CN107564645A - One kind has low residual magnetism temperature coefficient high temperature samarium-cobalt permanent-magnetic material and preparation method - Google Patents
One kind has low residual magnetism temperature coefficient high temperature samarium-cobalt permanent-magnetic material and preparation method Download PDFInfo
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Abstract
The invention discloses one kind to have low residual magnetism temperature coefficient high temperature samarium-cobalt permanent-magnetic material and preparation method, and the expression formula of the permanent-magnet material is Sm1‑x‑yErxLay(Co1‑u‑v‑wFeuCuvZrw)z, wherein x=0.00~0.40, y=0.00~0.03, u=0.10~0.20, v=0.06~0.10, w=0.02~0.04, z=7.4~7.8.Using vacuum arc melting, ball powder-grinding, magnetic field orientating shaping, isostatic cool pressing, sintering, solid solution and aging technique, the Sm with low residual magnetism temperature coefficient is made1‑x‑yErxLay(Co1‑u‑v‑wFeuCuvZrw)zPermanent-magnet material.
Description
Technical field
There is low remanent magnetism temperature containing samarium Sm, erbium Er, lanthanum La, cobalt Co, iron Fe, copper Cu, zirconium Zr elements the present invention relates to one kind
Spend the new type high temperature samarium-cobalt permanent-magnetic material and preparation method of the nanometer cell structure of coefficient.
Background technology
Permanent-magnet material as a kind of important functional material, be widely applied to computer technology, that micro- communication technology,
Each key areas such as auto industry, aircraft industry, automatic technology, instrumental technique.The development experience of permanent-magnet material carbon steel,
Several developing stage such as AlNiCo systems alloy, hard ferrite, RE permanent magnetic alloy.The high temperature of low-temperature coefficient operation at high temperature
Permanent-magnet material is the hot issue of physics and Material Field research.
Sm2Co17Permanent magnet does not only have high intrinsic saturation induction density, and Curie temperature is also very high, about 926 DEG C, its
Intrinsic saturation induction density and Curie temperature are above SmCo5Alloy, it is most likely that develop into temperature in use more than 450 DEG C
High temperature permanent magnetic material.Sm2Co17Permanent magnet HCJ temperature coefficient is high, about -0.4%/DEG C.Therefore, in high-temperature power generation
Machine, high temperature resistant magnetic suspension bearing, high temperature instrument, wind-driven generator etc. have important application prospect.
Existing commercial samarium cobalt permanent magnet physical efficiency uses 300 DEG C, and residual magnetism temperature coefficient α is big, about -0.035%/DEG C.And document
The permanent magnet of the existing low residual magnetism temperature coefficient of middle preparation only has low temperature coefficient at 25~100 DEG C, can not use more
High temperature, the present invention by rare earth doped, prepared in the range of 25~400 DEG C residual magnetism temperature coefficient α for-
0.025%/DEG C, the requirement of high temperature precision instrument can be met.
The content of the invention
The technology of the present invention solves problem：Overcome the deficiencies in the prior art, there is provided one kind has low residual magnetism temperature coefficient high
Temperature samarium-cobalt permanent-magnetic material and preparation method, it is excellent by adding heavy rare earth element Er, LREE La, while modifying ingredients
Chemical industry skill, 400 DEG C of highest can be used by having prepared, while have the permanent magnet of low residual magnetism temperature coefficient at 25~400 DEG C, can
To meet the requirement of high temperature precision instrument.
The technology of the present invention solution：One kind has low residual magnetism temperature coefficient high temperature samarium-cobalt permanent-magnetic material, contains for one kind
There is the low residual magnetism temperature coefficient with nanometer cell structure of samarium Sm, erbium Er, lanthanum La, cobalt Co, iron Fe, copper Cu, zirconium Zr elements
High temperature new type high temperature samarium-cobalt permanent-magnetic material, the chemical formula of the new low residual magnetism temperature coefficient high temperature permanent magnetic material is Sm1-x- yErxLay(Co1-u-v-wFeuCuvZrw)z, wherein x=0.00~0.40, y=0.00~0.03, u=0.10~0.20, v=0.06
~0.10, w=0.02~0.04, z=7.4~7.8.Z is magnesium-yttrium-transition metal and rare earth ratio.Wherein add Er elements
The residual magnetism temperature coefficient of magnet can be reduced, addition La elements can regulate and control the microstructure of magnet, and then magnet is kept
Higher coercivity.
