CN115410785B - A coating for protecting the surface of samarium cobalt permanent magnet material and a method for protecting the surface of samarium cobalt permanent magnet material - Google Patents
A coating for protecting the surface of samarium cobalt permanent magnet material and a method for protecting the surface of samarium cobalt permanent magnet material Download PDFInfo
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- CN115410785B CN115410785B CN202110577559.0A CN202110577559A CN115410785B CN 115410785 B CN115410785 B CN 115410785B CN 202110577559 A CN202110577559 A CN 202110577559A CN 115410785 B CN115410785 B CN 115410785B
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- 239000000463 material Substances 0.000 title claims abstract description 121
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 title claims abstract description 102
- 238000000576 coating method Methods 0.000 title claims abstract description 88
- 239000011248 coating agent Substances 0.000 title claims abstract description 87
- KPLQYGBQNPPQGA-UHFFFAOYSA-N cobalt samarium Chemical compound [Co].[Sm] KPLQYGBQNPPQGA-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 33
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 23
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052751 metal Inorganic materials 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 19
- 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
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 6
- 239000000956 alloy Substances 0.000 claims abstract description 6
- 238000007747 plating Methods 0.000 claims description 50
- 238000004544 sputter deposition Methods 0.000 claims description 29
- 238000000151 deposition Methods 0.000 claims description 21
- 238000004140 cleaning Methods 0.000 claims description 17
- 238000007733 ion plating Methods 0.000 claims description 13
- 229910001362 Ta alloys Inorganic materials 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 abstract description 7
- 229910052758 niobium Inorganic materials 0.000 abstract description 4
- 230000002401 inhibitory effect Effects 0.000 abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 abstract 1
- 229910052804 chromium Inorganic materials 0.000 abstract 1
- 229910052735 hafnium Inorganic materials 0.000 abstract 1
- 229910052759 nickel Inorganic materials 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 56
- 229910052761 rare earth metal Inorganic materials 0.000 description 32
- 150000002910 rare earth metals Chemical class 0.000 description 31
- 238000005245 sintering Methods 0.000 description 30
- 230000002829 reductive effect Effects 0.000 description 24
- 239000007789 gas Substances 0.000 description 21
- 239000000843 powder Substances 0.000 description 20
- 238000010438 heat treatment Methods 0.000 description 16
- 230000008021 deposition Effects 0.000 description 14
- 238000009792 diffusion process Methods 0.000 description 14
- 238000012360 testing method Methods 0.000 description 14
- 238000005406 washing Methods 0.000 description 14
- 229910017052 cobalt Inorganic materials 0.000 description 13
- 239000010941 cobalt Substances 0.000 description 13
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 13
- 229910052772 Samarium Inorganic materials 0.000 description 12
- 229910004168 TaNb Inorganic materials 0.000 description 12
- 238000003723 Smelting Methods 0.000 description 10
- 230000032683 aging Effects 0.000 description 10
- 239000011247 coating layer Substances 0.000 description 10
- 239000002131 composite material Substances 0.000 description 10
- 230000000694 effects Effects 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
- 238000001514 detection method Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 229910052742 iron Inorganic materials 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
- 239000010949 copper Substances 0.000 description 6
- 239000000696 magnetic material Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 229910052777 Praseodymium Inorganic materials 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- 238000001755 magnetron sputter deposition Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 229910001172 neodymium magnet Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 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
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material 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
- 239000013077 target material Substances 0.000 description 1
- 229910002058 ternary alloy Inorganic materials 0.000 description 1
Classifications
-
- 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
本申请公开了一种用于钐钴永磁材料表面防护的镀层及钐钴永磁材料表面的防护方法，镀层包括以下成分中的至少一种：金属钽Ta；氧化钽TaOX1，X1为0～2.5之间的任意数字；氮化钽TaNX2，X2为0～1.6之间的任意数字；包括金属钽Ta和金属M的合金，M包括V、Nb、Zr、Hf、Cr、Al、Ni中的至少一种。本申请提供了一种用于钐钴永磁材料表面防护的镀层，该镀层既可阻隔永磁材料内部元素向外扩散，又可阻隔外部O元素向永磁材料内扩散，从而改善了钐钴永磁材料的耐高温性能，抑制了钐钴在高温环境的磁性能衰减。
The present application discloses a coating for protecting the surface of samarium cobalt permanent magnet materials and a method for protecting the surface of samarium cobalt permanent magnet materials, wherein the coating includes at least one of the following components: metal tantalum 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 including metal tantalum Ta and metal M, wherein M includes at least one of V, Nb, Zr, Hf, Cr, Al, and Ni. The present application provides a coating for protecting the surface of samarium cobalt permanent magnet materials, which can block the internal elements of the permanent magnet materials from diffusing outward, and can also block the external O elements from diffusing into the permanent magnet materials, thereby improving the high temperature resistance of the samarium cobalt permanent magnet materials and inhibiting the attenuation of the magnetic properties of samarium cobalt in high temperature environments.
