CN115410785A - Coating for surface protection of samarium-cobalt permanent magnet material and protection method for surface of samarium-cobalt permanent magnet material - Google Patents
Coating for surface protection of samarium-cobalt permanent magnet material and protection method for surface of samarium-cobalt permanent magnet material Download PDFInfo
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- CN115410785A CN115410785A CN202110577559.0A CN202110577559A CN115410785A CN 115410785 A CN115410785 A CN 115410785A CN 202110577559 A CN202110577559 A CN 202110577559A CN 115410785 A CN115410785 A CN 115410785A
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- 239000000463 material Substances 0.000 title claims abstract description 117
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 title claims abstract description 92
- KPLQYGBQNPPQGA-UHFFFAOYSA-N cobalt samarium Chemical compound [Co].[Sm] KPLQYGBQNPPQGA-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000000576 coating method Methods 0.000 title claims description 78
- 239000011248 coating agent Substances 0.000 title claims description 77
- 229910052751 metal Inorganic materials 0.000 claims abstract description 43
- 239000002184 metal Substances 0.000 claims abstract description 43
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 18
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 11
- 239000000956 alloy Substances 0.000 claims abstract description 11
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 9
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims abstract description 8
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001936 tantalum oxide Inorganic materials 0.000 claims abstract description 8
- 238000007747 plating Methods 0.000 claims description 57
- 238000004544 sputter deposition Methods 0.000 claims description 34
- 238000000151 deposition Methods 0.000 claims description 25
- 238000004140 cleaning Methods 0.000 claims description 19
- 238000007733 ion plating Methods 0.000 claims description 15
- 239000013077 target material Substances 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims 1
- 238000009792 diffusion process Methods 0.000 abstract description 14
- 238000005253 cladding Methods 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 5
- 239000010410 layer Substances 0.000 description 60
- 229910052761 rare earth metal Inorganic materials 0.000 description 31
- 150000002910 rare earth metals Chemical class 0.000 description 30
- 230000002829 reductive effect Effects 0.000 description 24
- 230000008569 process Effects 0.000 description 21
- 238000005245 sintering Methods 0.000 description 20
- 238000010438 heat treatment Methods 0.000 description 19
- 230000008021 deposition Effects 0.000 description 15
- 230000000694 effects Effects 0.000 description 15
- 238000012360 testing method Methods 0.000 description 14
- 229910052772 Samarium Inorganic materials 0.000 description 12
- 229910004168 TaNb Inorganic materials 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- 230000032683 aging Effects 0.000 description 11
- 239000000843 powder Substances 0.000 description 11
- 238000003723 Smelting Methods 0.000 description 10
- 229910017052 cobalt Inorganic materials 0.000 description 10
- 239000010941 cobalt Substances 0.000 description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 10
- 239000002131 composite material Substances 0.000 description 10
- 238000000465 moulding Methods 0.000 description 10
- 238000012545 processing Methods 0.000 description 10
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 10
- 238000003801 milling Methods 0.000 description 9
- 238000005406 washing Methods 0.000 description 9
- 239000010949 copper Substances 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 239000000696 magnetic material Substances 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 6
- 229910002056 binary alloy Inorganic materials 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
- 229910052726 zirconium Inorganic materials 0.000 description 6
- 238000005554 pickling Methods 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 229910052777 Praseodymium Inorganic materials 0.000 description 4
- 239000011247 coating layer Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 229910052758 niobium Inorganic materials 0.000 description 4
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 4
- 238000001755 magnetron sputter deposition Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 1
- VWVRASTUFJRTHW-UHFFFAOYSA-N 2-[3-(azetidin-3-yloxy)-4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]pyrazol-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound O=C(CN1C=C(C(OC2CNC2)=N1)C1=CN=C(NC2CC3=C(C2)C=CC=C3)N=C1)N1CCC2=C(C1)N=NN2 VWVRASTUFJRTHW-UHFFFAOYSA-N 0.000 description 1
- XYLOFRFPOPXJOQ-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-3-(piperazine-1-carbonyl)pyrazol-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound O=C(Cn1cc(c(n1)C(=O)N1CCNCC1)-c1cnc(NC2Cc3ccccc3C2)nc1)N1CCc2n[nH]nc2C1 XYLOFRFPOPXJOQ-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- NDYCBWZIOSTTHS-UHFFFAOYSA-N cobalt samarium Chemical compound [Co].[Co].[Co].[Co].[Co].[Sm] NDYCBWZIOSTTHS-UHFFFAOYSA-N 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000001540 jet deposition Methods 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 238000010405 reoxidation reaction Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 229910002058 ternary alloy Inorganic materials 0.000 description 1
Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/0551—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0552—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 in the form of particles, e.g. rapid quenched powders or ribbon flakes with a protective layer
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/026—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets protecting methods against environmental influences, e.g. oxygen, by surface treatment
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The application discloses a cladding material that is used for samarium cobalt permanent magnet material surface to protect and samarium cobalt permanent magnet material surface's protection method, cladding material include at least one of following composition: tantalum metal Ta; tantalum oxide TaO X1 X1 is any number between 0 and 2.5; tantalum nitride TaN X2 X2 is any number between 0 and 1.6; an alloy comprising metallic tantalum Ta and a metal M, M comprising at least one of V, nb, zr, hf, cr, al, ni. The application provides a cladding material for samarium cobalt permanent-magnet material surface protection, this cladding material both can obstruct the inside element of permanent-magnet material outdiffusion, can obstruct outside O element again and to permanent-magnet material internal diffusion to improve samarium cobalt permanent-magnet material's high temperature resistance performance, restrained samarium cobalt in the magnetic performance decay of high temperature environment.