The permanent-magnet material is Sm1-x-yErxLay(Co1-u-v-wFeuCuvZrw)z, wherein x=0.00~0.40, y=0.00
~0.03, u=0.10~0.20, v=0.06~0.10, w=0.02~0.04, z=7.4~7.8.
The permanent-magnet material is Sm0.9Er0.09La0.01(Co0.727Fe0.16Cu0.08Zr0.033)7.6；Or Sm0.8Er0.18La0.02
(Co0.727Fe0.16Cu0.08Zr0.033)7.6；Or Sm0.7Er0.27La0.03(Co0.727Fe0.16Cu0.08Zr0.033)7.6。
A kind of method for the new type high temperature samarium-cobalt permanent-magnetic material for preparing low residual magnetism temperature coefficient, using vacuum arc melting,
Ball powder-grinding, magnetic field orientating shaping, isostatic cool pressing, sintering, timeliness and aging technique, the height with low residual magnetism temperature coefficient is made
Warm permanent-magnet material.
As shown in figure 1, under the present invention includes with low residual magnetism temperature coefficient high temperature samarium-cobalt permanent-magnetic material preparation method
Row step：
The first step：Prepare target component foundry alloy
Use purity for 99.95% rare earth element Sm, Er, purity be 99.9% Co, purity be 99.9% Fe,
Cu, Zr element are configured to the foundry alloy of target component；
In the present invention, target component refers to according to chemical formula Sm1-x-yErxLay(Co1-u-v-wFeuCuvZrw)zMiddle requirement
Atom number carries out proportioning and weighs each element simple substance.
In the present invention, the purity of each element is mass percent purity.
Second step：Melting ingot casting
The target component foundry alloy that the first step is prepared is put in the water jacketed copper crucible of vacuum arc melting furnace, adjusts vacuum
The vacuum of room reaches 2 × 10-3~4 × 10-3Pa, high-purity hydrogen is then filled to -0.1 × 105~-0.3 × 105Pa, working
Electric arc melting 20~70 seconds under the conditions of voltage 30V~45V, operating current 630A~750A, after alloying element is completely melt, break
Arc forms alloy pig；Alloy pig is overturn, melt back 3~5 times, the uniform Sm of composition is made1-x-yErxLay(Co1-u-v- wFeuCuvZrw)zAlloy pig；
3rd step：Coarse crushing and ball milling
Filled with high-purity hydrogen to 0.1x105In Pa glove box, by Sm made from second step1-x-yErxLay(Co1-u-v- wFeuCuvZrw)zAlloy pig sieves after being smashed to pieces with iron mortar, obtains particle size<1.0mm coarse powder, is then existed using ball mill
120~180mins of ball milling under gasoline media protection, obtain the Sm that particle diameter is 3~5um1-x-yErxLay(Co1-u-v-wFeuCuvZrw)z
Powder；
The weight ratio of ball material is 8 in mechanical milling process:1~12:1；
Steel ball is using the spheroid of two kinds of different-diameters, a diameter of 10mm of A steel balls, a diameter of 5mm of B steel balls；
4th step：Pressing under magnetic field and isostatic pressed
Powder made from 3rd step is put into oriented moulding in magnetic field orientating forming machine, magnetic field size is 2T, will be orientated to
Magnetic base substrate after type is wrapped with preservative film, is put into isostatic pressing machine, is suppressed manually using 46# hydraulic oil as medium
200MPa, pressure 1h is kept to take out magnet base substrate；
5th step：Sintering and heat treatment
By Sm made from the 4th step1-x-yErxLay(Co1-u-v-wFeuCuvZrw)zBase substrate is put into the burner hearth of vacuum heat treatment furnace
It is interior, vacuum is adjusted in vacuum heat treatment furnace to 2 × 10-3~4 × 10-3Pa, high-purity hydrogen is passed through to -0.1 × 105~-0.3 ×
105Pa, after sintering 60~120mins at a temperature of 1175 DEG C~1200 DEG C, Sm is made1-x-yErxLay(Co1-u-v- wFeuCuvZrw)zAlloy；Then the alloy is put into quenching-in water under the conditions of hydrogen shield, being made has Th2Ni17Structure
SmCo2:17 single-phase alloys；Then 8~12h is incubated under 800~850 DEG C of high temperature, then with 0.5~0.7 DEG C/min speed
400 DEG C are slowly cooled to, insulation 9-11h quenchings, is taken out within preferably 10 hours, that is, being made has the low remanent magnetism temperature of nanometer cell structure
The high temperature permanent magnetic material of coefficient.