Description
Technical Field
The application relates to the technical field of materials, in particular to a coating for protecting the surface 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 th century, a first generation rare earth permanent magnet material 1:5 type samarium cobalt material (SmCo 5) was produced, a second generation rare earth permanent magnet material 2:17 type samarium cobalt permanent magnet material (Sm 2Co 17) was produced in the 70 th year, and a third generation permanent magnet material represented by neodymium iron boron (Nd-Fe-B) was produced in the 80 th year. China is the world's largest rare earth raw material reserve country and production country. The development of rare earth permanent magnet materials has been progressed for decades, and the market demands have prompted the development of technologies toward high performance.
The samarium cobalt permanent magnet material is widely applied in the environment with the temperature of more than 200 ℃ because of higher comprehensive magnetic performance and excellent temperature resistance. The high-performance samarium cobalt permanent magnet material is widely applied to the fields of high-speed rail, new energy automobile motors, water pumps, sensors and the like. The low temperature coefficient permanent magnet material is used in the fields of space satellite, aerospace and the like with excellent temperature stability. Gao Wenshan cobalt permanent magnet materials have been used in environments with temperatures of 550 ℃.
But the samarium cobalt permanent magnet material can generate magnetic property attenuation when working for a long time under the environment of 350 ℃. The formation of the surface aged layer is a main cause of the decay of magnetic properties. The surface protection coating with oxidation resistance and high stability is an effective method for inhibiting the formation of a surface aging layer.
Content of the application
The application provides a coating for protecting the surface of a samarium cobalt permanent magnet material and a protection method for the surface of the samarium cobalt permanent magnet material, which can improve the high temperature resistance of the samarium cobalt permanent magnet material.
In a first aspect, the application provides a coating for protecting the surface of a samarium cobalt permanent magnet material, which comprises at least one of the following components:
Metallic tantalum Ta;
tantalum oxide TaO X1, wherein 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 samarium cobalt permanent magnet material comprises a first-generation rare earth permanent magnet material 1:5 type samarium cobalt material (SmCo 5) and a second-generation rare earth permanent magnet material 2:17 type samarium cobalt permanent magnet material (Sm 2Co17). The material contains one or more of Fe, cu, zr, ti, si, sn, nb, V, ni, mo, B and rare earth elements La, ce, pr, nd, er, gd, dy, ho, tb, eu besides two basic components of Sm and Co.
For the metal tantalum Ta, the metal tantalum Ta has high melting point, good toughness and excellent chemical stability, so that the metal tantalum Ta coating is a high-temperature-resistant, friction-resistant and extreme chemical corrosion-resistant choice.
Further, the plating layer comprises one of the following components:
Metallic tantalum Ta;
tantalum oxide TaO X1, wherein 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 composition of the coating may be metallic tantalum Ta, denoted Ta coating, or tantalum oxide TaO X1, denoted TaO X1 coating.
Further, the alloy is composed of metallic tantalum Ta and a metal M, M comprising at least one of V, nb, zr, hf, cr, al, ni.
For example, the composition of the coating may be an alloy, which may be composed of metallic tantalum Ta and metallic Nb, where the coating is denoted as a TaNb binary alloy coating, and may be composed of metallic tantalum Ta, metallic Zr, and metallic Hf, where the coating is denoted as a TaZrHf ternary alloy coating.
Further, the plating layer comprises at least one layer body, each layer body is stacked, and each layer body comprises one of the following components:
Metallic tantalum Ta;
tantalum oxide TaO X1, wherein X1 is any number between 0 and 2.5;
Tantalum nitride TaN X2, X2 is any number between 0 and 1.6;
Comprises an alloy of tantalum Ta and a metal M, M being at least one of V, nb, zr, hf, cr, al, ni.
For example, the number of the layers may be one, two, or three.
Further, the components of each layer are respectively one of the following components:
Metallic tantalum Ta;
tantalum oxide TaO X1, wherein X1 is any number between 0 and 2.5;
Tantalum nitride TaN X2, X2 is any number between 0 and 1.6;
Comprises an alloy of tantalum Ta and a metal M, M being at least one of V, nb, zr, hf, cr, al, ni.
Further, the composition of each layer is different.
