CN104078230B - A kind of high-silicon electrical steel iron core of intergranular insulation and preparation method thereof - Google Patents
A kind of high-silicon electrical steel iron core of intergranular insulation and preparation method thereof Download PDFInfo
- Publication number
- CN104078230B CN104078230B CN201410354648.9A CN201410354648A CN104078230B CN 104078230 B CN104078230 B CN 104078230B CN 201410354648 A CN201410354648 A CN 201410354648A CN 104078230 B CN104078230 B CN 104078230B
- Authority
- CN
- China
- Prior art keywords
- electrical steel
- iron core
- silicon electrical
- ferro
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Soft Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention relates to high-silicon electrical steel iron core of a kind of intergranular insulation and preparation method thereof.Its technical scheme is: be that ferro-silicium powder, dehydrated alcohol, silane coupler and distilled water are sequentially added in reaction vessel by 1 (6 ~ 10) (0.04 ~ 0.1) (0.2 ~ 0.5) by the mass ratio of ferro-silicium powdered anhydrous ethanol silane coupler distilled water, stirring；It is added thereto to tetraethyl orthosilicate or methyl silicate again, adds ammonia, continue stirring；Washing, filters, and is dried；Then insulation 1 ~ 3h under the conditions of 600 ~ 800 DEG C, furnace cooling, compressing；Finally insert in sintering furnace, under the conditions of 950 ~ 1350 DEG C, sinter 1 ~ 10h, furnace cooling, obtain the high-silicon electrical steel iron core of intergranular insulation.The present invention has that technique is simple, the cycle is short, stock utilization is high and the feature of low cost, and the high-silicon electrical steel iron core iron loss of prepared intergranular insulation is low, steadiness good and service life is long.
Description
Technical field
The invention belongs to high-silicon electrical steel core technology field.It is specifically related to the high-silicon electrical steel iron core of a kind of intergranular insulation
And preparation method thereof.
Background technology
In recent years, along with propelling and the popularization and application of high efficiency motor of energy-saving and emission-reduction policy, following middle and small motor and micro-
The demand of high grade non-oriented electrical steel will be dramatically increased by machine field.It addition, along with main flow motor frequency conversion control model
The universal and exploitation of high-speed rotation motor, non-oriented electrical steel is proposed high frequency, high magnetic strength and the requirement of low iron loss.And
High-silicon electrical steel has the excellent soft magnetic characteristics such as low iron loss, high magnetic strength, high magnetic conduction and low magnetic hysteresis be flexible, is electromagnetic conversion dress
For realizing low energy consumption, low heating, microminaturization, low noise, high stable and the key of environmental protection.
It is known that owing to the eddy-current loss of iron core and square forward of electrical sheet gauge of sheet are relevant, so to use up
Amount reduces electrical sheet gauge of sheet, generally passes through milling method by its THICKNESS CONTROL at below 1mm, to reduce eddy-current loss.
But, for high-silicon electrical steel, especially when silicone content is more than 4.5wt%, B easily occurs in high-silicon electrical steel2And DO3In order
Phase, causes its plasticity and toughness drastically to decline, and elongation percentage is almost equal to zero, and rolling, molding and punching are abnormal difficult, produce and are subject to applying
Serious restriction, thus high-silicon electrical steel be difficult to by pair rolling method by its THICKNESS CONTROL within 1mm.
