CN101552063A - High-performance neodymium-iron-boron magnet with composite addition of titanium and zirconium - Google Patents
High-performance neodymium-iron-boron magnet with composite addition of titanium and zirconium Download PDFInfo
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- CN101552063A CN101552063A CNA2008101632287A CN200810163228A CN101552063A CN 101552063 A CN101552063 A CN 101552063A CN A2008101632287 A CNA2008101632287 A CN A2008101632287A CN 200810163228 A CN200810163228 A CN 200810163228A CN 101552063 A CN101552063 A CN 101552063A
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Abstract
The invention discloses a high-performance neodymium-iron-boron magnet with composite addition of titanium and zirconium, which is composed of the following components by weight percentage: 20 percent-33 percent of praseodymium-neodymium alloy, 0.1 percent-1 percent of titanium, 0.1 percent-0.5 percent of zirconium, 0.1 percent-10 percent of dysprosium, 0 percent-10 percent of gadolinium, 0 percent-10 percent of holmium, 0.9 percent-1.2 of percent boron, 0.1 percent-0.5 percent of aluminum, 0.1 percent-0.5 percent of copper, 0 percent-5 percent of terbium, 0 percent-3 percent of cobalt and the balance of iron and a small amount of inevitable impurities in materials. The high-performance neodymium-iron-boron magnet with composite addition of titanium and zirconium has high product performance and low production cost, improves the overall magnetic performance of the magnet and enhances the enterprise competitiveness.
Description
Technical field
The present invention relates to the Nd-Fe-Bo permanent magnet material technical field, particularly use the sintered Nd-Fe-B permanent magnetic material of compound interpolation replacement gallium (Ga) of titanium (Ti) and zirconium (Zr) and cobalt precious metals such as (Co), be specifically related to the high-performance neodymium-iron-boron magnet of the compound interpolation of titanium zirconium.
Background technology
Neodymium iron boron (NdFeB) magnetic material is the third generation permanent magnetic material of early eighties exploitation, and it has very strong magnetic property, is the strongest permanent magnet of current magnetic, is called as " permanent magnetism king ".Nd-Fe-Bo permanent magnet material is widely used in international and domestic emerging developing industry and pillar industry, as computer industry, information industry, telecommunications industry, auto industry, Magnetic resonance imaging industry, office automation etc. because of it has good cost performance.Along with raising to the magnet requirement on devices, especially the used device in information communication field is to the development of directions such as miniaturization, lightweight, high speed, low noiseization, require magnet performance to improve gradually, consumption to high-performance Fe-Nd-B magnet will constantly increase, so high-performance Ne-Fe-B permanent-magnet material is the emphasis of present industry development.
But the production of high-performance Ne-Fe-B permanent-magnet material is the production of high-performance neodymium-iron-boron magnet particularly, need to use more rare precious metal such as gallium and cobalt etc., because in recent years non-ferrous metal and rare earth element price sharp rise, this causes the production cost of high-performance Ne-Fe-B permanent-magnet material high, and existing high-performance Ne-Fe-B permanent-magnet material corrosion resistance is relatively poor, has seriously restricted the fast development of sintered NdFeB magnetic industry.
Pass through to add the relatively cheap metals of price such as zirconium in the prior art, substitute relatively costly metals such as niobium, cobalt in the neodymium iron boron magnetic body, thereby reduce production costs, applying for a patent publication number as China is among the CN101256860A " with the Nd-Fe-Bo permanent magnet material of zirconium to substitute niobium ", mention and use the alternative niobium of zirconium to reduce production costs, but only add a kind of relatively cheap zirconium, and addition only is 0.1%～0.5%, still can not effectively reduces cost.
Summary of the invention
The technical problem to be solved in the present invention is the above-mentioned deficiency at prior art, and the high-performance neodymium-iron-boron magnet of a kind of magnetic property height, the compound interpolation of titanium zirconium that production cost is low is provided.
