CN1332053C - Multiplex rare-earth ferroalloy (RERAFe#-[2]) powder and method for preparing same - Google Patents
Multiplex rare-earth ferroalloy (RERAFe#-[2]) powder and method for preparing same Download PDFInfo
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- CN1332053C CN1332053C CNB2004100680444A CN200410068044A CN1332053C CN 1332053 C CN1332053 C CN 1332053C CN B2004100680444 A CNB2004100680444 A CN B2004100680444A CN 200410068044 A CN200410068044 A CN 200410068044A CN 1332053 C CN1332053 C CN 1332053C
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 62
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 52
- 239000000843 powder Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 25
- 229910001021 Ferroalloy Inorganic materials 0.000 title description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 65
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 36
- 239000000956 alloy Substances 0.000 claims abstract description 36
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 29
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 28
- 229910052742 iron Inorganic materials 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- 239000011780 sodium chloride Substances 0.000 claims abstract description 14
- 238000009792 diffusion process Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000007935 neutral effect Effects 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 238000006722 reduction reaction Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 6
- 239000008187 granular material Substances 0.000 claims description 5
- -1 terbium peroxide Chemical class 0.000 claims description 5
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052771 Terbium Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229930000044 secondary metabolite Natural products 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 2
- GEZAXHSNIQTPMM-UHFFFAOYSA-N dysprosium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Dy+3].[Dy+3] GEZAXHSNIQTPMM-UHFFFAOYSA-N 0.000 claims description 2
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 2
- 238000009461 vacuum packaging Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000011575 calcium Substances 0.000 abstract description 21
- 229910052791 calcium Inorganic materials 0.000 abstract description 13
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 7
- 238000011084 recovery Methods 0.000 abstract description 5
- 238000004140 cleaning Methods 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 238000002791 soaking Methods 0.000 abstract description 2
- 238000005660 chlorination reaction Methods 0.000 abstract 2
- 150000003839 salts Chemical class 0.000 abstract 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 abstract 1
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 abstract 1
- TWJVNKMWXNTSAP-UHFFFAOYSA-N azanium;hydroxide;hydrochloride Chemical compound [NH4+].O.[Cl-] TWJVNKMWXNTSAP-UHFFFAOYSA-N 0.000 abstract 1
- 239000001110 calcium chloride Substances 0.000 abstract 1
- 235000011148 calcium chloride Nutrition 0.000 abstract 1
- 229910001628 calcium chloride Inorganic materials 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000000696 magnetic material Substances 0.000 description 7
- 229910001172 neodymium magnet Inorganic materials 0.000 description 7
- 229910052692 Dysprosium Inorganic materials 0.000 description 5
- 229910052779 Neodymium Inorganic materials 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 229910000640 Fe alloy Inorganic materials 0.000 description 4
- 238000003912 environmental pollution Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 230000005496 eutectics Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000007499 fusion processing Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000004080 punching Methods 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 229910000521 B alloy Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The present invention relates to multielement rare earth iron (RERAFe2) alloy powder and a preparing method thereof. Any two kinds of rare earth oxide are arbitrarily selected from Nd2O3, Dy2O3, Pr2O3 and Tb4O7 to be used as raw materials, and are prepared into rare earth oxide mixtures according to the weight percentage; then, calcium metal grains Ca, iron powder Fe and chlorination salt (NaCl or CaCl2) are added and are mixed to prepare a secondary mixture of rare earth oxide according to the weight percentage. Calcium metal grains are added with chlorination salt as a reducing agent; through stirring, argon Ar cleaning, positive pressure protection and heating, reduction diffusion reaction is performed; after cooling, NH4Cl water solution is used for soaking until the solution is brown; then, acetic acid water solution and water solution are used for cleaning until the pH valve is neutral; finally, filtration, water content removal and drying are performed to obtain the alloy powder. The alloy powder can be used as master alloy to be prepared into rare earth permanent-magnet materials, and has the characteristics of simple manufacturing process, low production cost, no environment pollution, stable and controllable metal content, high alloy recovery rate, etc.
