CN107610858A - A kind of amount containing cerium high inexpensive N35 neodymium iron boron magnetic bodies and its sintering method - Google Patents
A kind of amount containing cerium high inexpensive N35 neodymium iron boron magnetic bodies and its sintering method Download PDFInfo
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Abstract
A kind of amount containing cerium high inexpensive N35 neodymium iron boron magnetic bodies and its sintering method, belong to powder metallurgical technology, wt% by weight percentage weighs following raw material and is prepared by sintering process：Pu Nv ﹙ Pr Nd ﹚：12 ~ 27 , Shi ﹙ Ce ﹚：7 ~ 15 , Ni ﹙ Nb ﹚：0 ~ 0.5 , Lv ﹙ Al ﹚：0 ~ 1 , Tong ﹙ Cu ﹚：0 ~ 1 , Peng ﹙ B ﹚：0.9 ~ 1.1, cobalt (Co)：0 ~ 1.2, zirconium (Zr)：0 ~ 0.5, gadolinium (Gd)：0 ~ 3, remaining Wei Tie ﹙ Fe ﹚.This programme, part praseodymium neodymium is replaced Yong Shi ﹙ Ce ﹚（Pr‑Nd）, magnetic property index reaches N35 brands of sintered Nd-Fe-B national standards, and the corresponding trade mark magnet of production per kilogram can save 15 ~ 25 yuan of material cost.
Description
Technical field
The invention belongs to powder metallurgical technology, and in particular to for a kind of high inexpensive N35 neodymium-iron-borons of amount containing cerium
Body and its sintering method.
Background technology
In recent years, with the rapid expansion of neodymium iron boron magnetic body application field, the demand of raw material has been become increasingly
Greatly, but because the cost of rare earth mining is higher and as the increasing of national regulation and control dynamics, its material cost are also gradually increased.Price compared with
The element allocation ratios such as high praseodymium neodymium, holmium, gadolinium are higher, and cerium content is no more than 3（wt%）.It is excessive in present price amount of increase
In the case of, the price endurance of Downstream Market than relatively limited, portion downstream enterprise have selected using relatively inexpensive ferrite or
The materials such as aluminium nickel cobalt, SmCo replace neodymium iron boron magnetic body raw material in rare earth, this to neodymium iron boron magnetic body market bring it is larger not
Stability.In addition, Nd-Fe-B magnetic material fragility is high, specification is miscellaneous, easily occurs unfilled corner in electroplating process and size is bad etc.
Problem.And after electroplating the learies of neodymium iron boron magnetic body very greatly, be only finished appearance and size scrappage just 2 ~ 5% it
Between, because being often resulted in when client is otherwise to be required also, generation is bad to scrap phenomenon.Therefore reduce Sintered NdFeB magnet into
Originally it is one of urgent problem to be solved.
At present, domestic production neodymium iron boron magnetic body producer is more, the neodymium iron boron magnetic body of the different trades mark its production technology substantially phase
Together.The neodymium iron boron magnetic body that the trade mark is N35 is the larger magnet of current CD drive, robot, high end audio market demand
Material, production cost is higher, and the energy resource consumption in production process is big.Present industry common manufacturing method has following defect：（1）
Added using elements such as expensive heavy rare earth gadolinium, terbium, dysprosiums, cause material cost to remain high.（2）Cerium is alone or in combination
Addition, but addition can't be more than 5%（wt）, otherwise not only magnetic property deteriorates and does not reach the positive effect for reducing cost.
For the deficiencies in the prior art, there is provided a kind of high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium and its burning
Knot method, its amount containing cerium >=6 (wt%).
The content of the invention
It is an object of the invention to overcome the defects of mentioned above and deficiency, and provide a kind of amount containing cerium high low cost
N35 neodymium iron boron magnetic bodies.
Another object of the present invention is to provide the sintering method of above-mentioned neodymium iron boron magnetic body.
The present invention realizes that the technical scheme that its purpose uses is as follows.
A kind of high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium, by weight percentage wt% weigh following raw material and pass through burning
Knot technique is prepared：Pu Nv ﹙ Pr-Nd ﹚：12 ~ 27 , Shi ﹙ Ce ﹚：7 ~ 15 , Ni ﹙ Nb ﹚：0 ~ 0.5 , Lv ﹙ Al ﹚：0 ~ 1 , Tong ﹙ Cu ﹚：0
~ 1 , Peng ﹙ B ﹚：0.9 ~ 1.1, cobalt (Co)：0 ~ 1.2, zirconium (Zr)：0 ~ 0.5, gadolinium (Gd)：0 ~ 3, remaining Wei Tie ﹙ Fe ﹚.
