CN101798652A - Method for improving corrosion resistance and processability of neodymium-iron-boron through tin and titanium complex adding - Google Patents

Method for improving corrosion resistance and processability of neodymium-iron-boron through tin and titanium complex adding Download PDF

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Publication number
CN101798652A
CN101798652A CN 201010158358 CN201010158358A CN101798652A CN 101798652 A CN101798652 A CN 101798652A CN 201010158358 CN201010158358 CN 201010158358 CN 201010158358 A CN201010158358 A CN 201010158358A CN 101798652 A CN101798652 A CN 101798652A
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China
Prior art keywords
boron
tin
neodymium
neodymium iron
iron boron
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CN 201010158358
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袁文杰
王文慧
董义
刁树林
范耀林
陈雅
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TIANJIN TIANHE MAGNETIC MATERIAL TECHNOLOGY Co Ltd
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TIANJIN TIANHE MAGNETIC MATERIAL TECHNOLOGY Co Ltd
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Abstract

The invention discloses a method for improving corrosion resistance and processability of neodymium-iron-boron through tin and titanium complex adding, high performance sintered neodymium-iron-boron and a preparation method thereof. Tin and titanium account for 0.2 to 2.2 atom percent; a rare-earth element accounts for 12.9 to 14.2 atom percent; ferrum accounts for 75 to 78 atom percent; boron accounts for 5.8 to 6.3 atom percent; and other element accounts for 0.01 to 4.3 atom percent, wherein the other element is one or more of cobalt, nickel, aluminum, copper, zirconium, niobium, tungsten, manganese, gallium, silicon, carbon and oxygen. The neodymium-iron-boron material has the advantages of high corrosion resistance and high mechanical processing yield.