For example, the number of the layers may be two, which are respectively referred to as a first layer and a second layer coated on the first layer, the composition of the first layer may be tantalum nitride TaN X2, the second layer may be metallic tantalum Ta, and the coating is referred to as a TaN X2 +ta composite coating.
Further, the tantalum Ta metal is alpha phase or beta phase. The metallic tantalum Ta coating deposited at room temperature generally exhibits a tetragonal phase structure (beta phase,) Beta-phase tantalum Ta coatings are very hard but very brittle, often resulting in high coating stresses. The thermodynamically stable phase of Ta is the bcc structure (alpha phase,) The coating has high toughness and good ductility, and is an ideal coating.
Further, the total thickness of the plating layer is 0.5-200 mu m.
In a second aspect, the application provides a protection method for the surface of a samarium cobalt permanent magnet material, comprising the following steps:
Depositing the coating in any of the embodiments above on the surface of the samarium cobalt permanent magnet material.
Further, the plating layer is deposited by sputtering, ion plating or spray coating.
Further, before sputtering, cleaning the sputtered target, wherein the working air pressure is 0.1-5 Pa, the sputtering power per unit target area is 0.1-15W/cm 2, and the cleaning time is more than or equal to 1min.
Further, during sputter plating, the working air pressure is 0.1-5 Pa, the sputtering power per unit target area is 0.1-15W/cm 2, and bias voltage of-400 to-1V is applied.
Further, before sputtering, the target material 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 ion plated target is cleaned, the working air pressure is 0.5-5 Pa, the current density of unit target area is 0.5-5A/cm 2, and the cleaning time is more than or equal to 1min.
Further, when ion plating is performed, the working air pressure is 0.5-5 Pa, the current density of unit target area is 0.5-5A/cm 2, and bias voltage of-400 to-1V is applied.
In a further scheme, before ion plating, the ion plated target is cleaned, and the samarium cobalt permanent magnet material is subjected to acid washing, water washing and drying.
Compared with the prior art, the plating layer has the following beneficial effects:
the application provides a coating for protecting the surface of a samarium cobalt permanent magnet material, which can not only prevent the outward diffusion of elements in the permanent magnet material, but also prevent the inward diffusion of external O elements in the permanent magnet material, thereby improving the high temperature resistance of the samarium cobalt permanent magnet material and inhibiting the decay of the magnetic property of the samarium cobalt in a high temperature environment.
Drawings
FIG. 1 is a block diagram of a cross section of Sm 2Co17 permanent magnet material with a Ta coating.
Detailed description of the preferred embodiments
The present application will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present application more apparent. It should be understood that the detailed description and specific examples are intended for purposes of illustration only and are not intended to limit the scope of the application.
Example 1
The selected samarium cobalt permanent magnet material is as follows:
The first generation rare earth permanent magnet material is 1:5 samarium cobalt (sintered SmCo 5) with the mark of 22, and the main composition is Sm (rare earth samarium), pr (rare earth praseodymium) and Co (metal cobalt). The sintering SmCo 5 adopts a powder sintering process, and the process flow can be summarized as smelting, powder preparation, molding, sintering, detection and processing.
The selected plating layers are as follows:
Ta coating, ta is alpha phase.
The steps of depositing the coating are as follows:
(1) Two Ta targets (purity 99.95%) were mounted on a magnetron sputtering source in a vacuum chamber, and the angle of the Ta targets to the sample carousel horizontal plane was adjusted to 45 °.
(2) The samarium cobalt permanent magnet material is placed on a sample turntable after being subjected to acid washing, water washing and drying.
(3) The vacuum chamber is pre-vacuumized by a mechanical pump until the vacuum degree in the vacuum chamber is less than 20Pa, and then vacuumized by a molecular pump, so that the vacuum degree in the vacuum chamber is less than 8.0X10- 4 Pa.
(4) The Ta target was cleaned under conditions of Ar (99.999% purity) as a working gas, a working gas pressure of 0.5Pa, a sputtering power per target area of 2W/cm 2, and a cleaning time of 30min.
(5) And performing sputtering deposition on the samarium cobalt permanent magnet material under the deposition condition that Ar (purity is 99.999%) is adopted as working gas, working gas pressure is controlled to be 0.5Pa, sputtering power per unit target area is 4W/cm 2, bias voltage of-100V is applied, the temperature of the substrate is regulated to 400 ℃ by using a built-in heater, and deposition thickness is controlled to be 4 mu m, so that the Ta coating is deposited.
Example 2
The only difference from example 1 is that the samarium cobalt permanent magnet material was selected as follows:
The second-generation rare earth permanent magnet material is 2:17 samarium cobalt (sintered Sm 2Co17) with the brand of 26H, and comprises the components of Sm (rare earth samarium), co (metallic cobalt), cu (metallic copper), fe (metallic iron) and Zr (subgroup element zirconium). The sintering Sm 2Co17 adopts a powder sintering process, and the process flow can be summarized as smelting, powder preparation, molding, sintering, detection and processing.