Description
Technical field
The present invention relates to field of new, especially a kind of multielement rare earth iron RERAFe
2Alloy powder and preparation method thereof.
Background technology
Rare earth permanent-magnetic material NdFeB, mainly be to be prepared from by powder metallurgical technique, be widely used in industries such as electronics, machinery, especially high performance material by metals such as rare earth metal neodymium, iron and boron, more paid attention to using in national defense industry, its market outlook are very wide.In order to increase substantially the magnetic property of rare earth permanent-magnetic material NdFeB, especially improve HCJ and thermostability, often when the melting of rare earth permanent-magnetic material NdFeB powder metallurgy, all add a spot of rare earth metal rare earth, thereby improve the thermostability of rare earth permanent-magnetic material NdFeB, promptly under higher use temperature condition, its magnetic property can obviously not descend, and adds the rare earth of 1%-35% usually in the NdFeB permanent magnet material.The rare earth metal rare earth is except the additive that can be used as rare earth permanent-magnetic material NdFeB, and it can also be used for other rare earth functional materialss, as rareearth super magnetostrictive alloy FeDy
0.7B
0.3In magnetoopticmemory material FeDyTbGd.At present, multielement rare earth iron RERAFe
2The preparation method of alloy roughly has three kinds: one, through calciothermy, prepare the pure metal rare earth with rare earth fluorine, and be smelted into the multielement rare earth iron alloy that difference contains rare earth content through eutectic method again; Its two, produce the rare earth ferroalloy that height contains rare earth content with the eutectoid electrolytic process, be smelted into the multielement rare earth iron alloy that difference contains rare earth content through eutectic method again; Its three, utilize pure calcium reduction diffusion process directly to prepare the multielement rare earth iron alloy by oxide compound.These preparation methods' shortcoming is respectively: prepare rare earth ferroalloy with eutectic method, have the production cost height, shortcomings such as serious environmental pollution are arranged.The eutectoid electrolytic process prepares rare earth ferroalloy, and its content of rare earth is within the specific limits uncontrollable, brings difficulty to use; Advantages such as the calcium reduction diffusion process has non-environmental-pollution, and its alloy ingredient is controlled.But adopt calcium to have following shortcoming again merely: the reduzate calcium oxide as reductive agent, its fusing point is up to 2600 ℃, still be solid-state under reduction temperature, diffusion to the reduction of rare earth metal-rare-earth has inhibition, even the oxidized calcium of as-reduced metal-rare-earth can be comprised, not only purify and bring difficulty, and make it form rare earth ferroalloy with metallic iron to alloy.Thereby, want to form the fixing multielement rare earth iron alloy of forming, the add-on of its rare earth oxide is greater than theoretical amount, adds the rare earth oxide of 110%-120% usually, from and production cost is increased substantially.In above-mentioned Rare Earth Functional Materials, the rare earth metal rare earth all adds with form of pure metal, can't rapid melting in the molten process of freezing, alloy recovery is low, and production cost height, fusion process produce a large amount of slags, affect environmental pollution, and cause a lot of valuable rare earth metals losses, and make the formula components imbalance as the preparation of rare earth permanent-magnetic material, affect half-finished magnetic property.
Summary of the invention
The object of the invention is to overcome the defective of prior art and provides a kind of fusion process to melt fast, the alloy recovery height, and production cost is low, avoids valuable rare earth metal loss, does not influence the multielement rare earth iron RERAFe of work in-process magnetic property
2Alloy powder and preparation method thereof.