In order to solve the problems of the technologies described above, technical scheme of the present invention is: the high-performance neodymium-iron-boron magnet of the compound interpolation of titanium zirconium is made up of the component of following percetage by weight: praseodymium neodymium (PrNd) alloy 20%～33%, titanium (Ti) 0.1%～1%, zirconium (Zr) 0.1%～0.5%, dysprosium (Dy) 0.1%～10%, gadolinium (Ga) 0%～10%, holmium (Ho) 0%～10%, boron (B) 0.9%～1.2%, aluminium (Al) 0.1%～0.5%, copper (Cu) 0.1%～0.5%, terbium (Tb) 0～5%, cobalt (Co) 0～3%, surplus are a small amount of unavoidable impurities in iron (Fe) and the material.
Above-mentioned praseodymium neodymium alloy, the percentage by weight that adopts commercially available praseodymium are 20%～30% praseodymium neodymium alloy.
Above-mentioned dysprosium, the fusing point in practical operation when reducing batching processing fusion, adopting the percentage by weight of buying commercially available dysprosium is 75%～85% Dy-Fe alloy.
Above-mentioned zirconium, the fusing point in practical operation when reducing batching processing fusion, adopting the percentage by weight of buying commercially available zirconium is that 50%～60% ferrozirconium adds.
Above-mentioned boron, the fusing point in practical operation when reducing batching processing fusion, adopting the percentage by weight of buying commercially available boron is that 18%～20% ferro-boron adds.
The preparation section of the high-performance neodymium-iron-boron magnet of the compound interpolation of titanium zirconium of the present invention is:
Batching: each component is proportionally prepared burden, mix.
Melting: will be in proportion raw materials mixed pack in the vacuum spun furnace, when the air in the vacuum spun furnace is evacuated down to 5Pa, begin the melting of heating, when batching is rubescent to stove, close vacuum valve, charge into argon gas to 0.6Pa, and elevated temperature, melt fully until batching, refining was poured into a mould after 10 minutes again, powered-down is waited to get rid of when the sheet temperature is lower than 80 ℃ and is come out of the stove then.
Powder process: will get rid of sheet and be positioned in the hydrogen crushing furnace, feed hydrogen, treat product inhale fully hydrogen to 0.2Mpa stable after, close hydrogen valve, be warming up to 550～600 ℃, carried out dehydrogenation 6～9 hours, the powder after dehydrogenation is finished is put into airflow milling and is carried out powder process, control powder particles (laser particle analyzer) adds powder gasoline (the per kilogram powder adds 10～30 milligrams of gasoline) then and carries out stirring in 30～60 minutes between 3～5 μ m.
Moulding: the powder that stirs weight is in accordance with regulations weighed, put into the mould of moulding press, add compression moulding behind the magnetic field orientating, green compact are taken out in demagnetization then, and rapid Vacuum Package, the good green compact of Vacuum Package are put into the isostatic pressing machine 150～200Mpa that pressurizes, pressurize was taken out after 1～3 minute again.
Sintering: green compact are packed in the sintering basin, put into the sintering furnace sintering, sintering is 3～5 hours under 1050～1100 ℃ sintering temperature, takes out after 3～6 hours 480 ℃～600 ℃ tempering, and the Sintered NdFeB magnet operation is finished.
Advantage of the present invention and beneficial effect are:
1. rare rare earth materials such as gallium in the alternative high-performance neodymium-iron-boron magnet of compound interpolation titanium and zirconium and cobalt, improved the corrosion resistance of product: adopt experiment condition in 2 atmospheric pressure of pressure, 120 ℃ of temperature, relative humidity 95%, 168 hours time, average weightless less than 10mg/cm
2
2. rare rare earth materials such as gallium in the alternative high-performance neodymium-iron-boron magnet of compound interpolation titanium and zirconium and cobalt are reaching average weightlessness less than 10mg/cm
2Equal below-G conditions under, cobalt can add 1% less, has reduced the consumption of rare precious metals; Again because titanium and zirconium all are the profuse metallic elements of content in the stratum, its price is well below the price of expensive metal such as gallium and cobalt, and applying for a patent publication number with China is among the CN101256860A " with the Nd-Fe-Bo permanent magnet material of zirconium to substitute niobium ", the zirconium addition only is 0.1%～0.5% to compare, further reduced production cost, reduce the consumption of high price rare metal, promoted the market competitiveness of enterprise.
