CN117245088A - Auxiliary agent auxiliary preparation method for samarium iron and samarium iron nitrogen - Google Patents
Auxiliary agent auxiliary preparation method for samarium iron and samarium iron nitrogen Download PDFInfo
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- CN117245088A CN117245088A CN202311529143.7A CN202311529143A CN117245088A CN 117245088 A CN117245088 A CN 117245088A CN 202311529143 A CN202311529143 A CN 202311529143A CN 117245088 A CN117245088 A CN 117245088A
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- samarium iron
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- 239000012752 auxiliary agent Substances 0.000 title claims abstract description 30
- PRQMIVBGRIUJHV-UHFFFAOYSA-N [N].[Fe].[Sm] Chemical compound [N].[Fe].[Sm] PRQMIVBGRIUJHV-UHFFFAOYSA-N 0.000 title claims abstract description 26
- AWWAHRLLQMQIOC-UHFFFAOYSA-N [Fe].[Sm] Chemical compound [Fe].[Sm] AWWAHRLLQMQIOC-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 162
- 239000011575 calcium Substances 0.000 claims abstract description 93
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000006247 magnetic powder Substances 0.000 claims abstract description 70
- 238000010438 heat treatment Methods 0.000 claims abstract description 69
- 239000011812 mixed powder Substances 0.000 claims abstract description 65
- 238000009792 diffusion process Methods 0.000 claims abstract description 46
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 45
- 230000009467 reduction Effects 0.000 claims abstract description 41
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 37
- 239000001257 hydrogen Substances 0.000 claims abstract description 37
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 37
- 239000002245 particle Substances 0.000 claims abstract description 37
- 229910001954 samarium oxide Inorganic materials 0.000 claims abstract description 34
- 229940075630 samarium oxide Drugs 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 33
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000007789 gas Substances 0.000 claims abstract description 28
- 238000006356 dehydrogenation reaction Methods 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 238000005406 washing Methods 0.000 claims abstract description 18
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 238000005121 nitriding Methods 0.000 claims description 23
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 18
- 239000012535 impurity Substances 0.000 claims description 16
- 239000000725 suspension Substances 0.000 claims description 10
- 239000001103 potassium chloride Substances 0.000 claims description 9
- 235000011164 potassium chloride Nutrition 0.000 claims description 9
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 4
- 239000001110 calcium chloride Substances 0.000 claims description 4
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 2
- 239000003638 chemical reducing agent Substances 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000006722 reduction reaction Methods 0.000 description 38
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 238000002441 X-ray diffraction Methods 0.000 description 14
- 229910052772 Samarium Inorganic materials 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 11
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 229910000859 α-Fe Inorganic materials 0.000 description 9
- 238000001035 drying Methods 0.000 description 7
- 238000007885 magnetic separation Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 6
- 239000000956 alloy Substances 0.000 description 6
- 230000000630 rising effect Effects 0.000 description 6
- 238000009210 therapy by ultrasound Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000000053 physical method Methods 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0207—Using a mixture of prealloyed powders or a master alloy
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0235—Starting from compounds, e.g. oxides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/059—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and Va elements, e.g. Sm2Fe17N2
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses a method for preparing samarium iron and samarium iron nitrogen with the aid of an auxiliary agent, which comprises the following steps: 1. mixing iron powder, samarium oxide and calcium particles uniformly and doping inorganic salt to obtain mixed powder; 2. heat treatment and reduction to obtain Sm 2 Fe 17 CaO/Ca mixtureMixing the powder; 3. heat treatment in a mixed gas of hydrogen and ammonia to obtain Sm 2 Fe 17 N 3 CaO/Ca mixed powder; 4. grinding in washing liquid, and magnetically separating to obtain Sm 2 Fe 17 N 3 H x Magnetic powder; 5. dehydrogenation by heat treatment to obtain Sm 2 Fe 17 N 3 Magnetic powder. The invention adopts an auxiliary agent assisted reduction diffusion method, improves the fluidity of the reducing agent calcium particles by adding inorganic salt, promotes the calcium particles and samarium oxide to be uniformly mixed, and effectively improves Sm 2 Fe 17 And Sm 2 Fe 17 N 3 Crystallinity of the magnetic powder improves Sm 2 Fe 17 N 3 The magnetic property of the magnetic powder improves the utilization rate of calcium, has mild reaction conditions and good process stability, and is favorable for realizing industrial production.
Description
Technical Field
The invention belongs to the technical field of magnet materials, and particularly relates to a method for preparing samarium iron and samarium iron nitrogen with the aid of an auxiliary agent.
