CN108878092A - A kind of Ni-based thin soft magnetic sheet and preparation method thereof - Google Patents
A kind of Ni-based thin soft magnetic sheet and preparation method thereof Download PDFInfo
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- CN108878092A CN108878092A CN201810725933.5A CN201810725933A CN108878092A CN 108878092 A CN108878092 A CN 108878092A CN 201810725933 A CN201810725933 A CN 201810725933A CN 108878092 A CN108878092 A CN 108878092A
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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
- H01F1/12—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 soft-magnetic materials
- H01F1/33—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 soft-magnetic materials mixtures of metallic and non-metallic particles; metallic particles having oxide skin
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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
- H01F41/02—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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F7/00—Magnets
- H01F7/02—Permanent magnets [PM]
- H01F7/0205—Magnetic circuits with PM in general
- H01F7/021—Construction of PM
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F7/00—Magnets
- H01F7/02—Permanent magnets [PM]
- H01F7/0205—Magnetic circuits with PM in general
- H01F7/021—Construction of PM
- H01F7/0215—Flexible forms, sheets
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Abstract
The invention belongs to field of magnetic material, especially a kind of Ni-based thin soft magnetic sheet and preparation method thereof；Nano flake including being stacked with into sandwich-like, coated nickel-particle between upper and lower nano flake, nickel particle average-size are 45.4 nanometers, and there is a micro protrusion on surface, interlayer with a thickness of 400 ~ 500 nanometers；Ni-based thin soft magnetic sheet of the invention, nano nickel particles are wrapped between carbon nano flake, and antioxygenic property is strong, and sandwich stability is strong；Preparation method of the invention, preparation method simple process, it is at low cost, it can be achieved that scale produce in enormous quantities；The nanometer of sandwich-like nickel carbon nano-flake material is synthesized and obtained, the development of nickel-base material is promoted；The compound shows good soft magnetic characteristic；Meanwhile nano nickel particles are wrapped between carbon nano flake, inoxidizability increases.
Description
Technical field
The invention belongs to field of magnetic material, especially a kind of Ni-based thin soft magnetic sheet and preparation method thereof.
Background technique
Soft magnetic materials is that a kind of magnetization occurs to be not more than the material of 1000A/m in Hc.Because this kind of material has many excellent
Different performance, soft magnetic materials utilization get more and more extensive concerning of people (Journal of Magnetism and Magnetic Materials.2018,456,390-399).However, the magnetic conductivity of soft magnetic materials is influenced by several factors
Such as the size of particles of magnetic material, disperse situation, occupied state etc..So the microstructure of artificial designing material is come in fact
The soft magnetic characteristic of existing material is a good selection.A seed nucleus has been prepared in the members of Satoshi Mori seminar
The manganese-zinc ferrite of shell structure/iron silicon presses against compound, research find this compound have low-loss and high magnetic permeability (Advanced Powder Technology.2018, 29, 1481–1486).What seminar has also obtained the soft magnetism of polymer overmold bright-coloured system
Material (ACS Appl. Mater. Interfaces.2018,10,16947-16951.), and its ambient stable is improved
Property, but exploitation is dispersed in carbon-based soft magnetic metallic material still and has larger challenge.
Summary of the invention
The technical problem to be solved by the present invention is to：Overcome deficiency in the prior art, a kind of Ni-based thin soft magnetic sheet, the nickel are provided
Base thin soft magnetic sheet antioxygenic property is strong, and sandwich stability is strong, and it is a further object to provide a kind of Ni-based soft magnetisms
Preparation of sections method, it is the preparation method simple process, at low cost, industrialization large-scale production can be suitable for.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of Ni-based thin soft magnetic sheet, the nano flake including being stacked with into sandwich-like coat nickel between upper and lower nano flake
Grain, nickel particle average-size are 45.4 nanometers, and there is a micro protrusion on surface, interlayer with a thickness of 400 ~ 500 nanometers.
