CN109695017A - A kind of preparation method of high magnetic material - Google Patents
A kind of preparation method of high magnetic material Download PDFInfo
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- CN109695017A CN109695017A CN201811655243.3A CN201811655243A CN109695017A CN 109695017 A CN109695017 A CN 109695017A CN 201811655243 A CN201811655243 A CN 201811655243A CN 109695017 A CN109695017 A CN 109695017A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/085—Oxides of iron group metals
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/08—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of metallic material
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- 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
- H01F41/14—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 applying magnetic films to substrates
- H01F41/18—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 applying magnetic films to substrates by cathode sputtering
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- 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
- H01F41/14—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 applying magnetic films to substrates
- H01F41/22—Heat treatment; Thermal decomposition; Chemical vapour deposition
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- Manufacturing & Machinery (AREA)
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- General Chemical & Material Sciences (AREA)
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Abstract
The invention discloses a kind of preparation methods of high magnetic material, are related to a kind of preparation method of high magnetic material, are mainly used in the application of field of magnetic material.The technical problem to be solved is that nano particle and magnetic material parent are combined, high magnetic intensity material is prepared.Be characterized in that: magnetic nanoparticle is embedded among magnetic parent, it is generated in preparation process or after preparing magnetic parent by annealing, it anneals while magnetic field is added, the interaction between magnetic Nano and magnetic parent will be increased, increase curie point and the intensity of magnetization, the optimum temperature of annealing will be different with the different of material.Material is prepared simply, can prepare high performance material using magnetron sputtering method, hydro-thermal method and thermal decomposition method, the invention of this material can be for, in sensor, the material new using offer of magnetic storage, transformer, communication, wireless charging field selects in magnetic material.
Description
Technical field
The present invention relates to a kind of preparation methods of high magnetic material, are mainly used in the application of field of magnetic material.
Background technique
Magnetic material mainly has soft magnetism and hard magnetic material.It is usually to have Fe, Co, Ni and their compound are formed.Hard Magnetic
Material requirements coercivity is high, and soft magnetic materials needs coercivity small.However, either Hard Magnetic or soft magnetic materials, the intensity of magnetization is all
It is that the higher the better for requirement.The investigation of materials of high magnetic intensity is made slow progress between last 100 years, in addition to FeCo alloy and Fe8N is ground
Outside studying carefully, almost without other materials, moreover, Fe8The stability of N is always a problem.
Summary of the invention:
A kind of preparation method of high magnetic material of the present invention the technical problem to be solved is that: nano particle and magnetism material
Material parent combines, and prepares high magnetic intensity material, provides new material selection for the application of magnetic material.
A kind of preparation method of high magnetic material of the present invention is adopted the technical scheme that: magnetic nanoparticle is embedded in magnetic
Among sexupara body, the chemical component of the material is by mole meter: nano particle 0-50%；Magnetic matrix/fertile material
50%-100%；The magnanimity of magnetic nanoparticle can from 10% to 50%, magnetic nanoparticle is less than 10 nanometers, magnetic Nano
Particle can be Fe, Co, Ni, Gd and rare earth metal or NiO, CoO, Co3O4、FeO、Fe2O3、Fe3O4It is antiferromagnetic and ferrous
Magnetic nano particle,
Preparation method can pass through following several preparation approachs:
(1) preparation method of film high magnetic material: for Ni/NiO, using magnetic control sputtering device grow layer of Ni, one layer
NiO, then layer of Ni, then another layer NiO, repeats five times in this way, and every layer of thickness needs accurate control, and only about 1-2 receives
Rice is thick；The lower annealing of magnetism: usually after 10 multilayer films of preparation, the film of preparation is annealed under the atmosphere of hydrogen, the temperature of annealing