Background
In recent years, with the rapid development of the electronic and electric industry, the development trend of miniaturization, light weight and integration of electronic equipment has put higher demands on bonded permanent magnets. Nd 2 Fe 14 B/Sm 2 Fe 17 N 3 Composite bonded magnets are attracting attention for their excellent magnetic properties. Magnetic powder as the "parent of magnet" and high-performance anisotropic Sm 2 Fe 17 N 3 The magnetic powder is important for the preparation of the composite bonded magnet. In addition, rare earth Sm is generally considered as a byproduct of rare earth Nd extraction, so Sm 2 Fe 17 N 3 Is beneficial to the balanced utilization of rare earth resources in China.
For samarium-iron-nitrogen magnetic powder, the general preparation method can be classified into a physical method and a reduction diffusion method, wherein the physical method is to prepare Sm through the steps of alloy smelting-crushing and the like 2 Fe 17 After which nitridation to form Sm 2 Fe 17 N 3 Magnetic powder; the reduction diffusion method is to separate Sm/Fe from oxygen by high temperatureThe compound precursor is reduced and then subjected to element interdiffusion to form Sm 2 Fe 17 After which nitridation to form Sm 2 Fe 17 N 3 Magnetic powder. The latter is advantageous mainly in that the process is based on elemental interdiffusion to give Sm 2 Fe 17 The powder, rather than peritectic reaction involved in the physical method, can effectively avoid the residue of alpha-Fe in the product, thereby improving the magnetic property of the magnetic powder; on the other hand, the reduction diffusion method does not need a crushing step, the surface of the magnetic powder is relatively flat and smooth, and the Sm is improved due to fewer surface defects 2 Fe 17 N 3 Key factors of magnetic powder magnetic properties. Therefore, the reduction diffusion method is a preparation method for easily obtaining the magnetic powder with higher magnetic property.
However, the existing reduction diffusion process generally uses Ca as a reducing agent, a large amount of Ca is required to be used in the reaction to ensure that the Ca is fully contacted with samarium/iron oxide to achieve the effect of complete reduction, and the use of a large amount of Ca inevitably leads to the sudden increase of the preparation cost and the subsequent difficulty of impurity removal; in addition, the fluidity of the molten Ca at high temperature is poor, which is not beneficial to the mutual diffusion of samarium and iron and easily leads to Sm 2 Fe 17 Poor alloy crystallinity, etc.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing samarium iron and samarium iron nitrogen with the aid of an auxiliary agent aiming at the defects of the prior art. The method adopts an auxiliary agent assisted reduction diffusion method, and adopts molten inorganic salt as a medium to improve the fluidity of the reducing agent calcium particles by doping the inorganic salt in the reduction diffusion process, promote the uniform mixing of the calcium particles and the samarium oxide, and effectively improve Sm 2 Fe 17 And Sm 2 Fe 17 N 3 The crystallinity of the magnetic powder improves the utilization rate of calcium, greatly saves the process cost and solves the problem of Sm prepared by the prior art 2 Fe 17 And Sm 2 Fe 17 N 3 The magnetic powder has poor crystallinity and large using amount of the reducing agent Ca.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for preparing samarium iron and samarium iron nitrogen with the aid of an auxiliary agent is characterized by comprising the following steps of:
step one, mixing powder: uniformly mixing iron powder, samarium oxide and calcium particles, and doping inorganic salt to obtain mixed powder;
step two, reduction diffusion: performing heat treatment on the mixed powder obtained in the first step under a protective atmosphere, reducing by calcium particles, and diffusing by using heat driving to obtain Sm 2 Fe 17 CaO/Ca mixed powder;
step three, nitriding: sm obtained in the second step 2 Fe 17 Performing heat treatment on the mixed powder of CaO and Ca in the mixed gas of hydrogen and ammonia to obtain Sm 2 Fe 17 N 3 CaO/Ca mixed powder;
step four, removing impurities: sm obtained in the third step 2 Fe 17 N 3 Grinding mixed powder of CaO/Ca in washing liquid to form suspension, and magnetically separating to obtain Sm 2 Fe 17 N 3 H x Magnetic powder;
step five, dehydrogenation: under vacuum, sm obtained in the fourth step 2 Fe 17 N 3 H x Heat treating the magnetic powder to obtain Sm 2 Fe 17 N 3 Magnetic powder.
Sm is taken as the raw material in the fourth step of the invention 2 Fe 17 N 3 Grinding mixed powder of CaO/Ca in washing liquid to form suspension, extracting Sm by magnetic separation such as magnet 2 Fe 17 N 3 H x The magnetic powder is separated from CaO/Ca to remove CaO/Ca impurities, and simultaneously auxiliary methods such as ultrasonic and grinding can be adopted to accelerate the impurity removal rate.
The method for preparing samarium iron and samarium iron nitrogen with the aid of the auxiliary agent is characterized in that the molar ratio of samarium oxide to iron powder in the first step is 1:11-14.5.
