CN112687442A - Preparation method of reticular multi-layer samarium cobalt nanowire - Google Patents
Preparation method of reticular multi-layer samarium cobalt nanowire Download PDFInfo
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- CN112687442A CN112687442A CN202110059508.9A CN202110059508A CN112687442A CN 112687442 A CN112687442 A CN 112687442A CN 202110059508 A CN202110059508 A CN 202110059508A CN 112687442 A CN112687442 A CN 112687442A
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- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 title claims abstract description 42
- 239000002070 nanowire Substances 0.000 title claims abstract description 32
- KPLQYGBQNPPQGA-UHFFFAOYSA-N cobalt samarium Chemical compound [Co].[Sm] KPLQYGBQNPPQGA-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229920006289 polycarbonate film Polymers 0.000 claims abstract description 50
- 238000010884 ion-beam technique Methods 0.000 claims abstract description 20
- 239000004417 polycarbonate Substances 0.000 claims abstract description 20
- 238000004070 electrodeposition Methods 0.000 claims abstract description 17
- 239000002052 molecular layer Substances 0.000 claims abstract description 7
- 238000005516 engineering process Methods 0.000 claims abstract description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 14
- 238000000151 deposition Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 239000002090 nanochannel Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 229910000366 copper(II) sulfate Inorganic materials 0.000 claims description 5
- 230000001678 irradiating effect Effects 0.000 claims description 5
- 229920000515 polycarbonate Polymers 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 4
- 239000004327 boric acid Substances 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 4
- 239000001509 sodium citrate Substances 0.000 claims description 4
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 4
- 238000003486 chemical etching Methods 0.000 claims description 3
- 239000008139 complexing agent Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 2
- 238000007747 plating Methods 0.000 claims description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 2
- 238000007669 thermal treatment Methods 0.000 claims description 2
- 230000003307 reticuloendothelial effect Effects 0.000 claims 1
- 230000008878 coupling Effects 0.000 abstract description 2
- 238000010168 coupling process Methods 0.000 abstract description 2
- 238000005859 coupling reaction Methods 0.000 abstract description 2
- 230000005347 demagnetization Effects 0.000 abstract description 2
- 230000003993 interaction Effects 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 6
- 230000005476 size effect Effects 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000006250 one-dimensional material Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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- Other Surface Treatments For Metallic Materials (AREA)
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Abstract
The invention discloses a preparation method of a reticular multilayer samarium cobalt nanowire, which is characterized in that a polycarbonate film (PC) template containing a 3D reticular structure channel is prepared by high-energy heavy ion beams, and a pulse electrodeposition technology is utilized to prepare a network (SmCo)1‑xCuxthe/Cu nanowire is in a mutually connected net structure, can be directly used as a magnetic nano device, and enhances the coercivity by introducing the non-magnetic nano layer Cu to enhance the demagnetization coupling interaction of samarium cobalt.
Description
Technical Field
The invention relates to a preparation method of a samarium cobalt magnet, in particular to a preparation method of a reticular samarium cobalt nanowire, belonging to the technical field of permanent magnet materials.
Background
The one-dimensional nano magnetic material is used as the research foundation of other low-dimensional nano materials, is closely related to nano electronic devices and micro sensors, has wide application prospect in the aspects of developing nano electronic devices in the micro field and the like, and can be used as nano devices, needle points of scanning tunnel microscopes, optical fibers, sensitive materials, connecting lines of super-large-scale integrated circuits, micro drill bits, reinforcing agents of composite materials and the like. Samarium cobalt permanent magnet materials are still of great value as first and second generation permanent magnets due to their advantages of significant magnetic anisotropy, high curie temperature, etc. Samarium cobalt nanometer line is as one-dimensional material, and nanometer material has small size effect, surface effect, quantum size effect and macroscopic quantum tunnel effect etc. is the key material of nanometer assembly technique.
At present, the preparation method of samarium cobalt low-dimensional material mainly comprises vapor deposition, sputtering, spin coating, electrodeposition and the like, magnetron sputtering and the like have the defects of high cost, high process requirement and the like, and researchers try to find a process with low cost and simple operation. Electrodeposition is an excellent material preparation means, has the advantages of simple equipment, low cost, high production efficiency and the like, and researchers make attempts to prepare rare earth permanent magnetic materials by electrodeposition. Wherein the Hebei industry university utilizes electrodeposition and an AAO alumina template to prepare samarium cobalt nanowires, and the ratio of Sm to Co ions is adjusted to find that when the ratio of Sm to Co ions is 6: 1, the obtained magnetic performance is optimal, but the nanowire prepared by the method cannot stand and cannot be directly used as a device, so that the application of the nanowire as a nanometer device is limited to a certain extent, and the coercivity of the obtained SmCo nanowire is low due to the nanometer size effect.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of the samarium-cobalt reticular magnetic nanowire.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a preparation method of the samarium-cobalt net-shaped magnetic nanowire comprises the following steps:
1) manufacturing a mesh PC channel template: the method comprises the steps of irradiating the surface of a polycarbonate film (PC) by using a high-energy heavy ion beam, taking the heavy ion beam as a normal line in the irradiation process, firstly adjusting the angle of the polycarbonate film to enable the irradiation angle of the polycarbonate film and the heavy ion beam to be alpha, then rotating the polycarbonate film to enable the irradiation angle of the carbonate film and the heavy ion beam to be-alpha, irradiating the polycarbonate by using the heavy ion beam twice, forming a net-shaped nano-channel network in the polycarbonate film, putting the polycarbonate film into Na (OH) solution, expanding holes of the nano-channel network by using a chemical etching method to form a PC channel template with a 3D net-shaped structure, and finally plating a layer of Au/Pt film on the surface of the polycarbonate film by using an electronic evaporation method.