The object of the invention realizes by following technical proposal:
A kind of multielement rare earth iron RERAFe
2Alloyed powder is characterized in that this alloyed powder is at rare earth oxide neodymium oxide Nd
2O
3, Dysprosium trioxide Dy
2O
3, praseodymium sesquioxide Pr
2O
3, terbium peroxide Tb
4O
7In to choose at least arbitrarily two kinds of rare earth oxides be raw material, process by weight percentage and make rare earth oxide compound RE
2O
3+ RA
2O
3:
Rare earth oxide RE
2O
360-87%
Rare earth oxide RA
2O
313-40%
In the rare earth oxide compound that makes, add granules of metal Ca Ca, iron powder Fe, chlorate NaCl or CaCl again
2, be treated to by weight percentage:
Rare earth oxide RE
2O
3+ RA
2O
320-80%
Granules of metal Ca Ca 8.5-50%
Iron powder Fe 10.7-63.1%
Chlorate NaCl or CaCl
20-15%
Rare earth oxide secondary compound by said ratio makes directly makes multielement rare earth iron RERAFe through reduction-diffusion process
2Alloy powder.
Multielement rare earth iron RERAFe
2The preparation method of alloy powder, soon rare earth oxide secondary compound is placed on and stirs 1.5-5 hour in the mixing machine to uniform mixing; Be placed on after the stirring on the press at 500-800kg/cm
2Pressure depress to the material piece; After above-mentioned material piece placed vacuum furnace to vacuumize to reach 2Pa, clean 1-3 time with pure argon gas Ar; With stove applying argon gas positive pressure protection heating down again, make it carry out reduction diffusion reaction at 850-1150 ℃, kept temperature 4-10 hour; The reduction reaction furnace cooling that finishes is treated that test portion is cooled to below 60 ℃ promptly to come out of the stove; Cooling test portion after coming out of the stove is directly put into 1-10%NH
4Soaked 1-15 hour in the Cl aqueous solution; Add again water stirring and washing to solution show brown till; Use 2-4% (volume percent) aqueous acetic acid and the 1%EDTA aqueous solution to clean then 1-2 time; The pH value that is washed till solution with clear water is neutral at last; Filter to remove moisture, again with dehydrated alcohol dash filter 2 times the precipitation alloy powder; Place the vacuum drying oven below 60 ℃ to dry 1-2 hour above-mentioned precipitation alloy powder; Take out the final vacuum packing and become product.
Described material is block-shaped to be ring-type or square or strip or trapezoidal or triangle or cylindrical.
Described vacuum furnace is vacuum resistance furnace or vacuum sintering furnace.
Compared with prior art, the present invention has adopted directly and has made raw material with calcium metal Ca and chlorate NaCl or CaCl by multiple rare-earth oxide
2Directly prepare multielement rare earth iron RERAFe as reducing agent
2Alloyed powder has been brought into play CaONaCl and CaOCaCl
2Fusing point be respectively the low melting point advantage of 801 ℃ and 782 ℃, be more conducive to the diffusion of reducing metal and the formation of intermetallic compound after making fusing, make preparation technology simple, production cost is low, non-environmental-pollution, and the metal-rare-earth stable content is controlled, the alloy recovery height, avoid valuable rare earth metal loss and magnetic property impact, the foundry alloy as preparation rare earth permanent-magnetic material NdFeB has immeasurable practical value.
Embodiment
RA in the title of the present invention, RE represent any rare earth, RA
2O
3, RE
2O
3Represent any rare earth oxide.The present invention adds alloying element according to the smelting process principle with the mother alloy form, is more conducive to fusing, makes alloy ingredient more even.Because metal-rare-earth in actual applications, all in ferruginous alloy, thereby it is particularly reasonable to add rare earth with multielement rare earth iron mother alloy form, makes production technique simple, and production cost is low, the alloy recovery height.
