CN109448948A - A kind of Fe/CNT ring-type powder core composite material and preparation method - Google Patents
A kind of Fe/CNT ring-type powder core composite material and preparation method Download PDFInfo
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- CN109448948A CN109448948A CN201811256372.5A CN201811256372A CN109448948A CN 109448948 A CN109448948 A CN 109448948A CN 201811256372 A CN201811256372 A CN 201811256372A CN 109448948 A CN109448948 A CN 109448948A
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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
Abstract
The invention discloses a kind of Fe/CNT ring-type powder core composite material and preparation methods, comprising the following steps: (1) high-purity iron powder surface preparation；(2) carbon nanotube and iron powder are pre-mixed in V-type batch mixer；(3) high-energy ball milling is pre-mixed powder, prepares Fe/CNT composite powder；(4) Fe/CNT composite powder is heat-treated；(5) Fe/CNT composite powder is pressed into toroidal core sample；(6) toroidal core sample high-temperature heat treatment under argon atmosphere.Compared with prior art, above-mentioned preparation process is simple to operation, and the used time is short, uniform doping, and gained composite material compactness is preferable, and magnetic property is stablized.
Description
Technical field
The invention belongs to iron-based soft magnetic technical field of composite preparation, and in particular to a kind of Fe/CNT ring-type powder core is multiple
Condensation material and preparation method thereof.
Background technique
Soft-magnetic composite material is usually made of ferromagnetic particle and surface coated insulating layer, therefore resistance with higher
Rate, magnetic isotropy and relatively low magnetic loss.The loss of general powder core is made of three parts: magnetic hystersis loss, vortex damage
Consumption and residual loss, wherein the eddy-current loss that about 9% loss is exchanged from electromagnetism, therefore prepare good magnetic property and loss
Low soft-magnetic composite material is still problem.The mode for usually reducing eddy-current loss is to coat one layer on ferromagnetic particle surface
Insulating properties medium, such as organic material, inorganic material, in-situ passivation material, by the way that iron particle is carried out insulation processing, preferably
Powder resistivity is improved, to reduce the loss that electromagnetism exchanges under medium-high frequency.But as shared by magnetic-particle in unit volume
Percentage decline, causes the reduced performances such as magnetic conductivity and saturation induction density.
Summary of the invention
Problem to be solved by this invention is in view of the deficiencies of the prior art, it is compound to provide a kind of Fe/CNT ring-type powder core
Material and preparation method thereof, using high-energy ball milling, the high temperature anneal and cold pressing and subsequent high temperature be tempered and etc. prepare carbon
Nanotube adulterates toroidal core composite material, overcomes material magnetization intensity, magnetic conductivity and saturation induction after insulating wrapped strong
The problem of degree decline.
The purpose of the present invention is achieved by the following technical programs:
In a first aspect, the preparation method of above-mentioned Fe/CNT ring-type powder core composite material, specifically, comprising the following steps:
(1) high-purity iron powder surface preparation；
(2) treated carbon nanotube and step (1), and iron powder is pre-mixed；
(3) powder after high-energy ball milling step (2) premixing, is made Fe/CNT composite powder；
(4) high-temperature heat treatment is carried out to Fe/CNT composite powder in step (3)；
(5) the Fe/CNT composite powder after step (4) high-temperature heat treatment is pressed into toroidal core；
(6) toroidal core carries out high-temperature heat treatment under argon atmosphere in step (5)；
Detailed process are as follows:
The high-purity iron powder is successively cleaned by ultrasonic 10-20min in acetone and alcohol and removes surface and oil contaminant, vacuum and low temperature
Drying；
Iron powder after carbon nanotube and surface treated is subjected to premixing flour according to mass ratio for 0.25-5:100 and handles 10-
20min；
It is in mass ratio the ball milling under argon atmosphere protection after 1:20-50 is mixed by above-mentioned pre-mix powder and stainless steel ball
1-3h；
Powder after ball milling is annealed 1-3h at 550-650 DEG C；
Fe/CNT composite powder after annealing is mixed with zinc stearate, is pressed into annular magnetic under 800-1000MPa pressure
Core sample；
Toroidal core sample is made annealing treatment into 1-3h at 600-700 DEG C under the argon atmosphere of flowing.
Preferably, the temperature of the vacuum and low temperature drying is 120 DEG C, time 2h.
Preferably, the stainless steel ball is 304 stainless steel abrading-balls, diameter 5mm.
Preferably, the outer diameter of the toroidal core is 20mm, internal diameter 12mm, with a thickness of 3mm.
Preferably, the carbon nanotube is that 0.5-2:100 is premixed according to mass ratio with the iron powder after surface treated
Powder handles 15min.
