CN109859945A - A kind of preparation method of high temperature samarium-cobalt permanent-magnetic material - Google Patents
A kind of preparation method of high temperature samarium-cobalt permanent-magnetic material Download PDFInfo
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- CN109859945A CN109859945A CN201910157231.6A CN201910157231A CN109859945A CN 109859945 A CN109859945 A CN 109859945A CN 201910157231 A CN201910157231 A CN 201910157231A CN 109859945 A CN109859945 A CN 109859945A
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Abstract
The invention discloses a kind of preparation methods of high temperature samarium-cobalt permanent-magnetic material, and steps are as follows: samarium-cobalt permanent-magnetic material is first, in accordance with Sm (Co1‑u‑v‑wCuuFevZrw)zIngredient is carried out, wherein u=0.082-0.088, v=0.093-0.143, w=0.027-0.028 and z=6.2-6.5;The raw material merging vacuum induction melting furnace matched then is subjected to melting, obtains the uniform alloy pig of ingredient;Alloy pig is obtained into the alloy powder in granularity SDM=3.2-3.8 μ m by airflow milling is broken afterwards;Then powder is suppressed by magnetic field orientating and static pressure is waited to obtain green compact;Green compact are finally subjected to multisection type sintering, solid solution and ageing treatment.Combination of invention under the premise of not adding microelement (Mn and Er etc.) through samarium metal, metallic cobalt, five kinds of metallic copper, metallic iron and metal zirconium metals solves the problems, such as resistant to high temperature at 500 DEG C of 2:17 type samarium cobalt permanent magnet.
Description
Technical field
The invention belongs to samarium-cobalt permanent-magnetic material preparation technical fields, especially the preparation side with a kind of high temperature samarium-cobalt permanent-magnetic material
Method is related.
Background technique
Samarium-cobalt permanent-magnetic material is widely used in motor, sensing with the advantages that high temperature resistant, corrosion-resistant and higher magnetic property
The high-tech areas such as device, detector, engine and radar, but it is directed to some Special use environment (superelevation of aerospace field
Warm condition) remain the problem that magnetic property at high temperature is relatively low and maximum operating temperature is relatively low.
Summary of the invention
Aiming at the problem that above-mentioned background technique, the present invention is intended to provide a kind of preparation method of high temperature samarium-cobalt permanent-magnetic material.
For this purpose, the invention adopts the following technical scheme: a kind of preparation method of high temperature samarium-cobalt permanent-magnetic material, including
Step 1, samarium-cobalt permanent-magnetic material is first, in accordance with Sm (Co1-u-v-wCuuFevZrw)zIngredient is carried out, wherein u=0.082-
0.088, v=0.093-0.143, w=0.027-0.028 and z=6.2-6.5;
The raw material merging vacuum induction melting furnace matched is carried out melting, obtains the uniform alloy pig of ingredient by step 2;
Alloy pig is obtained the alloy powder in granularity SDM=3.2-3.8 μ m by airflow milling is broken by step 3;
Powder is suppressed by magnetic field orientating and static pressure is waited to obtain green compact by step 4;
Green compact are carried out multisection type sintering, solid solution and ageing treatment by step 5.
As supplement to above-mentioned technical proposal and perfect, the invention also includes following technical characteristics.
In step 2, the raw material matched successively are put according to the sequencing of Fe-Zr-Fe-Co-Cu-Sm into vacuum sense
Smelting furnace is answered, the bell that vacuum induction melting furnace is closed after the completion of charging carries out vacuumize process, as vacuum degree≤7Pa in furnace
Start low-power heating, excludes the moisture of crucible, burner hearth and raw material and the gas of absorption, stop as vacuum degree≤5Pa in furnace
It only vacuumizes opening Ar gas charge valve and is filled with Ar gas into burner hearth, stop inflation when air pressure reaches -0.06 ± 0.03MPa and start
High-power (65 ± 5KW) heats 15 ± 5min of melting, and water cooling ingot casting copper mold is cast straight to after melting and is quickly cooled down shape
At the alloy pig of single 1:7 phase.
In step 3, airflow milling powder is carried out again after alloy pig is carried out coarse crushing.
In step 4, the specific steps are two aspects of, magnetic field orientating die mould and equal static pressure, the wherein mistake of magnetic field orientating die mould
Alignment magnetic field need >=1.8T in journey, the oxygen content need≤5000PPM in press-space.