Further, the nickel particle is dispersed between two layers of carbon nano flake, and agglomeration is unobvious.
The method for preparing Ni-based thin soft magnetic sheet, the described method comprises the following steps：
（1）Prepare the hydroxide thin slice of nickel：By aequum and certain density ethylene glycol solution, ammonia spirit, sodium carbonate
Solution and nickel nitrate aqueous solution are added in reaction kettle, and stirring half an hour forms homogeneous solution.It is dry to be put into air dry oven；
（2）Prepare interlayer glucose/nickel hydroxide precursor：The mixing of the hydroxide of a certain amount of glucose and nickel, turns
It moves on in reaction kettle, it is dry to be put into air dry oven；
（3）Prepare Ni-based interlayer carbon complex：Step 2 is obtained into interlayer glucose/nickel hydroxide precursor and is placed on quartz
Guan Zhong is calcined under the conditions of nitrogen atmosphere.
Further, the step（1）The volume of middle ethylene glycol solution is 10mL, and the volume of ammonium hydroxide is 12mL, sodium carbonate
Concentration of aqueous solution is 1mol/L, and volume 4mL, nickel nitrate aqueous solution concentration is 1mol/L, volume 4mL.
Further, the step（1）In, reaction condition 180o16 h under C.
Further, the step（2）In, the quality of glucose is 0.9g, and the quality of the hydroxide of nickel is 0.1g, water
Volume be 30mL, reaction condition 180o8 h under C.
Further, the step（3）Middle calcination condition is in a nitrogen atmosphere, in 800 oC3 h of lower calcining, heating speed
Rate is 2 oC/min。
It is using the beneficial effect of technical solution of the present invention：
1, Ni-based thin soft magnetic sheet of the invention, nano nickel particles are wrapped between carbon nano flake, and antioxygenic property is strong, interlayer
Structural stability is strong；
2, preparation method of the invention, preparation method simple process, it is at low cost, it can be achieved that scale produce in enormous quantities.Synthesis is simultaneously
And the nanometer nickel carbon nano-flake material of sandwich-like has been obtained, promote the development of nickel-base material.The compound shows good
Good soft magnetic characteristic.Meanwhile nano nickel particles are wrapped between carbon nano flake, inoxidizability increases.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is the X ray diffracting spectrum of the Ni-based interlayer carbon nano flake of soft magnetism made from the embodiment of the present invention 1；
Fig. 2 is the SEM photograph of the Ni-based interlayer carbon nano flake of soft magnetism made from the embodiment of the present invention 1；
Fig. 3 is the TEM photo of the Ni-based interlayer carbon nano flake of soft magnetism made from the embodiment of the present invention 1；
Fig. 4 is the hysteresis loop figure of the Ni-based interlayer carbon nano flake of soft magnetism made from the embodiment of the present invention 1.
Fig. 5 is the magnetic conductivity figure of the Ni-based interlayer carbon nano flake of soft magnetism made from the embodiment of the present invention 1.
Specific embodiment
The following examples can make those skilled in the art that the present invention be more fully understood, but these embodiments are not
Limiting the scope of the invention." one embodiment " or " embodiment " referred to herein, which refers to, may be included in the present invention at least
A particular feature, structure, or characteristic in one implementation.In the present specification different places occur " in one embodiment
In " the same embodiment not is referred both to, nor the individual or selective embodiment mutually exclusive with other embodiments.
Embodiment 1
A kind of Ni-based interlayer carbon nano flake of soft magnetism is the Ni-based carbon nano flake of sandwich-like, and nano flake is stacked with, interlayer
Thickness is about 400 ~ 500 nanometers；Nickel particle is wrapped in one layer of centre by upper and lower two panels nano flake, and nickel particle growth causes table
There are some protrusions in face, and mean nickel particle size is 45.4 nanometers.The present invention uses the method and high-temperature heat treatment system of two step hydro-thermals
For a kind of Ni-based interlayer carbon nano flake of soft magnetism.