Embodiment
The present invention will be further described below in conjunction with specific embodiment, but the present invention not only limits to following examples:
Embodiment one:
Batching: the proportioning by following percentage by weight is prepared burden: 30% praseodymium neodymium alloy (content of neodymium accounts for 75% in the alloy), 1% boron, 0.7% dysprosium, 0.5% aluminium, 0.1% zirconium, 0.2% titanium, 0.5% cobalt, 0.2% bronze medal, surplus are a small amount of unavoidable impurities in iron and the material; In order to reduce the batching fusing point, under the constant situation of dysprosium, boron, three kinds of materials of zirconium shared percentage by weight in guaranteeing above-mentioned each comfortable batching, adopt the form of alloy to add; Be that boron adds with the ferro-boron form, the content of boron is 18.5% in the alloy; Dysprosium adds with the Dy-Fe alloy form, and the content of dysprosium is 79.5% in the alloy; Zirconium adds with the ferrozirconium form, and the content of zirconium is 50% in the alloy.
With melting 100Kg Nd Fe B alloys is example, and each set of dispense is such as shown in the table 1-1:
Each set of dispense ratio among the table 1-1 embodiment one
Single by above proportioning, each raw material mixing is encased in the vacuum spun furnace.
Melting: the raw material that will mix are in proportion packed in the vacuum spun furnace, when the air in the vacuum spun furnace is evacuated down to 5Pa, begin the melting of heating, when batching is rubescent to stove, close vacuum valve, charge into argon gas to 0.6Pa, and elevated temperature, melt fully until batching, refining was poured into a mould after 10 minutes again, powered-down is waited to get rid of when the sheet temperature is lower than 80 ℃ and is come out of the stove then.
Powder process: will get rid of sheet and be positioned in the hydrogen crushing furnace, feed hydrogen, treat product inhale fully hydrogen to 0.2Mpa stable after, close hydrogen valve, be warming up to 550～600 ℃, carried out dehydrogenation 6～9 hours, the powder after dehydrogenation is finished is put into airflow milling and is carried out powder process, control powder particles (laser particle analyzer) adds powder gasoline (the per kilogram powder adds 10～30 milligrams of gasoline) then and carries out stirring in 30～60 minutes between 3～5 μ m.
Moulding: the powder that stirs weight is in accordance with regulations weighed, put into the mould of moulding press, add compression moulding behind the magnetic field orientating, green compact are taken out in demagnetization then, and rapid Vacuum Package, the good green compact of Vacuum Package are put into the isostatic pressing machine 150～200Mpa that pressurizes, pressurize was taken out after 1～3 minute again.
Sintering: green compact are packed in the sintering basin, put into the sintering furnace sintering, sintering is 3～5 hours under 1050～1100 ℃ sintering temperature, takes out after 3～6 hours 480 ℃～600 ℃ tempering, and the Sintered NdFeB magnet operation is finished.
Sintered NdFeB magnet by above operation production, use the compound interpolation of 0.2% titanium and 0.1% zirconium to replace 1% cobalt, the cancellation gallium is made sintered Nd-Fe-B alloy, detect according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, magnetic property is shown in table 1-2:
Table 1-2 adds the magnetic property (reach with the neodymium iron boron magnetic body that does not add zirconium, titanium and compare) of the neodymium iron boron magnetic body of zirconium, titanium
| Remanent magnetism Br/KGs | HCJ/KOe | Coercivity H b/KOe | Magnetic energy product BH (max)/MGOe | |
| Embodiment one | 13.91 | 15.17 | 13.62 | 47.18 |
| The neodymium iron boron magnetic body of no zirconium, titanium | 13.88 | 14.7 | 13.41 | 46.44 |
Contrast above data as can be known, use the compound interpolation of 0.2% titanium and 0.1% zirconium to replace 1% cobalt, behind the cancellation gallium, the magnetic property of magnet has all obtained certain raising, and cost savings 5～10%.