Example 3
The selected samarium cobalt permanent magnet material is as follows:
The first generation rare earth permanent magnet material is 1:5 samarium cobalt (sintered SmCo 5) with the mark of 22, and the main composition is Sm (rare earth samarium), pr (rare earth praseodymium) and Co (metal cobalt). The sintering SmCo 5 adopts a powder sintering process, and the process flow can be summarized as smelting, powder preparation, molding, sintering, detection and processing.
The selected plating layers are as follows:
Ta coating, ta is alpha phase.
The steps of depositing the coating are as follows:
(1) Two Ta arc targets (99.95% purity) were mounted on an arc source within a vacuum chamber.
(2) The samarium cobalt permanent magnet material is placed on a sample turntable after being subjected to acid washing, water washing and drying.
(3) The vacuum chamber is pre-vacuumized by a mechanical pump until the vacuum degree in the vacuum chamber is less than 20Pa, and then vacuumized by a molecular pump, so that the vacuum degree in the vacuum chamber is less than 8.0X10- 4 Pa.
(4) The Ta arc target is cleaned under the conditions that Ar (purity is 99.999%) is adopted as working gas, working air pressure is controlled to be 1Pa, current density per unit target area is 1A/cm 2, and cleaning time is 30min.
(5) And (3) performing multi-arc deposition on the samarium cobalt permanent magnet material workpiece, wherein the deposition condition is that Ar (purity is 99.999%) is adopted as working gas, the working gas pressure is controlled to be 1Pa, the current density of unit target area is 1A/cm 2, a bias voltage of-200V is applied, the temperature of the substrate is regulated to 400 ℃ by using a built-in heater, and the deposition thickness is controlled to be 8 mu m, so that the Ta coating is deposited.
Example 4
The only difference from example 3 is that the samarium cobalt permanent magnet material was selected as follows:
the second-generation rare earth permanent magnet material is 2:17 samarium cobalt (sintered Sm 2Co17) with the brand of 26H, and comprises the following components of Sm (rare earth samarium), co (metallic cobalt), cu (metallic copper), fe (metallic iron) and Zr (subgroup element zirconium). The sintering Sm 2Co17 adopts a powder sintering process, and the process flow can be summarized as smelting, powder preparation, molding, sintering, detection and processing.
Example 5
The selected samarium cobalt permanent magnet material is as follows:
The first generation rare earth permanent magnet material is 1:5 samarium cobalt (sintered SmCo 5) with the mark of 22, and the main composition is Sm (rare earth samarium), pr (rare earth praseodymium) and Co (metal cobalt). The sintering SmCo 5 adopts a powder sintering process, and the process flow can be summarized as smelting, powder preparation, molding, sintering, detection and processing.
The selected plating layers are as follows:
TaN X2 +Ta composite coating, and Ta is alpha phase.
The steps of depositing the coating are as follows:
(1) Two Ta targets (purity 99.95%) were mounted on a magnetron sputtering source in a vacuum chamber, and the angle of the Ta targets to the sample carousel horizontal plane was adjusted to 45 °.
(2) The samarium cobalt permanent magnet material is placed on a sample turntable after being subjected to acid washing, water washing and drying.
(3) The vacuum chamber is pre-vacuumized by a mechanical pump until the vacuum degree in the vacuum chamber is less than 20Pa, and then vacuumized by a molecular pump, so that the vacuum degree in the vacuum chamber is less than 8.0X10- 4 Pa.
(4) The Ta target was cleaned under conditions of Ar (99.999% purity) as a working gas, a working gas pressure of 0.5Pa, a sputtering power per target area of 2W/cm 2, and a cleaning time of 30min.
(5) And performing sputter deposition on the samarium cobalt permanent magnet material workpiece under the deposition condition that Ar (purity is 99.999%) and N 2 (purity is 99.999%) are adopted as working gases, and the working pressure is controlled to be 0.5Pa, and the deposition thickness is 0.1 mu m, so that a TaN X2 coating is deposited. It should be noted that the substrate temperature need not be adjusted with a built-in heater.
(6) N 2 is closed, 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 only difference from example 5 is that the samarium cobalt permanent magnet material was selected as follows:
the second-generation rare earth permanent magnet material is 2:17 samarium cobalt (sintered Sm 2Co17) with the brand of 26H, and comprises the following components of Sm (rare earth samarium), co (metallic cobalt), cu (metallic copper), fe (metallic iron) and Zr (subgroup element zirconium). The sintering Sm 2Co17 adopts a powder sintering process, and the process flow can be summarized as smelting, powder preparation, molding, sintering, detection and processing.