A kind of preparation method of the above-mentioned Ni-based interlayer carbon nano flake of soft magnetism, specifically includes the following steps：
Step 1, the hydroxide thin slice of nickel is prepared：By the ethylene glycol solution of 10mL, the ammonia spirit of 12mL, the 1mol/L of 4mL
It is to stir half small in 50mL reaction kettle that the 1mol/L nickel nitrate aqueous solution of aqueous sodium carbonate and 4mL, which are added to capacity,
When form homogeneous solution.It is put into 180 in air dry ovenoIt is dried after reacting 16 h under the conditions of C；
Step 2, interlayer glucose/nickel hydroxide precursor is prepared：The hydroxide of the nickel of the glucose and 0.1g of 0.9g
It is blended in the water of 30mL, is transferred in the reaction kettle of 50mL, be put into 180 in air dry ovenoAfter reacting 8 h under the conditions of C
It is dry；
Step 3, Ni-based interlayer carbon complex is prepared：Step 2 is obtained into interlayer glucose/nickel hydroxide precursor and is placed on stone
Ying Guanzhong, nitrogen atmosphere, 800 oC3 h of lower calcining, heating rate 2 oC/min。
Fig. 1 is the X ray diffracting spectrum of the Ni-based interlayer carbon nano flake of soft magnetism made from the embodiment of the present invention 1, can from Fig. 1
To find out, wherein the characteristic peak of W metal and standard PDF#04-0850 card are corresponded, and illustrate that W metal crystallinity is good,
The characteristic peak of carbon can also be found out simultaneously.
Fig. 2 is the SEM photograph of the Ni-based interlayer carbon nano flake of soft magnetism made from the embodiment of the present invention 1, can from Fig. 2
Out, Ni-based carbon nano flake is sandwich, and thickness of interlayer is about 400 ~ 500nm, and nickel particle growth causes thin slice to have protrusion.
Fig. 3 is the TEM photo of the Ni-based interlayer carbon nano flake of soft magnetism made from embodiment 1, from figure 3, it can be seen that nickel
Grain is dispersed among upper layer and lower layer carbon nano flake, and agglomeration is unobvious, and the granular size of mean nickel particle is 45.4nm.
Fig. 4 is the hysteresis loop figure of the Ni-based interlayer carbon nano flake of soft magnetism made from embodiment 1, from fig. 4, it can be seen that nickel
Base interlayer carbon nano flake shows soft magnetic characteristic, and magnetic field strength is close to 8kOe, saturation magnetisation value 52.3emu/g.
Fig. 5 is the magnetic conductivity figure of the Ni-based interlayer carbon nano flake of soft magnetism made from embodiment 1, from fig. 5, it can be seen that Ni-based
The real part of the magnetic conductivity of interlayer carbon nano flake is near 1.2.
The Ni-based interlayer carbon nano flake of soft magnetism of the present invention, synthesis technology is simple, easy to operate, may be implemented to industrialize big rule
Mould production.Promote metallic nickel/carbon material synthesis development.In addition, due to its special nanostructure, metallic nickel is not easy by oxygen
Change and corrosion, inoxidizability enhance.Characteristic with soft magnetic materials.
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.It is all in essence of the invention
Within mind and principle, any modification, equivalent substitution, improvement and etc. done be should all be included in the protection scope of the present invention.This
The technical scope of item invention is not limited to the contents of the specification, it is necessary to its technology is determined according to scope of the claims
Property range.
Claims (8)
1. a kind of Ni-based thin soft magnetic sheet, it is characterised in that：Nano flake including being stacked with into sandwich-like, upper and lower nano flake
Between coated nickel-particle, nickel particle average-size be 45.4 nanometers, there is micro protrusion on surface, and interlayer is received with a thickness of 400 ~ 500
Rice.
2. a kind of Ni-based thin soft magnetic sheet according to claim 1, it is characterised in that：The nickel particle is dispersed in two layers of carbon and receives
Between rice thin slice, agglomeration is unobvious.