Description
Technical Field
The application relates to the technical field of materials, in particular to a plating layer for surface protection of a samarium cobalt permanent magnet material and a protection method for the surface of the samarium cobalt permanent magnet material.
Background
In the 60 s of the 20 th century, a first-generation rare earth permanent magnet material 1:5 type samarium cobalt (SmCo 5) was born, in the 70 s a second-generation rare earth permanent magnet material 2. China is the world's largest reserve and producing country of rare earth materials. After decades of development of rare earth permanent magnetic materials, the market demand has promoted the development of the technology towards high performance.
Samarium cobalt permanent magnet material is widely used in the environment of temperature above 200 ℃ because of its higher comprehensive magnetic property and excellent temperature resistance. The high-performance samarium cobalt permanent magnet material is widely applied to the fields of high-speed rails, new energy automobile motors, water pumps, sensors and the like. The low temperature coefficient permanent magnetic material is used in the fields of space satellites, aerospace and the like due to excellent temperature stability. High temperature resistant samarium cobalt permanent magnet materials have been used in environments with temperatures of 550 c.
However, samarium cobalt permanent magnet materials can suffer from magnetic property degradation when operated for a long time in an environment with a temperature of 350 ℃. The formation of the surface-aged layer is a main cause of the deterioration of magnetic properties. An oxidation-resistant, highly stable surface protective coating is an effective method for inhibiting the formation of surface-aged layers.
Content of application
The application provides a cladding material and samarium cobalt permanent-magnet material surface's protection method that is used for samarium cobalt permanent-magnet material surface to protect can improve samarium cobalt permanent-magnet material's high temperature resistance.
In a first aspect, the present application provides a coating for surface protection of a samarium cobalt permanent magnet material comprising at least one of the following:
tantalum metal Ta;
tantalum oxide TaO X1 X1 is any number between 0 and 2.5;
tantalum nitride TaN X2 X2 is any number between 0 and 1.6;
an alloy comprising metallic tantalum Ta and a metal M, M comprising at least one of V, nb, zr, hf, cr, al, ni.
Wherein the samarium cobalt permanent magnet material comprises a first generation rare earth permanent magnet material 1:5 type samarium cobalt material (SmCo) 5 ) And the second-generation rare earth permanent magnet material 2 2 Co 17 ). The material contains two basic components of Sm and Co, and also contains one or more of Fe, cu, zr, ti, si, sn, nb, V, ni, mo and B and rare earth elements of La, ce, pr, nd, er, gd, dy, ho, tb and Eu.
The metal tantalum Ta has high melting point, good toughness and excellent chemical stability, so that the metal tantalum Ta coating becomes a selection for resisting high temperature, friction and extreme chemical corrosion.
Further, the composition of the coating is one of the following components:
tantalum metal Ta;
tantalum oxide TaO X1 X1 is any number between 0 and 2.5;
tantalum nitride TaN X2 X2 is any number between 0 and 1.6;
an alloy comprising metallic tantalum Ta and a metal M, M comprising at least one of V, nb, zr, hf, cr, al, ni.
For example, the coating may be tantalum metal Ta, which is referred to as Ta coating, or tantalum oxide TaO X1 Is marked as TaO X1 And (4) plating.
In a further scheme, the alloy consists of metal tantalum Ta and metal M, wherein M comprises at least one of V, nb, zr, hf, cr, al and Ni.
For example, the composition of the plating layer may be an alloy, the alloy may be composed of metal tantalum Ta and metal Nb, in this case, the plating layer is denoted as a TaNb binary alloy plating layer, the alloy may also be composed of metal tantalum Ta, metal Zr, and metal Hf, in this case, the plating layer is denoted as a tazrf ternary alloy plating layer.
In a further aspect, the coating comprises at least one layer, wherein the layers are stacked, and each layer comprises one of the following components:
tantalum metal Ta;
tantalum oxide TaO X1 X1 is any number between 0 and 2.5;
tantalum nitride TaN X2 X2 is any number between 0 and 1.6;
the alloy comprises metal tantalum Ta and metal M, wherein M is at least one of V, nb, zr, hf, cr, al and Ni.