Example 7
The selected samarium cobalt permanent magnet material is as follows:
The second-generation rare earth permanent magnet material is 2:17 samarium cobalt (sintered Sm 2Co17), the brand is Gao Wenshan cobalt-resistant T-550, the highest service temperature of the brand samarium cobalt reaches 550 ℃, and the second-generation rare earth permanent magnet material comprises Sm (rare earth samarium), co (metallic cobalt), cu (metallic copper), fe is metallic iron and Zr (subgroup element zirconium). The sintering Sm 2Co17 with the brand of T-550 adopts a powder sintering process, and the process flow can be summarized as smelting, powder making, molding, sintering, detecting and processing.
And (3) selecting a coating:
TaO X1 coating.
The steps of depositing the coating are as follows:
(1) Two Ta targets (purity 99.95%) were mounted on a magnetron sputtering source in a vacuum chamber, and the angle of the Ta targets to the sample carousel horizontal plane was adjusted to 45 °.
(2) The samarium cobalt permanent magnet material is placed on a sample turntable after being subjected to acid washing, water washing and drying.
(3) The vacuum chamber is pre-vacuumized by a mechanical pump until the vacuum degree in the vacuum chamber is less than 20Pa, and then vacuumized by a molecular pump, so that the vacuum degree in the vacuum chamber is less than 8.0X10- 4 Pa.
(4) The Ta target was cleaned under conditions of Ar (99.999% purity) as a working gas, a working gas pressure of 0.5Pa, a sputtering power per target area of 2W/cm 2, and a cleaning time of 30min.
(5) And performing sputter deposition on the samarium cobalt permanent magnet material workpiece under the deposition condition that Ar (purity is 99.999%) and O 2 (purity is 99.999%) are adopted as working gases, and the working pressure is controlled to be 0.5Pa, and the deposition thickness is 2 mu m, so that the TaO X1 coating is deposited. It should be noted that the substrate temperature need not be adjusted with a built-in heater.
Example 8
The only difference from example 7 is that the samarium cobalt permanent magnet material was selected as follows:
The second-generation rare earth permanent magnet material is 2:17 samarium cobalt (sintered Sm 2Co17) with the brand of 26H, and comprises the following components of Sm (rare earth samarium), co (metallic cobalt), cu (metallic copper), fe (metallic iron) and Zr (subgroup element zirconium). The sintering Sm 2Co17 with the brand of 26H adopts a powder sintering process, and the process flow can be summarized as smelting, powder making, molding, sintering, detecting and processing.
Example 9
The selected samarium cobalt permanent magnet material is as follows:
The first generation rare earth permanent magnet material is 1:5 samarium cobalt (sintered SmCo 5) with the mark of 22, and the main composition is Sm (rare earth samarium), pr (rare earth praseodymium) and Co (metal cobalt). The sintering SmCo 5 adopts a powder sintering process, and the process flow can be summarized as smelting, powder preparation, molding, sintering, detection and processing.
The selected plating layers are as follows:
and (3) a TaNb binary alloy coating.
The steps of depositing the coating are as follows:
(1) Two TaNb binary alloy targets (50 at% Ta:50at% Nb, purity 99.95%) were mounted on a sputter source in a vacuum chamber, and the angle of the TaNb binary alloy targets to the horizontal plane of the sample turntable was adjusted to 45 degrees.
(2) The samarium cobalt permanent magnet material is placed on a sample turntable after being subjected to acid washing, water washing and drying.
(3) The vacuum chamber is pre-vacuumized by a mechanical pump until the vacuum degree in the vacuum chamber is less than 20Pa, and then vacuumized by a molecular pump, so that the vacuum degree in the vacuum chamber is less than 8.0X10- 4 Pa.
(4) And cleaning the TaNb binary alloy target under the conditions that Ar (purity is 99.999%) is adopted as working gas, the working gas pressure is controlled to be 0.5Pa, the sputtering power per unit target area is 2W/cm 2, and the cleaning time is 30min.
(5) And performing sputtering deposition on the samarium cobalt permanent magnet material under the deposition condition that Ar (purity is 99.999%) is adopted as working gas, working gas pressure is controlled to be 0.5Pa, sputtering power per unit target area is 4W/cm 2, bias voltage of-100V is applied, a built-in heater is used for heating the substrate to 400 ℃, and deposition thickness is controlled to be 4 mu m, so that the TaNb binary alloy coating is deposited.