Drastically decline for high-silicon electrical steel plasticity and toughness, roll forming difficulty etc. problem, Chinese scholars is high silicon electrician
Reason that steel brittleness increases, how to strengthen its plasticity and toughness and how to avoid the aspect such as fragility of electrical sheet and carried out substantial amounts of grinding
Study carefully, it is proposed that many new technology and methods, advance the development of high-silicon electrical steel effectively.The purpose of technological innovation is intended to pass through
Structure control improves its plasticity and toughness and machinability, or avoids tradition rolling mill practice completely, uses new method to prepare high silicon electricity
Work steel sheet.As the reaction-injection moulding based on rapid solidification (cooling) technology and melt rapid quenching mold methods such as (solidifications)
Can effectively suppress or reduce the formation of ordered phase, to improve the machinability of high-silicon electrical steel.Also can be by adding microalloy
Element also optimizes existing rolling technique, such as " a kind of containing chromium height silicon steel thin belt and preparation method thereof " (CN103276174A) patent skill
Art and " a kind of high silicon steel thin belt and preparation method thereof " (CN101935800B) patented technology, use the most conventional hot rolling cold rolling,
Or forging hot rolling warm-rolling cold-rolling process, steps up the ductility of high-silicon electrical steel, it is possible to be successfully obtained excellent performance
Ultra-thin high-silicon electrical steel thin plate.Another kind of Research Thinking is to avoid existing rolling technique, and development is based on deposition-diffusion method
Correlation technique, such as chemical gaseous phase deposition, plasma activated chemical vapour deposition, hot submersion siliconising, embedding siliconising, magnetron sputtering, melts
The technology such as salt electro-deposition, electro beam physics vapour deposition, laser melting coating, electrophoretic deposition, and for example " hot-dip silicon process prepares high silicon silicon
The method of steel strip and silicon strip continuous preparation device " (CN103320737A) patented technology and " with magnetron sputtering continuous two-sided
The industrialized production system of codeposition technique height silicon strip " (CN101319306A) patented technology, all can obtain excellent performance
High-silicon electrical steel thin plate.
Although domestic and international researcher has been carried out extensive and deep basis for the various problems that high-silicon electrical steel is relevant and has been ground
Study carefully work, but above-mentioned prior art or because of relatively costly or because of by environmental constraints or because technical maturity is not or because of material
The problems such as utilization rate is relatively low and constrain it and apply further.
Summary of the invention
It is contemplated that overcome the deficiencies in the prior art, it is therefore an objective to iron loss is low, steadiness good, service life to provide one
Long, stock utilization is high and production cost is low high-silicon electrical steel iron core of intergranular insulation and preparation method thereof.
To achieve these goals, the comprising the concrete steps that of preparation method of the present invention:
The first step, ferro-silicium powder surface modifications
By the mass ratio of ferro-silicium powdered anhydrous ethanol silane coupler distilled water be 1 (6 ~ 10) (0.04 ~
0.1) (0.2 ~ 0.5), is sequentially added into ferro-silicium powder, dehydrated alcohol, silane coupler and distilled water in reaction vessel,
Under the conditions of 40 ~ 70 DEG C, stir 1 ~ 3h, obtain the mixed solution of ferro-silicium powder containing surface modification.
Second step, the preparation of nucleocapsid heterojunction structure composite powder
Under 40 ~ 70 DEG C and stirring condition, first in the mixed solution of the described ferro-silicium powder containing surface modification
Add tetraethyl orthosilicate or methyl silicate, add ammonia, under the conditions of 40 ~ 70 DEG C, continue stirring 8 ~ 24h；With distillation washing
Wash 2 ~ 3 times, with absolute ethanol washing 5 ~ 8 times, filter, vacuum drying, obtain nucleocapsid heterojunction structure composite powder.
Wherein: the mass ratio of ferro-silicium powder tetraethyl orthosilicate is 1:(0.1 ~ 2), ferro-silicium powder positive silicic acid first
The mass ratio of ester is 1:(0.1 ~ 2)；The mass ratio of ferro-silicium powder ammonia is 1:(0.02 ~ 0.4).
3rd step, annealing heat treatment
Described nucleocapsid heterojunction structure composite powder is inserted in annealing furnace, under the conditions of 600 ~ 800 DEG C, is incubated 1 ~ 3h, with
Stove is cooled to room temperature, it is thus achieved that the nucleocapsid heterojunction structure composite powder annealing heat treated.