The present invention makes rare earth oxide compound RE take any two rare earth oxide as raw materials by weight
2O
3+ RA
2O
3, in the rare earth oxide compound that makes, add again granules of metal Ca Ca, iron powder Fe, chlorate NaCl or CaCl
2, make by weight percentage the rare earth oxide secondary mixed material, this compound directly prepares multielement rare earth iron RERAFe by reduction-diffusion process
2Be filled with argon Ar after alloyed powder, this alloyed powder are processed premenstruum (premenstrua) and carry out reduction diffusion reaction, its reaction equation is as follows:
RA
2O
3+RE
2O
3+6Ca+4Fe+6NaCl＝2RERAFe
2+6CaO·NaCl
RA
2O
3+RE
2O
3+6Ca+4Fe+6CaCl
2＝2RERAFe
2+6CaO·CaCl
2
Reduction reaction complete with stove cooling, aqueous solution soaking to solution aobvious brown till, expect that piece becomes powdery this moment; Be neutral with aqueous acetic acid and EDTA aqueous cleaning to the pH value of solution then; Filter to remove moisture, again with absolute ethyl alcohol punching filter the precipitation alloyed powder; With above-mentioned precipitation alloyed powder place vacuum drying chamber dry multielement rare earth iron RERAFe
2Alloyed powder.
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
With Nd
2O
3(or Dy
2O
3) 100 grams, Dy
2O
3(or Nd
2O
3) 15 grams, Ca grain 80 grams, Fe powder 363 grams, NaCl (or CaCl
2) 17 grams, in mixer, stir and mix after 2 hours, compound is placed on the press with 500kg/cm
2Pressure test portion is pressed into annular material piece; put into generic container (using stainless steel); and place the vacuum resistance heating furnace; vacuumize reach 2Pa after; be filled with again pure argon gas Ar and clean 2 times, under the argon Ar protection, be heated to 950 ℃ with stove, be incubated 10 hours; cool to the furnace then below 60 ℃, take out test portion and place 5%NH
4Soaked 6 hours in the Cl aqueous solution, water cleans and presents brownly to solution under stirring condition, uses then 2% (volume) aqueous acetic acid and 1%EDTA aqueous cleaning 2 times, is washed to filter after solution is neutral (pH value), and with absolute ethyl alcohol punching filter 2 times, carry out vacuum drying 2 hours, gained alloyed powder 451.5 grams contain 18.9%Nd (or Dy) in the alloy again, 3.1%Dy (or Nd), 77.1%Fe, 0.16%Ca, 0.23%O.
Embodiment 2
With Dy
2O
3(or Pr
2O
3) 120 grams, Pr
2O
3(or Dy
2O
3) 30 grams, Ca grain 16 grams, Fe powder 20 grams, CaCl
2(or NaCl) 1.5 grams by the annular material piece that the implementation method of embodiment 1 is made, are put into the vacuum resistance heating furnace; vacuumize reach 2Pa after; under the protection of Ar gas, be heated to 1000 ℃, be incubated 8 hours, press the method processing reaction material of embodiment 1; gained alloyed powder 107.2 grams; contain 63.2%Dy (or Pr) in the alloy, 15.3%Pr (or Dy), 19.7%Fe; 0.13%Ca, 0.24%O.
Embodiment 3
With Nd
2O
3(or Dy
2O
3) 800 grams, Dy
2O
3(or Nd
2O
3) 200 grams, Ca grain 1659 grams, Fe powder 587 grams, NaCl (or CaCl
2) 72 grams, by the annular material piece that the implementation method of embodiment 1 is made, put into the vacuum resistance heating furnace; vacuumize reach 2Pa after; under the protection of Ar gas, be heated to 1100 ℃, be incubated 7 hours, press the method processing reaction material of embodiment 1; gained alloyed powder 1385.6 grams; contain 46.3%Nd (or Dy) in the alloy, 11.9%Dy (or Nd), 39.2%Fe; 0.12%Ca, 0.17%O.
Embodiment 4
With Dy
2O
3(or Tb
4O
7) 288 grams, Tb
4O
7(or Dy
2O
3) 192 grams, Ca grain 230 grams, Fe powder 492.5 grams, CaCl
2(or NaCl) 212 grams by the annular material piece that the implementation method of embodiment 1 is made, are put into the vacuum resistance heating furnace; vacuumize reach 2Pa after; under the protection of Ar gas, be heated to 1100 ℃, be incubated 7 hours, press the method processing reaction material of embodiment 1; gained alloyed powder 857.3 grams; contain 27.4%Dy (or Tb) in the alloy, 18.6%Tb (or Dy), 52.2%Fe; 0.15%Ca, 0.29%O.