In four steps, handled by high temperature sintering and secondary time effect is handled, realized Sm1-x-yErxLay
(Co1-u-v-wFeuCuvZrw)zRedistribution of element inside powder, from prepared by average cell footpath 100nm or so refinement nanometer
Cell structure.
In 3rd step, the weight ratio of ball and material is 6 in mechanical milling process:1~14:1, preferably 8:1~12:1.
In 3rd step, steel ball is using the spheroid of two kinds of different-diameters, a diameter of 10mm of A steel balls, the diameter of B steel balls
For 5mm, drawn using both balls by Process Exploration, the powder that both balls prepare out is more preferable.
Using Sm made from the above method1-x-yErxLay(Co1-u-v-wFeuCuvZrw)zThe new height of low residual magnetism temperature coefficient
Warm permanent-magnet material, its room temperature residual magnetic flux density are 8000-10000Gs；400 DEG C of residual magnetic flux densities are 7000-
8000Gs。
Using Sm made from the above method1-x-yErxLay(Co1-u-v-wFeuCuvZrw)zThe new height of low residual magnetism temperature coefficient
Warm permanent-magnet material, its room temperature HCJ are 20000-27000Oe；400 DEG C of HCJs are 10000-12000Oe.
The permanent-magnet material 25~200 DEG C of residual magnetism temperature coefficient α for 0.012~0.015%/DEG C, at 25~300 DEG C
Residual magnetism temperature coefficient α for 0.017~0.020%/DEG C, 25~400 DEG C of residual magnetism temperature coefficient α be 0.023~
0.027%/DEG C.
The present invention compared with prior art the advantages of be：
(1) maximum operation (service) temperature of commercial samarium cobalt permanent magnet body is 300 DEG C, and the present invention is mixed by designing composition and element
Miscellaneous, optimize technique, which has been prepared, can use 400 DEG C of permanent magnet.
(2) the residual magnetism temperature coefficient α of commercial permanent magnet is big, 25~300 DEG C of residual magnetism temperature coefficient α for -0.035%/DEG C,
And the present invention is adulterated by heavy rare earth element Er and LREE La, the residual magnetism temperature coefficient α at 25~300 DEG C has been prepared
For 0.017~0.020%/DEG C.
(3) temperature range of the magnet of the low residual magnetism temperature coefficient prepared in the prior art is small, usually 25~100 DEG C,
And the present invention have low residual magnetism temperature coefficient temperature range it is big, 25~300 DEG C of residual magnetism temperature coefficient α be 0.017~
0.020%/DEG C, 25~400 DEG C of residual magnetism temperature coefficient α be 0.023~0.027%/DEG C.
Brief description of the drawings
Fig. 1 is the flow chart of preparation method of the present invention；
Fig. 2 is Sm in the present invention0.9Er0.09La0.01(Co0.727Fe0.16Cu0.08Zr0.033)7.6Magnetic property at room temperature；
Fig. 3 is Sm in the present invention0.9Er0.09La0.01(Co0.727Fe0.16Cu0.08Zr0.033)7.6Performance under 200 DEG C of magnetic；
Fig. 4 is Sm in the present invention0.8Er0.18La0.02(Co0.727Fe0.16Cu0.08Zr0.033)7.6Magnetic property at room temperature；
Fig. 5 is Sm in the present invention0.8Er0.18La0.02(Co0.727Fe0.16Cu0.08Zr0.033)7.6Magnetic property at 300 DEG C；
Fig. 6 is Sm in the present invention0.7Er0.27La0.03(Co0.727Fe0.16Cu0.08Zr0.033)7.6Magnetic property at room temperature
Fig. 7 is Sm in the present invention0.7Er0.27La0.03(Co0.727Fe0.16Cu0.08Zr0.033)7.6Magnetic property at 400 DEG C.