For example, the number of the layers may be one, two, or three.
In a further scheme, the components of each layer body are respectively one of the following components:
tantalum metal Ta;
tantalum oxide TaO X1 X1 is any number between 0 and 2.5;
tantalum nitride TaN X2 X2 is any number between 0 and 1.6;
the alloy comprises metal Ta and metal M, wherein M is at least one of V, nb, zr, hf, cr, al and Ni.
In a further aspect, the layers are of different compositions.
For example, the number of the layers may be two, which are respectively referred to as a first layer and a second layer covering the first layer, and the composition of the first layer may be tantalum nitride TaN X2 The second layer may be Ta metal and the coating layer may be TaN X2 And + Ta composite coating.
In a further scheme, the metal tantalum Ta is in an alpha phase or a beta phase. Metallic tantalum Ta coatings deposited at room temperature generally exhibit a tetragonal phase structure (beta phase,
) The beta-phase tantalum Ta coating is very hard but very brittle, often resulting in high coating stress. The thermodynamically stable phase of Ta is a bcc structure (alpha phase,
) High toughness and good ductility, and is an ideal plating layer.
In a further proposal, the total thickness of the plating layer is 0.5 to 200 μm.
In a second aspect, the application provides a method for protecting a surface of a samarium cobalt permanent magnet material, comprising the steps of:
the plating of any of the embodiments described above is deposited on the surface of a samarium cobalt permanent magnet material.
Further, the plating layer is deposited by sputtering plating, ion plating or spraying.
In a further scheme, before sputtering plating, the target material for sputtering plating is cleaned, the working air pressure is 0.1-5 Pa, and the sputtering power per unit target area is 0.1-15W/cm 2 The cleaning time is more than or equal to 1min.
Further, when sputtering plating is carried out, the working air pressure is 0.1-5 Pa, and the sputtering power per unit target area is 0.1-15W/cm 2 And applying a bias voltage of-400 to-1V.
According to the further scheme, before sputtering plating, the target material for sputtering plating is cleaned, and the samarium cobalt permanent magnet material is subjected to acid washing, water washing and drying.
In a further scheme, before ion plating, the target material for ion plating is cleaned, the working air pressure is 0.5-5 Pa, and the current density of the unit target area is 0.5-5A/cm 2 The cleaning time is more than or equal to 1min.
In the further proposal, when the ion plating is carried out, the working air pressure is 0.5 to 5Pa, and the current density per unit target area is 0.5 to 5A/cm 2 And applying a bias voltage of-400 to-1V.
According to the further scheme, before ion plating, the target material subjected to ion plating is cleaned, and the samarium cobalt permanent magnet material is subjected to acid washing, water washing and drying.
Compared with the prior art, the coating has the following beneficial effects:
the application provides a cladding material for samarium cobalt permanent-magnet material surface protection, this cladding material both can obstruct the inside element of permanent-magnet material outdiffusion, can obstruct outside O element again and to permanent-magnet material internal diffusion to improve samarium cobalt permanent-magnet material's high temperature resistance performance, restrained samarium cobalt in the magnetic performance decay of high temperature environment.
Drawings
FIG. 1 shows Sm with a Ta coating 2 Co 17 Structure of the cross section of permanent magnetic material.
Detailed description of the preferred embodiment
In order to make the objects, technical solutions and advantages of the present application more apparent, the present application is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present application and are not intended to limit the present application.
Example 1
The selected samarium cobalt permanent magnet material is as follows:
first-generation rare earth permanent magnet material 1:5 samarium cobalt (sintered SmCo) 5 ) The mark is 22, and the main components are as follows: sm (rare earth metal samarium), pr (rare earth metal praseodymium), co (metal cobalt). Sintered SmCo 5 By adopting a powder sintering process, the process flow can be summarized as smelting, milling, molding, sintering, detecting and processing.
The selected plating layer is as follows:
ta coating, wherein Ta is an alpha phase.
The steps of depositing the coating are as follows:
(1) Two Ta targets (with purity of 99.95%) were mounted on a magnetron sputtering source in a vacuum chamber, and the angle between the Ta targets and the horizontal plane of the sample turntable was adjusted to 45 °.
(2) Samarium cobalt permanent magnet material is placed on the sample carousel after pickling, washing, drying.
(3) Firstly, using a mechanical pump to pre-pump vacuum to a vacuum degree of less than 20pa in the vacuum chamber, and then using a molecular pump to pump vacuum to make the vacuum degree in the vacuum chamber reach 8.0 × 10- 4 Pa or less.
(4) Cleaning the Ta target under the following conditions: ar (with the purity of 99.999 percent) is adopted as working gas, the working pressure is controlled to be 0.5Pa, and the sputtering power of unit target area is 2W/cm 2 The cleaning time is 30min.