Embodiment 5
With Nd
2O
3(or Tb
4O
7) 637.5 grams, Tb
4O
7(or Nd
2O
3) 212.5 grams, Ca grain 408 grams, Fe powder 697 grams, NaCl (or CaCl
2) 0 gram, by the annular material piece that the implementation method of embodiment 1 is made, put into the vacuum resistance heating furnace; vacuumize reach 2Pa after; under the protection of Ar gas, be heated to 1100 ℃, be incubated 7 hours, press the method processing reaction material of embodiment 1; gained alloyed powder 1358.3 grams; contain 38.4%Nd (or Tb) in the alloy, 12.6%Tb (or Nd), 46.7%Fe; 0.13%Ca, 0.27%O.
Embodiment 6
With Nd
2O
3(or Dy
2O
3) 3600 grams, Dy
2O
3(or Nd
2O
3) 900 grams, Ca grain 2160 grams, Fe powder 2638 grams, NaCl (or CaCl
2) 324 grams, by the annular material piece that the implementation method of embodiment 1 is made, put into the vacuum resistance heating furnace; vacuumize reach 2Pa after; under the protection of Ar gas, be heated to 1100 ℃, be incubated 9 hours, press the method processing reaction material of embodiment 1; gained alloyed powder 6207.2 grams; contain 46.6%Nd (or Dy) in the alloy, 11.4%Dy (or Nd), 39.7%Fe; 0.14%Ca, 0.17%O.
Utilize embodiment 6 gained alloyed powders 6207.2 grams, requirement according to the spindle prescription, be made into 18 kilograms prescription with other metal (such as iron, aluminium, copper etc.) with rare earth, on 20 kilograms of vaccum sensitive stoves successively melting 10 on 18 kilograms of Nd Fe B alloys ingots, after process pulverizing, moulding, sintering are made magnet, measure through China National Measuring Science Research Inst., its magnetic property is suitable with the traditional Fe-80Dy of adding, but HCJ increases.
Claims (4)
1, a kind of multielement rare earth iron RERAFe
2Alloyed powder is characterized in that this alloyed powder is at rare earth oxide neodymium oxide Nd
2O
3, Dysprosium trioxide Dy
2O
3, praseodymium sesquioxide Pr
2O
3, terbium peroxide Tb
4O
7In to choose at least arbitrarily two kinds of rare earth oxides be raw material, process by weight percentage and make rare earth oxide compound RE
2O
3+ RA
2O
3:
Rare earth oxide RE
2O
360-87%
Rare earth oxide RA
2O
313-40%
In the rare earth oxide compound that makes, add granules of metal Ca Ca, iron powder Fe, chlorate NaCl or CaCl again
2, be treated to by weight percentage:
Rare earth oxide RE
2O
3+ RA
2O
320-80%
Granules of metal Ca Ca 8.5-50%
Iron powder Fe 10.7-63.1%
Chlorate NaCl or CaCl
20.8-15%
Rare earth oxide secondary compound by said ratio makes directly makes multielement rare earth iron RERAFe through reduction-diffusion process
2Alloy powder.
2, a kind of by the described multielement rare earth iron of claim 1 RERAFe
2The preparation method of alloy powder is characterized in that described reduction-diffusion process is about to rare earth oxide secondary compound and is placed in the mixing machine and stirs 1.5-5 hour to uniform mixing; Above-mentioned compound is placed on the press at 500-800kg/cm
2Pressure depress to the material piece; After above-mentioned material piece placed vacuum furnace to vacuumize to reach 2Pa, clean 1-3 time with pure argon gas Ar; With stove applying argon gas positive pressure protection heating down again, make it carry out reduction diffusion reaction at 850-1150 ℃, kept temperature 4-10 hour; The reduction reaction furnace cooling that finishes is treated that test portion is cooled to below 60 ℃ promptly to come out of the stove; Cooling test portion after coming out of the stove is directly put into 1-10%NH
4Soaked 1-15 hour in the Cl aqueous solution; Add again water stirring and washing to solution show brown till; Use 2-4% (volume percent) aqueous acetic acid and the 1%EDTA aqueous solution to clean then 1-2 time; The pH value that is washed till solution with clear water is neutral at last; Filter to remove moisture, again with dehydrated alcohol dash filter 2 times the precipitation alloy powder; Place the vacuum drying oven below 60 ℃ to dry 1-2 hour above-mentioned precipitation alloy powder; Take out the final vacuum packing and become product.