Embodiment
Below in conjunction with the accompanying drawings and the present invention is discussed in detail in specific embodiment.But following embodiment is only limitted to explain this hair
Bright, protection scope of the present invention should include the full content of claim, be not limited only to the present embodiment.
Embodiment 1：Sm processed0.9Er0.09La0.01(Co0.727Fe0.16Cu0.08Zr0.033)7.6With low residual magnetism temperature coefficient high temperature
Use samarium-cobalt permanent-magnetic material
The first step：Prepare target component foundry alloy
Using rare earth element Sm, Er of purity 99.95%, La, purity 99.9% Co, Fe, Cu, Zr, press
Sm0.9Er0.09La0.01(Co0.727Fe0.16Cu0.08Zr0.033)7.6Chemical formula alloyage, alloy gross mass are 482.5276g, are used
Electronic balance accurate weighing 110.5180g Sm, 13.5370g Er, 1.1379g La, 258.1952g Co, 53.7389g
Fe, 30.6238g Cu, 18.1273g Zr.
Second step：Melting ingot casting
The target component foundry alloy that the first step is prepared is put in the water jacketed copper crucible of vacuum arc melting furnace, adjusts vacuum
The vacuum of room reaches 2 × 10-3~4 × 10-3Pa, high-purity hydrogen is then filled to -0.1 × 105~-0.3 × 105Pa, working
20~70s of electric arc melting under the conditions of voltage 30V~45V, operating current 630A~750A, after alloying element is completely melt, break
Arc forms alloy pig；Alloy pig is overturn, melt back 3~5 times, the uniform Sm of composition is made0.9Er0.09La0.01
(Co0.727Fe0.16Cu0.08Zr0.033)7.6Alloy pig；
3rd step：Coarse crushing and ball milling
Filled with high-purity hydrogen to 0.1x105In Pa glove box, by Sm made from second step0.9Er0.09La0.01
(Co0.727Fe0.16Cu0.08Zr0.033)7.6Alloy pig sieves after being smashed to pieces with iron mortar, obtains particle size<1.0mm coarse powder, so
Ball mill 120~180mins of ball milling under gasoline media protection is used afterwards, obtains the Sm that particle diameter is 3~5um0.9Er0.09La0.01
(Co0.727Fe0.16Cu0.08Zr0.033)7.6Powder；
The weight ratio of ball material is 8 in mechanical milling process:1~12:1；
Steel ball is using the spheroid of two kinds of different-diameters, a diameter of 10mm of A steel balls, a diameter of 5mm of B steel balls；
4th step：Pressing under magnetic field and isostatic pressed
Powder made from 3rd step is put into oriented moulding in magnetic field orientating forming machine, magnetic field size is 2T, will be orientated to
Magnetic base substrate after type is wrapped with preservative film, is put into isostatic pressing machine, is suppressed manually using 46# hydraulic oil as medium
200MPa, pressure 1h is kept to take out magnet base substrate；
5th step：Sintering and heat treatment
By Sm made from the 4th step0.9Er0.09La0.01(Co0.727Fe0.16Cu0.08Zr0.033)7.6Base substrate is put into vacuum heat
In the burner hearth of stove, vacuum is adjusted in vacuum heat treatment furnace to 2 × 10-3~4 × 10-3Pa, high-purity hydrogen is passed through to 0.1 × 105
~0.8 × 105Pa, after sintering 60~120mins at a temperature of 1175 DEG C~1200 DEG C, it is made -0.1 × 105~-0.3 ×
105Pa alloys；Then the alloy is put into quenching-in water under the conditions of hydrogen shield, being made has Th2Ni17The SmCo2 of structure:
17 single-phase alloys；Then 8~12h is incubated under 800~850 DEG C of high temperature, it is then slowly cold with 0.5~0.7 DEG C/min speed
But to 400 DEG C, insulation 10h quenchings, take out, that is, the high temperature permanent magnetic material with low residual magnetism temperature coefficient is made.