4th step, the preparation of high-silicon electrical steel powder compact
By compressing for the described nucleocapsid heterojunction structure composite powder made annealing treatment, it is thus achieved that high-silicon electrical steel powder pressure
Base.
The preparation of the high-silicon electrical steel iron core of the 5th step, intergranular insulation
Described high-silicon electrical steel powder compact is inserted in sintering furnace, under the conditions of 950 DEG C ~ 1350 DEG C, sinters 1 ~ 10h,
Cool to room temperature with the furnace, obtain the high-silicon electrical steel iron core of intergranular insulation.
The Si content of described ferro-silicium powder is 4.0 ~ 7.5wt%.
Described annealing furnace is the annealing furnace of vacuum protection or for the annealing furnace of inert gas shielding.
Described sintering furnace is the sintering furnace of vacuum protection or for the sintering furnace of inert gas shielding.
Described compressing pressure is 100Mpa ~ 600Mpa.
Owing to using technique scheme, the invention have the advantages that
1) preparation method of the high-silicon electrical steel iron core of intergranular disclosed by the invention insulation, avoids existing high-silicon electrical steel
Being difficult to the bottleneck rolled, a step sinter molding can obtain high-silicon electrical steel iron core, it is not necessary to rolling, compared with prior art technique
Simply, the cycle is short, low cost.
2) present invention uses surface coated method at ferro-silicium Surface coating silicon dioxide insulating layer, it is achieved that ferrum silicon
Insulation between alloying pellet, it is to avoid the use of existing high-silicon electrical steel leaf insulator coating, improves high-silicon electrical steel iron core
Steadiness, extend service life.
3) the high-silicon electrical steel iron core of the intergranular insulation that prepared by the present invention, its eddy current is limited in the ferrum in insulating wrapped district
In silicon alloy, eddy-current loss is little compared with existing high-silicon electrical steel iron core, and iron loss is low.
Prepared by this detailed description of the invention intergranular insulation high-silicon electrical steel iron core after testing: saturation induction density is
158~186emu/g；Resistivity is 1.9 × 10-2Ω * m ~ insulation；Iron loss P5/50It is 0.25 ~ 0.50W/kg, P5/400Be 5.85 ~
10.32W/kg, P5/1000It is 20.93 ~ 36.92W/kg.
4) preparation method of the high-silicon electrical steel iron core that the present invention proposes, can directly prepare ring by the design of mould
Shape, E shape, back-shaped and fan-shaped and other Special-shaped iron core, it is not necessary to punching process, stock utilization is high, low cost.
Therefore, the present invention has that technique is simple, the cycle is short, stock utilization is high and the feature of low cost；Prepared crystalline substance
Between insulation high-silicon electrical steel iron core iron loss low, steadiness is good, and service life is long.
Accompanying drawing explanation
Fig. 1 is the section SEM figure of the high-silicon electrical steel iron core of a kind of intergranular insulation prepared by the present invention；
Fig. 2 be shown in Fig. 1 intergranular insulation high-silicon electrical steel iron core different frequency under iron loss spectrogram；
Fig. 3 is the pictorial diagram of the high-silicon electrical steel iron core of the intergranular insulation shown in Fig. 1.
Detailed description of the invention
The present invention will be further described with detailed description of the invention below in conjunction with the accompanying drawings, not the limit to its protection domain
System.
The Si content of ferro-silicium powder described in this detailed description of the invention is 4.0 ~ 7.5wt%, the most superfluous in embodiment
State.
Embodiment 1
A kind of high-silicon electrical steel iron core of intergranular insulation and preparation method thereof.Comprising the concrete steps that of described preparation method:
The first step, ferro-silicium powder surface modifications
By the mass ratio of ferro-silicium powdered anhydrous ethanol silane coupler distilled water be 1 (6 ~ 7) (0.04 ~
0.05) (0.2 ~ 0.25), is sequentially added into reaction vessel by ferro-silicium powder, dehydrated alcohol, silane coupler and distilled water
In, under the conditions of 40 ~ 45 DEG C, stir 1.5 ~ 2h, obtain the mixed solution of ferro-silicium powder containing surface modification.