Performance is as follows when the N35 neodymium iron boron magnetic bodies test temperature is 20 DEG C：Remanent magnetism Br >=11.9kGs, magnetic strength coercivity
Hcb >=11.5kOe, HCJ Hcj >=12.8kOe, maximum magnetic energy product（BH）M >=33.9MGOe, squareness Hk >=98.2%
Hcj。
A kind of sintering method of the high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium, comprises the following steps：
Step 1. raw material weighing and proportioning：Wt% by weight percentage weighs following raw material：Pu Nv ﹙ Pr-Nd ﹚：12 ~ 27 , Shi ﹙
Ce ﹚：7 ~ 15 , Ni ﹙ Nb ﹚：0 ~ 0.5 , Lv ﹙ Al ﹚：0 ~ 1 , Tong ﹙ Cu ﹚：0 ~ 1 , Peng ﹙ B ﹚：0.9 ~ 1.1, cobalt (Co)：0 ~ 1.2, zirconium
(Zr)：0 ~ 0.5, gadolinium (Gd) 0 ~ 3, remaining Wei Tie ﹙ Fe ﹚；
Step 2. smelting sheet casting:Raw material in step 1 are put into vacuum rapid hardening furnace in order successively, after raw material fully melts
Stand, then cast forms flakey slab, after slab temperature is less than 40 DEG C, slab is collected standby；
Step 3. hydrogen comminution powder：It is broken that hydrogen is carried out to slab using hydrogen crushing furnace；
Step 4. magnetic is molded：Magnetic is molded in full-automatic pressing under magnetic field press and obtains pressed compact；
Step 5. sinters：Pressed compact after shaping is sintered.
Further, in step 2, the raw material in step 1 are put into vacuum rapid hardening furnace in order successively, add power to preheat 30
~ 40 minutes, 1350 ~ 1435 DEG C of smelting temperature, smelting time 40 ~ 45 minutes, stood after raw material fully melts.
Further, in step 3, after hydrogen is broken, hydrogen flour is worn into 2.5 ~ 3.5um magnetics through airflow milling, in three-dimensional material mixer
Middle stirring 1 ~ 3.5 hour, being put into stainless steel cask, to be filled with high pure nitrogen standby.
Further, in step 4, when magnetic is molded, alignment magnetic field 1.8T, 4 ~ 8MPa of pressure during shaping, 30 seconds dwell times.
As a preferred embodiment, in step 5, the pressed compact after shaping is sintered in vacuum sintering furnace, vacuum sintering furnace
Vacuum is better than 5.0 × 10-2Pa, heat temperature raising, 1020 ~ 1100 DEG C is carried out first and is sintered 3 ~ 5 hours, then carries out 870 ~ 950
DEG C heat treatment 2 ~ 3 hours, then carry out 460 ~ 650 DEG C be heat-treated 3 ~ 5 hours, be finally cooled to 60 ~ 90 DEG C and obtain blank, go out
Stove, the various parameters of blank qualified storage after testing.
As another kind preferably, in step 5, the pressed compact after shaping carries out microwave sintering, first stage under excess oxygen：
Heat temperature raising, first 350 ~ 360 DEG C of progress Isothermal sinter 3 hours；Second stage：It is small then to carry out 760 ~ 820 DEG C of heat treatments 1.5
When；Phase III：It is warming up to 1100 DEG C and is incubated 3 hours；Then cooled down, cooling is divided into two stages：First stage：With
510 DEG C/h cooling velocity will be cooled to 925 DEG C after sintering into parison, second stage, then by naturally cooling to 65 DEG C
Blank is obtained, is come out of the stove, the various parameters of blank qualified storage after testing.
The technical program has advantages below：
1. praseodymium neodymium in the production of traditional N35 Sintered NdFeB magnets（Pr-Nd）Content accounts for 32.5 ~ 32.8 (wt%), at present praseodymium neodymium valency
Lattice 400,000 yuan of , Shi ﹙ Ce ﹚ prices per ton are per ton less than 150,000 yuan, replace part praseodymium neodymium Yong Shi ﹙ Ce ﹚（Pr-Nd）, magnetic property index
Reach N35 brands of sintered Nd-Fe-B national standards, the corresponding trade mark magnet of production per kilogram can save 15 ~ 25 yuan of material cost.
2. increasing Tong ﹙ Cu ﹚ in formula, the weightlessness of product is reduced.The corrosion process of sintered Nd Fe B permanent magnets with regard to its essence and
Speech belongs to selective corrosion.The chemical characteristic and its distribution of rich neodymium phase are the passes for the corrosion resistance for determining NdFeB alloys
Key factor.Cu will not substitute the Fe in principal phase, and be dissolved in rich neodymium phase, and magnet is improved by changing the composition of rich neodymium phase
Corrosion resistance, the weightlessness of product is reduced, while reducing cost, enhance heatproof, the corrosion resistance of product.