The magnetic property of 25 DEG C and 200 DEG C of sample is measured with permanent-magnet material superhigh temperature measuring system NIM-500C, demagnetization is bent
Line is shown in accompanying drawing 2 and 3, and magnetic property data are shown in Table 1.Wherein Br is remanent magnetism, and unit is Gauss, is represented with Gs, and Hcj is intrinsic coercive
Power, unit are oersted, are represented with Oe, and (BH) max is maximum magnetic energy product, and unit is person's Gauss oersted, is represented with GOe.
Table 1.Sm0.9Er0.09La0.01(Co0.727Fe0.16Cu0.08Zr0.033)7.6Magnetic property and residual magnetism temperature coefficient
Embodiment 2：Sm processed0.8Er0.18La0.02(Co0.727Fe0.16Cu0.08Zr0.033)7.6With low residual magnetism temperature coefficient high temperature
Use samarium-cobalt permanent-magnetic material
The first step：Prepare target component foundry alloy
Using rare earth element Sm, Er of purity 99.95%, Co, Fe, Cu, Zr of purity 99.9%, press
Sm0.8Er0.18La0.02(Co0.727Fe0.16Cu0.08Zr0.033)7.6Chemical formula alloyage, alloy gross mass are 496.9990g, are used
The Sm of electronic balance accurate weighing 100.6302,27.1477g Er, 2.3313g La, 264.5804g Co, 55.1414g
Fe, 31.3976g Cu, 18.5958g Zr.
Second step：Melting ingot casting
The target component foundry alloy that the first step is prepared is put in the water jacketed copper crucible of vacuum arc melting furnace, adjusts vacuum
The vacuum of room reaches 2 × 10-3~4 × 10-3Pa, high-purity hydrogen is then filled to -0.1 × 105~-0.3 × 105Pa, working
20~70s of electric arc melting under the conditions of voltage 30V~45V, operating current 630A~750A, after alloying element is completely melt, break
Arc forms alloy pig；Alloy pig is overturn, melt back 3~5 times, the uniform Sm of composition is made0.8Er0.18La0.02
(Co0.727Fe0.16Cu0.08Zr0.033)7.6Alloy pig；
3rd step：Coarse crushing and ball milling
Filled with high-purity hydrogen to 0.1x105In Pa glove box, by Sm made from second step0.8Er0.18La0.02
(Co0.727Fe0.16Cu0.08Zr0.033)7.6Alloy pig sieves after being smashed to pieces with iron mortar, obtains particle size<1.0mm coarse powder, so
Ball mill 120~180mins of ball milling under gasoline media protection is used afterwards, obtains the Sm that particle diameter is 3~5um0.8Er0.18La0.02
(Co0.727Fe0.16Cu0.08Zr0.033)7.6Powder；
The weight ratio of ball material is 8 in mechanical milling process:1~12:1；
Steel ball is using the spheroid of two kinds of different-diameters, a diameter of 10mm of A steel balls, a diameter of 5mm of B steel balls；
4th step：Pressing under magnetic field and isostatic pressed
Powder made from 3rd step is put into oriented moulding in magnetic field orientating forming machine, magnetic field size is 2T, will be orientated to
Magnetic base substrate after type is wrapped with preservative film, is put into isostatic pressing machine, is suppressed manually using 46# hydraulic oil as medium
200MPa, pressure 1h is kept to take out magnet base substrate；
5th step：Sintering and heat treatment
By Sm made from the 4th step0.8Er0.18La0.02(Co0.727Fe0.16Cu0.08Zr0.033)7.6Base substrate is put into vacuum heat
In the burner hearth of stove, vacuum is adjusted in vacuum heat treatment furnace to 2 × 10-3~4 × 10-3Pa, high-purity hydrogen is passed through to -0.1 × 105
~-0.3 × 105Pa, after sintering 60~120mins at a temperature of 1175 DEG C~1200 DEG C, Sm is made0.8Er0.18La0.02
(Co0.727Fe0.16Cu0.08Zr0.033)7.6Alloy；Then the alloy is put into quenching-in water under the conditions of hydrogen shield, tool is made
There is Th2Ni17The SmCo2 of structure:17 single-phase alloys；Then 8~12h is incubated under 800~850 DEG C of high temperature, then with 0.5~
0.7 DEG C/min speed slowly cools to 400 DEG C, insulation 10h quenchings, takes out, that is, the height with low residual magnetism temperature coefficient is made
Warm permanent-magnet material.