The method for preparing samarium iron and samarium iron nitrogen with the aid of the auxiliary agent is characterized in that the molar ratio of samarium oxide to calcium particles in the first step is 1:3.6-6.
The method for preparing samarium iron and samarium iron nitrogen with the aid of the auxiliary agent is characterized in that the inorganic salt in the first step is potassium chlorideOr calcium chloride. The inorganic salt has a melting point of 770 deg.C, and Sm during heat treatment 2 Fe 17 The molten state is formed during phase formation, and the reducing agent can play a role in improving the fluidity of the reducing agent calcium, promote the calcium particles and the samarium oxide to be uniformly mixed, and improve Sm 2 Fe 17 And Sm 2 Fe 17 N 3 Crystallinity of the magnetic powder; meanwhile, the utilization rate of calcium is improved, and the cost is effectively controlled. In addition, the two inorganic salts are easily removed, thereby avoiding the introduction of impurities.
The method for preparing samarium iron and samarium iron nitrogen with the aid of the auxiliary agent is characterized in that the mass percentage of inorganic salt in the mixed powder in the first step is 4% -10%. The invention ensures that the inorganic salt content in the mixed powder is enough to play a role of a fused salt auxiliary agent by controlling the content of the inorganic salt, thereby assisting Sm 2 Fe 17 Sm and Sm 2 Fe 17 N 3 Pure phase formation and avoids the dilution of the concentration of the reduced calcium caused by the excessive content of inorganic salt and the influence on the reduction effect in the reduction diffusion of the reduced calcium, thereby leading to Sm 2 Fe 17 Sm and Sm 2 Fe 17 N 3 Cannot form a phase or cannot form a pure phase.
The method for preparing samarium iron and samarium iron nitrogen with the aid of the auxiliary agent is characterized in that the heat treatment temperature in the second step is 850-1150 ℃ and the time is 1.5-6 h. The invention ensures Sm by controlling the temperature and time of heat treatment, namely reduction diffusion 2 Fe 17 Sm and Sm 2 Fe 17 N 3 Smooth phase formation, and Sm caused by too low temperature or too short time is avoided 2 Fe 17 Sm and Sm 2 Fe 17 N 3 Poor or even impossible phase formation, and avoids serious agglomeration and even Sm caused by excessive temperature or excessive time 2 Fe 17 Or Sm 2 Fe 17 N 3 Decomposition problem.
The method for preparing samarium iron and samarium iron nitrogen with the aid of the auxiliary agent is characterized in that the volume ratio of hydrogen to ammonia in the hydrogen/ammonia mixed gas in the third step is 1-8:2. The invention ensures Sm by controlling the composition volume of the hydrogen/ammonia mixed gas 2 Fe 17 N 3 Is shaped smoothly and has excellent magnetic properties.
The method for preparing samarium iron and samarium iron nitrogen with the aid of the auxiliary agent is characterized in that the flow rate of the hydrogen/ammonia mixed gas in the third step is 0.6L/min-1.0L/min. The invention ensures the uniformity of nitriding process by controlling the flow rate of the hydrogen/ammonia mixed gas.
The method for preparing samarium iron and samarium iron nitrogen with the aid of the auxiliary agent is characterized in that the temperature of the heat treatment in the third step is 300-500 ℃ and the time is 3-6 hours. The invention ensures nitriding effect and avoids Sm by controlling the temperature and time of heat treatment, i.e. nitriding 2 Fe 17 N 3 Is decomposed.
Sm prepared by the auxiliary agent 2 Fe 17 And Sm 2 Fe 17 N 3 The method is characterized in that the temperature of the heat treatment in the fifth step is 100-400 ℃ and the time is 1-3 h.
Compared with the prior art, the invention has the following advantages:
1. the invention adopts the auxiliary agent assisted reduction diffusion method, and adopts the molten inorganic salt formed by the heat treatment as a medium to improve the fluidity of the reducing agent calcium particles by doping the inorganic salt in the reduction diffusion process, promote the uniform mixing of the calcium particles and the samarium oxide, facilitate the reduction of the samarium oxide and effectively improve the Sm 2 Fe 17 And samarium iron nitrogen Sm 2 Fe 17 N 3 The crystallinity of the magnetic powder improves the utilization rate of calcium, reduces the dosage of the reducing agent calcium particles, greatly saves the process cost and reduces the subsequent impurity removal difficulty.
2. The invention prepares Sm, fe, N and Sm 2 Fe 17 N 3 In the process of reducing diffusion, nitriding and impurity removal of magnetic powder, nitriding is Sm 2 Fe 17 To Sm 2 Fe 17 N 3 The nitrogen atoms are utilized to permeate from outside to inside in the conversion process, and the nitriding depth can be effectively controlled by controlling the ratio of the hydrogen to the ammonia in the hydrogen/ammonia mixed gas and the nitriding time of heat treatment, so that the ideal nitriding effect is obtained, and the overspray nitriding guide is avoidedAbnormal nitrogen content or Sm 2 Fe 17 N 3 Decompose to adapt to Sm with different particle sizes 2 Fe 17 N 3 The CaO/Ca mixed powder expands the application range of the invention.