In step 5, it is sintered specific steps are as follows: the green compact after static pressure will be waited to be placed in vacuum sintering furnace, rear fire door of closing is taken out very
Sky is begun to warm up as vacuum degree≤5Pa, starts to inflate after 10 ± 5min of heat preservation when sintering temperature rises 900 ± 10 DEG C of system
(inert gas) stopping after air pressure reaches -0.05 ± 0.01MPa in furnace body is inflated, and heating sintering is continued thereafter with, 1205
60 ± 30min is kept the temperature at ± 5 DEG C and carries out maximum temperature sintering, is then kept the temperature 120 ± 30min at 1185 ± 10 DEG C and is located in advance
Reason, room temperature processed air-cooled immediately after to be pre-treated;
It is dissolved specific steps are as follows: by the blank merging vacuum drying oven of sintering, rear fire door of closing is vacuumized, as vacuum degree≤5Pa
Start to be filled with inert gas and heat, 10 ± 5min of heat preservation at 1160 ± 5 DEG C is warming up to the speed of 4 ± 1 DEG C/min first, after
1165 ± 5 DEG C are warming up to the speed of 2 DEG C/min, and keeps the temperature 180 ± 5min under this temperature, it is immediately air-cooled, during being somebody's turn to do
The volatilization of samarium metal can effectively be prevented by being filled with inert gas;
Timeliness specific steps are as follows: by the blank merging vacuum drying oven after solid solution, rear fire door of closing is vacuumized, as vacuum degree≤5Pa
When start to be filled with inert gas and heat, the aging technique that the present invention uses is multistage aging, the heating rate of 4 DEG C/min first
600 ± 30min is kept the temperature after being warming up to 840 ± 5 DEG C, after with the rate of temperature fall of 0.8 ± 0.2 DEG C/min be cooled to 600 ± 5 DEG C, after
400 ± 5 DEG C are cooled to the rate of temperature fall of 1.5 ± 0.5 DEG C/min, keeps the temperature 120 ± 30min afterwards, it is rear air-cooled to room temperature.
The present invention can achieve following the utility model has the advantages that the present invention is led under the premise of not adding microelement (Mn and Er etc.)
The combination for crossing samarium metal, metallic cobalt, five kinds of metallic copper, metallic iron and metal zirconium metals solves at 500 DEG C of 2:17 type samarium cobalt permanent magnet
Problem resistant to high temperature.
Specific embodiment
With Sm (Co0.791Cu0.087Fe0.093Zr0.027)6.298For a specific embodiment of the invention is done furtherly
It is bright:
1 ingredient: choose high-purity raw material (Sm/RE >=99.7%, Co >=99.6%, Cu+Ag >=99.95%, Zr+Hf >=
99.3%, Fe >=99.75%) according to Sm (Co0.791Cu0.087Fe0.093Zr0.027)6.298、Sm
(Co0.745Cu0.084Fe0.142Zr0.027)6.497With Sm (Co0.768Cu0.082Fe0.121Zr0.027)6.399Atomic ratio carry out ingredient;
2 meltings: the raw material matched successively are put according to the sequencing of Fe-Zr-Fe-Co-Cu-Sm into melting kettle, charging
The bell for closing vacuum induction melting furnace after the completion carries out vacuumize process, starts low-power as vacuum degree≤7Pa in furnace and adds
Heat excludes the moisture of crucible, burner hearth and raw material and the gas of absorption, stops vacuumizing opening as vacuum degree≤5Pa in furnace
Ar gas charge valve is filled with Ar gas into burner hearth, when air pressure reaches -0.06 ± 0.03MPa stop inflation start it is high-power (65 ±
15 ± 5min of melting 5KW) is heated, water cooling ingot casting copper mold is cast straight to after melting and rapidly cools to form single 1:7 phase
Alloy pig;
3 powder processed: carrying out airflow milling powder after alloy pig is carried out coarse crushing again, and wherein airflow milling powder process uses indifferent gas
Body (nitrogen or argon gas) is protected from powder oxidation, and the particle size range of revolving speed control powder is discussed additionally by the sorting of airflow milling
SMD=3.2-3.8 μ m, powder particles carefully will lead to degree of oxidation partially and rise and then cause remanent magnetism and intrinsic coercivity equimagnetic
Performance parameter reduces, if the higher reduction for will lead to individual particle powder polycrystalline ratio and rising and then leading to remanent magnetism of granularity, thus it is whole
A pulverizing process needs strict control mill room oxygen content and powder particles.