The magnetic property of 25 DEG C and 300 DEG C of sample is measured with permanent-magnet material superhigh temperature measuring system NIM-500C, demagnetization is bent
Line is shown in attached Figure 4 and 5, and magnetic property data are shown in Table 2.Wherein Br is remanent magnetism, and unit is Gauss, is represented with Gs, and Hcj is intrinsic coercive
Power, unit are oersted, are represented with Oe, and (BH) max is maximum magnetic energy product, and unit is Gauss oersted, is represented with GOe..
Table 2.Sm0.8Er0.18La0.02(Co0.727Fe0.16Cu0.08Zr0.033)7.6Magnetic property and residual magnetism temperature coefficient
Embodiment 3：Sm processed0.7Er0.27La0.03(Co0.727Fe0.16Cu0.08Zr0.033)7.6With low residual magnetism temperature coefficient high temperature
Use samarium-cobalt permanent-magnetic material
The first step：Prepare target component foundry alloy
Using rare earth element Sm, Er of purity 99.95%, La, purity 99.9% Co, Fe, Cu, Zr, press
Sm0.7Er0.27La0.03(Co0.727Fe0.16Cu0.08Zr0.033)7.6Chemical formula alloyage, alloy gross mass are 542.0294g, are used
Electronic balance accurate weighing 95.4715g Sm, 44.7627g Er, 3.7916g La, 287.0876g Co, 59.8626g
Fe, 34.0675g Cu, 20.1261g Zr.
Second step：Melting ingot casting
The target component foundry alloy that the first step is prepared is put in the water jacketed copper crucible of vacuum arc melting furnace, adjusts vacuum
The vacuum of room reaches 2 × 10-3~4 × 10-3Pa, high-purity hydrogen is then filled to -0.1 × 105~-0.3 × 105Pa, working
Electric arc melting 20~70 seconds under the conditions of voltage 30V~45V, operating current 630A~750A, after alloying element is completely melt, break
Arc forms alloy pig；Alloy pig is overturn, melt back 3~5 times, the uniform Sm of composition is made0.7Er0.27La0.03
(Co0.727Fe0.16Cu0.08Zr0.033)7.6Alloy pig；
3rd step：Coarse crushing and ball milling
Filled with high-purity hydrogen to 0.1x105In Pa glove box, by Sm made from second step0.7Er0.27La0.03
(Co0.727Fe0.16Cu0.08Zr0.033)7.6Alloy pig sieves after being smashed to pieces with iron mortar, obtains particle size<1.0mm coarse powder, so
Ball mill 120~180mins of ball milling under gasoline media protection is used afterwards, obtains the Sm that particle diameter is 3~5um0.7Er0.27La0.03
(Co0.727Fe0.16Cu0.08Zr0.033)7.6Powder；
The weight ratio of ball material is 8 in mechanical milling process:1~12:1；
Steel ball is using the spheroid of two kinds of different-diameters, a diameter of 10mm of A steel balls, a diameter of 5mm of B steel balls；
4th step：Pressing under magnetic field and isostatic pressed
Powder made from 3rd step is put into oriented moulding in magnetic field orientating forming machine, magnetic field size is 2T, will be orientated to
Magnetic base substrate after type is wrapped with preservative film, is put into isostatic pressing machine, is suppressed manually using 46# hydraulic oil as medium
200MPa, pressure 1h is kept to take out magnet base substrate；
5th step：Sintering and heat treatment
By Sm made from the 4th step0.7Er0.27La0.03(Co0.727Fe0.16Cu0.08Zr0.033)7.6Base substrate is put into vacuum heat
In the burner hearth of stove, vacuum is adjusted in vacuum heat treatment furnace to 2 × 10-3~4 × 10-3Pa, high-purity hydrogen is passed through to -0.1 × 105
~-0.3 × 105Pa, after sintering 60~120mins at a temperature of 1175 DEG C~1200 DEG C, Sm is made0.7Er0.27La0.03
(Co0.727Fe0.16Cu0.08Zr0.033)7.6Alloy；Then the alloy is put into quenching-in water under the conditions of hydrogen shield, tool is made
There is Th2Ni17The SmCo2 of structure:17 single-phase alloys；Then 8~12h is incubated under 800~850 DEG C of high temperature, then with 0.5~
0.7 DEG C/min speed slowly cools to 400 DEG C, insulation 10h quenchings, takes out, that is, the height with low residual magnetism temperature coefficient is made
Warm permanent-magnet material.