3, multielement rare earth iron RERAFe according to claim 2
2The preparation method of alloy powder is characterized in that described material is block-shaped for ring-type or square or strip or trapezoidal or trilateral or cylindrical.
4, multielement rare earth iron RERAFe according to claim 2
2The preparation method of alloy powder is characterized in that described vacuum furnace is vacuum resistance furnace or vacuum sintering furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100680444A CN1332053C (en) | 2004-11-11 | 2004-11-11 | Multiplex rare-earth ferroalloy (RERAFe#-[2]) powder and method for preparing same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100680444A CN1332053C (en) | 2004-11-11 | 2004-11-11 | Multiplex rare-earth ferroalloy (RERAFe#-[2]) powder and method for preparing same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1603444A CN1603444A (en) | 2005-04-06 |
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| CN101618459B (en) * | 2008-07-02 | 2013-03-13 | 北京中科三环高技术股份有限公司 | Method for preparing DyGaFe alloy powder by reduction-diffusion method |
| CN101618460B (en) * | 2008-07-02 | 2012-09-19 | 宁波科宁达工业有限公司 | Method for preparing DyGa alloy |
| CN105689731B (en) * | 2016-01-28 | 2017-07-07 | 湖北大学 | A kind of Fe3The low temperature preparation method of Si magnetic nanoparticle powders |
| CN108231313A (en) * | 2017-12-28 | 2018-06-29 | 北京京磁电工科技有限公司 | The slab technique of sintered NdFeB ultra-high coercive force magnet |
| CN108907216A (en) * | 2018-07-19 | 2018-11-30 | 兰州大学 | High-frequency high temperature R2Co17The reduction scattering preparation of based magnetic powder |
| CN114703387A (en) * | 2022-01-24 | 2022-07-05 | 中天捷晟(天津)新材料科技有限公司 | Terbium-iron alloy preparation method |
| JP7726230B2 (en) * | 2022-03-18 | 2025-08-20 | 住友金属鉱山株式会社 | Method for producing rare earth transition metal alloy powder |
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| US4681623A (en) * | 1985-06-24 | 1987-07-21 | Sumitomo Metal Mining Company Limited | Process for producing alloy powder containing rare earth metals |
| JP2001140005A (en) * | 1999-11-15 | 2001-05-22 | Sumitomo Metal Mining Co Ltd | Method for producing alloy powder for rare earth magnet and alloy powder produced by the method |
| CN1424164A (en) * | 2002-12-30 | 2003-06-18 | 北京科技大学 | Process for producing rare-earth-iron-boron permanent magnet alloy powder by reduction diffusion |
| CN1436871A (en) * | 2002-02-06 | 2003-08-20 | 徐军 | Prepn of ternary Tb-Dy-Fe alloy |
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| US4681623A (en) * | 1985-06-24 | 1987-07-21 | Sumitomo Metal Mining Company Limited | Process for producing alloy powder containing rare earth metals |
| JP2001140005A (en) * | 1999-11-15 | 2001-05-22 | Sumitomo Metal Mining Co Ltd | Method for producing alloy powder for rare earth magnet and alloy powder produced by the method |
| CN1436871A (en) * | 2002-02-06 | 2003-08-20 | 徐军 | Prepn of ternary Tb-Dy-Fe alloy |
| CN1424164A (en) * | 2002-12-30 | 2003-06-18 | 北京科技大学 | Process for producing rare-earth-iron-boron permanent magnet alloy powder by reduction diffusion |
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