Example 10
The only difference from example 9 is that the samarium cobalt permanent magnet material was selected as follows:
The second-generation rare earth permanent magnet material is 2:17 samarium cobalt (sintered Sm 2Co17) with the brand of 26H, and comprises the components of Sm (rare earth samarium), co (metallic cobalt), cu (metallic copper), fe (metallic iron) and Zr (subgroup element zirconium). The sintering Sm 2Co17 adopts a powder sintering process, and the process flow can be summarized as smelting, powder preparation, molding, sintering, detection and processing.
Test example 1
The SmCo 5 permanent magnet material with Ta coating of example 1, the Sm 2Co17 permanent magnet material with Ta coating of example 2, the corresponding SmCo 5 permanent magnet material without any coating (denoted as comparative example 1), the corresponding Sm 2Co17 permanent magnet material without any coating (denoted as comparative example 2) were subjected to isothermal heat treatment under the conditions of 500 ℃ in air, and then the magnetic properties before and after heat treatment were tested using a Vibrating Sample Magnetometer (VSM), and the results are shown in the following table:
The SmCo 5 permanent magnet material with Ta coating of example 1 and the SmCo 17 permanent magnet material with Ta coating of example 2 were subjected to heat treatment at 500 ℃ for 192 hours in an aerobic atmosphere, the remanence (Br) was reduced by-23.24% and 15.10%, respectively, while the SmCo 5 permanent magnet material without any coating of comparative example 1 was pulverized, and the remanence of the SmCo 17 permanent magnet material without any coating of comparative example 2 was reduced by 64.16%, whereby it was found that the Ta coating had a remarkable high temperature protective effect on the samarium cobalt permanent magnet material because Sm outward diffusion and O inward diffusion were suppressed by the dense Ta coating, the formation of a surface aged layer was prevented, and the loss of magnetic properties was reduced.
Test example 2
The SmCo 5 permanent magnet material with Ta coating of example 3 and the Sm 2Co17 permanent magnet material with Ta coating of example 4 were subjected to a heat treatment under the conditions of 500 ℃ and air environment, and then the magnetic properties before and after the heat treatment were tested by using a Vibrating Sample Magnetometer (VSM), and the results are shown in the following table:
The SmCo 5 permanent magnet material with Ta coating of example 3 and the SmCo 17 permanent magnet material with Ta coating of example 4 were subjected to heat treatment at 500 ℃ for 192 hours in an aerobic atmosphere, the remanence (Br) was reduced by 19.32% and 10.58%, respectively, while the SmCo 5 permanent magnet material without any coating of comparative example 1 was pulverized, and the remanence of the SmCo 17 permanent magnet material without any coating of comparative example 2 was reduced by 64.16%, whereby it was found that the Ta coating had a remarkable high temperature protective effect on the samarium cobalt permanent magnet material because Sm outward diffusion and O inward diffusion were suppressed by the dense Ta coating, the formation of a surface aged layer was prevented, and the loss of magnetic properties was reduced.
In addition, compared with the Ta plating layers in the embodiment 1 and the embodiment 2, the Ta plating layers in the embodiment 3 and the embodiment 4 have better high-temperature protection effect on the samarium cobalt permanent magnet material, because the embodiment 3 and the embodiment 4 adopt multi-arc ion plating to deposit the Ta plating layer, compared with the embodiment 1 and the embodiment 2, the Ta plating layers have two changes, namely, the thickness is increased by 1 time and is 8 mu m, and the second, the density of the plating layer is improved by applying negative bias, and the two changes enable the Ta plating layer to have better protection effect.
Test example 3
The SmCo 5 permanent magnet material with a TaN X2 +ta composite coating of example 5 and the Sm 2Co17 permanent magnet material with a TaN X2 +ta composite coating of example 6 were subjected to isothermal heat treatment under the conditions of 500 ℃ and air environment, and then magnetic properties before and after heat treatment were measured using a Vibrating Sample Magnetometer (VSM), and the results are shown in the following table:
The SmCo 5 permanent magnetic material with the TaN X2 +ta composite coating layer of example 5 and the Sm 2Co17 permanent magnetic material with the TaN X2 +ta composite coating layer of example 6 undergo heat treatment for 192 hours at 500 ℃ in an aerobic atmosphere, the remanence (Br) is reduced by 22.44% and 14.54%, respectively, while the SmCo 5 permanent magnetic material without any coating layer of comparative example 1 is pulverized, and the remanence of the SmCo 17 permanent magnetic material without any coating layer of comparative example 2 is reduced by 64.16%, whereby it is known that the TaN X2 +ta composite coating layer improves the high temperature stability of the samarium cobalt permanent magnetic material, because Sm outward diffusion and O inward diffusion are suppressed by the dense TaN X2 +ta composite coating layer.