3. increasing Ni ﹙ Nb ﹚ in formula, magnet HCJ is improved（Hcj）, ensure that properties of product are more stable.Nb was both
Do not substitute, be also insoluble in rich neodymium phase, form shaft-like cenotype Nb (FeCo) B phases.The coercivity of Sintered NdFeB magnet comes
Magnetic coupling is mainly gone in source, and the formation of this cenotype is of great advantage to going magnetic coupling, therefore can improve magnet HCJ
（Hcj）, simultaneously because Nb (FeCo) B fusing points are higher, to the great benefit of uniformity consistency of magnet microstructure so that magnet
Can more it stablize.
4. using multi-steps sintering, heat treatment, sintering time saves 4 hours than conventional sintering technique, reduces cost of material,
Reduce energy resource consumption, more meet national energy-saving emission reduction policy.
5. using microwave sintering, the crystallite dimension of sintered body is significantly reduced, the phenomenon of particle fusion is less, realizes microcosmic
Liquid-phase sintering between interface, sintering temperature can be reduced, and ensure the comprehensive magnetic energy of magnet.
Brief description of the drawings
Fig. 1 is the SEM figures of neodymium iron boron magnetic body difference sintering process.
Embodiment
The present invention is described in further detail below.
Embodiment 1.
A kind of high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium, it passes through sintering by following percentage by weight wt% component
Technique is prepared：Pu Nv ﹙ Pr-Nd ﹚：21.5 , Shi ﹙ Ce ﹚：11 , Ni ﹙ Nb ﹚：0.2 , Lv ﹙ Al ﹚：0.9 , Tong ﹙ Cu ﹚：0.15 , Peng ﹙
B﹚：1.0, remaining Wei Tie ﹙ Fe ﹚.
Performance is as follows when obtained N35 neodymium iron boron magnetic bodies test temperature is 20 DEG C：Remanent magnetism Br=11.9kGs, magnetic strength coercivity
Hcb=11.5kOe, HCJ Hcj=12.8kOe, maximum magnetic energy product（BH）M=33.9MGOe, squareness Hk=98.2%Hcj.
A kind of sintering method of the high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium, comprises the following steps：
Step 1. raw material weighing and proportioning：(wt%) weighs following raw material by weight percentage：The , Shi ﹙ Ce ﹚ of Pu Nv ﹙ Pr-Nd ﹚ 21.5
11 , Ni ﹙ Nb ﹚, 0.2 , Lv ﹙ Al ﹚, 0.9 , Tong ﹙ Cu ﹚ 0.15 , Peng ﹙ B ﹚ 1.0, remaining Wei Tie ﹙ Fe ﹚；
Step 2. smelting sheet casting:Raw material in step 1 are put into vacuum rapid hardening furnace in order successively, add power to preheat 40 points
Clock, 1350 DEG C of smelting temperature, smelting time 40 minutes, being stood after raw material fully melts, then cast forms flakey slab,
Cooling water temperature is maintained at less than 20 DEG C and cooled down 120 minutes, after slab temperature is less than 40 DEG C, slab is collected standby；
Step 3. hydrogen comminution powder：It is broken that hydrogen is carried out to slab using hydrogen crushing furnace, hydrogen flour is then worn into 3.0 ~ 3.2um through airflow milling
Magnetic, stirred 2.5 hours in three-dimensional material mixer, being put into stainless steel cask, to be filled with high pure nitrogen standby；
Step 4. magnetic is molded：Magnetic material is molded in full-automatic pressing under magnetic field press and obtains pressed compact, alignment magnetic field 1.8T, during shaping
Pressure 4.5MPa, 30 seconds dwell times；
Step 5. sinters：Pressed compact after shaping is sintered in vacuum sintering furnace, the vacuum of vacuum sintering furnace better than 5.0 ×
10-2Pa, heat temperature raising, first 1050 DEG C of progress Isothermal sinter 3.5 hours, then 900 DEG C of progress heat treatment 2.5 hours, then
Carry out 555 DEG C to be heat-treated 5 hours, be finally cooled to 70 DEG C and obtain blank, come out of the stove.Then blank is processed into the production of D10 × 10
Product, test normal temperature magnetic property, weightlessness（Be placed on 2 normal atmosphere pressures, 100% humidity, 121 DEG C, taken out after 48 hours, by oxygen
Change layer to remove, weights before and after testing experiment）.