2) Chemical electrodeposition: preparing Sm with a certain concentration2(SO4)3，CoSO4And CuSO4Mixed solution as a chemicalAn electrodeposition solution, one or more of boric acid, citric acid and sodium citrate are used as complexing agents, the reticular PC channel template obtained in the step 1 is placed into the electrodeposition solution, an electrochemical workstation is utilized, an Au/Pt thin film on the template is used as a cathode, Ag/AgCl is used as a reference electrode and Pt is used as a counter electrode, a pulse electrodeposition technology is adopted, the deposition potential is switched between-2V and-0.4V, 2.4V is used for depositing SmCo materials, 0.4V is used for depositing Cu, the pulse duration of the-2.4V is 500 ms-1 s, the pulse duration of the-0.4V is 1 s-2 s, and a reticular (SmCo) is deposited in a polycarbonate thin film1-xCuxCu multilayer nanowire, where x is less than or equal to 0.05, (SmCo)1-xCuxThe thickness of the Cu nano layer is 10nm to 20nm, and the thickness of the Cu nano layer is 1nm to 2 nm.
3) Removing the template: the (SmCo) obtained in step 21-xCuxPutting the polycarbonate film of the/Cu nanowire into a dichloromethane solution, and dissolving the polycarbonate film to obtain a net shape (SmCo)1-xCuxA Cu nanowire.
4) Aging treatment: subjecting the resultant web (SmCo) obtained in step 3 to a thermal treatment1-xCuxthe/Cu nano-wire is 600-850oAnd C, carrying out aging treatment for 2-4 h under the protection of nitrogen, and cooling to room temperature along with the furnace.
Specifically, the energy of the high-energy heavy ion beam in the step 1 is 5 MeV-10 MeV, the diameter of an irradiation area is 2cm, and the frequency is 1 Hz-2 Hz; the thickness of the polycarbonate film is 20-100 mu m; the irradiation angle alpha of the carbonate film and the heavy ion beam is 20o~45oThe diameter of the reticular nano channel obtained after the pore is opened is 50 nm-200 nm; the thickness of the Au/Pt film on the plated surface of the polycarbonate film is 500 nm-1 mu m.
Specifically, Sm described in step 22(SO4)3,CoSO4And CuSO4In the mixed solution, the atomic ratio of Sm to Co to Cu is 1: 5-8.5: 0.002-0.008.
Specifically, the concentration of the dichloromethane solution in the step 3 is 0.5 molL-1~2 molL-1。
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) through preparing a polycarbonate film (PC) three-dimensional nano-channel template, depositing samarium-cobalt reticular nanowires on the template, wherein the obtained nanowires form a mutually connected reticular structure and can be directly used as a magnetic nano device;
(2) according to the invention, the nonmagnetic nano-layer Cu is introduced into the samarium cobalt nanowire to form a SmCo/Cu multilayer nanowire structure, so that the demagnetization coupling interaction of samarium cobalt is enhanced, and the coercivity is improved.
Detailed Description
The present invention will be further described with reference to the following specific embodiments and comparative examples.
Example 1
1) Manufacturing a mesh PC channel template: irradiating the surface of a polycarbonate film (PC) by using high-energy heavy ion beams with the energy of 5MeV and the frequency of 1Hz, wherein the thickness of the polycarbonate film (PC) is 30 mu m, and in the irradiation process, the heavy ion beams are taken as normal lines, the angle of the polycarbonate film is firstly adjusted, so that the irradiation angle of the polycarbonate film and the heavy ion beams is 45 oRotating the polycarbonate film to make the irradiation angle between the polycarbonate film and the heavy ion beam be-45 DEG oAfter the polycarbonate film is irradiated by heavy ion beams twice, a reticular nano-channel network is formed inside the polycarbonate film, the polycarbonate film is put into Na (OH) solution, the pores of the nano-channel network are expanded by a chemical etching method to form a PC channel template with a 3D reticular structure, the pore diameter is 50nm, and finally, an Au film with the thickness of 500nm is plated on the surface of the polycarbonate film by using an electronic evaporation method;
2) chemical electrodeposition: 0.5mol L of the mixture is prepared-1 Sm2(SO4)3, 5 mol L-1CoSO4And 0.008 mol L-1 CuSO4Putting the reticular PC channel template obtained in the step 1 into the electro-deposition solution by taking boric acid and sodium citrate as complexing agents and boric acid and sodium citrate as chemical electro-deposition solutions, using an electrochemical workstation, taking an Au thin film on the template as a cathode, Ag as a reference electrode and Pt as a counter electrode, adopting a pulse electro-deposition technology, switching the deposition potential between-2V and-0.4V, depositing a SmCo material at-2.4V, and depositing a SmCo material at-0.4VCu, pulse duration of-2.4V is 500ms, pulse duration of-0.4V is 1s, and network (SmCo) is obtained by deposition in polycarbonate film0.97Cu0.03Cu multilayer nanowire, where x is less than or equal to 0.05, (SmCo)0.97Cu0.03The thickness of (2) is 10nm, and the thickness of the Cu nanolayer is 1 nm.