Description

The method of the corrosion-resistant and processibility of tin titanium compound interpolation improvement neodymium iron boron
Technical field
The invention belongs to the materials processing of neodymium iron boron magnetic, particularly a kind of method of corrosion-resistant and processibility of tin titanium compound interpolation improvement neodymium iron boron.
Background technology
R 2Fe 14The Type B compound-material is present magnetic energy product the highest permanent magnet material, particularly sintered Nd-Fe-B permanent magnet, and the coercive force of its superelevation and remanent magnetism make it obtain the title of " magnetic king ".High-coercive force and high remanent magnetism make it that bigger magneticflux-density is provided in application, have dwindled the volume of equipment greatly.But along with the expansion of the Application Areas of neodymium iron boron, people are to R 2Fe 14The erosion resistance and the workability of Type B compound-material have proposed requirement.
The neodymium iron boron type compound is a kind of being easy in moist hot environment and the compound of corrosion failure.Under present condition, most NbFeB sintered permanent magnetism of using the generally high temperature hygrothermal environment that completely cut off outside of the means by coating protect the neodymium iron boron mother metal itself not to be corroded.The drawback of coating protection is that the neodymium iron boron mother metal is corroded rapidly in environment for use, and sudden disabler takes place after coating destroys, and does not almost have tangible omen before it destroys.Because this sudden function that causes owing to corroding rapidly of NdFeB material is destroyed and is made the inefficacy of equipment be difficult to obtain effective early warning.
The workability of neodymium iron boron is another difficult point that neodymium iron boron is broken through Application Areas, for baroque different in nature part, after the compression molding, need to its carry out chamfering, round as a ball, draw mechanical workouts such as hole, cutting.Because the hardness height of neodymium iron boron, toughness is little, has inevitably caused arrisdefect in the course of processing, falls the limit, knocks mechanical workout damages such as spot.Owing to permanent magnet uses as the energy storage material that magnetic energy is provided, its outer shape produces very big influence to the performance of itself simultaneously, in case the mechanical hard defects of its outside appearance are represented the inefficacy of its function substantially.
Summary of the invention
Technical problem to be solved by this invention is: the method that a kind of corrosion-resistant and processibility of tin titanium compound interpolation improvement neodymium iron boron is provided.
Technical scheme of the present invention is:
A kind of method of corrosion-resistant and processibility of tin titanium compound interpolation improvement neodymium iron boron is characterized in that: the steps include:
Material composition: the atom percentage composition of its prescription is: tin element and titanium elements 0.2-2.2%, rare earth element 12.9-14.2%, ferro element 75-78%, boron 5.8-6.3%, other elements: one or more 0.01-4.3% in cobalt, nickel, aluminium, copper, zirconium, niobium, tungsten, gallium, silicon, carbon, the oxygen;
1) utilize rapid hardening thin slice prepared Nd-Fe-B alloys thin slice or utilize casting ingot process to prepare the Nd-Fe-B alloys steel ingot, broken and air-flow grinding process prepares the Nd-Fe-B alloys powder that mean particle size is 3-10 μ m by hydrogen;
2) powder compression moulding under the magnetic field of 1.2-3T, its density is 3.0-4.7g/cm after the moulding 3
3) base substrate is put into high vacuum sintering furnace, through 1045-1100 ℃ of sintering 3-5h under the vacuum tightness 0.02Pa, slow cooling carries out the insulation of 3-5h and handles to 350-800 ℃ then, is cooled to 70 ℃ at last rapidly and comes out of the stove;
In powder metallurgy process, take various anti-oxidation measures, as vacuum melting, atmosphere protection, vacuum sintering, interpolation antioxidant.
Effect of the present invention is:
The method of the corrosion-resistant and processibility of tin titanium compound interpolation improvement neodymium iron boron is to add tin and two kinds of elements of titanium by the while in neodymium iron boron, and reaches the erosion resistance of raising neodymium iron boron and the purpose of workability by specific melting-airflow milling-sintering process.In the NdFeB material of the interpolation titanium elements of trace, the erosion resistance of neodymium iron boron can slightly improve, when adding a large amount of titanium elements, the magnetic property of neodymium iron boron descends very big, pass through to use the method for tin and the compound interpolation of titanium among the present invention, guaranteeing to add under the constant situation of element atomic percentage conc, improved the erosion resistance of NdFeB material greatly, simultaneously because the compound interpolation of two kinds of elements, the high cryogenic mechanics performance of material improves, and toughness strengthens, and has reduced the probability that causes structural impairment owing to thermal shock, simultaneously improve the destruction of NdFeB material in the course of processing greatly, improved yield rate.
Embodiment