In addition, compared with the Ta plating layers in the embodiments 1 and 2, the TaN X2 +ta composite plating layers in the embodiments 5 and 6 have better high-temperature protection effect on the samarium cobalt permanent magnet material, because the TaN X2 plating layer and the Ta plating layer have different structures, so that the interface between the TaN X2 plating layer and the Ta plating layer forms a more effective diffusion barrier layer, the inhibition effect on the diffusion of O and Sm is improved, and meanwhile, the TaN X2 plating layer can be used as an induction layer, and the Ta plating layer can be induced to form an alpha-phase structure at room temperature, so that the Ta plating layer has better protection effect and higher bonding strength.
Test example 4
The Sm 2Co17 permanent magnet materials with TaO X1 coating and the corresponding Gao Wenshan cobalt-resistant permanent magnet materials without any coating (denoted as comparative example 3) of example 7 and example 8 were subjected to isothermal heat treatment under the conditions of 500 ℃ and air environment, and then the magnetic properties before and after heat treatment were tested by using a Vibrating Sample Magnetometer (VSM), and the results are shown in the following table:
After the Sm 2Co17 permanent magnet material with TaO X1 coating and the Sm 2Co17 permanent magnet material with TaO X1 coating and the Sm 2Co17 permanent magnet material with 26H of example 7 are subjected to heat treatment for 192 hours in a 500 ℃ high-temperature aerobic environment, the residual magnetism (Br) is reduced by 2.94% and 5.45%, respectively. Whereas the residual magnetism of the Sm 2Co17 permanent magnet material of the comparative example 2, which is not provided with any coating layer, and the Sm 2Co17 permanent magnet material of the comparative example 2, which is not provided with any coating layer, and which is provided with 26H, is respectively reduced by 48.91% and 64.16%, it is clear that the TaO X1 coating layer significantly improves the high temperature stability of the samarium cobalt permanent magnet material, because the diffusion of Sm outwards and the diffusion of O inwards are suppressed by the dense TaO X1 coating layer.
In addition, compared with the Ta plating layer in the embodiment 2, the Ta plating layer in the embodiment 4 and the TaN X2 +Ta composite plating layer in the embodiment 6, the TaO X1 plating layer in the embodiment 8 has better high-temperature protection effect on the samarium cobalt permanent magnet material, because the TaO X1 plating layer is in a stable oxide state, the TaO X1 plating layer does not react with O in the air any more, so that the TaO X1 plating layer has very excellent oxidation resistance, and the TaO X1 plating layer does not fall off due to reoxidation in the air, so that the TaO X1 always has stable protection effect.
Test example 5
The SmCo 5 permanent magnet material with a TaNb coating of example 9 and the Sm 2Co17 permanent magnet material with a TaNb coating of example 10 were subjected to a heat treatment under the conditions of 500 ℃ and an air atmosphere, and then the magnetic properties before and after the heat treatment were tested using a Vibrating Sample Magnetometer (VSM), and the results are shown in the following table:
The SmCo 5 permanent magnet material with a TaNb coating of example 9 and the SmCo 17 permanent magnet material with a TaNb coating of example 10 undergo heat treatment for 192 hours at a high temperature and in an aerobic environment at 500 ℃, the remanence (Br) is reduced by 17.90% and 8.9%, respectively, while the SmCo 5 permanent magnet material without any coating of comparative example 1 is pulverized, and the remanence of the SmCo 17 permanent magnet material without any coating of comparative example 2 is reduced by 64.16%, thus the TaNb coating has obvious high temperature protection effect on the samarium cobalt permanent magnet material because Ta and Nb sputtering yield are close, the deposited TaNb coating has no too large component segregation, ta and Nb can form a denser coating than Ta, the outward diffusion and the inward diffusion of O of Sm can be effectively inhibited, the surface aging layer is prevented from being formed, and the loss of magnetic performance is reduced.
Test example 6
6.1 Under the same other conditions as in example 2, the influence of the working gas pressure for sputter plating on the magnetic properties of the permanent magnet material with a coating was examined, and the examination was carried out with reference to test example 1, with the results shown in the following table:
As can be seen from the table, when the working air pressure is 0.1-5 Pa, the sputtering plating is ensured, and meanwhile, the magnetic property loss after high-temperature aging is reduced. When the operating gas pressure is too low, sputtering is not possible. When the working air pressure is too high, the density of the plating layer is reduced, and the protective performance is reduced.