(5) Carrying out sputtering deposition on samarium cobalt permanent magnet material, wherein the deposition conditions are as follows: ar (purity is 99.999%) is used as working gas, the working pressure is controlled to be 0.5Pa, and the sputtering power per unit target area is 4W/cm 2 A bias voltage of-100V was applied, the substrate temperature was adjusted to 400 ℃ with a built-in heater, and the deposition thickness was controlled to 4 μm, thereby depositing a Ta plating layer.
Example 2
The only difference from example 1 is that samarium cobalt permanent magnet material was chosen as:
second-generation rare earth permanent magnet material 2 2 Co 17 ) The brand is 26H, and the components are as follows: sm (rare earth metal samarium), co (metal cobalt), cu (metal copper), fe (metal iron), zr (subgroup element zirconium). Sintered Sm 2 Co 17 Adopts a powder sintering process, and the process flow canThe method comprises the steps of smelting, powder making, molding, sintering, detecting and processing.
Example 3
The selected samarium cobalt permanent magnet material is as follows:
first-generation rare earth permanent magnet material 1:5 samarium cobalt (sintered SmCo) 5 ) The mark is 22, and the main components are as follows: sm (rare earth metal samarium), pr (rare earth metal praseodymium), co (metal cobalt). Sintered SmCo 5 By adopting a powder sintering process, the process flow can be summarized as smelting, milling, molding, sintering, detecting and processing.
The selected plating layers are as follows:
ta coating layer, ta is alpha phase.
The steps of depositing the coating are as follows:
(1) Two Ta arc targets (99.95% pure) were mounted on an arc source in a vacuum chamber.
(2) Samarium cobalt permanent magnet material is placed on the sample carousel after pickling, washing, drying.
(3) Firstly, using a mechanical pump to pre-pump vacuum to a vacuum degree of less than 20pa in the vacuum chamber, and then using a molecular pump to pump vacuum to make the vacuum degree in the vacuum chamber reach 8.0 × 10- 4 Pa or less.
(4) Cleaning the Ta arc target under the following conditions: ar (purity is 99.999%) is used as working gas, the working pressure is controlled to be 1Pa, and the current density per unit target area is 1A/cm 2 The cleaning time is 30min.
(5) Carrying out multi-arc deposition on a samarium cobalt permanent magnet material workpiece, wherein the deposition conditions are as follows: ar (purity is 99.999%) is used as working gas, the working pressure is controlled to be 1Pa, and the current density per unit target area is 1A/cm 2 A bias voltage of-200V was applied, the substrate temperature was adjusted to 400 ℃ with a built-in heater, and the deposition thickness was controlled to 8 μm, thereby depositing a Ta plating layer.
Example 4
The difference from example 3 is only that samarium cobalt permanent magnet material was chosen:
second-generation rare earth permanent magnet material 2 2 Co 17 ) The brand is 26H, and the components are as follows: sm (rare earth metal samarium), co (metal cobalt), cu (metal copper) and Fe are metalsIron, zr (subgroup element zirconium). Sintered Sm 2 Co 17 By adopting a powder sintering process, the process flow can be summarized as smelting, milling, molding, sintering, detecting and processing.
Example 5
The selected samarium cobalt permanent magnet material is as follows:
first-generation rare earth permanent magnet material 1:5 samarium cobalt (sintered SmCo) 5 ) The mark is 22, and the main components are as follows: sm (rare earth metal samarium), pr (rare earth metal praseodymium), co (metal cobalt). Sintered SmCo 5 By adopting a powder sintering process, the process flow can be summarized as smelting, milling, molding, sintering, detecting and processing.
The selected plating layers are as follows:
TaN X2 and + Ta composite coating, wherein Ta is an alpha phase.
The steps of depositing the coating are as follows:
(1) Two Ta targets (with purity of 99.95%) were mounted on a magnetron sputtering source in a vacuum chamber, and the angle between the Ta targets and the horizontal plane of the sample turntable was adjusted to 45 °.
(2) Samarium cobalt permanent magnet material is placed on the sample carousel after pickling, washing, drying.
(3) Firstly, using a mechanical pump to pre-pump vacuum to a vacuum degree of less than 20pa in the vacuum chamber, and then using a molecular pump to pump vacuum to make the vacuum degree in the vacuum chamber reach 8.0 × 10- 4 Pa or less.
(4) Cleaning the Ta target under the following conditions: ar (purity is 99.999%) is used as working gas, the working pressure is controlled to be 0.5Pa, and the sputtering power per unit target area is 2W/cm 2 The cleaning time is 30min.