Corrosion-resistant and the workability method of tin titanium compound interpolation improvement neodymium iron boron:
The atom percentage composition of its prescription is: tin element and titanium elements 0.2-2.2%, rare earth element 12.9-14.2%, ferro element 75-78%, boron 5.8-6.3%, one or more 0.01-4.3% in other element cobalt, nickel, aluminium, copper, zirconium, niobium, tungsten, gallium, silicon, carbon, the oxygen;
Its preparation process is:
1, according to prescription various raw materials is mixed in proportion;
2, utilize rapid hardening thin slice prepared Nd-Fe-B alloys thin slice or utilize casting ingot process to prepare the Nd-Fe-B alloys steel ingot, broken and air-flow grinding process prepares the Nd-Fe-B alloys powder that mean particle size is 3-10 μ m by hydrogen;
2, powder compression moulding under the magnetic field of 1.2-3T, its density is 3.0-4.7g/cm after the moulding 3
3, base substrate is put into high vacuum sintering furnace, through 1045-1100 ℃ of sintering 3-5h under the vacuum tightness 0.02Pa, slow cooling carries out the insulation of 3-5h and handles to 350-800 ℃ then.Being cooled to 70 ℃ at last rapidly comes out of the stove.
Various anti-oxidation measure in the aforesaid method in powder metallurgy process is as vacuum melting, atmosphere protection, vacuum sintering, interpolation antioxidant etc.Its anti-oxidation measure may be interpreted as the impurity of avoiding material composition to depart from and introducing from air.
Various raw-material prescriptions compositions (atomic percent) are among the present invention: tin element and titanium elements 0.2-2.2%, rare earth element 12.9-14.2%, ferro element 75-78%, boron 5.8-6.3%, one or more 0.1-2.3% in other element cobalt, nickel, aluminium, copper, zirconium, niobium, tungsten, gallium, silicon, carbon, the oxygen.
The making step of the NdFeB material that the corrosion-resistant workability of heatproof described in the present invention is good is:
1, batching: various raw materials are mixed in proportion according to prescription;
2, utilize rapid hardening thin slice prepared neodymium iron boron phase thin slice or utilize casting ingot process to prepare neodymium iron boron phase steel ingot, the broken or Mechanical Crushing by hydrogen, broken back makes the neodymium iron boron phase powder that granularity is 3-10 μ m by airflow milling technology;
3, powder compression moulding under the magnetic field of 1.2-3T, its density is 3.0-4.7g/cm after the moulding 3
4, base substrate is put into high vacuum sintering furnace, through 1045-1100 ℃ of sintering 3-5h under the vacuum tightness 0.02Pa, slow cooling carries out the insulation of 3-5h and handles to 350-800 ℃ then.Being cooled to 70 ℃ at last rapidly comes out of the stove.
Concrete case
Following example is set forth for further specifying the present invention, but example under the present invention is not limited thereto.
Case study on implementation 1
1) adopt rapid hardening thin slice casting technique to prepare Nd-Fe-B alloys, its nominal composition atomic percent is:
Nd is 12.94%, and Fe is 78.87%, and B is 5.89%, and Dy is 0.42%, and Co is 0.53%, and Ti is 0.20%, and Sn is 0.04%, and Al is 1.1%, and Cu is 0.01%;
2) with hydrogen broken-airflow milling technology carries out powder process, neodymium iron boron particulate median size is 3.2 μ m after the powder process;
3) compression moulding in the magnetic field of 1.8T;
4) blank after the moulding is carried out waiting static pressure 5-18 minute under the pressure of 15-20Mpa;
5) carry out product section yield statistics in magnetism testing and corrosion-resistant zero-G test and the actual production, the condition of zero-G test is 2.7 normal atmosphere of pressure, 130 ℃ of temperature, humidity 100%RH, 240 hours time.
The performance of the sample by above-mentioned prepared and the contrast of common neodymium iron boron are listed as follows:
Sample ??B r??(KGs) ??H cj??(KOe) ??(BH) max??(MGOe) Weightless (mg/cm 2) Yield rate (1000)
The compound interpolation neodymium iron boron of titanium tin ??13.86 ??17.91 ??46.55 ??0.76 ??98.6%
With the performance neodymium iron boron product ??13.85 ??17.89 ??46.53 ??5.35 ??91.3%
Case study on implementation 2
1) adopt rapid hardening thin slice casting technique to prepare Nd-Fe-B alloys, the atomic percent of its nominal composition is: Nd is that Nd is 13.36%, and Fe is 78.67%, and B is 5.89%, Dy is 0.33%, and Co is 0.3%, and Ti is 0.5%, Sn is 0.23%, and Al is 0.6%, and Cu is 0.1%;
2) with hydrogen broken-airflow milling technology carries out powder process, neodymium iron boron particulate median size is 3.2 μ m after the powder process;
3) compression moulding in the magnetic field of 1.8T;
4) blank after the moulding is carried out waiting static pressure 5-18 minute under the pressure of 15-20Mpa;
5) carry out product section yield statistics in magnetism testing and corrosion-resistant zero-G test and the actual production, the condition of zero-G test is 2.7 normal atmosphere of pressure, 130 ℃ of temperature, humidity 100%RH, 240 hours time.
The performance of the sample by above-mentioned prepared and the contrast of common neodymium iron boron are listed as follows:
Sample ??B r??(KGs) ??H cj??(KOe) ??(BH) max??(MGOe) Weightless (mg/cm 2) Yield rate (1000)
The compound interpolation neodymium iron boron of titanium tin ??13.9 ??15.1 ??46.63 ??0.36 ??99.0%
With the performance neodymium iron boron product ??13.92 ??15.15 ??46.71 ??5.25 ??91.4%