Comparative example 1：N35 Sintered NdFeB magnets are produced according to conventional procedures：
The ﹚ of ﹙ 1 (wt%) by weight percentage weigh following raw material：Pu Nv ﹙ Pr-Nd ﹚：25.7 , Shi ﹙ Ce ﹚：1.0 , Lv ﹙ Al ﹚：
0.75, gadolinium (Gd)：5.4 , Peng ﹙ B ﹚：1.0, copper（Cu）：0.17, remaining Wei Tie ﹙ Fe ﹚；
Above-mentioned raw materials are put into vacuum rapid hardening furnace by the ﹚ of ﹙ 2, add power to preheat 40 minutes, 1370 DEG C of smelting temperature, smelting time 42
Minute, stood after various raw material fully melt and pour into slab, cooling water temperature is maintained at less than 20 DEG C and cooled down 120 minutes
After slab temperature is less than 40 DEG C, cooling terminates, and slab is collected standby；
The ﹚ of ﹙ 3 carry out hydrogen to slab using hydrogen crushing furnace and crushed, and hydrogen flour then are worn into 3.0 ~ 3.2um powders through airflow milling, mixed
Stirred 2.5 hours in material machine, being put into stainless steel cask, to be filled with high pure nitrogen standby；
The ﹚ powders of ﹙ 4 are molded in full-automatic pressing under magnetic field press, alignment magnetic field 1.8T, pressure 4.5MPa during shaping, the dwell time
30 seconds；
Pressed compact after the ﹚ of ﹙ 5 shapings is sintered in vacuum sintering furnace, and vacuum is higher than 5.0 × 10-2Pa heats up, 1060 DEG C of perseverances
Temperature is sintered 3.5 hours, next 900 DEG C of constant temperature heat treatment 3 hours, and then 535 DEG C of constant temperature are heat-treated 5 hours, are finally cooled to 70
DEG C blank is come out of the stove.Then blank is processed into D10*10 product, test normal temperature magnetic property.
Table 1：N35 Sintered NdFeB magnet magnetic property contrast tables
| Group | Remanent magnetism Br/kGs | Magnetic strength coercivity H b/kOe | HCJ Hcj/kOe | Maximum magnetic energy product（BH）m/MGOe | Squareness Hk/Hcj |
| Embodiment 1 | 11.9 | 11.5 | 12.8 | 33.9 | 98.2% |
| Comparative example 1 | 11.86 | 11.4 | 12.2 | 33.1 | 96.5% |
Table 1 shows that the indices of embodiment 1 are superior to comparative example 1.
Table 2：Allocation ratio and formulation cost contrast table
Table 2 shows, the formulation cost of embodiment 1 reduces by 18.5 yuan/KG compared with comparative example formulation cost, i.e., 15.43%.
Embodiment 2.
A kind of high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium, it passes through sintering by following percentage by weight wt% component
Technique is prepared：Pu Nv ﹙ Pr-Nd ﹚：12 , Shi ﹙ Ce ﹚：15 , Lv ﹙ Al ﹚：1 , Peng ﹙ B ﹚：1.1, cobalt (Co)：1.2, zirconium (Zr)：
0.25, gadolinium (Gd)：1.5, remaining Wei Tie ﹙ Fe ﹚.
Performance is as follows when obtained N35 neodymium iron boron magnetic bodies test temperature is 20 DEG C：Remanent magnetism Br=12.1kGs, magnetic strength coercivity
Hcb=12.2kOe, HCJ Hcj=12.5kOe, maximum magnetic energy product（BH）M=35.4MGOe, squareness Hk=98.5%Hcj.
A kind of sintering method of the high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium, comprises the following steps：
Step 1. raw material weighing and proportioning：(wt%) weighs following raw material by weight percentage：Pu Nv ﹙ Pr-Nd ﹚：12 , Shi ﹙ Ce ﹚：
15 , Lv ﹙ Al ﹚：1 , Peng ﹙ B ﹚：1.1, cobalt (Co)：1.2, zirconium (Zr)：0.25, gadolinium (Gd) 1.5, remaining Wei Tie ﹙ Fe ﹚；[0035] step
Rapid 2. smelting sheet casting:Raw material in step 1 are put into vacuum rapid hardening furnace in order successively, add power to preheat 30 minutes, melting
1450 DEG C of temperature, smelting time 45 minutes, stands after raw material fully melts, and then cast forms flakey slab, cooling water
Temperature is maintained at less than 26 DEG C and cooled down 150 minutes, after slab temperature is less than 40 DEG C, slab is collected standby；
Step 3. hydrogen comminution powder：It is broken that hydrogen is carried out to slab using hydrogen crushing furnace, hydrogen flour is then worn into 2.7 ~ 3.5um through airflow milling
Magnetic, stirred 2.5 hours in three-dimensional material mixer, being put into stainless steel cask, to be filled with high pure nitrogen standby；
Step 4. magnetic is molded：Magnetic material is molded in full-automatic pressing under magnetic field press and obtains pressed compact, alignment magnetic field 1.8T, during shaping
Pressure 8MPa, 30 seconds dwell times；
Step 5. sinters：Pressed compact after shaping is sintered in vacuum sintering furnace, the vacuum of vacuum sintering furnace better than 5.0 ×
10-2Pa, first heat temperature raising, 1100 DEG C of progress Isothermal sinter 3 hours, then carries out 950 DEG C and is heat-treated 2.5 hours, Ran Houjin
650 DEG C of row is heat-treated 3 hours, is finally cooled to 65 DEG C and is obtained blank, comes out of the stove.Then blank is processed into the product of D10 × 10,
Test normal temperature magnetic property, weightlessness（Be placed on 2 normal atmosphere pressures, 100% humidity, 121 DEG C, taken out after 48 hours, will aoxidize
Layer removes, weights before and after testing experiment）.