It is highly preferred that the iron powder after the carbon nanotube and surface treated is that 1:100 carries out premixing flour according to mass ratio
Handle 15min.
Preferably, the powder after the ball milling is annealed 2h at 600 DEG C.
Preferably, the zinc stearate and the Fe/CNT composite powder mass ratio after annealing are 1.5:100.
Preferably, the toroidal core sample is made annealing treatment into 2h at 650 DEG C under the argon atmosphere of flowing.
Second aspect, the system that Fe/CNT ring-type powder core composite material passes through above-mentioned Fe/CNT ring-type powder core composite material
Preparation Method is made.
The beneficial effects of the present invention are:
Compared with prior art, the present invention is by using high-energy ball milling, the high temperature anneal and cold pressing and subsequent high temperature
Tempering and etc. preparation Fe/CNT ring-type powder core composite material, simple process is easy to operate, and the used time is short, uniform doping.Gained is multiple
Condensation material compactness is preferable, and magnetic property is stablized, magnetic conductivity and high frequency stability with higher, lower magnetic loss, when carbon is received
When mitron doping is 1wt%, magnetic conductivity is maximum, and magnetic loss is minimum.
Detailed description of the invention
Fig. 1 is the permeability curcve of Fe/CNT ring-type powder core composite material when adulterating different content carbon nanotube.
Fig. 2 is the damage curve of Fe/CNT ring-type powder core composite material when adulterating different content carbon nanotube.
Specific embodiment
The principles and features of the present invention are described below, and the given examples are served only to explain the present invention, is not intended to limit
Determine the scope of the present invention.
Embodiment
Fe/CNT ring-type powder core composite material is prepared, detailed process is as follows:
S1. 5.00g high-purity iron powder is weighed, is successively cleaned by ultrasonic 15min in acetone, alcohol, removes iron power removing surface and oil contaminant,
Then it is being placed in a vacuum drying oven, 120 DEG C of low temperature, dry 2h takes out spare.
S2. according to 1.00wt%, iron powder premixing flour 15min in V-type batch mixer in 0.0500gCNT, with S1 is weighed.
S3. according to powder and stainless steel ball ratio 1:50,250g stainless steel abrading-ball is weighed, premixed powder in abrading-ball and S2 is put
Enter in stainless steel jar mill, under argon atmosphere protection, high-energy ball milling 2h is ground using 304 stainless steel jar mills and 304 stainless steels
Ball.
S4. gained composite powder after ball milling is taken out, anneal 2h at 600 DEG C, eliminates internal stress.
S5. the Fe/CNT composite powder after annealing is mixed with 1.5wt% zinc stearate, is then acted in 1000MPa pressure
Under be pressed into toroidal core sample, outer diameter 20mm, internal diameter 12mm, with a thickness of 3mm.
S6. toroidal core sample is made annealing treatment into 2h at 650 DEG C, the argon atmosphere of flowing obtains Fe/CNT ring
Shape powder core composite material.
With reference to the accompanying drawing and above-described embodiment further illustrates the present invention.Unless stated otherwise, present invention implementation is adopted
Reagent raw material is conventional reagent raw material, unless stated otherwise, the method equipment used for the method for this field routine and
Equipment prepares the pure iron powder core for not adulterating CNT as control under the same conditions.
Fig. 1 is the magnetic conductivity for adulterating the Fe/CNT ring-type powder core composite material of different content carbon nanotube, as seen from the figure,
In the range of 0-3wt%, when doping is 1wt%, magnetic conductivity is maximum, and when doping is 3wt%, magnetic conductivity is minimum, in conjunction with
Doping be 0.25wt%, 0.5wt% and 2wt% when composite material magnetic conductivity it is found that with nanotube doping increase,
Downward trend after first increase is presented in magnetic conductivity, and maximum value is reached at 1wt%.
Fig. 2 is the magnetic loss of Fe/CNT ring-type powder core composite material when adulterating different content carbon nanotube, as seen from the figure,
The magnetic loss of different dopings is not much different, but still can be seen that magnetic loss is relatively minimum when doping is 1wt%.
In conclusion the present invention improves the magnetic property of Fe/CNT composite material by adulterating micro carbon nanotube, one
Determine the magnetic conductivity for improving iron powder within the scope of doping, reduces magnetic loss.Compared with the existing technology, preparation method technique letter of the present invention
Single easy to operate, the used time is short, uniform doping, and gained composite material compactness is preferable, and magnetic property is stablized, magnetic conductivity with higher and
High frequency stability, compared with low-loss, when being doped to 1wt%, magnetic conductivity is maximum, is lost minimum.