4 die moulds: die mould is primarily referred to as magnetic field orientating die mould and waits two aspects of static pressure, wherein the mistake of magnetic field orientating die mould
Alignment magnetic field need >=1.8T in journey, the oxygen content need≤5000PPM in press-space.
5 sintering: the green compact after static pressure will be waited to be placed in vacuum sintering furnace, rear fire door of closing vacuumizes, as vacuum degree≤5Pa
When begin to warm up, start to inflate (inert gas) until furnace after 10 ± 5min of heat preservation when sintering temperature rises 900 ± 10 DEG C of system
Internal air pressure stops inflation after reaching -0.05 ± 0.01MPa, continues thereafter with heating sintering, keep the temperature 60 at 1205 ± 5 DEG C ±
30min carries out maximum temperature sintering, then keeps the temperature 120 ± 30min at 1185 ± 10 DEG C and is pre-processed, end to be pre-treated
Room temperature processed air-cooled immediately afterwards.It can effectively be prevented compared with traditional vacuum-sintering in the sintering process using inert gas sintering
The volatilization of samarium metal, in addition the present invention uses multisection type sintering to can be further improved blank compared with traditional single hop sintering close
Degree, while bigger cell structure can also be obtained, promote Fe element to enter 2:17R phase, and then it is (surplus to improve every magnetic parameter
Magnetic and squareness etc.).
6 solid solutions: by the blank merging vacuum drying oven of sintering, rear fire door of closing is vacuumized, and starts as vacuum degree≤5Pa
Be filled with inert gas and heat, 10 ± 5min of heat preservation is warming up at 1160 ± 5 DEG C with the speed of 4 ± 1 DEG C/min first, after with 2
DEG C/speed of min is warming up to 1165 ± 5 DEG C, and keeps the temperature 180 ± 5min under this temperature, immediately air-cooled, should during be filled with
Inert gas can effectively prevent the volatilization of samarium metal, and then reduce intrinsic coercivity temperature coefficient.
7 timeliness: by the blank merging vacuum drying oven after solid solution, rear fire door of closing is vacuumized, and opens as vacuum degree≤5Pa
Beginning is filled with inert gas and heats, and for multistage aging, the heating rate of 4 DEG C/min first heats up the aging technique that the present invention uses
600 ± 30min is kept the temperature after to 840 ± 5 DEG C, after with the rate of temperature fall of 0.8 ± 0.2 DEG C/min be cooled to 600 ± 5 DEG C, after with 1.5
The rate of temperature fall of ± 0.5 DEG C/min is cooled to 400 ± 5 DEG C, keeps the temperature 120 ± 30min afterwards, rear air-cooled to room temperature.
The detection of 8 magnetic properties:
Claims (5)
1. a kind of preparation method of high temperature samarium-cobalt permanent-magnetic material, it is characterised in that the following steps are included:
Step 1, samarium-cobalt permanent-magnetic material is first, in accordance with Sm (Co1-u-v-wCuuFevZrw)zIngredient is carried out, wherein u=0.082-0.088,
V=0.093-0.143, w=0.027-0.028 and z=6.2-6.5;
The raw material merging vacuum induction melting furnace matched is carried out melting, obtains the uniform alloy pig of ingredient by step 2;
Alloy pig is obtained the alloy powder in granularity SDM=3.2-3.8 μ m by airflow milling is broken by step 3;
Powder is suppressed by magnetic field orientating and static pressure is waited to obtain green compact by step 4;
Green compact are carried out multisection type sintering, solid solution and ageing treatment by step 5.
2. a kind of preparation method of high temperature samarium-cobalt permanent-magnetic material according to claim 1, it is characterised in that: in step 2,
The raw material matched successively are put according to the sequencing of Fe-Zr-Fe-Co-Cu-Sm into vacuum induction melting furnace, charging is completed
The bell for closing vacuum induction melting furnace afterwards carries out vacuumize process, starts low-power heating, row as vacuum degree≤7Pa in furnace
Except the moisture of crucible, burner hearth and raw material and the gas of absorption, as vacuum degree≤5Pa in furnace, stopping vacuumizes opening Ar gas and fills
Air valve is filled with Ar gas into burner hearth, stops inflation beginning high-power (65 ± 5KW) when air pressure reaches -0.06 ± 0.03MPa and adds
15 ± 5min of hot smelting is cast straight to water cooling ingot casting copper mold and rapidly cools to form the alloy of single 1:7 phase after melting
Ingot.