Embodiment 3.
A kind of high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium, it passes through sintering by following percentage by weight wt% component
Technique is prepared：Pu Nv ﹙ Pr-Nd ﹚：27 , Shi ﹙ Ce ﹚：The , Tong ﹙ Cu ﹚ of 7 , Ni ﹙ Nb ﹚ 0.5：1 , Peng ﹙ B ﹚：0.9, cobalt (Co)：0.6,
Zirconium (Zr)：0.5, gadolinium (Gd)：3, remaining Wei Tie ﹙ Fe ﹚.
Performance is as follows when obtained N35 neodymium iron boron magnetic bodies test temperature is 20 DEG C：Remanent magnetism Br=13.3kGs, magnetic strength coercivity
Hcb=12.9kOe, HCJ Hcj=13.3kOe, maximum magnetic energy product（BH）M=37.2MGOe, squareness Hk=98.7%Hcj.
A kind of sintering method of the high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium, comprises the following steps：
Step 1. raw material weighing and proportioning：(wt%) weighs following raw material by weight percentage：Pu Nv ﹙ Pr-Nd ﹚：27 , Shi ﹙ Ce ﹚：
The , Tong ﹙ Cu ﹚ of 7 , Ni ﹙ Nb ﹚ 0.5：1 , Peng ﹙ B ﹚：0.9, cobalt (Co)：0.6, zirconium (Zr)：0.5, gadolinium (Gd)：3, remaining Wei Tie ﹙ Fe ﹚；
Step 2. smelting sheet casting:Raw material in step 1 are put into vacuum rapid hardening furnace in order successively, add power to preheat 35 points
Clock, 1350 DEG C of smelting temperature, smelting time 40 minutes, being stood after raw material fully melts, then cast forms flakey slab,
Cooling water temperature is maintained at less than 26 DEG C and cooled down 150 minutes, after slab temperature is less than 40 DEG C, slab is collected standby；
Step 3. hydrogen comminution powder：It is broken that hydrogen is carried out to slab using hydrogen crushing furnace, hydrogen flour is then worn into 2.7 ~ 3.2um through airflow milling
Magnetic, stirred 1 hour in three-dimensional material mixer, being put into stainless steel cask, to be filled with high pure nitrogen standby；
Step 4. magnetic is molded：Magnetic material is molded in full-automatic pressing under magnetic field press and obtains pressed compact, alignment magnetic field 1.8T, during shaping
Pressure 4MPa, 30 seconds dwell times；
Step 5. sinters：Pressed compact after shaping is sintered in vacuum sintering furnace, the vacuum of vacuum sintering furnace better than 5.0 ×
10-2Pa, first heat temperature raising, 1020 DEG C of progress Isothermal sinter 5 hours, then carries out 870 DEG C and is heat-treated 2 hours, then carry out
460 DEG C are heat-treated 5 hours, are finally cooled to 65 DEG C and obtain blank, come out of the stove.Then blank is processed into the product of D10 × 10, surveyed
Try normal temperature magnetic property, weightlessness（Be placed on 2 normal atmosphere pressures, 100% humidity, 121 DEG C, taken out after 48 hours, by oxide layer
Remove, weights before and after testing experiment）.
Embodiment 4.
A kind of high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium, it passes through sintering by following percentage by weight wt% component
Technique is prepared：Pu Nv ﹙ Pr-Nd ﹚：21.5 , Shi ﹙ Ce ﹚：11 , Ni ﹙ Nb ﹚：0.2 , Lv ﹙ Al ﹚：0.9 , Tong ﹙ Cu ﹚：0.15 , Peng ﹙
B﹚：1.0, remaining Wei Tie ﹙ Fe ﹚.
