under 4.9Mpa prestress.
Claims (10)
1, a kind of one-step preparation process of rare earth ultra-magnetostriction material is characterized in that: this preparation technology comprises the steps:
(1), adopts the vacuum chamber that is provided with smelting pot, heat-preservation cylinder and detachable heat-preservation cylinder base in it, wherein, the heat-preservation cylinder base is a hollow form, and bring water outlet into, the heat-preservation cylinder base connects can make its upper and lower mobile drive unit, with the proportioning raw materials of the rare earth ultra-magnetostriction material of the surface cleaning after treatment target component to the material design, the smelting pot of packing into then, vacuum chamber is under vacuum or the protection of inert gas state, carries out alloy melting again;
(2), to the logical water coolant of heat-preservation cylinder base, and heat-preservation cylinder heated to more than the rare earth ultra-magnetostriction material fusing point 100 ℃-250C °, it is the directional freeze temperature, molten alloy is poured in the heat-preservation cylinder, after the cast, by the drop-down rare earth ultra-magnetostriction material of drive unit,, obtain the bar of the rare earth ultra-magnetostriction material of directional freeze up to all pulling out heat-preservation cylinder;
(3), heat-preservation cylinder is cooled to thermal treatment temp after, by drive unit bar is risen in the heat-preservation cylinder and to heat-treat,, obtain high-performance＜110 at last through thermal treatment〉rare earth ultra-magnetostriction material of texture.
2, the one-step preparation process of rare earth ultra-magnetostriction material according to claim 1 is characterized in that: in described step (2), the directional freeze temperature is 1300 ℃-1550 ℃.
3, the one-step preparation process of rare earth ultra-magnetostriction material according to claim 1 and 2 is characterized in that: in described step (2), drop-down speed is 30mm/h-240mm/h.
4, the one-step preparation process of rare earth ultra-magnetostriction material according to claim 3 is characterized in that: in described step (3), thermal treatment temp is 800 ℃-1250 ℃, and heat treatment time is 1.0-3.0h.
5, the one-step preparation process of rare earth ultra-magnetostriction material according to claim 4, it is characterized in that: in described step (1), the type of heating of the alloy melting of smelting pot is selected from a kind of in induction heating, resistive heating, electrical spark heating and the plasma heating.
6, the employed equipment of one-step preparation process of the described rare earth ultra-magnetostriction material of a kind of claim 1, it is characterized in that: this equipment is to be provided with smelting pot in vacuum chamber from top to bottom successively, heat-preservation cylinder and detachable heat-preservation cylinder base, wherein, the heat-preservation cylinder base is a hollow form, and bring water outlet into, and connection water inlet pipe and water outlet pipe, the heat-preservation cylinder base connects can be made on it, mobile down drive unit, vacuum-chamber wall is provided with aeration aperture, and is furnished with inflation valve, outside vacuum chamber, be provided with vacuum extractor, and join by vacuum lines and the vacuum chamber that is provided with vacuum valve.
7, equipment according to claim 6 is characterized in that: described heat-preservation cylinder is made up of lagging material, and is provided with the heating element by temperature controller control, and the heat-preservation cylinder base is by highly heat-conductive material, as copper production.
8, according to claim 6 or 7 described equipment, it is characterized in that: described drive unit comprises servomotor, reduction box and lifts leading screw, and servomotor connects the lower end that lifts leading screw by reduction box, and the heat-preservation cylinder base connects the upper end that lifts leading screw.
9, the rare earth ultra-magnetostriction material of single stage method according to claim 1 preparation is characterized in that: this rare earth ultra-magnetostriction material be RE (Fe, M)
2-xRE is rare earth element one or more of totally 17 kinds that comprise Y and Sc, and M is Mn, Ni, Al, Co etc., can partly substitute Fe, 0≤x≤0.10.
10, rare earth ultra-magnetostriction material according to claim 9 is characterized in that: described rare earth ultra-magnetostriction material has axial crystalline＜110〉texture.
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| CN03156926.9A CN1247829C (en) | 2003-09-15 | 2003-09-15 | Rareearth supermagnetostrictive material one step preparation and apparatus and products thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102181656A (en) * | 2011-04-07 | 2011-09-14 | 武汉钢铁(集团)公司 | Method for smelting high-purity steel through vacuum induction furnace |
| CN102392174A (en) * | 2011-10-27 | 2012-03-28 | 东北大学 | Method and device for preparing magnetostrictive material |
| CN103627944A (en) * | 2012-08-29 | 2014-03-12 | 四平兴大密封件有限公司 | Powder metallurgy rare earth super-magnetostrictive bar material and preparation technology therefor |
| CN105986310A (en) * | 2015-03-06 | 2016-10-05 | 有研稀土新材料股份有限公司 | Rare earth magnetostriction material and preparation method thereof |
-
2003
- 2003-09-15 CN CN03156926.9A patent/CN1247829C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102181656A (en) * | 2011-04-07 | 2011-09-14 | 武汉钢铁(集团)公司 | Method for smelting high-purity steel through vacuum induction furnace |
| CN102181656B (en) * | 2011-04-07 | 2012-07-25 | 武汉钢铁(集团)公司 | Method for smelting high-purity steel through vacuum induction furnace |
| CN102392174A (en) * | 2011-10-27 | 2012-03-28 | 东北大学 | Method and device for preparing magnetostrictive material |
| CN102392174B (en) * | 2011-10-27 | 2013-04-10 | 东北大学 | Method and device for preparing magnetostrictive material |
| CN103627944A (en) * | 2012-08-29 | 2014-03-12 | 四平兴大密封件有限公司 | Powder metallurgy rare earth super-magnetostrictive bar material and preparation technology therefor |
| CN105986310A (en) * | 2015-03-06 | 2016-10-05 | 有研稀土新材料股份有限公司 | Rare earth magnetostriction material and preparation method thereof |
| CN105986310B (en) * | 2015-03-06 | 2018-06-01 | 有研稀土新材料股份有限公司 | Rare earth giant magnetostrictive material preparation method and rare earth giant magnetostrictive material |
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| Publication number | Publication date |
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| CN1247829C (en) | 2006-03-29 |
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