3. the method for preparation such as Ni-based thin soft magnetic sheet of any of claims 1-2, it is characterised in that：The method packet
Include following steps：
（1）Prepare the hydroxide thin slice of nickel：By aequum and certain density ethylene glycol solution, ammonia spirit, sodium carbonate
Solution and nickel nitrate aqueous solution are added in reaction kettle, and stirring half an hour forms homogeneous solution.
4. it is dry to be put into air dry oven；
（2）Prepare interlayer glucose/nickel hydroxide precursor：The mixing of the hydroxide of a certain amount of glucose and nickel, turns
It moves on in reaction kettle, it is dry to be put into air dry oven；
（3）Prepare Ni-based interlayer carbon complex：Step 2 is obtained into interlayer glucose/nickel hydroxide precursor and is placed on quartz
Guan Zhong is calcined under the conditions of nitrogen atmosphere.
5. the preparation method of Ni-based thin soft magnetic sheet according to claim 3, it is characterised in that：The step（1）Middle second two
The volume of alcoholic solution is 10mL, and the volume of ammonium hydroxide is 12mL, and aqueous sodium carbonate concentration is 1mol/L, volume 4mL, nickel nitrate
Concentration of aqueous solution is 1mol/L, volume 4mL.
6. the preparation method of Ni-based thin soft magnetic sheet according to claim 3, it is characterised in that：The step（1）In, reaction
Condition is 180o16 h under C.
7. the preparation method of Ni-based thin soft magnetic sheet according to claim 3, it is characterised in that：The step（2）In, grape
The quality of sugar is 0.9g, and the quality of the hydroxide of nickel is 0.1g, and the volume of water is 30mL, reaction condition 180o8 under C
h。
8. the preparation method of Ni-based thin soft magnetic sheet according to claim 3, it is characterised in that：The step（3）Middle calcining
Condition is in a nitrogen atmosphere, in 800 o3 h, heating rate 2 are calcined under C oC/min。
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| CN105887160A (en) * | 2015-01-12 | 2016-08-24 | 刘艳娇 | Preparation method for thermoelectrical composite thin film with nano nickel loaded on graphene |
| CN107325283A (en) * | 2017-07-21 | 2017-11-07 | 张娟 | A kind of soluble polyaniline doped graphene cladding nano nickel composite wave-suction material and preparation method thereof |
| US20180126368A1 (en) * | 2016-11-07 | 2018-05-10 | Council Of Scientific & Industrial Research | Process for the production of graphene sheets with tunable functionalities from seaweed promoted by deep eutectic solvents |
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2018
- 2018-07-04 CN CN201810725933.5A patent/CN108878092B/en active Active
Patent Citations (7)
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|---|---|---|---|---|
| JP2003201121A (en) * | 2001-12-27 | 2003-07-15 | National Institute Of Advanced Industrial & Technology | Method for manufacturing laminated manganese oxide nanocomplex |
| CN102576876A (en) * | 2009-08-10 | 2012-07-11 | 巴特尔纪念研究院 | Self assembled multi-layer nanocomposite of graphene and metal oxide materials |
| CN104538595A (en) * | 2014-12-10 | 2015-04-22 | 南京师范大学 | Lithium ion battery cathode material embedded nano metal loaded carbon nanosheet as well as preparation method and application thereof |
| CN105887160A (en) * | 2015-01-12 | 2016-08-24 | 刘艳娇 | Preparation method for thermoelectrical composite thin film with nano nickel loaded on graphene |
| CN105390676A (en) * | 2015-11-02 | 2016-03-09 | 北京师范大学 | Quick preparation method for graphene base metal or metal oxide with sandwich structure |
| US20180126368A1 (en) * | 2016-11-07 | 2018-05-10 | Council Of Scientific & Industrial Research | Process for the production of graphene sheets with tunable functionalities from seaweed promoted by deep eutectic solvents |
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