Ni/NiO optimum temperature is spent at 200 degree, and the intensity of magnetization that magnetic field is added is greater than 0.1 tesla；
(2) preparation method of nano particle high magnetic material: for Ni/NiO, nickel acetate (1M) and
Ethylene glycol (100ml) is heated to 194 degree.Nickel acetate resolves into Ni, and certain density oxygen is passed into
In container, Ni/NiO is formed, and equally, thermal decomposition method, hydro-thermal method can prepare high magnetic material；
Magnetic nanoparticle is embedded among magnetic parent, and magnetic-particle can generate in preparation process, can also be with
It is generated after the magnetic parent of preparation by annealing, anneal while magnetic field is added, will increased between magnetic Nano and magnetic parent
Interaction, increases curie point and the intensity of magnetization, and the optimum temperature of annealing will be different with the different of material, Fe/Fe3O4400
Degree, usually in 100-400 degree, the magnetic field provided needs to be greater than 0.1 tesla the temperature of annealing,
A kind of preparation method of high magnetic material of the present invention the utility model has the advantages that material preparation is simple, material is two kinds of members
The compound of element, can prepare high performance material using magnetron sputtering method, hydro-thermal method and thermal decomposition method；
Under room temperature, performance all improves a lot than magnetic matrix/parent intensity of magnetization, under low temperature, higher property
It can be observed, it means that the improvement of technique will further improve the performance of material.
The invention of this material can be in magnetic material in sensor, magnetic storage, transformer, communication, wireless charging field
Application new material selection is provided.
The performance of the material prepared under the method for the present invention all improves a lot than magnetic matrix/parent intensity of magnetization.
For example, 54emu/g of the intensity of magnetization 180emu/g. compared to Ni that Ni/NiO film prepares display under magnetron sputtering is improved
Very much, the intensity of magnetization that Fe/Fe3O4 film is shown reaches 220emu/g of the 400emu/g. compared to Fe and also improves very much, and
And the intensity of magnetization than Fe8N also improves very much.
Specific embodiment
Embodiment 1: a kind of preparation method of high magnetic material of the present invention for Ni/NiO, is grown using magnetic control sputtering device
Layer of Ni, layer of Ni O, then layer of Ni, then another layer NiO, repeats five times in this way, and every layer of thickness needs accurate control, greatly
About there was only 1-2 nanometer thickness, the lower annealing of magnetism: usually after 10 multilayer films of preparation, the film of preparation is moved back under the atmosphere of hydrogen
Fire.For the temperature Ni/NiO optimum temperature of annealing at 200 degree, the intensity of magnetization that magnetic field is added is greater than 0.1 tesla；
Magnetron sputtering selects U.S. Discovery system, and the target diameter of metallic nickel is two inches, purity 99.99%,
Substrate is quartz, and size 10mm*10mm*1mm is first plated in 2nm Ni on quartz substrate, then plates 2nm NiO, this is logical
It crosses and is passed through certain oxygen and is aoxidized by Ni, plate totally 10 layers of Ni and NiO in turn in this way, topmost plate one layer of 10nm Al for one layer, prevent
Only Ni is aoxidized, and the sample plated, which is taken in annealing furnace, anneals, and in annealing process, the magnetic field 2000Oe is added among the sample of annealing,
Annealing temperature is 100-400 degree, the results showed that 200 degree of annealing obtain high magnetic material.
Magnetic nanoparticle is embedded among magnetic parent, and magnetic-particle can generate in preparation process, can also be with
It is generated after the magnetic parent of preparation by annealing, anneal while magnetic field is added, will increased between magnetic Nano and magnetic parent
Interaction, increases curie point and the intensity of magnetization, and the optimum temperature of annealing will be different with the different of material, Fe/Fe3O4400
Degree, usually in 100-400 degree, the magnetic field provided needs to be greater than 0.1 tesla the temperature of annealing.
For embodiment 2:Ni/NiO, nickel acetate (1M) and ethylene glycol (100ml) are heated to
194 degree, nickel acetate resolves into Ni, and at this moment, certain density oxygen is passed into container, and Ni/NiO is formed, equally,
Thermal decomposition method, hydro-thermal method can prepare high magnetic material.
