CN101423902B

CN101423902B - Processing method of R-T-B series alloy powder for radiation magnetic loop

Info

Publication number: CN101423902B
Application number: CN2008102269708A
Authority: CN
Inventors: 陈国安; 王浩颉; 王湛; 钮萼; 饶晓雷; 胡伯平
Original assignee: Beijing Zhong Ke San Huan High Tech Co Ltd
Current assignee: Beijing Zhong Ke San Huan High Tech Co Ltd
Priority date: 2008-11-21
Filing date: 2008-11-21
Publication date: 2012-02-15
Anticipated expiration: 2028-11-21
Also published as: CN101423902A

Abstract

The invention provides an R-T-B system alloy powder treatment method for radiation magnetic rings. The method comprises the following steps: raw alloy is melted in vacuum or inert gas so as to cast an ingot; a raw alloy ingot is subjected to coarse or hydrogen crushing in inert atmosphere; any two substances selected from polyethylene oxide composite polymers, fatty acid, fatty acid derivatives and hydrocarbon are added to and mixed with powder after coarse or hydrogen crushing; alloy coarse powder is subjected to micro-grinding in a nitrogen environment by use of a jet mill; the alloy powder is annealed in inert gas, vacuum or reducing atmosphere; carbonyl iron powder and at least one alicyclic hydrocarbon are added to and mixed with the annealed alloy powder; the mixed powder is taken to form an annular formed body in a magnetic field; the annular formed body is sintered in vacuum or inert gas atmosphere. The method has the advantages that the method is uniform in the density of the radiation ring, high in one-time molding rate and wide in pressure application range, increases the magnetic energy product of the radiation ring, and improves surface magnetic uniformity.

Description

The treatment process of R-T-B series alloy powder for radiation magnetic loop

Technical field

The present invention relates to a kind of treatment process, specifically, relate to a kind of treatment process of R-T-B series alloy powder for radiation magnetic loop rare earth alloy powder.

Background technology

High performance for magnet requires to improve day by day at present, and is therefore also increasingly high for the requirement of rare earth alloy powder, as requires high workability, compression moulding excellent performance.Adopted the mixing pulp of method that adds organic solvents such as n-butene, terepthaloyl moietie to carry out granulation to rare earth alloy powder among the patent CN0280727.6,96190684.7; The granulation powder has effectively improved the flowability and the formability of R-Fe-B series alloy powder; And sticker can access effective removal in follow-up sintering process, and thick granulation powder is had relatively high expectations to the pressure of press.Add mineral wet goods mixture at powder among the patent CN200310100706.7, the direct Wet-pressing molding of slurry, mould structure changes greatly, and before the sintering timeliness, needs to increase the operation of deoiling, and production efficiency descends to some extent.

The special oriented moulding mode of radiation ring (no matter be bipolar to fill or four extremely to filling) cause flowability, formability to be had higher requirement to rare earth alloy powder; Organic solvents such as mentioned n-paraffin, isoparaffin add in the powder as lubricant or forming agent in traditional Triple Pressed Stearic Acid or stearate and the above-mentioned patent, and the once shaped rate of radiation ring compacting is all very low.And after through the present invention powder being handled following advantage can be arranged: (1) resulting radiation ring density is even, and the once shaped rate is high, and does not find defective and crackle in the molded blank; (2) applied widely for the required pressure of compacting, 1～300MPa all can; (3) the needed magnetic field of orientation is little; (4) magnetic energy product of radiation ring increases, and the table magnetic homogeneity of 360 degree and short transverse improves.

Summary of the invention

The objective of the invention is to increase substantially the once shaped rate of radiation ring, and can improve the magnetic property and the table magnetic homogeneity of radiation ring.

According to the present invention, the invention provides a kind of treatment process of R-T-B series alloy powder for radiation magnetic loop, the treating method comprises following steps:

(1) raw alloy carries out conventional melting ingot casting in vacuum or rare gas element;

(2) it is broken the raw alloy ingot casting to be carried out coarse breaking/hydrogen in inert atmosphere, obtains particle diameter and be hundreds of microns powder;

(3) adding two kinds of materials that 0.01～1wt.% is selected from polyethylene oxide composition polymer, lipid acid, derivative of fatty acid and hydrocarbon polymer in the powder after coarse breaking/hydrogen fragmentation mixed 1～10 hour;