(5) Sputtering deposition is carried out on a samarium cobalt permanent magnet material workpiece, and the deposition conditions are as follows: ar (purity 99.999%) and N are adopted 2 (purity: 99.999%) as working gas, and controlling the working gas pressure to be 0.5Pa and the deposition thickness to be 0.1 μm, thereby depositing TaN X2 And (7) plating. It should be noted that no built-in heater is required to regulate the substrate temperature.
(6) Turning off N 2 Ar (with the purity of 99.999%) is used as working gas, and the deposition thickness is controlled to be 3.9 mu m, so that the Ta coating is deposited.
Example 6
The difference from example 5 is only that samarium cobalt permanent magnet material was chosen:
second-generation rare earth permanent magnet material 2 2 Co 17 ) The brand is 26H, and the components are as follows: sm (rare earth metal samarium), co (metal cobalt) and Cu (metal copper), fe is metal iron and Zr (subgroup element zirconium). Sintered Sm 2 Co 17 By adopting a powder sintering process, the process flow can be summarized as smelting, milling, molding, sintering, detecting and processing.
Example 7
The selected samarium cobalt permanent magnet material is as follows:
the second-generation rare earth permanent magnet material 2 2 Co 17 ) The high-temperature-resistant samarium cobalt T-550 is used as a mark, the highest service temperature of the samarium cobalt reaches 550 ℃, and the samarium cobalt has the following components: sm (rare earth metal samarium), co (metal cobalt), cu (metal copper), fe (metal iron), zr (subgroup element zirconium). Sintered Sm with T-550 trademark 2 Co 17 By adopting a powder sintering process, the process flow can be summarized as smelting, milling, molding, sintering, detecting and processing.
The selected plating layer:
TaO X1 and (7) plating.
The steps of depositing the coating are as follows:
(1) Two Ta targets (with purity of 99.95%) were mounted on a magnetron sputtering source in a vacuum chamber, and the angle between the Ta targets and the horizontal plane of the sample turntable was adjusted to 45 °.
(2) Samarium cobalt permanent magnet material is placed on the sample carousel after pickling, washing, drying.
(3) Firstly, using a mechanical pump to pre-pump vacuum to a vacuum degree of less than 20pa in the vacuum chamber, and then using a molecular pump to pump vacuum to make the vacuum degree in the vacuum chamber reach 8.0 × 10- 4 Pa or less.
(4) Cleaning the Ta target under the following conditions: ar (purity is 99.999%) is used as working gas, the working pressure is controlled to be 0.5Pa, and the sputtering power per unit target area is 2W/cm 2 The cleaning time is 30min.
(5) Sputtering of samarium cobalt permanent magnet material workpiecePerforming jet deposition under the following deposition conditions: ar (purity 99.999%) and O are used 2 (purity: 99.999%) as working gas, the working gas pressure was controlled to 0.5Pa, and the deposition thickness was 2 μm, thereby depositing TaO X1 And (7) plating. It should be noted that no built-in heater is required to regulate the substrate temperature.
Example 8
The only difference from example 7 is that samarium cobalt permanent magnet material was chosen as:
second-generation rare earth permanent magnet material 2 2 Co 17 ) The brand is 26H, and the components are as follows: sm (rare earth metal samarium), co (metal cobalt), cu (metal copper), fe (metal iron), zr (subgroup element zirconium). Sintered Sm with 26H mark 2 Co 17 By adopting a powder sintering process, the process flow can be summarized as smelting, milling, molding, sintering, detecting and processing.
Example 9
The selected samarium cobalt permanent magnet material is as follows:
first-generation rare earth permanent magnet material 1:5 samarium cobalt (sintered SmCo) 5 ) The mark is 22, and the main components are as follows: sm (rare earth metal samarium), pr (rare earth metal praseodymium), and Co (metal cobalt). Sintered SmCo 5 By adopting a powder sintering process, the process flow can be summarized as smelting, milling, molding, sintering, detecting and processing.
The selected plating layers are as follows:
and (4) coating TaNb binary alloy.
The steps of depositing the coating are as follows:
(1) Two TaNb binary alloy targets (50at% Ta, 50at% Nb, purity 99.95%) were mounted on a sputtering source in a vacuum chamber, and the angle of the TaNb binary alloy target to the horizontal plane of the sample turntable was adjusted to 45 °.
(2) Samarium cobalt permanent magnet material is placed on the sample carousel after pickling, washing, drying.
(3) Firstly, using a mechanical pump to pre-pump vacuum to a vacuum degree of less than 20pa in the vacuum chamber, and then using a molecular pump to pump vacuum to make the vacuum degree in the vacuum chamber reach 8.0 × 10- 4 Pa or less.
(4) Cleaning the TaNb binary alloy target under the following conditions: miningAr (purity is 99.999%) is used as working gas, the working pressure is controlled to be 0.5Pa, and the sputtering power per unit target area is 2W/cm 2 The cleaning time is 30min.