6.2 Under the same other conditions as in example 2, the influence of the sputtering power per target area for sputter plating on the magnetic properties of the permanent magnet material having a plating layer was examined, and the examination was performed with reference to test example 1, with the results shown in the following table:
As can be seen from the table, when the sputtering power per unit target area is 0.1-15W/cm 2, the magnetic property loss after high-temperature aging is reduced while the sputtering plating is ensured. When the sputtering power is too low, sputtering is impossible. The sputtering power is too high, the grains are coarse, and the protective performance of the coating is reduced.
6.3 Under the same other conditions as in example 2, the influence of the cleaning time for sputter plating on the magnetic properties of the permanent magnet material with a coating was examined, and the examination was carried out with reference to test example 1, with the results shown in the following table:
as can be seen from the table, when the cleaning time is more than or equal to 1min, the quality of the coating is improved, and the magnetic property loss after high-temperature aging is reduced.
6.4 Under the same other conditions as in example 2, the influence of the bias voltage for sputter plating on the magnetic properties of the plated permanent magnet material was examined, and the examination was made with reference to test example 1, with the results shown in the following table:
as can be seen from the table, when the bias voltage is-400 to-1V, the magnetic property loss after high-temperature aging is reduced.
6.5 Under the same other conditions as in example 4, the influence of the working gas pressure for ion plating on the magnetic properties of the permanent magnet material having a plating layer was examined, and the examination was carried out with reference to test example 2, with the results shown in the following table:
As can be seen from the table, when the working air pressure is 0.5-5 Pa, the ion plating is ensured, and meanwhile, the magnetic property loss after high-temperature aging is reduced.
6.6 Under the same other conditions as in example 4, the effect of the current density per target area for ion plating on the magnetic properties of the permanent magnet material having a plating layer was examined, and the examination was performed with reference to test example 2, with the results shown in the following table:
from the above table, it can be seen that the magnetic property loss after high temperature aging is reduced when the current density per unit target area is 0.5-5A/cm 2.
6.7 Under the same other conditions as in example 4, the effect of the ion plating cleaning time on the magnetic properties of the plated permanent magnet material was examined, and the examination was carried out with reference to test example 2, with the results shown in the following table:
As can be seen from the table, when the cleaning time is more than or equal to 1min, the magnetic property loss after high-temperature aging is reduced.
6.8 Under the same other conditions as in example 4, the influence of the bias voltage for ion plating on the magnetic properties of the permanent magnet material having a plating layer was examined, and the examination was made with reference to test example 2, with the results shown in the following table:
as can be seen from the table, when the bias voltage is-400 to-1V, the magnetic property loss after high-temperature aging is reduced.
The foregoing description of the preferred embodiments of the application is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the application.
Claims (9)
1. The coating for protecting the surface of the samarium cobalt permanent magnet material is characterized by comprising at least one of the following components:
tantalum oxide TaO X1, wherein 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 plating layer comprises two or more layers, each layer is stacked, and each layer comprises one of the following components:
tantalum oxide TaO X1, wherein X1 is any number between 0 and 2.5;
Tantalum nitride TaN X2, X2 is any number between 0 and 1.6;
Comprises an alloy of tantalum Ta and a metal M, M being at least one of V, nb, zr, hf, cr, al, ni.
2. The coating of claim 1, wherein the coating is,
The metal tantalum Ta is alpha phase or beta phase.
3. The coating of claim 1, wherein the coating is,
The thickness of the plating layer is 0.5-200 mu m.
4. The protection method for the surface of the samarium cobalt permanent magnet material is characterized by comprising the following steps of:
Depositing the coating of any one of claims 1-3 on the surface of the samarium cobalt permanent magnet material.
5. The protection method of claim 4, wherein,
The plating is deposited by sputter plating, ion plating or spray coating.
6. The protection method of claim 5, wherein,
Before the sputtering plating, cleaning the sputtering plated target, wherein the working air pressure is 0.1-5 Pa, the sputtering power per unit target area is 0.1-15W/cm 2, and the cleaning time is more than or equal to 1min.
7. The protection method of claim 5, wherein,
When the sputtering plating is carried out, the working air pressure is 0.1-5 Pa, the sputtering power per unit target area is 0.1-15W/cm 2, and a bias voltage of-400 to-1V is applied.
8. The protection method of claim 5, wherein,
Before ion plating, cleaning the ion plated target, wherein the working air pressure is 0.5-5 Pa, the current density of unit target area is 0.5-5A/cm 2, and the cleaning time is more than or equal to 1min.
9. The protection method of claim 5, wherein,
When the ion plating is carried out, the working air pressure is 0.5-5 Pa, the current density of unit target area is 0.5-5A/cm 2, and a bias voltage of-400 to-1V is applied.
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