(4) use airflow milling under nitrogen environment that alloy coarse meal micro mist is broken, obtain median size 1～10 μ m, specific surface area is 1.5～2.5m ²The screening powder of the even particle size distribution of/g;

(5) powdered alloy is annealed under rare gas element, vacuum or reducing atmosphere;

(6) add 0.05～5wt.% carbonyl iron dust and at least a cycloaliphates in the powdered alloy after annealing and mixed 1～8 hour, obtain mixed powder; Wherein said cycloaliphates is hexanaphthene, pimelinketone or toluene pimelinketone;

(7) this mixed powder is formed the ring-type molding in magnetic field;

(8) with this ring-type molding in vacuum or inert gas atmosphere at 1000～1150 ℃ of sintering that carry out 1～10 hour, behind the sintering again to sintered compact respectively 800～1000 ℃ carry out 1～3 hour, 450～600 ℃ of ageing treatment of carrying out 2～5 hours.

Wherein, the polyethylene oxide composition polymer is polyethylene oxide alkyl ethers or polyethylene oxide mono fatty acid ester; Lipid acid is triglyceride level or lecithin; Derivative of fatty acid is Zinic stearas, calcium stearate or StAl; Hydrocarbon polymer is paraffin or naphthalene.

Wherein, in step (5), reducing atmosphere is hydrogen, ammonia.Annealing region is 100～1000 ℃, and annealing time is 0.5～10 hour.Being preferably annealing region is 200～800 ℃, and annealing time is 1～5 hour.

Wherein, in step (6), in powdered alloy, add 0.1～3wt.% carbonyl iron dust and at least a cycloaliphates and mixed 2～5 hours, obtain mixed powder.In addition, in step (6), the loose density of resulting powder particle is 2.5～3g/cm ³, tap density is 3～4.5g/cm ³, flowability>=32s/50g.

Wherein, in step (7), the compacting pressure that is shaped in the magnetic field is 1～300MPa; The compacting pressure that preferably is shaped in the magnetic field is 2～100MPa; More preferably, the compacting pressure that is shaped in the magnetic field is 3～50MPa.

In addition, in step (7), externally-applied magnetic field is set at 0.5～2T, wherein, and externally-applied magnetic field or be static magnetic field, or be pulsed magnetic field.

The treatment process of R-T-B series alloy powder for radiation magnetic loop of the present invention at length is described below.

At first (1) raw alloy can preferably be made with near quick setting scale ingot casting method or other known smelting processes (high-frequency induction melting water-cooled copper modulus method, reduction-diffusion process) in Ar atmosphere in vacuum or rare gas element.(2) use jaw crusher, stamp mill etc. in inert atmosphere, to carry out coarse breaking on the raw alloy ingot casting, its particle diameter is reached about hundreds of microns.Also can make raw alloy thin slice storage of hydrogen and embrittlement, thereby obtain the alloy coarse meal.The hydrogen fragmentation is positioned thick broken, also can omit the coarse breaking operation of machinery.(3) add the verivate or the hydrocarbon polymer of polyethylene oxide composition polymer about 0.01%～1wt.%, lipid acid, lipid acid in the powder after the coarse breaking; Like polyethylene oxide alkyl ethers, polyethylene oxide mono fatty acid ester, Zinic stearas, calcium stearate, StAl, paraffin and naphthalene etc., mixed 1～10 hour.(4) use airflow milling under nitrogen environment that alloy coarse meal micro mist is broken, obtain median size 1～10 μ m, specific surface area is 1.5～2.5m ²The screening powder of the even particle size distribution of/g.(5) powdered alloy being crossed 60 and 320 purposes sieve makes the size-grade distribution of powder more even.(6) with annealing under powdered alloy any one state in rare gas element, vacuum or reducing atmosphere (like hydrogen, ammonia etc.), be more preferably reducing atmosphere (like hydrogen).Annealing region is 100～1000 ℃, and more preferably 200～800 ℃, annealing time is 0.5～10 hour, more preferably 1～5 hour; (7) in powder, add 0.05～5wt.% then, more preferably at least a (like hexanaphthene, pimelinketone or the toluene pimelinketone etc.) in the carbonyl iron dust of 0.1～3wt.% and the alicyclic hydrocarbon type mix, and mixing time is 1～8 hour, more preferably 2～5 hours.Resulting powder particle regular shape, epigranular, good fluidity, its loose density are 2.5～3g/cm ³, tap density is 3～4.5g/cm ³, flowability>=32s/50g.Therefore (8) this mixed powder is shaped in magnetic field, powder particle has good fillibility to mould, can high precision and make the ring-type molding efficiently.The compacting pressure that is shaped in the magnetic field can be set at 0.01～3ton/cm2 (1～300MPa) scope, more preferably 2～100MPa.Compacting pressure can be a constant, also can be to increase gradually or reduce, or irregular.The low more then orientation degree of compacting pressure is good more, can hang down to 3～50MPa through the compacting pressure of ring-type shaping thing after the above-mentioned powder treatment, can guarantee enough fabrication strengths again simultaneously.Externally-applied magnetic field can be set at 0.5～2T, can be static magnetic field, also can be pulsed magnetic field.And very little through the required magnetic field of orientation after the above-mentioned powder treatment, 0.5T just can make ring-type shaping thing orientation saturated.(9) with molding in vacuum or inert gas atmosphere at 1000～1150 ℃ of sintering that carry out 1～10 hour, behind the sintering sintered compact is handled 800～1000 ℃, 450～600 ℃ split ag(e)ings of carrying out 1～5 hour respectively.