3. a kind of preparation method of high temperature samarium-cobalt permanent-magnetic material according to claim 1, it is characterised in that: in step 3,
Airflow milling powder is carried out again after alloy pig is carried out coarse crushing.
4. a kind of preparation method of high temperature samarium-cobalt permanent-magnetic material according to claim 1, it is characterised in that: in step 4,
The specific steps are two aspects of, magnetic field orientating die mould and equal static pressure, wherein alignment magnetic field during magnetic field orientating die mould
Need >=1.8T, the oxygen content need≤5000PPM in press-space.
5. a kind of preparation method of high temperature samarium-cobalt permanent-magnetic material according to claim 1, it is characterised in that: in step 5,
It is sintered specific steps are as follows: the green compact after static pressure will be waited to be placed in vacuum sintering furnace, rear fire door of closing vacuumizes, as vacuum degree≤5Pa
When begin to warm up, start to inflate (inert gas) until furnace after 10 ± 5min of heat preservation when sintering temperature rises 900 ± 10 DEG C of system
Internal air pressure stops inflation after reaching -0.05 ± 0.01MPa, continues thereafter with heating sintering, keep the temperature 60 at 1205 ± 5 DEG C ±
30min carries out maximum temperature sintering, then keeps the temperature 120 ± 30min at 1185 ± 10 DEG C and is pre-processed, end to be pre-treated
Room temperature processed air-cooled immediately afterwards;
It is dissolved specific steps are as follows: by the blank merging vacuum drying oven of sintering, rear fire door of closing is vacuumized, as vacuum degree≤5Pa
Start to be filled with inert gas and heat, 10 ± 5min of heat preservation at 1160 ± 5 DEG C is warming up to the speed of 4 ± 1 DEG C/min first, after
1165 ± 5 DEG C are warming up to the speed of 2 DEG C/min, and keeps the temperature 180 ± 5min under this temperature, it is immediately air-cooled, during being somebody's turn to do
The volatilization of samarium metal can effectively be prevented by being filled with inert gas;
Timeliness specific steps are as follows: by the blank merging vacuum drying oven after solid solution, rear fire door of closing is vacuumized, as vacuum degree≤5Pa
When start to be filled with inert gas and heat, the aging technique that the present invention uses is multistage aging, the heating rate of 4 DEG C/min first
600 ± 30min is kept the temperature after being warming up to 840 ± 5 DEG C, after with the rate of temperature fall of 0.8 ± 0.2 DEG C/min be cooled to 600 ± 5 DEG C, after
400 ± 5 DEG C are cooled to the rate of temperature fall of 1.5 ± 0.5 DEG C/min, keeps the temperature 120 ± 30min afterwards, it is rear air-cooled to room temperature.
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CN110444383A (en) * | 2019-07-24 | 2019-11-12 | 北矿磁材(阜阳)有限公司 | A kind of high HkThe preparation method of SmCo sintered permanent magnet |
CN110957089A (en) * | 2019-11-21 | 2020-04-03 | 杭州科德磁业有限公司 | Preparation method of samarium cobalt permanent magnet material |
CN111243804A (en) * | 2019-11-29 | 2020-06-05 | 南京安德海睿智能科技有限公司 | Rare earth permanent magnet with hydrogen resistance and preparation method thereof |
CN111370191A (en) * | 2020-03-20 | 2020-07-03 | 杭州永磁集团有限公司 | Heavy rare earth element-free samarium-cobalt permanent magnet material with low coercive force temperature coefficient and high temperature and preparation method thereof |
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CN110444383A (en) * | 2019-07-24 | 2019-11-12 | 北矿磁材(阜阳)有限公司 | A kind of high HkThe preparation method of SmCo sintered permanent magnet |
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CN111243804A (en) * | 2019-11-29 | 2020-06-05 | 南京安德海睿智能科技有限公司 | Rare earth permanent magnet with hydrogen resistance and preparation method thereof |
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CN111370191A (en) * | 2020-03-20 | 2020-07-03 | 杭州永磁集团有限公司 | Heavy rare earth element-free samarium-cobalt permanent magnet material with low coercive force temperature coefficient and high temperature and preparation method thereof |
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CN113436874A (en) * | 2021-05-27 | 2021-09-24 | 北矿科技股份有限公司 | Sm2Co17Molded high-temperature magnet and preparation method thereof |
CN113436874B (en) * | 2021-05-27 | 2023-04-18 | 北矿科技股份有限公司 | Sm 2 Co 17 Molded high-temperature magnet and preparation method thereof |
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