A kind of sintering method of the high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium, comprises the following steps：
Step 1. raw material weighing and proportioning：(wt%) weighs following raw material by weight percentage：Pu Nv ﹙ Pr-Nd ﹚：21.5 , Shi ﹙
Ce ﹚：11 , Ni ﹙ Nb ﹚：0.2 , Lv ﹙ Al ﹚：0.9 , Tong ﹙ Cu ﹚：0.15 , Peng ﹙ B ﹚：1.0, remaining Wei Tie ﹙ Fe ﹚；
Step 2. smelting sheet casting:Raw material in step 1 are put into vacuum rapid hardening furnace in order successively, add power to preheat 40 points
Clock, 1410 DEG C of smelting temperature, smelting time 41 minutes, being stood after raw material fully melts, then cast forms flakey slab,
Cooling water temperature is maintained at less than 26 DEG C and cooled down 150 minutes, after slab temperature is less than 40 DEG C, slab is collected standby；
Step 3. hydrogen comminution powder：It is broken that hydrogen is carried out to slab using hydrogen crushing furnace, hydrogen flour is then worn into 2.5 ~ 2.7um through airflow milling
Magnetic, stirred 3.5 hours in three-dimensional material mixer, being put into stainless steel cask, to be filled with high pure nitrogen standby；
Step 4. magnetic is molded：Magnetic material is molded in full-automatic pressing under magnetic field press and obtains pressed compact, alignment magnetic field 1.8T, during shaping
Pressure 7MPa, 30 seconds dwell times；
Step 5. sinters：Pressed compact after shaping carries out microwave sintering, first stage under excess oxygen：Heat temperature raising, enter first
350 ~ 360 DEG C of row Isothermal sinter 3 hours；Second stage：760 ~ 820 DEG C are then carried out to be heat-treated 1.5 hours；Phase III：Rise
Warm to 1100 DEG C are incubated 3 hours；Then cooled down, cooling is divided into two stages：First stage：With 510 DEG C/h cooling speed
Degree will be cooled to 925 DEG C after sintering into parison, second stage, then obtains blank by naturally cooling to 65 DEG C, comes out of the stove.So
Blank is processed into the product of D10 × 10, test normal temperature magnetic property, weightlessness afterwards（It is placed on 2 normal atmospheres pressure, 100% wet
Degree, 121 DEG C, taken out after 48 hours, oxide layer is removed, weights before and after testing experiment）.
During sintering, excess oxygen, be advantageous to avoid the generation of reducing atmosphere.
For the present embodiment by microwave sintering, the phenomenon of particle fusion is less, realizes the liquid-phase sintering between micro interface,
Sintering temperature can be reduced, and ensures the comprehensive magnetic energy of magnet.
From figure 1 it appears that compared with traditional Muffle furnace sintering, microwave sintering can significantly reduce the crystal grain of sintered body
Size.In conventional sintering sample, the phenomenon of little particle melting and abnormal growth is found so that single domain particle reduces, and have impact on
Neodymium iron boron magnetic body imitation frosted glass performance.And in the neodymium iron boron magnetic body of microwave sintering, sintering temperature is low, the time is short, the phenomenon of particle fusion
It is less, realize the liquid-phase sintering between micro interface.
Performance is as follows when obtained N35 neodymium iron boron magnetic bodies test temperature is 20 DEG C：Remanent magnetism Br=14.5kGs, magnetic strength coercivity
Hcb=14.3kOe, HCJ Hcj=14.8kOe, maximum magnetic energy product（BH）M=48.7MGOe, squareness Hk=98.2%Hcj.
Embodiment 5.
A kind of high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium, it passes through sintering by following percentage by weight wt% component
Technique is prepared：Pu Nv ﹙ Pr-Nd ﹚：12 , Shi ﹙ Ce ﹚：15 , Lv ﹙ Al ﹚：1 , Peng ﹙ B ﹚：1.1, cobalt (Co)：1.2, zirconium (Zr)：
0.25, gadolinium (Gd)：1.5, remaining Wei Tie ﹙ Fe ﹚.
A kind of sintering method of the high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium, comprises the following steps：
Step 1. raw material weighing and proportioning：(wt%) weighs following raw material by weight percentage：Pu Nv ﹙ Pr-Nd ﹚：12 , Shi ﹙ Ce ﹚：
15 , Lv ﹙ Al ﹚：1 , Peng ﹙ B ﹚：1.1, cobalt (Co)：1.2, zirconium (Zr)：0.25, gadolinium (Gd)：1.5, remaining Wei Tie ﹙ Fe ﹚；
Step 2. smelting sheet casting:Raw material in step 1 are put into vacuum rapid hardening furnace in order successively, add power to preheat 30 points
Clock, 1450 DEG C of smelting temperature, smelting time 45 minutes, being stood after raw material fully melts, then cast forms flakey slab,
Cooling water temperature is maintained at less than 26 DEG C and cooled down 150 minutes, after slab temperature is less than 40 DEG C, slab is collected standby；
Step 3. hydrogen comminution powder：It is broken that hydrogen is carried out to slab using hydrogen crushing furnace, hydrogen flour is then worn into 2.7 ~ 3.5um through airflow milling
Magnetic, stirred 2.5 hours in three-dimensional material mixer, being put into stainless steel cask, to be filled with high pure nitrogen standby；
Step 4. magnetic is molded：Magnetic material is molded in full-automatic pressing under magnetic field press and obtains pressed compact, alignment magnetic field 1.8T, during shaping
Pressure 8MPa, 30 seconds dwell times；
Step 5. sinters：Pressed compact after shaping carries out microwave sintering, first stage under excess oxygen：Heat temperature raising, enter first
350 ~ 360 DEG C of row Isothermal sinter 3 hours；Second stage：760 ~ 820 DEG C are then carried out to be heat-treated 1.5 hours；Phase III：Rise
Warm to 1100 DEG C are incubated 3 hours；Then cooled down, cooling is divided into two stages：First stage：With 510 DEG C/h cooling speed
Degree will be cooled to 925 DEG C after sintering into parison, second stage, then obtains blank by naturally cooling to 65 DEG C, comes out of the stove.So
Blank is processed into the product of D10 × 10, test normal temperature magnetic property, weightlessness afterwards（It is placed on 2 normal atmospheres pressure, 100% wet
Degree, 121 DEG C, taken out after 48 hours, oxide layer is removed, weights before and after testing experiment）.