And the beneficial effect after through the present invention powder being handled is: (1) resulting radiation ring density is even; The once shaped rate is high; And do not find defective and crackle in the molded blank, the once shaped rate of radiation ring 50% is brought up to 90% after the powder treatment when being untreated; (2) applied widely for the required pressure of compacting, 1～300MPa all can; (3) the needed magnetic field of orientation is little; (4) magnetic energy product of radiation ring increases, and the magnetic energy product of radiation ring is brought up to 30MGOe by 25MGOe; The table magnetic homogeneity of (5) 360 degree and short transverse improves, and the table magnetic homogeneity of radiation ring 360 degree brings up to 8% by 12%.

Embodiment

Below will combine embodiment that the present invention is further specified, embodiments of the invention only are used to technical scheme of the present invention is described, and non-limiting the present invention.

Selecting R-T-B for use is sintering radiation ring magnet

This R-T-B is the rare earth element (R) that sintering radiation ring magnet contains 27～35wt.%.That R can select from Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu is a kind of, two kinds or more kinds of.When R quantity not sufficient 27wt.%, principal phase generates insufficient, separates out the α-Fe phase of soft magnetism, causes coercive force significantly to reduce; When the R amount surpassed 35wt.%, the volume ratio of principal phase reduced, thereby residual flux density reduces.Therefore the R amount is set at 27～35wt.%, preferred 28～34wt.%, more preferably 29～33wt.%.

This R-T-B is the B that sintering radiation ring magnet contains 0.5～4wt.%.When B deficiency 0.5wt.%, can not obtain high coercive force; When B ultrasonic was crossed 4wt.%, residual flux density had a declining tendency.Therefore B is set at 0.5～4wt.%, preferred 0.6～1.5wt.%, more preferably 0.8～1.2wt.%.

This R-T-B is the Co that sintering radiation ring magnet contains 0.1～2.0wt.%, and corrosion proof raising mutually is very effective with crystal boundary to Tc, preferred 0.2～1.0wt.%, more preferably 0.3～0.8wt.%.

This R-T-B is the Al that sintering radiation ring magnet also can contain 0.01～0.8wt.%, in the elements such as the Ga of the Cu of 0.01～0.8wt.%, the Zr of 0.01～0.3wt.%, 0.01～0.5wt.% and Sn, V a kind of, two or more.

Along with the increase of oxygen level, the rare earth oxide of non magnetic phase increases, and the R enrichment reduces mutually, makes magnetic properties reduce, so the oxygen amount is preferably below the 5000ppm, more preferably below the 3000ppm.

Embodiment 1

Employing is got rid of the band legal system and is equipped with raw alloy, and it consists of 5.0Pr-22.0Nd-4.8Dy-0.2Al-0.1Cu-0.5Co-0.2Ga-0.1Zr-1.0B-surplus Fe.Then carry out the broken processing of hydrogen, at room temperature make raw alloy inhale hydrogen, in Ar atmosphere, carry out 500 ℃ * 1 hour dehydrogenation.The StAl and the paraffin wax that add 0.1wt.% mixed 1 hour, obtained the powder particle that median size is 4 μ m after the airflow milling, crossed the powder 1 that 60 and 300 purposes sieve obtains even particle size distribution then.More unprocessed with handle after the blank product parameters.