Second step, the preparation of nucleocapsid heterojunction structure composite powder
Under 40 ~ 45 DEG C and stirring condition, first in the mixed solution of the described ferro-silicium powder containing surface modification
Add tetraethyl orthosilicate, add ammonia, under the conditions of 40 ~ 45 DEG C, continue stirring 8 ~ 10h；With distilled water wash 2 ~ 3 times, by nothing
Water-ethanol washs 5 ~ 6 times, filters, and vacuum drying obtains nucleocapsid heterojunction structure composite powder.
Wherein: the mass ratio of ferro-silicium powder tetraethyl orthosilicate is 1:(0.1 ~ 0.4)；Ferro-silicium powder ammonia
Mass ratio is 1:(0.02 ~ 0.05).
3rd step, annealing heat treatment
Described nucleocapsid heterojunction structure composite powder is inserted in the annealing furnace of vacuum protection, under the conditions of 600 ~ 650 DEG C
Insulation 1.5 ~ 2h, cools to room temperature with the furnace, it is thus achieved that the nucleocapsid heterojunction structure composite powder annealing heat treated.
4th step, the preparation of high-silicon electrical steel powder compact
By compressing for the described nucleocapsid heterojunction structure composite powder made annealing treatment, compressing pressure is 100 ~
200Mpa, it is thus achieved that high-silicon electrical steel powder compact.
The preparation of the high-silicon electrical steel iron core of the 5th step, intergranular insulation
Described high-silicon electrical steel powder compact is inserted in the sintering furnace of vacuum protection, burn under the conditions of 950 ~ 1000 DEG C
Knot 2 ~ 4h, cools to room temperature with the furnace, obtains the high-silicon electrical steel iron core of intergranular insulation.
The high-silicon electrical steel iron core of the intergranular insulation prepared by the present embodiment is after testing: saturation induction density is 184 ~
186emu/g；Resistivity is 2.8 × 10-2~3.0×10-2Ω*m；Iron loss P5/50It is 0.42 ~ 0.43W/kg, P5/400Be 8.93 ~
9.01W/kg, P5/1000It is 31.95 ~ 32.24W/kg.
Embodiment 2
A kind of high-silicon electrical steel iron core of intergranular insulation and preparation method thereof.Comprising the concrete steps that of described preparation method:
The first step, ferro-silicium powder surface modifications
By the mass ratio of ferro-silicium powdered anhydrous ethanol silane coupler distilled water be 1 (7 ~ 8) (0.05 ~
0.06) (0.25 ~ 0.3), is sequentially added into reaction vessel by ferro-silicium powder, dehydrated alcohol, silane coupler and distilled water
In, under the conditions of 45 ~ 50 DEG C, stir 2.5 ~ 3h, obtain the mixed solution of ferro-silicium powder containing surface modification.
Second step, the preparation of nucleocapsid heterojunction structure composite powder
Under 45 ~ 50 DEG C and stirring condition, first in the mixed solution of the described ferro-silicium powder containing surface modification
Add methyl silicate, add ammonia, under the conditions of 45 ~ 50 DEG C, continue stirring 10 ~ 12h；With distilled water wash 2 ~ 3 times, use
Absolute ethanol washing 6 ~ 7 times, filters, and vacuum drying obtains nucleocapsid heterojunction structure composite powder.
Wherein: the mass ratio of ferro-silicium powder methyl silicate is 1:(0.4 ~ 0.6)；Ferro-silicium powder ammonia
Mass ratio is 1:(0.05 ~ 0.1).