Performance is as follows when obtained N35 neodymium iron boron magnetic bodies test temperature is 20 DEG C：Remanent magnetism Br=15.2kGs, magnetic strength coercivity
Hcb=14.8kOe, HCJ Hcj=15.8kOe, maximum magnetic energy product（BH）M=48.4MGOe, squareness Hk=98.8%Hcj.
Embodiment 6.
A kind of high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium, it passes through sintering by following percentage by weight wt% component
Technique is prepared：Pu Nv ﹙ Pr-Nd ﹚：27 , Shi ﹙ Ce ﹚：The , Tong ﹙ Cu ﹚ of 7 , Ni ﹙ Nb ﹚ 0.5：1 , Peng ﹙ B ﹚：0.9, cobalt (Co)：0.6,
Zirconium (Zr)：0.5, gadolinium (Gd)：3, remaining Wei Tie ﹙ Fe ﹚.
A kind of sintering method of the high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium, comprises the following steps：
Step 1. raw material weighing and proportioning：(wt%) weighs following raw material by weight percentage：Pu Nv ﹙ Pr-Nd ﹚：27 , Shi ﹙ Ce ﹚：
The , Tong ﹙ Cu ﹚ of 7 , Ni ﹙ Nb ﹚ 0.5：1 , Peng ﹙ B ﹚：0.9, cobalt (Co)：0.6, zirconium (Zr)：0.5, gadolinium (Gd)：3, remaining Wei Tie ﹙ Fe ﹚；
Step 2. smelting sheet casting:Raw material in step 1 are put into vacuum rapid hardening furnace in order successively, add power to preheat 35 points
Clock, 1350 DEG C of smelting temperature, smelting time 40 minutes, being stood after raw material fully melts, then cast forms flakey slab,
Cooling water temperature is maintained at less than 26 DEG C and cooled down 150 minutes, after slab temperature is less than 40 DEG C, slab is collected standby；
Step 3. hydrogen comminution powder：It is broken that hydrogen is carried out to slab using hydrogen crushing furnace, hydrogen flour is then worn into 2.7 ~ 3.2um through airflow milling
Magnetic, stirred 1 hour in three-dimensional material mixer, being put into stainless steel cask, to be filled with high pure nitrogen standby；
Step 4. magnetic is molded：Magnetic material is molded in full-automatic pressing under magnetic field press and obtains pressed compact, alignment magnetic field 1.8T, during shaping
Pressure 4MPa, 30 seconds dwell times；
Step 5. sinters：Pressed compact after shaping carries out microwave sintering, first stage under excess oxygen：Heat temperature raising, enter first
350 ~ 360 DEG C of row Isothermal sinter 3 hours；Second stage：760 ~ 820 DEG C are then carried out to be heat-treated 1.5 hours；Phase III：Rise
Warm to 1100 DEG C are incubated 3 hours；Then cooled down, cooling is divided into two stages：First stage：With 510 DEG C/h cooling speed
Degree will be cooled to 925 DEG C after sintering into parison, second stage, then obtains blank by naturally cooling to 65 DEG C, comes out of the stove.So
Blank is processed into the product of D10 × 10, test normal temperature magnetic property, weightlessness afterwards（It is placed on 2 normal atmospheres pressure, 100% wet
Degree, 121 DEG C, taken out after 48 hours, oxide layer is removed, weights before and after testing experiment）.
Performance is as follows when obtained N35 neodymium iron boron magnetic bodies test temperature is 20 DEG C：Remanent magnetism Br=15.9kGs, magnetic strength coercivity
Hcb=15.4kOe, HCJ Hcj=14.8kOe, maximum magnetic energy product（BH）M=49.2MGOe, squareness Hk=98.5%Hcj.
The present invention is illustrated according to embodiment, on the premise of present principles are not departed from, if the present apparatus can also make
Dry modification and improvement.It should be pointed out that all technical schemes obtained using modes such as equivalent substitution or equivalent transformations, all fall within this
In the protection domain of invention.