Unprocessed: powder 1 is shaped on extremely to the pressurising machine four, and compacting pressure is 50MPa, and externally-applied magnetic field is 1.0T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 1:

Table 1

Embodiment 2

Employing is got rid of the band legal system and is equipped with raw alloy, and it consists of 5.0Pr-22.0Nd-4.8Dy-0.2Al-0.1Cu-0.5Co-0.2Ga-0.1Zr-1.0B-surplus Fe.Then carry out the broken processing of hydrogen, at room temperature make raw alloy inhale hydrogen, in Ar atmosphere, carry out 500 ℃ * 1 hour dehydrogenation.The Zinc Stearate and the triglyceride level that add 0.1wt.% mixed 1 hour, obtained the powder particle that median size is 4 μ m after the airflow milling, crossed the powder 1 that 60 and 300 purposes sieve obtains even particle size distribution then.More unprocessed with handle after the blank product parameters.

Handle: with powder 1 600 ℃ of anneal 3 hours under vacuum atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 1.0wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.See also table 2.

Table 2

Embodiment 3

Employing is got rid of the band legal system and is equipped with raw alloy, and it consists of 5.0Pr-22.0Nd-4.8Dy-0.2Al-0.1Cu-0.5Co-0.2Ga-0.1Zr-1.0B-surplus Fe.Then carry out the broken processing of hydrogen, at room temperature make raw alloy inhale hydrogen, in Ar atmosphere, carry out 500 ℃ * 1 hour dehydrogenation.The StAl and the paraffin wax that add 0.01wt.% mixed 1 hour, and obtaining median size after the airflow milling is that (specific surface area is 1.5m to 1 μ m ²/ g) powder particle is crossed 60 and 300 purposes then and is sieved the powder 1 that obtains even particle size distribution.More unprocessed with handle after the blank product parameters.

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.05wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 3:

Table 3

Embodiment 4

Handle: with powder 1 500 ℃ of anneal 2 hours under vacuum atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 4:

Table 4

Embodiment 5

Handle: with powder 1 500 ℃ of anneal 2 hours under hydrogen atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 5:

Table 5

Embodiment 6

Handle: with powder 1 500 ℃ of anneal 2 hours under ammonia atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 6:

Table 6

Embodiment 7

Handle: with powder 1 200 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 7:

Table 7

Embodiment 8

Employing is got rid of the band legal system and is equipped with raw alloy, and it consists of 5.0Pr-22.0Nd-4.8Dy-0.2Al-0.1Cu-0.5Co-0.2Ga-0.1Zr-1.0B-surplus Fe.Then carry out the broken processing of hydrogen, at room temperature make raw alloy inhale hydrogen, in Ar atmosphere, carry out 500 ℃ * 1 hour dehydrogenation.The StAl and the paraffin wax that add 1wt.% mixed 1 hour, and obtaining median size after the airflow milling is that (specific surface area is 2.5m to 10 μ m ²/ g) powder particle is crossed 60 and 300 purposes then and is sieved the powder 1 that obtains even particle size distribution.More unprocessed with handle after the blank product parameters.

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 8:

Table 8

Embodiment 9

Handle: with powder 1 800 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 9:

Table 9

Embodiment 10

Handle: with powder 1 500 ℃ of anneal 1 hour under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 10:

Table 10

Embodiment 11

Handle: with powder 1 500 ℃ of anneal 5 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 8:

Table 11

Embodiment 12

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.1wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 12:

Table 12

Embodiment 13

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 1.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 13:

Table 13

Embodiment 14

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 3wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 14:

Table 14

Embodiment 15

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 1 hour with hexanaphthene toward the carbonyl iron dust that wherein adds 1.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 15:

Table 15

Embodiment 16

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 5 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 1.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 16:

Table 16

Embodiment 17

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with pimelinketone toward the carbonyl iron dust that wherein adds 1.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 17:

Table 17

Embodiment 18

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with the toluene pimelinketone toward the carbonyl iron dust that wherein adds 1.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 18:

Table 18

Embodiment 19

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 3MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 19:

Table 19

Embodiment 20

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 25MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 20:

Table 20

Embodiment 21

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 50MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 21:

Table 21

Embodiment 22

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.1wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 22:

Table 22

Embodiment 23

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 1.2T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 23:

Table 23

Embodiment 24

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is static magnetic field 2.0T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 24:

Table 24

Embodiment 25

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is pulsed magnetic field 2.0T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 25:

Table 25

Embodiment 26

Employing is got rid of the band legal system and is equipped with raw alloy, and it consists of 5.0Pr-22.0Nd-4.8Dy-0.2Al-0.1Cu-0.5Co-0.2Ga-0.1Zr-1.0B-surplus Fe.Then carry out the broken processing of hydrogen, at room temperature make raw alloy inhale hydrogen, in Ar atmosphere, carry out 500 ℃ * 1 hour dehydrogenation.The polyethylene oxide alkyl ethers and the lecithin that add 0.1wt.% mixed 1 hour, obtained the powder particle that median size is 4 μ m after the airflow milling, crossed the powder 1 that 60 and 300 purposes sieve obtains even particle size distribution then.More unprocessed with handle after the blank product parameters.

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 26:

Table 26

Embodiment 27

Employing is got rid of the band legal system and is equipped with raw alloy, and it consists of 5.0Pr-22.0Nd-4.8Dy-0.2Al-0.1Cu-0.5Co-0.2Ga-0.1Zr-1.0B-surplus Fe.Then carry out the broken processing of hydrogen, at room temperature make raw alloy inhale hydrogen, in Ar atmosphere, carry out 500 ℃ * 1 hour dehydrogenation.The polyethylene oxide alkyl ethers and the calcium stearate that add 0.1wt.% mixed 1 hour, obtained the powder particle that median size is 4 μ m after the airflow milling, crossed the powder 1 that 60 and 300 purposes sieve obtains even particle size distribution then.More unprocessed with handle after the blank product parameters.

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 27:

Table 27

Embodiment 28

Employing is got rid of the band legal system and is equipped with raw alloy, and it consists of 5.0Pr-22.0Nd-4.8Dy-0.2Al-0.1Cu-0.5Co-0.2Ga-0.1Zr-1.0B-surplus Fe.Then carry out the broken processing of hydrogen, at room temperature make raw alloy inhale hydrogen, in Ar atmosphere, carry out 500 ℃ * 1 hour dehydrogenation.The polyethylene oxide alkyl ethers and the naphthalene that add 0.1wt.% mixed 1 hour, obtained the powder particle that median size is 4 μ m after the airflow milling, crossed the powder 1 that 60 and 300 purposes sieve obtains even particle size distribution then.More unprocessed with handle after the blank product parameters.

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 28:

Table 28

Embodiment 29

Employing is got rid of the band legal system and is equipped with raw alloy, and it consists of 5.0Pr-22.0Nd-4.8Dy-0.2Al-0.1Cu-0.5Co-0.2Ga-0.1Zr-1.0B-surplus Fe.Then carry out the broken processing of hydrogen, at room temperature make raw alloy inhale hydrogen, in Ar atmosphere, carry out 500 ℃ * 1 hour dehydrogenation.The polyethylene oxide mono fatty acid ester and the lecithin that add 0.1wt.% mixed 1 hour, obtained the powder particle that median size is 4 μ m after the airflow milling, crossed the powder 1 that 60 and 300 purposes sieve obtains even particle size distribution then.More unprocessed with handle after the blank product parameters.

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 29:

Table 29

Embodiment 30

Employing is got rid of the band legal system and is equipped with raw alloy, and it consists of 5.0Pr-22.0Nd-4.8Dy-0.2Al-0.1Cu-0.5Co-0.2Ga-0.1Zr-1.0B-surplus Fe.Then carry out the broken processing of hydrogen, at room temperature make raw alloy inhale hydrogen, in Ar atmosphere, carry out 500 ℃ * 1 hour dehydrogenation.The polyethylene oxide mono fatty acid ester and the calcium stearate that add 0.1wt.% mixed 1 hour, obtained the powder particle that median size is 4 μ m after the airflow milling, crossed the powder 1 that 60 and 300 purposes sieve obtains even particle size distribution then.More unprocessed with handle after the blank product parameters.