Above said content is only preferable experiment embodiment result of the invention, not makees any form to the present invention
On limitation above embodiments are made according to the technical essence of the invention therefore without departing from the technical solutions of the present invention
Any modification, equivalent variations and modification, in the range of still falling within the limited technical solution of claims of the present invention.
Claims (10)
- The preparation method of 1.Fe/CNT ring-type powder core composite material, which comprises the following steps:(1) high-purity iron powder surface preparation；(2) treated carbon nanotube and step (1), and iron powder is pre-mixed；(3) powder after high-energy ball milling step (2) premixing, is made Fe/CNT composite powder；(4) high-temperature heat treatment is carried out to Fe/CNT composite powder in step (3)；(5) the Fe/CNT composite powder after step (4) high-temperature heat treatment is pressed into toroidal core；(6) toroidal core carries out high-temperature heat treatment under argon atmosphere in step (5)；Detailed process are as follows:The high-purity iron powder is successively cleaned by ultrasonic in acetone and alcohol to 10-20min and removes surface and oil contaminant, vacuum and low temperature dries It is dry；Iron powder after carbon nanotube and surface treated is subjected to premixing flour according to mass ratio for 0.25-5:100 and handles 10- 20min；It is in mass ratio the ball milling 1-3h under argon atmosphere protection after 1:20-50 is mixed by above-mentioned pre-mix powder and stainless steel ball；Powder after ball milling is annealed 1-3h at 550-650 DEG C；Fe/CNT composite powder after annealing is mixed with zinc stearate, is pressed into toroidal core under 800-1000MPa pressure；Toroidal core is made annealing treatment into 1-3h at 600-700 DEG C under the argon atmosphere of flowing.
- 2. the preparation method of Fe/CNT ring-type powder core composite material according to claim 1, which is characterized in that the vacuum The temperature of low temperature drying is 120 DEG C, time 2h.
- 3. the preparation method of Fe/CNT ring-type powder core composite material according to claim 1, which is characterized in that described stainless Steel ball is 304 stainless steel abrading-balls, diameter 5mm.
- 4. the preparation method of Fe/CNT ring-type powder core composite material according to claim 1, which is characterized in that the carbon is received Iron powder after mitron and surface treated carries out premixing flour according to mass ratio for 0.5-2:100 and handles 15min.
- 5. according to claim 1 or the preparation method of the 4 Fe/CNT ring-type powder core composite materials, which is characterized in that described Iron powder after carbon nanotube and surface treated carries out premixing flour according to mass ratio for 1:100 and handles 15min.
- 6. the preparation method of Fe/CNT ring-type powder core composite material according to claim 1, which is characterized in that the ball milling Powder afterwards is annealed 2h at 600 DEG C.
- 7. the preparation method of Fe/CNT ring-type powder core composite material according to claim 1, which is characterized in that the tristearin Fe/CNT composite powder mass ratio after sour zinc and annealing is 1.5:100.
- 8. the preparation method of Fe/CNT ring-type powder core composite material according to claim 1, which is characterized in that in flowing The toroidal core sample is made annealing treatment into 2h at 650 DEG C under argon atmosphere.
- 9. the preparation method of Fe/CNT ring-type powder core composite material according to claim 1, which is characterized in that the annular The outer diameter of magnetic core is 20mm, internal diameter 12mm, with a thickness of 3mm.
- 10.Fe/CNT ring-type powder core composite material, which is characterized in that pass through any one of the claim 1-9 Fe/CNT ring The preparation method of shape powder core composite material is made.
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| CN201811256372.5A CN109448948B (en) | 2018-10-26 | 2018-10-26 | Fe/CNT (carbon nanotube) annular magnetic powder core composite material and preparation method thereof |
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| CN201811256372.5A CN109448948B (en) | 2018-10-26 | 2018-10-26 | Fe/CNT (carbon nanotube) annular magnetic powder core composite material and preparation method thereof |
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| CN103435972A (en) * | 2013-08-26 | 2013-12-11 | 中国科学院深圳先进技术研究院 | Nickel-zinc ferrite-multiwalled carbon nanotube-epoxy resin composite and preparation method thereof as well as complex and preparation method thereof |
| CN105369166A (en) * | 2015-12-09 | 2016-03-02 | 北京工业大学 | Preparation method of metal-based carbon nanotube reinforced composite material |
| CN107670640A (en) * | 2017-10-18 | 2018-02-09 | 宁波市疾病预防控制中心 | Immobilized quaternary ammonium salt magnetic functional material of CNT and its preparation method and application |
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2018
- 2018-10-26 CN CN201811256372.5A patent/CN109448948B/en active Active
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