3rd step, annealing heat treatment
Described nucleocapsid heterojunction structure composite powder is inserted in the annealing furnace of vacuum protection, under the conditions of 650 ~ 700 DEG C
Insulation 2 ~ 2.5h, cools to room temperature with the furnace, it is thus achieved that the nucleocapsid heterojunction structure composite powder annealing heat treated.
4th step, the preparation of high-silicon electrical steel powder compact
By compressing for the described nucleocapsid heterojunction structure composite powder made annealing treatment, compressing pressure is 200 ~
300Mpa, it is thus achieved that high-silicon electrical steel powder compact.
The preparation of the high-silicon electrical steel iron core of the 5th step, intergranular insulation
Described high-silicon electrical steel powder compact is inserted in the sintering furnace of vacuum protection, under the conditions of 1000 ~ 1050 DEG C
Sintering 4 ~ 6h, cools to room temperature with the furnace, obtains the high-silicon electrical steel iron core of intergranular insulation.
The high-silicon electrical steel iron core of the intergranular insulation prepared by the present embodiment is after testing: saturation induction density is 180 ~
182emu/g；Resistivity is 1.4 × 10-2~1.6×10-2Ω*m；Iron loss P5/50It is 0.36 ~ 0.37W/kg, P5/400Be 7.66 ~
7.74W/kg, P5/1000It is 27.41 ~ 27.69W/kg.
Embodiment 3
A kind of high-silicon electrical steel iron core of intergranular insulation and preparation method thereof.Comprising the concrete steps that of described preparation method:
The first step, ferro-silicium powder surface modifications
By the mass ratio of ferro-silicium powdered anhydrous ethanol silane coupler distilled water be 1 (8 ~ 9) (0.06 ~
0.07) (0.3 ~ 0.35), is sequentially added into reaction vessel by ferro-silicium powder, dehydrated alcohol, silane coupler and distilled water
In, under the conditions of 50 ~ 55 DEG C, stir 1 ~ 1.5h, obtain the mixed solution of ferro-silicium powder containing surface modification.
Second step, the preparation of nucleocapsid heterojunction structure composite powder
Under 50 ~ 55 DEG C and stirring condition, first in the mixed solution of the described ferro-silicium powder containing surface modification
Add tetraethyl orthosilicate, add ammonia, under the conditions of 50 ~ 55 DEG C, continue stirring 12 ~ 14h；With distilled water wash 2 ~ 3 times, use
Absolute ethanol washing 7 ~ 8 times, filters, and vacuum drying obtains nucleocapsid heterojunction structure composite powder.
Wherein: the mass ratio of ferro-silicium powder tetraethyl orthosilicate is 1:(0.6 ~ 1)；The matter of ferro-silicium powder ammonia
Amount ratio is 1:(0.1 ~ 0.15).
3rd step, annealing heat treatment
Described nucleocapsid heterojunction structure composite powder is inserted in the annealing furnace of vacuum protection, under the conditions of 700 ~ 750 DEG C
Insulation 2.5 ~ 3h, cools to room temperature with the furnace, it is thus achieved that the nucleocapsid heterojunction structure composite powder annealing heat treated.
4th step, the preparation of high-silicon electrical steel powder compact
By compressing for the described nucleocapsid heterojunction structure composite powder made annealing treatment, compressing pressure is 300 ~
400Mpa, it is thus achieved that high-silicon electrical steel powder compact.
The preparation of the high-silicon electrical steel iron core of the 5th step, intergranular insulation
Described high-silicon electrical steel powder compact is inserted in the sintering furnace of inert gas shielding, at 1050 ~ 1100 DEG C of bars
Sinter 6 ~ 8h under part, cool to room temperature with the furnace, obtain the high-silicon electrical steel iron core of intergranular insulation.