(5) Carrying out sputtering deposition on samarium cobalt permanent magnet material, wherein the deposition conditions are as follows: ar (with the purity of 99.999 percent) is adopted as working gas, the working pressure is controlled to be 0.5Pa, and the sputtering power of unit target area is 4W/cm 2 And applying a bias voltage of-100V, heating the substrate to 400 ℃ by using a built-in heater, and controlling the deposition thickness to be 4 mu m so as to deposit the TaNb binary alloy coating.
Example 10
The only difference from example 9 is that the samarium cobalt permanent magnet material selected was:
second-generation rare earth permanent magnet material 2 2 Co 17 ) The trademark is 26H, and the components are as follows: sm (rare earth metal samarium), co (metal cobalt), cu (metal copper), fe (metal iron), zr (subgroup element zirconium). Sintered Sm 2 Co 17 By adopting a powder sintering process, the process flow can be summarized as smelting, milling, molding, sintering, detecting and processing.
Test example 1
SmCo with Ta coating of example 1 5 Permanent magnet Material, sm with Ta coating of example 2 2 Co 17 Permanent magnet material, corresponding SmCo without any coating 5 Permanent magnet material (designated as comparative example 1), corresponding Sm without any coating 2 Co 17 The permanent magnet material (marked as comparative example 2) is subjected to isothermal heat treatment under the following conditions: magnetic properties before and after heat treatment were measured at 500 ℃, in an air atmosphere, and then using a Vibrating Sample Magnetometer (VSM), and the results are shown in the following table:
SmCo with Ta coating of example 1 5 Permanent magnet material and SmCo with Ta coating of example 2 17 After the permanent magnetic material is subjected to 192 hours of heat treatment at the high temperature of 500 ℃ in an aerobic environment, the remanence (Br) is respectively reduced by-23.24 percent and 15.10 percent% of comparative example 1 SmCo without any coating 5 Permanent magnet powdering, smCo of comparative example 2 without any coating 17 The remanence of the permanent magnet material is reduced by 64.16%, so that the Ta coating has an obvious high-temperature protection effect on the samarium cobalt permanent magnet material, and the reason is that the outward diffusion of Sm and the inward diffusion of O are inhibited through the compact Ta coating, the surface aging layer is prevented from being formed, and the loss of magnetic property is reduced.
Test example 2
SmCo with Ta coating of example 3 5 Permanent magnet material, sm with Ta coating of example 4 2 Co 17 Carrying out isothermal heat treatment on the permanent magnet material, wherein the heat treatment conditions are as follows: magnetic properties before and after heat treatment were measured at 500 ℃, in an air atmosphere, and then using a Vibrating Sample Magnetometer (VSM), and the results are shown in the following table:
SmCo with Ta coating of example 3 5 Permanent magnet material and SmCo with Ta coating of example 4 17 After the permanent magnet material is subjected to 192-hour heat treatment in a high-temperature aerobic environment at 500 ℃, the remanence (Br) is respectively reduced by 19.32 percent and 10.58 percent, while the SmCo without any coating of comparative example 1 5 Permanent magnet powdering, smCo of comparative example 2 without any coating 17 The remanence of the permanent magnet material is reduced by 64.16%, so that the Ta coating has obvious high-temperature protection effect on the samarium cobalt permanent magnet material, and the reason is that the outward diffusion of Sm and the inward diffusion of O are inhibited through the compact Ta coating, the surface aging layer is prevented from being formed, and the loss of magnetic performance is reduced.
In addition, compared with the Ta plating layers in the embodiments 1 and 2, the Ta plating layers in the embodiments 3 and 4 have better high-temperature protection effect on the samarium cobalt permanent magnet material, because the embodiments 3 and 4 deposit the Ta plating layers by multi-arc ion plating, compared with the embodiments 1 and 2, the two changes are provided, firstly, the thickness is increased by 1 time and is 8 μm, and secondly, the density of the plating layers is improved by applying negative bias, and the two changes enable the Ta plating layers to have better protection effect.
Test example 3
TaN for example 5 X2 SmCo of + Ta composite coating 5 Permanent magnet material, taN of example 6 X2 Sm of + Ta composite coating 2 Co 17 Carrying out isothermal heat treatment on the permanent magnet material, wherein the heat treatment conditions are as follows: magnetic properties before and after heat treatment were measured at 500 ℃, in an air atmosphere, and then using a Vibrating Sample Magnetometer (VSM), and the results are shown in the following table:
example 5 with TaN X2 SmCo of + Ta composite coating 5 Permanent magnet material and TaN of example 6 X2 Sm of + Ta composite coating 2 Co 17 After the permanent magnet material is subjected to 192-hour heat treatment in a high-temperature aerobic environment at 500 ℃, the remanence (Br) is reduced by 22.44 percent and 14.54 percent respectively, while the SmCo without any coating of comparative example 1 5 Permanent magnet material powdering, smCo of comparative example 2 without any plating 17 The remanence of the permanent magnetic material is reduced by 64.16 percent, so that TaN is obtained X2 The + Ta composite coating improves the high-temperature stability of the samarium cobalt permanent magnet material because of the dense TaN X2 The + Ta composite plating layer inhibits outward diffusion of Sm and inward diffusion of O.