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 30:

Table 30

Embodiment 31

Employing is got rid of the band legal system and is equipped with raw alloy, and it consists of 5.0Pr-22.0Nd-4.8Dy-0.2Al-0.1Cu-0.5Co-0.2Ga-0.1Zr-1.0B-surplus Fe.Then carry out the broken processing of hydrogen, at room temperature make raw alloy inhale hydrogen, in Ar atmosphere, carry out 500 ℃ * 1 hour dehydrogenation.The lecithin and the calcium stearate that add 0.1wt.% mixed 1 hour, obtained the powder particle that median size is 4 μ m after the airflow milling, crossed the powder 1 that 60 and 300 purposes sieve obtains even particle size distribution then.More unprocessed with handle after the blank product parameters.

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 31:

Table 31

Embodiment 32

Employing is got rid of the band legal system and is equipped with raw alloy, and it consists of 5.0Pr-22.0Nd-4.8Dy-0.2Al-0.1Cu-0.5Co-0.2Ga-0.1Zr-1.0B-surplus Fe.Then carry out the broken processing of hydrogen, at room temperature make raw alloy inhale hydrogen, in Ar atmosphere, carry out 500 ℃ * 1 hour dehydrogenation.The lecithin and the naphthalene that add 0.1wt.% mixed 1 hour, obtained the powder particle that median size is 4 μ m after the airflow milling, crossed the powder 1 that 60 and 300 purposes sieve obtains even particle size distribution then.More unprocessed with handle after the blank product parameters.

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 32:

Table 32

Embodiment 33

Employing is got rid of the band legal system and is equipped with raw alloy, and it consists of 5.0Pr-22.0Nd-4.8Dy-0.2Al-0.1Cu-0.5Co-0.2Ga-0.1Zr-1.0B-surplus Fe.Then carry out the broken processing of hydrogen, at room temperature make raw alloy inhale hydrogen, in Ar atmosphere, carry out 500 ℃ * 1 hour dehydrogenation.The calcium stearate and the naphthalene that add 0.1wt.% mixed 1 hour, obtained the powder particle that median size is 4 μ m after the airflow milling, crossed the powder 1 that 60 and 300 purposes sieve obtains even particle size distribution then.More unprocessed with handle after the blank product parameters.

Handle: with powder 1 500 ℃ of anneal 2 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 33:

Table 33

Embodiment 34

Handle: with powder 1 100 ℃ of anneal 0.5 hour under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 34:

Table 34

Embodiment 35

Handle: with powder 1 100 ℃ of anneal 10 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 35:

Table 35

Embodiment 36

Handle: with powder 1 1000 ℃ of anneal 0.5 hour under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 36:

Table 36

Embodiment 37

Handle: with powder 1 1000 ℃ of anneal 10 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 37:

Table 37

Embodiment 38

Handle: with powder 1 500 ℃ of anneal 3 hours under Ar atmosphere, mixing obtained powder 2 in 2 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 38:

Table 38

Embodiment 39

Handle: with powder 1 500 ℃ of anneal 3 hours under Ar atmosphere, mixing obtained powder 2 in 8 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 39:

Table 39

Embodiment 40

Handle: with powder 1 500 ℃ of anneal 3 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.The loose density of this powder is 2.5g/cm ³, tap density is 3g/cm ³, flowability is 36s/50g.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 40:

Table 40

Embodiment 41

Handle: with powder 1 500 ℃ of anneal 3 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.The loose density of this powder is 3g/cm ³, tap density is 4.5g/cm ³, flowability is 36s/50g.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 41:

Table 41

Embodiment 42

Handle: with powder 1 500 ℃ of anneal 3 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 1MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 42:

Table 42

Embodiment 43

Handle: with powder 1 500 ℃ of anneal 3 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 2MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 43:

Table 43

Embodiment 44

Handle: with powder 1 500 ℃ of anneal 3 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 100MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 44:

Table 44

Embodiment 45

Handle: with powder 1 500 ℃ of anneal 3 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 300MPa, and externally-applied magnetic field is 0.5T; Then 1080 ℃ of sintering 5 hours, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 45:

Table 45

Embodiment 46

Employing is got rid of the band legal system and is equipped with raw alloy, and it consists of 4.0Pr-24.0Nd-4.8Dy-0.2Al-0.1Cu-0.5Co-0.2Ga-0.1Zr-1.0B-surplus Fe.Then carry out the broken processing of hydrogen, at room temperature make raw alloy inhale hydrogen, in Ar atmosphere, carry out 500 ℃ * 1 hour dehydrogenation.The StAl and the paraffin wax that add 0.1wt.% mixed 1 hour, obtained the powder particle that median size is 4 μ m after the airflow milling, crossed the powder 1 that 60 and 300 purposes sieve obtains even particle size distribution then.More unprocessed with handle after the blank product parameters.