The high-silicon electrical steel iron core of the intergranular insulation prepared by the present embodiment is after testing: saturation induction density is 176 ~
178emu/g；Resistivity is 8.0 × 10-1~8.2×10-1Ω*m；Iron loss P5/50It is 0.33 ~ 0.34W/kg, P5/400Be 7.14 ~
7.22W/kg, P5/1000It is 25.55 ~ 25.83W/kg.
Embodiment 4
A kind of high-silicon electrical steel iron core of intergranular insulation and preparation method thereof.Comprising the concrete steps that of described preparation method:
The first step, ferro-silicium powder surface modifications
By the mass ratio of ferro-silicium powdered anhydrous ethanol silane coupler distilled water be 1 (9 ~ 10) (0.07 ~
0.08) (0.35 ~ 0.40), is sequentially added into reaction vessel by ferro-silicium powder, dehydrated alcohol, silane coupler and distilled water
In, under the conditions of 55 ~ 60 DEG C, stir 2 ~ 2.5h, obtain the mixed solution of ferro-silicium powder containing surface modification.
Second step, the preparation of nucleocapsid heterojunction structure composite powder
Under 55 ~ 60 DEG C and stirring condition, first in the mixed solution of the described ferro-silicium powder containing surface modification
Add methyl silicate, add ammonia, under the conditions of 55 ~ 60 DEG C, continue stirring 14 ~ 16h；With distilled water wash 2 ~ 3 times, use
Absolute ethanol washing 5 ~ 6 times, filters, and vacuum drying obtains nucleocapsid heterojunction structure composite powder.
Wherein: the mass ratio of ferro-silicium powder methyl silicate is 1:(1 ~ 1.2)；The matter of ferro-silicium powder ammonia
Amount ratio is 1:(0.15 ~ 0.2).
3rd step, annealing heat treatment
Described nucleocapsid heterojunction structure composite powder is inserted in the annealing furnace of vacuum protection, under the conditions of 750 ~ 800 DEG C
Insulation 1 ~ 1.5h, cools to room temperature with the furnace, it is thus achieved that the nucleocapsid heterojunction structure composite powder annealing heat treated.
4th step, the preparation of high-silicon electrical steel powder compact
By compressing for the described nucleocapsid heterojunction structure composite powder made annealing treatment, compressing pressure is 400 ~
500Mpa, it is thus achieved that high-silicon electrical steel powder compact.
The preparation of the high-silicon electrical steel iron core of the 5th step, intergranular insulation
Described high-silicon electrical steel powder compact is inserted in the sintering furnace of inert gas shielding, at 1100 ~ 1150 DEG C of bars
Sinter 8 ~ 10h under part, cool to room temperature with the furnace, obtain the high-silicon electrical steel iron core of intergranular insulation.
The high-silicon electrical steel iron core of the intergranular insulation prepared by the present embodiment is after testing: saturation induction density is 175 ~
177emu/g；Resistivity is insulation；Iron loss P5/50It is 0.29 ~ 0.30W/kg, P5/400It is 6.11 ~ 6.19W/kg, P5/1000For
21.86~22.14W/kg。
Embodiment 5
A kind of high-silicon electrical steel iron core of intergranular insulation and preparation method thereof.Comprising the concrete steps that of described preparation method:
The first step, ferro-silicium powder surface modifications
By the mass ratio of ferro-silicium powdered anhydrous ethanol silane coupler distilled water be 1 (6 ~ 6.5) (0.08 ~
0.09) (0.4 ~ 0.45), is sequentially added into reaction vessel by ferro-silicium powder, dehydrated alcohol, silane coupler and distilled water
In, under the conditions of 60 ~ 65 DEG C, stir 1.5 ~ 2h, obtain the mixed solution of ferro-silicium powder containing surface modification.
Second step, the preparation of nucleocapsid heterojunction structure composite powder
Under 60 ~ 65 DEG C and stirring condition, first in the mixed solution of the described ferro-silicium powder containing surface modification
Add methyl silicate, add ammonia, under the conditions of 60 ~ 65 DEG C, continue stirring 16 ~ 18h；With distilled water wash 2 ~ 3 times, use
Absolute ethanol washing 7 ~ 8 times, filters, and vacuum drying obtains nucleocapsid heterojunction structure composite powder.