3. Sm obtained by high-temperature reduction diffusion 2 Fe 17 The main component of the mixed powder of CaO and Ca is Sm 2 Fe 17 Alloy powder containing small amount of CaO or Ca and other impurities can be used as Sm 2 Fe 17 Alloy powder is applied and nitrided to obtain Sm 2 Fe 17 N 3 The magnetic powder has good crystallinity; meanwhile, the invention does not need the steps of crushing and the like, ensures Sm 2 Fe 17 N 3 The magnetic powder has good appearance, smooth and flat surface and fewer defects, and improves Sm 2 Fe 17 N 3 Magnetic properties of magnetic powder.
4. Non-nitrided Sm 2 Fe 17 The alloy is easy to oxidize, and the reduction diffusion in the second step and the nitridation in the third step in the preparation method only need to switch the atmosphere, can be continuously carried out in one device, and avoid Sm 2 Fe 17 The alloy contacts with oxidizing atmosphere such as air, and the like, thereby further ensuring Sm 2 Fe 17 N 3 The quality of the magnetic powder.
5. The preparation method has the advantages of simple preparation steps, mild reaction conditions, low cost, good product crystallinity and good process stability, and is favorable for realizing industrial production.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 shows Sm prepared in example 1 of the present invention 2 Fe 17 N 3 XRD pattern of magnetic powder.
FIG. 2 is a view of Sm prepared in example 2 of the present invention 2 Fe 17 N 3 XRD pattern of magnetic powder.
FIG. 3 is Sm prepared in example 3 of the present invention 2 Fe 17 N 3 XRD pattern of magnetic powder.
FIG. 4 is a preparation of example 4 of the present inventionSm of (V) 2 Fe 17 N 3 XRD pattern of magnetic powder.
FIG. 5 is Sm prepared in example 5 of the present invention 2 Fe 17 N 3 XRD pattern of magnetic powder.
FIG. 6 is a sample of Sm prepared in comparative example 1 of the present invention 2 Fe 17 N 3 XRD pattern of magnetic powder.
FIG. 7 is a diagram showing Sm prepared in comparative example 2 according to the present invention 2 Fe 17 N 3 XRD pattern of magnetic powder.
Detailed Description
Example 1
The embodiment comprises the following steps:
step one, mixing powder: uniformly mixing iron powder, samarium oxide and calcium particles, and doping potassium chloride to obtain mixed powder; the molar ratio of the samarium oxide to the iron powder is 1:11, the molar ratio of the samarium oxide to the calcium particles is 1:3.6, and the mass percentage of the potassium chloride in the mixed powder is 4%;
step two, reduction diffusion: performing heat treatment, reduction and diffusion on the mixed powder obtained in the step one under the protection atmosphere of nitrogen, reducing by calcium particles, and performing diffusion by using heat drive to obtain Sm 2 Fe 17 CaO/Ca mixed powder; the heating rate of the heat treatment reduction diffusion is 3.33 ℃/min, the temperature is 900 ℃, and the time is 6 hours;
step three, nitriding: sm obtained in the second step 2 Fe 17 Performing heat treatment nitridation on the mixed powder of CaO and Ca in the mixed gas of hydrogen and ammonia to obtain Sm 2 Fe 17 N 3 CaO/Ca mixed powder; the volume ratio of the hydrogen to the ammonia in the hydrogen/ammonia mixed gas is 4:1, and the flow rate of the hydrogen/ammonia mixed gas is 1.0L/min; the temperature rising rate of the heat treatment nitriding is 3.33 ℃/min, the temperature is 300 ℃, and the time is 6 hours;
step four, removing impurities: sm obtained in the third step 2 Fe 17 N 3 Placing the mixed powder of CaO/Ca in a washing solution, fully stirring, carrying out ultrasonic treatment and grinding to form a suspension, carrying out magnetic separation, washing and drying to obtain Sm 2 Fe 17 N 3 H x Magnetic powder;
step five, dehydrogenation: under vacuum, sm obtained in the fourth step 2 Fe 17 N 3 H x Carrying out heat treatment dehydrogenation on the magnetic powder to obtain Sm 2 Fe 17 N 3 Magnetic powder; the heating rate of the dehydrogenation by heat treatment is 3.33 ℃/min, the temperature is 150 ℃ and the time is 1h.