In addition, compared with the Ta plating layers in examples 1 and 2, taN in examples 5 and 6 was used X2 The + Ta composite coating has better high-temperature protection effect on samarium-cobalt permanent magnet materials because of TaN X2 The structure of the coating is different from that of the Ta coating, so TaN X2 The interface of the coating and the Ta coating forms a more effective diffusion barrier layer, the inhibition effect on O and Sm diffusion is improved, and simultaneously, the TaN coating X2 The coating can be used as an inducing layer, and can induce the Ta coating to form an alpha-phase structure at room temperature, so that the Ta coating has better protection effect and higher bonding strength.
Test example 4
TaO having the same properties as those of examples 7 and 8 X1 Sm of plating layer 2 Co 17 The permanent magnet material and the corresponding high-temperature-resistant samarium cobalt permanent magnet material without any plating layer (marked as comparative example 3) are subjected to isothermal heat treatment under the following conditions: magnetic properties before and after heat treatment were measured at 500 ℃, in an air atmosphere, and then using a Vibrating Sample Magnetometer (VSM), and the results are shown in the following table:
example 7 with TaO X1 Sm of plating layer with mark number of T-550 2 Co 17 Permanent magnet material and TaO with example 8 X1 Coated Sm of 26H brand 2 Co 17 After the permanent magnetic material is subjected to 192-hour heat treatment at the high temperature of 500 ℃ in an aerobic environment, the remanence (Br) is reduced by 2.94 percent and 5.45 percent respectively. Sm of reference example 2, having No coating, brand T-550 2 Co 17 Permanent magnet material and Sm of comparative example 2, no coating, reference 26H 2 Co 17 The remanence of the permanent magnetic material is respectively reduced by 48.91% and 64.16%, so that the TaO is known X1 The plating significantly improves the high temperature stability of samarium cobalt permanent magnet materials because of the dense TaO X1 And a plating layer for suppressing outward diffusion of Sm and inward diffusion of O.
Further, the same Ta plating layer as in example 2, ta plating layer as in example 4, taN plating layer as in example 6 X2 TaO in example 8 compared with + Ta composite coating X1 The coating has a better high temperature protection effect on samarium cobalt permanent magnet materials because of the TaO X1 The coating is in a stable oxide state, so that TaO X1 The coating layer no longer reacts with O in the air, so that TaO X1 The plating layer has excellent oxidation resistance, taO X1 The coating layer can not fall off due to reoxidation in the air, so that TaO X1 Has stable protection effect all the time.
Test example 5
SmCo with TaNb coating for example 9 5 Permanent magnetMaterials, sm with TaNb coating of example 10 2 Co 17 Carrying out isothermal heat treatment on the permanent magnet material, wherein the heat treatment conditions are as follows: magnetic properties before and after heat treatment were measured at 500 ℃, in an air atmosphere, and then using a Vibrating Sample Magnetometer (VSM), and the results are shown in the following table:
SmCo with TaNb coating of example 9 5 Permanent magnet material and SmCo with TaNb coating of example 10 17 After the permanent magnet material is subjected to heat treatment for 192 hours in a high-temperature aerobic environment at 500 ℃, the remanence (Br) is reduced by 17.90 percent and 8.9 percent respectively, compared with the SmCo without any coating of comparative example 1 5 Permanent magnet powdering, smCo of comparative example 2 without any coating 17 The remanence of the permanent magnet material is reduced by 64.16%, so that the TaNb coating has an obvious high-temperature protection effect on the samarium-cobalt permanent magnet material, and the reason is that the sputtering yield of Ta and Nb is close, the deposited TaNb coating does not have too large component segregation, ta and Nb can form a coating which is denser than Ta, sm outward diffusion and O inward diffusion can be effectively inhibited, a surface aging layer is prevented from being formed, and the loss of magnetic performance is reduced.
Test example 6
6.1 the effect of working gas pressure for sputter plating on the magnetic properties of a permanent magnet material having a plated layer was examined under the same conditions as in example 2 in a manner similar to that of test example 1, and the results are shown in the following table:
as can be seen from the above table, when the working air pressure is 0.1 to 5Pa, the magnetic property loss after high-temperature aging is reduced while the sputtering plating is ensured. When the working air pressure is too low, sputtering cannot be performed. When the working air pressure is too high, the density of the plating layer is reduced, and the protective performance is reduced.