Thermal decomposition method prepares the material of high magnetic-particle.Detailed process is as follows.Nickel acetate (1M) first uses alcohol
Dissolution is then and ethylene glycol (100ml) Hybrid Heating is to 194 degree, and 194 degree are exactly ethylene glycol's
Gasification temperature.Therefore, temperature is highly stable, and the copper sheet of 10mm*10mm*1mm size is put into mixed solution, at this moment certain dense
The oxygen of degree is passed into heating container, in this way, nickel acetate (1M) pyrolysis is grown in copper base at Ni/NiO film
On, the Ni/NiO of this method preparation, the intensity of magnetization can achieve 180emu/g.
Claims (2)
1. a kind of preparation method of high magnetic material, it is characterised in that: magnetic nanoparticle is embedded among magnetic parent, the material
The chemical component of material is by mole meter: nano particle 0-50%, and magnetic matrix/fertile material 50%-100%, magnetism is received
The magnanimity of rice grain can from 10% to 50%, magnetic nanoparticle less than 10 nanometers, magnetic nanoparticle can be Fe, Co,
Ni, Gd and rare earth metal or NiO, CoO, Co3O4、FeO、Fe2O3、Fe3O4Antiferromagnetic and ferrimagnetism magnetic nanoparticle,
Preparation method can pass through following several preparation approachs:
(1) preparation method of film high magnetic material: for Ni/NiO, using magnetic control sputtering device grow layer of Ni, layer of Ni O,
Layer of Ni again, then another layer NiO, repeats five times in this way, and every layer of thickness needs accurate control, only about 1-2 nanometer thickness,
The lower annealing of magnetism, after usually preparing 10 multilayer films, the film of preparation is annealed under the atmosphere of hydrogen, and the temperature of annealing is usual
In 100-400 degree, different materials, the temperature of annealing needs to adjust, and the magnetic field provided needs to be greater than 0.2 tesla；
(2) preparation method of nano particle high magnetic material: for Ni/NiO, nickel acetate (1M) and ethylene
Glycol (100ml) is heated to 194 degree.Nickel acetate resolves into Ni, and certain density oxygen is passed into container,
Ni/NiO is formed, and equally, thermal decomposition method, hydro-thermal method can prepare high magnetic material.
2. the preparation method of high magnetic material according to claim 1, it is characterised in that: magnetic nanoparticle is embedded in magnetism
Among parent, magnetic-particle can generate in preparation process, can also be generated, be moved back by annealing after preparing magnetic parent
Magnetic field is added simultaneously in fire, will increase the interaction between magnetic Nano and magnetic parent, increases curie point and the intensity of magnetization, move back
The optimum temperature of fire will be different with the different of material.Ni/NiO optimum temperature is at 200 degree, Fe/Fe3O4At 400 degree, magnetic is added
The intensity of magnetization of field is greater than 0.1 tesla.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811655243.3A CN109695017A (en) | 2018-12-29 | 2018-12-29 | A kind of preparation method of high magnetic material |
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| CN201811655243.3A CN109695017A (en) | 2018-12-29 | 2018-12-29 | A kind of preparation method of high magnetic material |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103824673A (en) * | 2014-02-27 | 2014-05-28 | 中山大学 | Magnetic nano-particle film with exchange bias effect and preparation method thereof |
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- 2018-12-29 CN CN201811655243.3A patent/CN109695017A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103824673A (en) * | 2014-02-27 | 2014-05-28 | 中山大学 | Magnetic nano-particle film with exchange bias effect and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 刘先松等: "单分散Ni球制备及Ni/NiO的磁性研究", 《稀有金属材料与工程》 * |
| 王文鼐 等: "Ni/NiO界面的高场磁化研究", 《物理学报》 * |
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