Embodiment two:
Batching: prepare burden by following proportioning: 28.2% praseodymium neodymium alloy (neodymium content accounts for 75% in the alloy), 1% boron, 1% terbium, 1% dysprosium, 0.5% aluminium, 0.1% titanium, 0.1% zirconium, 0.5% cobalt, 0.2% bronze medal, surplus are a small amount of unavoidable impurities in iron and the material; In order to reduce the batching fusing point, under the constant situation of dysprosium, boron, three kinds of materials of zirconium shared percentage by weight in guaranteeing above-mentioned each comfortable batching, adopt the form of alloy to add; Be that boron is formed with ferro-boron, the boron ratio is 18.5%, and dysprosium is a Dy-Fe alloy, and the ratio of dysprosium is 79.5%, and Zr is a ferrozirconium, and wherein zirconium content 50%.
With melting 100Kg Nd Fe B alloys is example, and each set of dispense is such as shown in the table 2-1:
Each set of dispense ratio among the table 2-1 embodiment two
Single by above proportioning, each raw material is mixed in the vacuum spun furnace of packing into, other preparation section is with embodiment one.
Sintered NdFeB magnet after preparation section is finished, be to use the compound interpolation of 0.1% titanium and 0.1% zirconium to replace 1% cobalt, cancellation gallium, the sintered Nd-Fe-B alloy of making, detect according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, magnetic property is shown in table 2-2:
Table 2-2 adds the magnetic property (reach with the neodymium iron boron magnetic body that does not add zirconium, titanium and compare) of the neodymium iron boron magnetic body of zirconium, titanium
| Remanent magnetism Br/KGs | HCJ/KOe | Coercivity H b/KOe | Magnetic energy product BH (max)/MGOe |
| Embodiment two | 13.87 | 17.64 | 13.46 | 46.48 |
| The neodymium iron boron magnetic body of no zirconium, titanium | 13.85 | 17.26 | 13.45 | 46.36 |
From above data as can be known, use the compound interpolation of 0.1% titanium and 0.1% zirconium to replace 1% cobalt, behind the cancellation gallium, the magnetic property of magnet has all obtained certain raising, and cost savings 5～10%.
Embodiment three:
Batching: prepare burden by following proportioning: 24.5% praseodymium neodymium alloy (wherein the neodymium content in the praseodymium neodymium alloy accounts for 75%), 1% boron, 6% dysprosium, 0.5% aluminium, 0.2% titanium, 0.1% zirconium, 0.5% cobalt, 0.2% bronze medal, surplus are a small amount of unavoidable impurities in iron and the material; In order to reduce the batching fusing point, under the constant situation of dysprosium, boron, three kinds of materials of zirconium shared percentage by weight in guaranteeing above-mentioned each comfortable batching, adopt the form of alloy to add; Be that boron adds with ferro-boron, the content of boron is 18.5% in the alloy; Dysprosium adds with the Dy-Fe alloy form, and the content of dysprosium is 79.5% in the alloy; Zirconium adds with the ferrozirconium form, and the content of zirconium is 50% in the alloy.
With melting 100Kg Nd Fe B alloys is example, and each set of dispense is such as shown in the table 3-1:
Each set of dispense ratio among the table 3-1 embodiment three
Single by above proportioning, each raw material is mixed in the vacuum spun furnace of packing into, its preparation section is with embodiment one.
The Sintered NdFeB magnet of gained after production process is finished, be to use the compound interpolation of 0.2% zirconium and 0.1% titanium to replace 1% cobalt, cancellation gallium, the sintered Nd-Fe-B alloy of making, detect according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, magnetic property is shown in table 3-2:
Table 3-2 adds the magnetic property (reach with the neodymium iron boron magnetic body that does not add zirconium, titanium and compare) of the neodymium iron boron magnetic body of zirconium, titanium
| Remanent magnetism Br/KGs | HCJ/KOe | Coercivity H b/KOe | Magnetic energy product BH (max)/MGOe | |
| Embodiment three | 12.74 | 25.71 | 12.56 | 39.94 |
| The neodymium iron boron magnetic body of no zirconium, titanium | 12.6 | 25.62 | 12.38 | 39.13 |
From above data as can be known, use the compound interpolation of 0.2% titanium and 0.1% zirconium to replace 1% cobalt, behind the cancellation gallium, the magnetic property of magnet has all obtained certain raising, cost savings 5～10%.