The magnetic property of 25 DEG C and 400 DEG C of sample is measured with permanent-magnet material superhigh temperature measuring system NIM-500C, demagnetization is bent
Line is shown in accompanying drawing 6 and 7, and magnetic property data are shown in Table 3.Wherein Br is remanent magnetism, and unit is Gauss, is represented with Gs, and Hcj is intrinsic coercive
Power, unit are oersted, are represented with Oe, and (BH) max is maximum magnetic energy product, and unit is Gauss oersted, is represented with GOe.
Table 3.Sm0.7Er0.27La0.03(Co0.727Fe0.16Cu0.08Zr0.033)7.6Magnetic property and residual magnetism temperature coefficient
In a word, by examples above as can be seen that the present invention by adding heavy rare earth element Er, while adjusting component,
Optimize Technology for Heating Processing, prepared in 25~200 DEG C of temperature ranges, residual magnetism temperature coefficient α be -0.014%/DEG C, 25
Within the temperature range of~300 DEG C, residual magnetism temperature coefficient α be 0.019%/DEG C, within the temperature range of 25~400 DEG C, remanent magnetism temperature
Spend factor alpha be 0.025%/DEG C.
It should be noted that according to the various embodiments described above of the present invention, those skilled in the art are can to realize this hair completely
The content of the four corner of bright independent claims and appurtenance, implementation process and the same the various embodiments described above of method；And this hair
Bright do not elaborate partly belongs to techniques well known.
It is described above, part embodiment only of the present invention, but protection scope of the present invention is not limited thereto, and is appointed
What those skilled in the art the invention discloses technical scope in, the change or replacement that can readily occur in should all be covered
Within protection scope of the present invention.
Claims (10)
1. one kind has low residual magnetism temperature coefficient high temperature samarium-cobalt permanent-magnetic material, it is characterised in that：The chemistry of the permanent-magnet material
Formula is Sm1-x-yErxLay(Co1-u-v-wFeuCuvZrw)z, wherein atom number ratio is：X=0.00~0.40, y=0.00~
0.03, u=0.10~0.20, v=0.06~0.10, w=0.02~0.04, z=7.4~7.8.
2. according to claim 1 have low residual magnetism temperature coefficient high temperature samarium-cobalt permanent-magnetic material, it is characterised in that：It is described
Permanent-magnet material is Sm1-x-yErxLay(Co1-u-v-wFeuCuvZrw)z, wherein x=0.1~0.20, y=0.00~0.03, u=0.15
~0.17, v=0.07~0.09, w=0.030~0.035, z=7.5~7.6.
3. according to claim 1 have low residual magnetism temperature coefficient high temperature samarium-cobalt permanent-magnetic material, it is characterised in that：It is described
Permanent-magnet material is Sm0.9Er0.09La0.01(Co0.727Fe0.16Cu0.08Zr0.033)7.6；Or Sm0.8Er0.18La0.02
(Co0.727Fe0.16Cu0.08Zr0.033)7.6；Or Sm0.7Er0.27La0.03(Co0.727Fe0.16Cu0.08Zr0.033)7.6。
4. according to claim 1 have low residual magnetism temperature coefficient high temperature samarium-cobalt permanent-magnetic material, it is characterised in that：It is described
Permanent-magnet material is 8000-10000Gs in room temperature residual magnetic flux density；400 DEG C of residual magnetic flux densities of high temperature are 7000-
8000Gs。
5. according to claim 1 have low residual magnetism temperature coefficient high temperature samarium-cobalt permanent-magnetic material, it is characterised in that：It is described
Permanent-magnet material is 20000-27000Oe in room temperature HCJ；400 DEG C of HCJs of high temperature are 10000-12000Oe.