6.2 in the same manner as in example 2 except that the influence of the sputtering power per target area for sputtering on the magnetic properties of the permanent magnet material having a plated layer was examined, the examination is made with reference to test example 1, and the results are shown in the following table:
as can be seen from the above table, the sputtering power per unit target area is 0.1-15W/cm 2 During the process, the loss of magnetic performance after high-temperature aging is reduced while the sputtering plating is ensured. When the sputtering power is too low, sputtering cannot be performed. The sputtering power is too high, the crystal grains are coarse, and the protective performance of the plating layer is reduced.
6.3 the effect of the cleaning time for sputter plating on the magnetic properties of the permanent-magnet material with a plated layer was examined under the same conditions as in example 2, in a manner similar to that of test example 1, and the results are shown in the following table:
as can be seen from the table above, when the cleaning time is greater than or equal to 1min, the quality of the coating is improved, and the loss of the magnetic property after high-temperature aging is reduced.
6.4 in the same manner as in example 2 except that the influence of the bias voltage for sputter plating on the magnetic properties of the permanent magnet material having a plated layer was examined, reference was made to test example 1, and the results are given in the following table:
as can be seen from the above table, the loss of magnetic properties after high temperature aging is reduced when the bias voltage is-400 to-1V.
6.5 in the same manner as in example 4 except that the working gas pressure for ion plating was examined for the influence on the magnetic properties of the permanent magnet material having a plated layer, the examination was made in a manner as referred to test example 2, and the results are shown in the following table:
as can be seen from the above table, when the working air pressure is 0.5 to 5Pa, the loss of magnetic performance after high-temperature aging is reduced while the ion plating is ensured.
6.6 the effect of the current density per target area for ion plating on the magnetic properties of the permanent magnet material with a plated layer was examined under the same conditions as in example 4 in a manner similar to that of test example 2, and the results are shown in the following table:
as can be seen from the above table, the current density per unit target area is 0.5 to 5A/cm 2 In this case, the loss of magnetic properties after high-temperature aging is reduced.
6.7 the effect of the cleaning time for ion plating on the magnetic properties of the permanent-magnet material with a plated layer was examined under the same conditions as in example 4 in a manner as described in test example 2, and the results are shown in the following table:
as can be seen from the above table, when the cleaning time is greater than or equal to 1min, the magnetic property loss after high-temperature aging is reduced.
6.8 the effect of the bias voltage for ion plating on the magnetic properties of the permanent magnet material having a plated layer was examined under the same conditions as in example 4 in a manner as described in test example 2, and the results are shown in the following table:
as can be seen from the above table, the loss of magnetic properties after high temperature aging is reduced when the bias voltage is-400 to-1V.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. A coating for surface protection of samarium cobalt permanent magnet materials, comprising at least one of the following components:
tantalum metal Ta;
tantalum oxide TaO X1 X1 is any number between 0 and 2.5;
tantalum nitride TaN X2 X2 is any number between 0 and 1.6;
an alloy comprising metallic tantalum Ta and a metal M, M comprising at least one of V, nb, zr, hf, cr, al, ni.
2. The coating of claim 1,
the plating layer comprises at least one layer body, wherein each layer body is superposed, and each layer body comprises one of the following components:
tantalum metal Ta;
tantalum oxide TaO X1 X1 is any number between 0 and 2.5;
tantalum nitride TaN X2 X2 is any number between 0 and 1.6;
the alloy comprises metal tantalum Ta and metal M, wherein M is at least one of V, nb, zr, hf, cr, al and Ni.
3. The coating of claim 1,
the metal tantalum Ta is an alpha phase or a beta phase.
4. The coating of claim 1,
the thickness of the plating layer is 0.5-200 μm.
5. A method for protecting the surface of a samarium cobalt permanent magnet material is characterized by comprising the following steps of:
depositing the coating of any of claims 1 to 4 on the surface of the samarium cobalt permanent magnet material.
6. The method of protection according to claim 5,
the coating is deposited by sputter plating, ion plating or spray coating.
7. The shielding method of claim 6,
before the sputtering plating, the target material of the sputtering plating is cleaned, the working air pressure is 0.1 to 5Pa, and the sputtering power per unit target area is 0.1 to 15W/cm 2 And the cleaning time is more than or equal to 1min.
8. The shielding method of claim 5,
when the sputtering plating is carried out, the working air pressure is 0.1 to 5Pa, and the sputtering power per unit target area is 0.1 to 15W/cm 2 And applying a bias voltage of-400 to-1V.
9. The shielding method of claim 5,
before the ion plating, cleaning the ion plated target material, wherein the working air pressure is 0.5-5 Pa, and the current density of the unit target area is 0.5-5A/cm 2 The cleaning time is more than or equal to 1min.
10. The method of protection according to claim 5,
when the ion plating is carried out, the working air pressure is 0.5 to 5Pa, and the current density per unit target area is 0.5 to 5A/cm 2 And applying a bias voltage of-400 to-1V.
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