FIG. 1 shows Sm prepared in this example 2 Fe 17 N 3 As can be seen from the XRD patterns of the magnetic powder in FIG. 1, the magnetic powder prepared in the embodiment has good crystallinity and a pure Sm 2 Fe 17 N 3 The diffraction peak of alpha-Fe did not appear.
Example 2
The embodiment comprises the following steps:
step one, mixing powder: uniformly mixing iron powder, samarium oxide and calcium particles, and doping potassium chloride to obtain mixed powder; the molar ratio of the samarium oxide to the iron powder is 1:14.5, the molar ratio of the samarium oxide to the calcium particles is 1:3.6, and the mass percentage of the potassium chloride in the mixed powder is 10%;
step two, reduction diffusion: performing heat treatment, reduction and diffusion on the mixed powder obtained in the step one under the protection atmosphere of nitrogen, reducing by calcium particles, and performing diffusion by using heat drive to obtain Sm 2 Fe 17 CaO/Ca mixed powder; the heating rate of the heat treatment reduction diffusion is 3.33 ℃/min, the temperature is 1050 ℃, and the time is 3 hours;
step three, nitriding: sm obtained in the second step 2 Fe 17 Performing heat treatment nitridation on the mixed powder of CaO and Ca in the mixed gas of hydrogen and ammonia to obtain Sm 2 Fe 17 N 3 CaO/Ca mixed powder; the volume ratio of the hydrogen to the ammonia in the hydrogen/ammonia mixed gas is 1:2, and the flow rate of the hydrogen/ammonia mixed gas is 0.6L/min; the temperature rising rate of the heat treatment nitriding is 3.33 ℃/min, the temperature is 500 ℃, and the time is 3 hours;
step four, removing impurities: sm obtained in the third step 2 Fe 17 N 3 Placing the mixed powder of CaO/Ca in a washing solution, fully stirring, carrying out ultrasonic treatment and grinding to form a suspension, carrying out magnetic separation, washing and drying to obtain Sm 2 Fe 17 N 3 H x Magnetic powder;
step five, dehydrogenation: under vacuum, sm obtained in the fourth step 2 Fe 17 N 3 H x Carrying out heat treatment dehydrogenation on the magnetic powder to obtain Sm 2 Fe 17 N 3 Magnetic powder; the heating rate of the dehydrogenation by heat treatment is 3.33 ℃/min, the temperature is 250 ℃, and the time is 3h.
FIG. 2 is a view of Sm prepared in this example 2 Fe 17 N 3 As can be seen from the XRD patterns of the magnetic powder in FIG. 2, the magnetic powder prepared in the embodiment has good crystallinity and a pure Sm 2 Fe 17 N 3 The diffraction peak of alpha-Fe did not appear.
Example 3
The embodiment comprises the following steps:
step one, mixing powder: uniformly mixing iron powder, samarium oxide and calcium particles, and doping potassium chloride to obtain mixed powder; the molar ratio of the samarium oxide to the iron powder is 1:11, the molar ratio of the samarium oxide to the calcium particles is 1:6, and the mass percentage of the potassium chloride in the mixed powder is 4.5%;
step two, reduction diffusion: performing heat treatment, reduction and diffusion on the mixed powder obtained in the step one under the protection atmosphere of nitrogen, reducing by calcium particles, and performing diffusion by using heat drive to obtain Sm 2 Fe 17 CaO/Ca mixed powder; the heating rate of the heat treatment reduction diffusion is 3.33 ℃/min, the temperature is 950 ℃, and the time is 6 hours;
step three, nitriding: sm obtained in the second step 2 Fe 17 Performing heat treatment nitridation on the mixed powder of CaO and Ca in the mixed gas of hydrogen and ammonia to obtain Sm 2 Fe 17 N 3 CaO/Ca mixed powder; the volume ratio of the hydrogen to the ammonia in the hydrogen/ammonia mixed gas is 3:1, and the flow rate of the hydrogen/ammonia mixed gas is 0.8L/min; the temperature rising rate of the heat treatment nitriding is 3.33 ℃/min, the temperature is 400 ℃, and the time is 3 hours;
step four, removing impurities: sm obtained in the third step 2 Fe 17 N 3 Placing the mixed powder of CaO/Ca in the washing liquid, fully stirring, ultrasonic treating andgrinding to form suspension, magnetic separating, washing and drying to obtain Sm 2 Fe 17 N 3 H x Magnetic powder;
step five, dehydrogenation: under vacuum, sm obtained in the fourth step 2 Fe 17 N 3 H x Carrying out heat treatment dehydrogenation on the magnetic powder to obtain Sm 2 Fe 17 N 3 Magnetic powder; the heating rate of the dehydrogenation by heat treatment is 3.33 ℃/min, the temperature is 200 ℃, and the time is 3h.