Claims (1)

1. the method for the corrosion-resistant and processibility of tin titanium compound interpolation an improvement neodymium iron boron is characterized in that: the steps include:
Material composition: the atom percentage composition of its prescription is: tin element and titanium elements 0.2-2.2%, rare earth element 12.9-14.2%, ferro element 75-78%, boron 5.8-6.3%, other elements: one or more 0.01-4.3% in cobalt, nickel, aluminium, copper, zirconium, niobium, tungsten, manganese, gallium, silicon, carbon, the oxygen;
1) utilize rapid hardening thin slice prepared Nd-Fe-B alloys thin slice or utilize casting ingot process to prepare the Nd-Fe-B alloys steel ingot, broken and air-flow grinding process prepares the Nd-Fe-B alloys powder that mean particle size is 3-10 μ m by hydrogen;
2) powder compression moulding under the magnetic field of 1.2-3T, its density is 3.0-4.7g/cm after the moulding 3
3) base substrate is put into high vacuum sintering furnace, through 1045-1100 ℃ of sintering 3-5h under the vacuum tightness 0.02Pa, slow cooling carries out the insulation of 3-5h and handles to 350-800 ℃ then, is cooled to 70 ℃ at last rapidly and comes out of the stove.
CN 201010158358 2010-04-28 2010-04-28 Method for improving corrosion resistance and processability of neodymium-iron-boron through tin and titanium complex adding Pending CN101798652A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102412044A (en) * 2011-11-16 2012-04-11 宁波同创强磁材料有限公司 Ultralow weightless sintered neodymium iron boron magnetic material and preparation method thereof
CN102447357A (en) * 2011-11-04 2012-05-09 无锡天宝电机有限公司 Preparation method capable of improving processability for sintered neodymium-iron-boron for motor
CN103121102A (en) * 2013-02-05 2013-05-29 中铝广西有色金源稀土股份有限公司 Sintering tempering method of neodymium iron boron magnetic materials

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5181973A (en) * 1990-02-14 1993-01-26 Tdk Corporation Sintered permanent magnet
CN1257290A (en) * 1998-12-11 2000-06-21 信越化学工业株式会社 Process for preparing rare earth base permanent magnet
JP2002339018A (en) * 2001-05-17 2002-11-27 Nissan Motor Co Ltd Alloy for anisotropic exchange-spring magnet and method for producing exchange-spring magnet
CN101051544A (en) * 2007-05-10 2007-10-10 浙江大学 Method for preparing high performance sintered neodymium-iron-boron air stream millby hydrogenation
CN101315825A (en) * 2007-05-31 2008-12-03 北京中科三环高技术股份有限公司 Fire resistant permanent magnet alloy and manufacturing method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5181973A (en) * 1990-02-14 1993-01-26 Tdk Corporation Sintered permanent magnet
CN1257290A (en) * 1998-12-11 2000-06-21 信越化学工业株式会社 Process for preparing rare earth base permanent magnet
JP2002339018A (en) * 2001-05-17 2002-11-27 Nissan Motor Co Ltd Alloy for anisotropic exchange-spring magnet and method for producing exchange-spring magnet
CN101051544A (en) * 2007-05-10 2007-10-10 浙江大学 Method for preparing high performance sintered neodymium-iron-boron air stream millby hydrogenation
CN101315825A (en) * 2007-05-31 2008-12-03 北京中科三环高技术股份有限公司 Fire resistant permanent magnet alloy and manufacturing method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102447357A (en) * 2011-11-04 2012-05-09 无锡天宝电机有限公司 Preparation method capable of improving processability for sintered neodymium-iron-boron for motor
CN102447357B (en) * 2011-11-04 2015-05-13 无锡天宝电机有限公司 Preparation method capable of improving processability for sintered neodymium-iron-boron for motor
CN102412044A (en) * 2011-11-16 2012-04-11 宁波同创强磁材料有限公司 Ultralow weightless sintered neodymium iron boron magnetic material and preparation method thereof
CN102412044B (en) * 2011-11-16 2014-01-22 宁波同创强磁材料有限公司 Ultralow weightless sintered neodymium iron boron magnetic material and preparation method thereof
CN103121102A (en) * 2013-02-05 2013-05-29 中铝广西有色金源稀土股份有限公司 Sintering tempering method of neodymium iron boron magnetic materials

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