Unprocessed: powder 1 is shaped on extremely to the pressurising machine four, and compacting pressure is 50MPa, and externally-applied magnetic field is 1.0T; Hydrostatic pressure is 200MPa; 1150 ℃ of sintering 1 hour under vacuum state then, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.

Handle: with powder 1 500 ℃ of anneal 3 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; 1150 ℃ of sintering 1 hour under vacuum state then, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 46:

Table 46

Embodiment 47

Unprocessed: powder 1 is shaped on extremely to the pressurising machine four, and compacting pressure is 50MPa, and externally-applied magnetic field is 1.0T; Hydrostatic pressure is 200MPa; 1000 ℃ of sintering 10 hours under vacuum state then, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.

Handle: with powder 1 500 ℃ of anneal 3 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; 1000 ℃ of sintering 10 hours under vacuum state then, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 47:

Table 47

Embodiment 48

Unprocessed: powder 1 is shaped on extremely to the pressurising machine four, and compacting pressure is 50MPa, and externally-applied magnetic field is 1.0T; Hydrostatic pressure is 200MPa; 1080 ℃ of sintering 4 hours under vacuum state then, 1000 ℃ of timeliness 1 hour, 600 ℃ of timeliness 3 hours.

Handle: with powder 1 500 ℃ of anneal 3 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; 1080 ℃ of sintering 4 hours under vacuum state then, 1000 ℃ of timeliness 1 hour, 600 ℃ of timeliness 3 hours.Referring to table 48:

Table 48

Embodiment 49

Unprocessed: powder 1 is shaped on extremely to the pressurising machine four, and compacting pressure is 50MPa, and externally-applied magnetic field is 1.0T; Hydrostatic pressure is 200MPa; 1080 ℃ of sintering 4 hours under vacuum state then, 800 ℃ of timeliness 3 hours, 600 ℃ of timeliness 3 hours.

Handle: with powder 1 500 ℃ of anneal 3 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; 1080 ℃ of sintering 4 hours under vacuum state then, 800 ℃ of timeliness 3 hours, 600 ℃ of timeliness 3 hours.Referring to table 49:

Table 49

Embodiment 50

Unprocessed: powder 1 is shaped on extremely to the pressurising machine four, and compacting pressure is 50MPa, and externally-applied magnetic field is 1.0T; Hydrostatic pressure is 200MPa; 1080 ℃ of sintering 4 hours under vacuum state then, 900 ℃ of timeliness 2 hours, 450 ℃ of timeliness 5 hours.

Handle: with powder 1 500 ℃ of anneal 3 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; 1080 ℃ of sintering 4 hours under vacuum state then, 900 ℃ of timeliness 2 hours, 450 ℃ of timeliness 5 hours.Referring to table 50:

Table 50

Embodiment 51

Unprocessed: powder 1 is shaped on extremely to the pressurising machine four, and compacting pressure is 50MPa, and externally-applied magnetic field is 1.0T; Hydrostatic pressure is 200MPa; 1080 ℃ of sintering 4 hours under vacuum state then, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 2 hours.

Handle: with powder 1 500 ℃ of anneal 3 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; 1080 ℃ of sintering 4 hours under vacuum state then, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 2 hours.Referring to table 51:

Table 51

Embodiment 52

Unprocessed: powder 1 is shaped on extremely to the pressurising machine four, and compacting pressure is 50MPa, and externally-applied magnetic field is 1.0T; Hydrostatic pressure is 200MPa; 1150 ℃ of sintering 1 hour under the argon gas state then, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.

Handle: with powder 1 500 ℃ of anneal 3 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; 1150 ℃ of sintering 1 hour under the argon gas state then, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 52:

Table 52

Embodiment 53

Unprocessed: powder 1 is shaped on extremely to the pressurising machine four, and compacting pressure is 50MPa, and externally-applied magnetic field is 1.0T; Hydrostatic pressure is 200MPa; 1000 ℃ of sintering 10 hours under the argon gas state then, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.

Handle: with powder 1 500 ℃ of anneal 3 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; 1000 ℃ of sintering 10 hours under the argon gas state then, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 53:

Table 53

Embodiment 54

Unprocessed: powder 1 is shaped on extremely to the pressurising machine four, and compacting pressure is 50MPa, and externally-applied magnetic field is 1.0T; Hydrostatic pressure is 200MPa; 1080 ℃ of sintering 4 hours under the argon gas state then, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.