FIG. 3 is a view of Sm prepared in this example 2 Fe 17 N 3 As can be seen from the XRD patterns of the magnetic powder in FIG. 3, the magnetic powder prepared in the embodiment has good crystallinity and a pure Sm 2 Fe 17 N 3 The diffraction peak of alpha-Fe did not appear.
Example 4
The embodiment comprises the following steps:
step one, mixing powder: uniformly mixing iron powder, samarium oxide and calcium particles, and doping potassium chloride to obtain mixed powder; the molar ratio of the samarium oxide to the iron powder is 1:11, the molar ratio of the samarium oxide to the calcium particles is 1:3.6, and the mass percentage of the potassium chloride in the mixed powder is 6%;
step two, reduction diffusion: performing heat treatment, reduction and diffusion on the mixed powder obtained in the step one under the protection atmosphere of nitrogen, reducing by calcium particles, and performing diffusion by using heat drive to obtain Sm 2 Fe 17 CaO/Ca mixed powder; the heating rate of the heat treatment reduction diffusion is 3.33 ℃/min, the temperature is 850 ℃, and the time is 6 hours;
step three, nitriding: sm obtained in the second step 2 Fe 17 Performing heat treatment nitridation on the mixed powder of CaO and Ca in the mixed gas of hydrogen and ammonia to obtain Sm 2 Fe 17 N 3 CaO/Ca mixed powder; the volume ratio of the hydrogen to the ammonia in the hydrogen/ammonia mixed gas is 2:1, and the flow rate of the hydrogen/ammonia mixed gas is 0.8L/min; the temperature rising rate of the heat treatment nitriding is 3.33 ℃/min, the temperature is 400 ℃, and the time is 6 hours;
step four, removing impurities: sm obtained in the third step 2 Fe 17 N 3 Placing the mixed powder of CaO/Ca in a washing solution, fully stirring, carrying out ultrasonic treatment and grinding to form a suspension, carrying out magnetic separation, washing and drying to obtain Sm 2 Fe 17 N 3 H x Magnetic powder;
step five, dehydrogenation: under vacuum, sm obtained in the fourth step 2 Fe 17 N 3 H x Carrying out heat treatment dehydrogenation on the magnetic powder to obtain Sm 2 Fe 17 N 3 Magnetic powder; the heating rate of the dehydrogenation by heat treatment is 3.33 ℃/min, the temperature is 400 ℃, and the time is 1h.
FIG. 4 shows Sm prepared in this example 2 Fe 17 N 3 As can be seen from the XRD patterns of the magnetic powder in FIG. 4, the magnetic powder prepared in the embodiment has good crystallinity and a pure Sm 2 Fe 17 N 3 The diffraction peak of alpha-Fe did not appear.
Example 5
The embodiment comprises the following steps:
step one, mixing powder: uniformly mixing iron powder, samarium oxide and calcium particles, and doping calcium chloride to obtain mixed powder; the molar ratio of the samarium oxide to the iron powder is 1:11, the molar ratio of the samarium oxide to the calcium particles is 1:3.6, and the mass percentage of the calcium chloride in the mixed powder is 6%;
step two, reduction diffusion: performing heat treatment, reduction and diffusion on the mixed powder obtained in the step one under the protection atmosphere of nitrogen, reducing by calcium particles, and performing diffusion by using heat drive to obtain Sm 2 Fe 17 CaO/Ca mixed powder; the heating rate of the heat treatment reduction diffusion is 3.33 ℃/min, the temperature is 1150 ℃, and the time is 1.5h;
step three, nitriding: sm obtained in the second step 2 Fe 17 Performing heat treatment nitridation on the mixed powder of CaO and Ca in the mixed gas of hydrogen and ammonia to obtain Sm 2 Fe 17 N 3 CaO/Ca mixed powder; the volume ratio of the hydrogen to the ammonia in the hydrogen/ammonia mixed gas is 2:1, and the flow rate of the hydrogen/ammonia mixed gas is 0.8L/min; the temperature rising rate of the heat treatment nitriding is 3.33 ℃/min, the temperature is 400 ℃, and the time is 6 hours;
step fourRemoving impurities: sm obtained in the third step 2 Fe 17 N 3 Placing the mixed powder of CaO/Ca in a washing solution, fully stirring, carrying out ultrasonic treatment and grinding to form a suspension, carrying out magnetic separation, washing and drying to obtain Sm 2 Fe 17 N 3 H x Magnetic powder;
step five, dehydrogenation: under vacuum, sm obtained in the fourth step 2 Fe 17 N 3 H x Carrying out heat treatment dehydrogenation on the magnetic powder to obtain Sm 2 Fe 17 N 3 Magnetic powder; the heating rate of the dehydrogenation by heat treatment is 3.33 ℃/min, the temperature is 100 ℃, and the time is 3h.