Claims (8)
1. the high inexpensive N35 neodymium iron boron magnetic bodies of a kind of amount containing cerium, it is characterised in that wt% by weight percentage weighs following original
Material is prepared by sintering process：Pu Nv ﹙ Pr-Nd ﹚：12 ~ 27 , Shi ﹙ Ce ﹚：7 ~ 15 , Ni ﹙ Nb ﹚：0 ~ 0.5 , Lv ﹙ Al ﹚：0~
1 , Tong ﹙ Cu ﹚：0 ~ 1 , Peng ﹙ B ﹚：0.9 ~ 1.1, cobalt (Co)：0 ~ 1.2, zirconium (Zr)：0 ~ 0.5, gadolinium (Gd)：0 ~ 3, remaining Wei Tie ﹙ Fe ﹚.
A kind of 2. high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium as claimed in claim 1, it is characterised in that the N35 neodymiums
Performance is as follows when iron boron magnet test temperature is 20 DEG C：Remanent magnetism Br >=11.9kGs, magnetic strength coercivity H b >=11.5kOe, it is intrinsic
Coercivity H j >=12.8kOe, maximum magnetic energy product（BH）M >=33.9MGOe, squareness Hk >=98.2%Hcj.
3. a kind of sintering method of the high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium as claimed in claim 1, including following step
Suddenly：
Step 1. raw material weighing and proportioning：Wt% by weight percentage weighs following raw material：Pu Nv ﹙ Pr-Nd ﹚：12 ~ 27 , Shi ﹙
Ce ﹚：7 ~ 15 , Ni ﹙ Nb ﹚：0 ~ 0.5 , Lv ﹙ Al ﹚：0 ~ 1 , Tong ﹙ Cu ﹚：0 ~ 1 , Peng ﹙ B ﹚：0.9 ~ 1.1, cobalt (Co)：0 ~ 1.2, zirconium
(Zr)：0 ~ 0.5, gadolinium (Gd) 0 ~ 3, remaining Wei Tie ﹙ Fe ﹚；
Step 2. smelting sheet casting:Raw material in step 1 are put into vacuum rapid hardening furnace in order successively, after raw material fully melts
Stand, then cast forms flakey slab, after slab temperature is less than 40 DEG C, slab is collected standby；
Step 3. hydrogen comminution powder：It is broken that hydrogen is carried out to slab using hydrogen crushing furnace；
Step 4. magnetic is molded：Magnetic is molded in full-automatic pressing under magnetic field press and obtains pressed compact；
Step 5. sinters：Pressed compact after shaping is sintered.
, will in step 2 4. a kind of sintering method of the high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium as claimed in claim 3
Raw material in step 1 are put into vacuum rapid hardening furnace in order successively, add power to preheat 30 ~ 40 minutes, smelting temperature 1350 ~ 1435
DEG C, smelting time 40 ~ 45 minutes, stood after raw material fully melts.
5. a kind of sintering method of the high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium as claimed in claim 3, in step 3, hydrogen
After broken, hydrogen flour is worn into 2.5 ~ 3.5um magnetics through airflow milling, is stirred 1 ~ 3.5 hour in three-dimensional material mixer, is put into stainless steel
It is standby that bucket is filled with high pure nitrogen.
6. a kind of sintering method of the high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium as claimed in claim 3, in step 4, magnetic
When powder is molded, alignment magnetic field 1.8T, 4 ~ 8MPa of pressure during shaping, 30 seconds dwell times.
7. a kind of sintering method of the high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium as claimed in claim 3, in step 5, into
Pressed compact after type is sintered in vacuum sintering furnace, and the vacuum of vacuum sintering furnace is better than 5.0 × 10-2Pa, heat temperature raising are first
First carry out 1020 ~ 1100 DEG C to sinter 3 ~ 5 hours, then carry out 870 ~ 950 DEG C and be heat-treated 2 ~ 3 hours, then carry out 460 ~ 650 DEG C
Heat treatment 3 ~ 5 hours, is finally cooled to 60 ~ 90 DEG C and obtains blank, come out of the stove, the various parameters of blank qualified storage after testing.
8. a kind of sintering method of the high inexpensive N35 neodymium iron boron magnetic bodies of amount containing cerium as claimed in claim 3, in step 5, into
Pressed compact after type carries out microwave sintering, first stage under excess oxygen：Heat temperature raising, 350 ~ 360 DEG C of constant temperature are carried out first and are burnt
Knot 3 hours；Second stage：760 ~ 820 DEG C are then carried out to be heat-treated 1.5 hours；Phase III：It is small to be warming up to 1100 DEG C of insulations 3
When；Then cooled down, cooling is divided into two stages：First stage：With 510 DEG C/h cooling velocity by the shaping after sintering
Base is cooled to 925 DEG C, second stage, then obtains blank by naturally cooling to 65 DEG C, comes out of the stove, and the various parameters of blank are through inspection
Survey qualified storage.
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