Handle: with powder 1 500 ℃ of anneal 3 hours under Ar atmosphere, mixing obtained powder 2 in 3 hours with hexanaphthene toward the carbonyl iron dust that wherein adds 0.5wt.%.Then powder 2 is shaped on same press, compacting pressure is 5MPa, and externally-applied magnetic field is 0.5T; Hydrostatic pressure is 200MPa; 1080 ℃ of sintering 4 hours under the argon gas state then, 900 ℃ of timeliness 2 hours, 600 ℃ of timeliness 3 hours.Referring to table 54:

Table 54

Need to prove that foregoing invention content and embodiment are intended to prove the practical application of technical scheme provided by the present invention, should not be construed as qualification protection domain of the present invention.Those skilled in the art are in spirit of the present invention and principle, when doing various modifications, being equal to replacement or improvement.Protection scope of the present invention is as the criterion with appended claims.

Claims

1. the treatment process of a R-T-B series alloy powder for radiation magnetic loop, wherein, R is a REE, comprises at least a element or more than one elements that are selected among Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and the Lu; T comprises Fe and unavoidable impurities; Wherein, the content of R is 27-35wt.%, and the content of B is 0.5-4wt.%, and surplus is T;

The treating method comprises following steps:

(2) it is broken the raw alloy ingot casting to be carried out coarse breaking or hydrogen in inert atmosphere, obtains particle diameter and be hundreds of microns powder;

(3) adding any two kinds of materials that 0.01～1wt.% is selected from polyethylene oxide composition polymer, lipid acid, derivative of fatty acid and the hydrocarbon polymer in the powder after coarse breaking or hydrogen fragmentation mixed 1～10 hour; Wherein, said hydrocarbon polymer is paraffin or naphthalene;

(5) powdered alloy is annealed under rare gas element, vacuum or reducing atmosphere, annealing region is 100～1000 ℃, and annealing time is 0.5～10 hour;

(6) add 0.05～5wt.% carbonyl iron dust and at least a cycloaliphates in the powdered alloy after annealing and mixed 1～8 hour, obtain mixed powder;

(7) this mixed powder is formed the ring-type molding in magnetic field;

(8) this ring-type molding is carried out 1～10 hour sintering at 1000～1150 ℃ in vacuum or inert gas atmosphere, behind the sintering again to sintered compact respectively 800～1000 ℃ carry out 1～3 hour, 450～600 ℃ of ageing treatment of carrying out 2～5 hours.

2. treatment process as claimed in claim 1, wherein, the polyethylene oxide composition polymer is polyethylene oxide alkyl ethers or polyethylene oxide mono fatty acid ester; Lipid acid is triglyceride level or lecithin; Derivative of fatty acid is Zinic stearas, calcium stearate or StAl.

3. treatment process as claimed in claim 1, wherein, in step (5), reducing atmosphere is hydrogen or ammonia.

4. treatment process as claimed in claim 1, wherein, in step (5), annealing region is 200～800 ℃, annealing time is 1～5 hour.

5. treatment process as claimed in claim 1 wherein, in step (6), is added 0.1～3wt.% carbonyl iron dust and at least a cycloaliphates and was mixed 2～5 hours in powdered alloy, obtain mixed powder.

6. like claim 1 or 5 described treatment processs, wherein, said cycloaliphates is hexanaphthene, pimelinketone or toluene pimelinketone.

7. like claim 1 or 5 described treatment processs, wherein, in step (6), the loose density of resulting powder particle is 2.5～3g/cm ³, tap density is 3～4.5g/cm ³, flowability>=32s/50g.

8. treatment process as claimed in claim 1, wherein, in step (7), the compacting pressure that is shaped in the magnetic field is 1～300MPa.

9. treatment process as claimed in claim 1, wherein, in step (7), externally-applied magnetic field is set at 0.5～2T, and wherein, externally-applied magnetic field is static magnetic field or pulsed magnetic field.

10. treatment process as claimed in claim 8, wherein, in step (7), the compacting pressure that is shaped in the magnetic field is 2～100Mpa.

11. treatment process as claimed in claim 10, wherein, in step (7), the compacting pressure that is shaped in the magnetic field is 3～50MPa.