FIG. 5 is a view of Sm prepared in this example 2 Fe 17 N 3 As can be seen from the XRD patterns of the magnetic powder in FIG. 5, the magnetic powder prepared in the embodiment has good crystallinity and a pure Sm 2 Fe 17 N 3 The diffraction peak of alpha-Fe did not appear.
Comparative example 1
The comparative example comprises the following steps:
step one, mixing powder: uniformly mixing iron powder, samarium oxide and calcium particles to obtain mixed powder; the molar ratio of the samarium oxide to the iron powder is 1:11, and the molar ratio of the samarium oxide to the calcium particles is 1:18;
step two, reduction diffusion: performing heat treatment, reduction and diffusion on the mixed powder obtained in the step one under the protection atmosphere of nitrogen, reducing by calcium particles, and performing diffusion by using heat drive to obtain Sm 2 Fe 17 CaO/Ca mixed powder; the heating rate of the heat treatment reduction diffusion is 3.33 ℃/min, the temperature is 950 ℃, and the time is 6 hours;
step three, nitriding: sm obtained in the second step 2 Fe 17 Performing heat treatment nitridation on the mixed powder of CaO and Ca in the mixed gas of hydrogen and ammonia to obtain Sm 2 Fe 17 N 3 CaO/Ca mixed powder; the volume ratio of the hydrogen to the ammonia in the hydrogen/ammonia mixed gas is 3:1, and the flow rate of the hydrogen/ammonia mixed gas is 0.8L/min; the temperature rising rate of the heat treatment nitriding is 3.33 ℃/min, the temperature is 400 ℃, and the time is 3 hours;
step fourRemoving impurities: sm obtained in the third step 2 Fe 17 N 3 Placing the mixed powder of CaO/Ca in a washing solution, fully stirring, carrying out ultrasonic treatment and grinding to form a suspension, carrying out magnetic separation, washing and drying to obtain Sm 2 Fe 17 N 3 H x Magnetic powder;
step five, dehydrogenation: under vacuum, sm obtained in the fourth step 2 Fe 17 N 3 H x Carrying out heat treatment dehydrogenation on the magnetic powder to obtain Sm 2 Fe 17 N 3 Magnetic powder; the heating rate of the dehydrogenation by heat treatment is 3.33 ℃/min, the temperature is 200 ℃, and the time is 3h.
FIG. 6 is Sm prepared in this comparative example 2 Fe 17 N 3 As can be seen from the XRD pattern of the magnetic powder in FIG. 6, the magnetic powder prepared in this example has a Sm 2 Fe 17 N 3 Diffraction peaks for α -Fe did not appear, but crystallinity was poor.
Comparative example 2
The comparative example comprises the following steps:
step one, mixing powder: uniformly mixing iron powder, samarium oxide and calcium particles to obtain mixed powder; the molar ratio of the samarium oxide to the iron powder is 1:11, and the molar ratio of the samarium oxide to the calcium particles is 1:6;
step two, reduction diffusion: performing heat treatment, reduction and diffusion on the mixed powder obtained in the step one under the protection atmosphere of nitrogen, reducing by calcium particles, and performing diffusion by using heat drive to obtain Sm 2 Fe 17 CaO/Ca mixed powder; the heating rate of the heat treatment reduction diffusion is 3.33 ℃/min, the temperature is 950 ℃, and the time is 6 hours;
step three, removing impurities: sm obtained in the second step 2 Fe 17 Placing the mixed powder of CaO/Ca in a washing solution, fully stirring, carrying out ultrasonic treatment and grinding to form a suspension, carrying out magnetic separation, washing and drying to obtain Sm 2 Fe 17 Magnetic powder.
FIG. 7 is Sm prepared in this comparative example 2 Fe 17 The XRD pattern of the magnetic powder was found to be inferior in crystallinity of the magnetic powder prepared in this example, and a significant diffraction peak of alpha-Fe was present, as seen from FIG. 7.
As can be seen from a comparison of comparative examples 1 to 2 and example 3, comparative example 1 produced Sm containing no alpha-Fe with a higher amount of reducing agent calcium than in example 3 without using inorganic salt as an auxiliary agent 2 Fe 17 N 3 Phase and less crystalline, while comparative example 2 was prepared with the same amount of reducing agent calcium as example 3, without using inorganic salts as adjuvants 2 Fe 17 The magnetic powder has poor crystallinity and obvious alpha-Fe diffraction peak, and is not suitable for continuous Sm 2 Fe 17 N 3 And (3) preparation.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.