Add the low weightless effect that titanium, zirconium prescription also can effectively improve product, under 2 atmospheric pressure, 120 ℃ of temperature, relative humidity 95%, the experimental condition of 168 hours time, add titanium, zirconium prescription significantly better than not adding titanium, zirconium prescription, the weightless comparing result of both sides sees Table 3:
Table 3 the present invention and the conventional weight-loss ratio that does not add the neodymium iron boron magnetic body of zirconium and titanium
| The trade mark | Weight (mg) before the test | Test back weight (mg) | Weight-loss ratio (mg/cm 2) | Remarks |
| 48M(10×10×10) | 7612.5 | 7559.1 | 8.9 | Add titanium zirconium prescription |
| 48M(10×10×10) | 7614.8 | 7489.3 | 20.91 | Do not add titanium zirconium prescription |
| 40UH(10×10×10) | 7659.7 | 7614.3 | 7.57 | Add titanium zirconium prescription |
| 40UH(10×10×10) | 7657.6 | 7559.7 | 16.31 | Do not add titanium zirconium prescription |
The test data of comprehensive above sintered NdFeB, use titanium, the compound interpolation of zirconium to replace rare metals such as more expensive relatively cobalt, gallium, can optimize the grain structure of neodymium iron boron, improve the performance of neodymium iron boron magnetic body, reduced the product weight-loss ratio, reach the purpose that replaces the part precious metal, finally reduced the production cost of enterprise.
Claims (1)
1. the high-performance neodymium-iron-boron magnet of the compound interpolation of a titanium zirconium, it is made up of following components in weight percentage: praseodymium neodymium alloy 20%～33%, titanium 0.1%～1%, zirconium 0.1%～0.5%, dysprosium 0.1%～10%, gadolinium 0%～10%, holmium 0%～10%, boron 0.9%～1.2%, aluminium 0.1%～0.5%, copper 0.1%～0.5%, terbium 0～5%, cobalt 0～3%, surplus are a small amount of unavoidable impurities in iron and the material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102509602A (en) * | 2011-11-21 | 2012-06-20 | 宁波市展发磁业科技有限公司 | High-performance magnetic material |
| CN104821226A (en) * | 2015-05-07 | 2015-08-05 | 安徽万磁电子有限公司 | Method for making high-square-degree sintered NdFeB permanent magnets with cerium, titanium, cobalt and zirconium compound additive |
| CN103413668B (en) * | 2012-11-13 | 2017-05-31 | 宁波宏垒磁业有限公司 | A kind of method for preparing dysprosium iron neodymium iron boron magnetic body |
| EP4016561A4 (en) * | 2019-12-24 | 2022-10-19 | Fujian Changting Golden Dragon Rare-Earth Co., Ltd. | High-cu and high-al neodymium iron boron magnet and preparation method therefor |
-
2008
- 2008-12-09 CN CNA2008101632287A patent/CN101552063A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102509602A (en) * | 2011-11-21 | 2012-06-20 | 宁波市展发磁业科技有限公司 | High-performance magnetic material |
| CN102509602B (en) * | 2011-11-21 | 2015-06-24 | 宁波市展发磁业科技有限公司 | High-performance magnetic material |
| CN103413668B (en) * | 2012-11-13 | 2017-05-31 | 宁波宏垒磁业有限公司 | A kind of method for preparing dysprosium iron neodymium iron boron magnetic body |
| CN104821226A (en) * | 2015-05-07 | 2015-08-05 | 安徽万磁电子有限公司 | Method for making high-square-degree sintered NdFeB permanent magnets with cerium, titanium, cobalt and zirconium compound additive |
| EP4016561A4 (en) * | 2019-12-24 | 2022-10-19 | Fujian Changting Golden Dragon Rare-Earth Co., Ltd. | High-cu and high-al neodymium iron boron magnet and preparation method therefor |
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Open date: 20091007 |