6. according to claim 1 have low residual magnetism temperature coefficient high temperature samarium-cobalt permanent-magnetic material, it is characterised in that：It is described
Permanent-magnet material 25~200 DEG C of residual magnetism temperature coefficient α for 0.012~0.015%/DEG C, in 25~300 DEG C of remanent magnetism temperature system
Number α be 0.017~0.020%/DEG C, 25~400 DEG C of residual magnetism temperature coefficient α be 0.023~0.027%/DEG C.
7. a kind of as described in claim 1-6 is one of any there is low residual magnetism temperature coefficient high temperature to be prepared with samarium-cobalt permanent-magnetic material
Method, it is characterised in that：Comprise the following steps：
The first step：Prepare target component foundry alloy
Use Fe, Cu that Co, purity that purity is 99.9% for 99.95% rare earth element Sm, Er, La, purity are 99.9%,
Zr elements are configured to the foundry alloy of target component；
Target component refers to according to chemical formula Sm1-x-yErxLay(Co1-u-v-wFeuCuvZrw)zThe atom number of middle requirement is matched somebody with somebody
Than weighing each element simple substance；
Second step：Melting ingot casting
The target component foundry alloy that the first step is prepared is put in the water jacketed copper crucible of vacuum arc melting furnace, adjusts vacuum chamber
Vacuum reaches 2 × 10-3~4 × 10-3Pa, high-purity hydrogen is then filled to -0.1 × 105~-0.3 × 105Pa, in operating voltage
20~70s of electric arc melting under the conditions of 30V~45V, operating current 630A~750A, after alloying element is completely melt, current interruption shape
Into alloy pig；Alloy pig is overturn, melt back, the uniform Sm of composition is made1-x-yErxLay(Co1-u-v-wFeuCuvZrw)zAlloy
Ingot；
3rd step：Coarse crushing and ball milling
Filled with high-purity hydrogen to 0.1x105In Pa glove box, by Sm made from second step1-x-yErxLay(Co1-u-v- wFeuCuvZrw)zAlloy pig sieves after being smashed to pieces with iron mortar, obtains particle size<1.0mm coarse powder, is then existed using ball mill
120~180mins of ball milling under gasoline media protection, obtain the Sm that particle diameter is 3~5um1-x-yErxLay(Co1-u-v-wFeuCuvZrw)z
Powder；
4th step：Pressing under magnetic field and isostatic pressed
Powder made from 3rd step is put into oriented moulding in magnetic field orientating forming machine, magnetic field size is 2T, after oriented moulding
Magnetic base substrate wrapped with preservative film, be put into isostatic pressing machine, 200MPa suppressed manually by medium of 46# hydraulic oil, protect
Hold pressure 1h and take out magnet base substrate；
5th step：Sintering and heat treatment
By Sm made from the 4th step1-x-yErxLay(Co1-u-v-wFeuCuvZrw)zBase substrate is put into the burner hearth of vacuum heat treatment furnace, is adjusted
Vacuum is saved in vacuum heat treatment furnace to 2 × 10-3~4 × 10-3Pa, high-purity hydrogen is passed through to -0.1 × 105~-0.3 ×
105Pa, after sintering 60~120mins at a temperature of 1175 DEG C~1200 DEG C, Sm is made1-x-yErxLay(Co1-u-v- wFeuCuvZrw)zAlloy；Then the alloy is put into quenching-in water under the conditions of hydrogen shield, being made has Th2Ni17Structure
SmCo2:17 single-phase alloys；Then 8~12h is incubated under 800~850 DEG C of high temperature, then with 0.5~0.7 DEG C/min speed
400 DEG C are slowly cooled to, insulation 9-11 hours quench, and quench within preferably 10 hours, and being made after taking-up has nanometer cell structure
The high temperature permanent magnetic material of low residual magnetism temperature coefficient.
8. preparation method according to claim 7, it is characterised in that：In 3rd step, ball and material in mechanical milling process
Weight ratio is 6:1~14:1, preferably 8:1~12:1.
9. preparation method according to claim 7, it is characterised in that：In 3rd step, steel ball is straight using two kinds of differences
The spheroid in footpath, a diameter of 10mm of A steel balls, a diameter of 5mm of B steel balls.
10. preparation method according to claim 7, it is characterised in that：In 3rd step, melt back 3~5 times.
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