Claims (10)
1. A method for preparing samarium iron and samarium iron nitrogen with the aid of an auxiliary agent is characterized by comprising the following steps of:
step one, mixing powder: uniformly mixing iron powder, samarium oxide and calcium particles, and doping inorganic salt to obtain mixed powder;
step two, reduction diffusion: performing heat treatment on the mixed powder obtained in the first step under a protective atmosphere, reducing by calcium particles, and diffusing by using heat driving to obtain Sm 2 Fe 17 CaO/Ca mixed powder;
step three, nitriding: sm obtained in the second step 2 Fe 17 Performing heat treatment on the mixed powder of CaO and Ca in the mixed gas of hydrogen and ammonia to obtain Sm 2 Fe 17 N 3 CaO/Ca mixed powder;
step four, removing impurities: sm obtained in the third step 2 Fe 17 N 3 Grinding mixed powder of CaO/Ca in washing liquid to form suspension, and magnetically separating to obtain Sm 2 Fe 17 N 3 H x Magnetic powder;
step five, dehydrogenation: under vacuum, sm obtained in the fourth step 2 Fe 17 N 3 H x Heat treating the magnetic powder to obtain Sm 2 Fe 17 N 3 Magnetic powder.
2. The method for preparing samarium iron and samarium iron nitrogen assisted by an auxiliary agent according to claim 1, wherein the molar ratio of samarium oxide to iron powder in the first step is 1:11-14.5.
3. The method for preparing samarium iron and samarium iron nitrogen assisted by an auxiliary agent according to claim 1, wherein the molar ratio of samarium oxide to calcium particles in the first step is 1:3.6-6.
4. The method for preparing samarium iron and samarium iron nitrogen with the aid of an auxiliary agent according to claim 1, wherein the inorganic salt in the first step is potassium chloride or calcium chloride.
5. The method for preparing samarium iron and samarium iron nitrogen with the aid of the auxiliary agent according to claim 1, wherein the mass percentage of inorganic salts in the mixed powder in the first step is 4% -10%.
6. The method for preparing samarium iron and samarium iron nitrogen with the aid of the auxiliary agent according to claim 1, wherein the heat treatment temperature in the second step is 850-1150 ℃ and the time is 1.5-6 h.
7. The method for preparing samarium iron and samarium iron nitrogen with the aid of the auxiliary agent according to claim 1, wherein the volume ratio of hydrogen to ammonia in the hydrogen/ammonia mixed gas in the third step is 1-8:2.
8. The method for preparing samarium iron and samarium iron nitrogen with the aid of an auxiliary agent according to claim 1, wherein the flow rate of the hydrogen/ammonia mixed gas in the third step is 0.6L/min-1.0L/min.
9. The method for preparing samarium iron and samarium iron nitrogen with the aid of the auxiliary agent according to claim 1, wherein the temperature of the heat treatment in the third step is 300-500 ℃ and the time is 3-6 h.
10. The method for preparing samarium iron and samarium iron nitrogen with the aid of the auxiliary agent according to claim 1, wherein the temperature of the heat treatment in the fifth step is 100-400 ℃ and the time is 1-3 h.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108274016A (en) * | 2018-03-14 | 2018-07-13 | 浙江工业大学 | A kind of method that spray-wall interaction reduction method directly prepares samarium ferroalloy powder |
| US20200016663A1 (en) * | 2016-03-04 | 2020-01-16 | National Institute Of Advanced Industrial Science And Technology | Samarium-iron-nitrogen alloy powder and method for producing same |
| US20220189669A1 (en) * | 2019-03-12 | 2022-06-16 | Tdk Corporation | Anisotropic magnetic powder, anisotropic magnet and method for manufacturing anisotropic magnetic powder |
| CN114898960A (en) * | 2022-03-24 | 2022-08-12 | 北矿科技股份有限公司 | Preparation method of nano-scale SmFeN magnetic powder |
| CN116741484A (en) * | 2022-03-04 | 2023-09-12 | 福建省长汀金龙稀土有限公司 | Samarium-iron alloy, samarium-iron-nitrogen permanent magnet material, and preparation methods and applications thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20200016663A1 (en) * | 2016-03-04 | 2020-01-16 | National Institute Of Advanced Industrial Science And Technology | Samarium-iron-nitrogen alloy powder and method for producing same |
| CN108274016A (en) * | 2018-03-14 | 2018-07-13 | 浙江工业大学 | A kind of method that spray-wall interaction reduction method directly prepares samarium ferroalloy powder |
| US20220189669A1 (en) * | 2019-03-12 | 2022-06-16 | Tdk Corporation | Anisotropic magnetic powder, anisotropic magnet and method for manufacturing anisotropic magnetic powder |
| CN116741484A (en) * | 2022-03-04 | 2023-09-12 | 福建省长汀金龙稀土有限公司 | Samarium-iron alloy, samarium-iron-nitrogen permanent magnet material, and preparation methods and applications thereof |
| CN114898960A (en) * | 2022-03-24 | 2022-08-12 | 北矿科技股份有限公司 | Preparation method of nano-scale SmFeN magnetic powder |
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