3) Removing the template: subjecting the resulting network-containing (SmCo) obtained in step 2 to0.97Cu0.03A polycarbonate film of/Cu multilayer nanowire, 0.5mol L of-1The polycarbonate film was sufficiently dissolved in the methylene chloride solution to obtain a network (SmCo)0.97Cu0.03A Cu multilayer nanowire.
4) Aging treatment: SmCo obtained in the step 30.97Cu0.03the/Cu multilayer nanowire is 600oC, carrying out aging treatment for 2 hours under the protection of nitrogen, and cooling to room temperature along with the furnace.
Prepared (SmCo)0.97Cu0.03The magnetic performance of a/Cu multilayer nanowire sample is tested by PPMS (polypropylene-random-Mass Spectrometry), and compared with samarium-cobalt nanowires prepared by AAO alumina templates in the literature, and the comparison result is shown in Table 1.
TABLE 1
Claims (3)
1. A preparation method of the reticular multi-layer samarium cobalt nanowire is characterized by comprising the following steps:
1) manufacturing a mesh PC channel template: irradiating the surface of a polycarbonate film (PC) by using a high-energy heavy ion beam, taking the heavy ion beam as a normal line in the irradiation process, firstly adjusting the angle of the polycarbonate film, enabling the irradiation angle of the polycarbonate film and the heavy ion beam to be alpha, then rotating the polycarbonate film, enabling the irradiation angle of the carbonate film and the heavy ion beam to be-alpha, irradiating the polycarbonate by using the heavy ion beam twice, forming a net-shaped nano-channel network in the inner part, putting the polycarbonate film into Na (OH) solution, expanding the holes of the nano-channel network by using a chemical etching method, forming a PC channel template with a 3D net-shaped structure, and finally plating an Au/Pt film on the surface of the polycarbonate film by using an electronic evaporation method;
2) chemical electrodeposition: preparing Sm with a certain concentration2(SO4)3，CoSO4And CuSO4The mixed solution is used as a chemical electrodeposition solution, one or more of boric acid, citric acid and sodium citrate is used as a complexing agent, the reticular PC channel template obtained in the step 1 is placed into the electrodeposition solution, an electrochemical workstation is utilized, an Au/Pt film on the template is used as a cathode, Ag/AgCl is used as a reference electrode and Pt is used as a counter electrode, a pulse electrodeposition technology is adopted, the deposition potential is switched between-2V and-0.4V, -2.4V is used for depositing SmCo material, -0.4V is used for depositing Cu, the pulse duration of the-2.4V is 500 ms-1 s, the pulse duration of the-0.4V is 1 s-2 s, and a reticular (SmCo) is deposited in a polycarbonate film1-xCuxCu multilayer nanowire, where x is less than or equal to 0.05, (SmCo)1-xCuxThe thickness of the Cu nano layer is 10nm to 20nm, and the thickness of the Cu nano layer is 1nm to 2 nm;
3) removing the template: the (SmCo) obtained in step 21-xCuxPutting the polycarbonate film of the/Cu nanowire into a dichloromethane solution, and dissolving the polycarbonate film to obtain a net shape (SmCo)1-xCuxA Cu nanowire;
4) aging treatment: subjecting the resultant web (SmCo) obtained in step 3 to a thermal treatment1-xCuxthe/Cu nano-wire is 600-850oAnd C, carrying out aging treatment for 2-4 h under the protection of nitrogen, and cooling to room temperature along with the furnace.
2. The method of making reticulated multilayer samarium cobalt nanowires of claim 1, wherein: the energy of the high-energy heavy ion beam is 5 MeV-10 MeV, the diameter of an irradiation area is 2cm, and the frequency is 1 Hz-2 Hz; the thickness of the polycarbonate film is 20-100 mu m; the irradiation angle alpha of the carbonate film and the heavy ion beam is 20o~45oThe diameter of the reticular nano channel obtained after the pore is opened is 50 nm-200 nm; the thickness of the Au/Pt film on the plated surface of the polycarbonate film is 500 nm-1 mu m.
3. The method of making samarium cobalt reticuloendothelial multilayer nanowires of claim 1, said Sm2(SO4)3,CoSO4And CuSO4In the mixed solution, the atomic ratio of Sm to Co to Cu is 1: 5-8.5: 0.002-0.008; the concentration of the dichloromethane solution is 0.5mol L-1~2 molL-1。
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