Wherein: the mass ratio of ferro-silicium powder methyl silicate is 1:(1.2 ~ 1.4)；Ferro-silicium powder ammonia
Mass ratio is 1:(0.2 ~ 0.25).
3rd step, annealing heat treatment
Described nucleocapsid heterojunction structure composite powder is inserted in the annealing furnace of inert gas shielding, at 600 ~ 700 DEG C of bars
It is incubated 1 ~ 2h under part, cools to room temperature with the furnace, it is thus achieved that the nucleocapsid heterojunction structure composite powder annealing heat treated.
4th step, the preparation of high-silicon electrical steel powder compact
By compressing for the described nucleocapsid heterojunction structure composite powder made annealing treatment, compressing pressure is 500 ~
600Mpa, it is thus achieved that high-silicon electrical steel powder compact.
The preparation of the high-silicon electrical steel iron core of the 5th step, intergranular insulation
Described high-silicon electrical steel powder compact is inserted in the sintering furnace of vacuum protection, under the conditions of 1150 ~ 1200 DEG C
Sintering 1 ~ 3h, cools to room temperature with the furnace, obtains the high-silicon electrical steel iron core of intergranular insulation.
The high-silicon electrical steel iron core of the intergranular insulation prepared by the present embodiment is after testing: saturation induction density is 168 ~
170emu/g；Resistivity is insulation；Iron loss P5/50It is 0.28 ~ 0.30W/kg, P5/400It is 6.04 ~ 6.12W/kg, P5/1000For
21.61~21.90W/kg。
Embodiment 6
A kind of high-silicon electrical steel iron core of intergranular insulation and preparation method thereof.Comprising the concrete steps that of described preparation method:
The first step, ferro-silicium powder surface modifications
By the mass ratio of ferro-silicium powdered anhydrous ethanol silane coupler distilled water be 1 (6.5 ~ 8) (0.09 ~
0.1) (0.45 ~ 0.5), is sequentially added into ferro-silicium powder, dehydrated alcohol, silane coupler and distilled water in reaction vessel,
Under the conditions of 65 ~ 70 DEG C, stir 2.5 ~ 3h, obtain the mixed solution of ferro-silicium powder containing surface modification.
Second step, the preparation of nucleocapsid heterojunction structure composite powder
Under 65 ~ 70 DEG C and stirring condition, first in the mixed solution of the described ferro-silicium powder containing surface modification
Add methyl silicate, add ammonia, under the conditions of 65 ~ 70 DEG C, continue stirring 18 ~ 20h；With distilled water wash 2 ~ 3 times, use
Absolute ethanol washing 7 ~ 8 times, filters, and vacuum drying obtains nucleocapsid heterojunction structure composite powder.
Wherein: the mass ratio of ferro-silicium powder methyl silicate is 1:(1.4 ~ 1.6)；Ferro-silicium powder ammonia
Mass ratio is 1:(0.25 ~ 0.3).
3rd step, annealing heat treatment
Described nucleocapsid heterojunction structure composite powder is inserted in the annealing furnace of inert gas shielding, at 700 ~ 800 DEG C of bars
It is incubated 2 ~ 3h under part, cools to room temperature with the furnace, it is thus achieved that the nucleocapsid heterojunction structure composite powder annealing heat treated.
4th step, the preparation of high-silicon electrical steel powder compact
By compressing for the described nucleocapsid heterojunction structure composite powder made annealing treatment, compressing pressure is 350 ~
400Mpa, it is thus achieved that high-silicon electrical steel powder compact.
The preparation of the high-silicon electrical steel iron core of the 5th step, intergranular insulation
Described high-silicon electrical steel powder compact is inserted in the sintering furnace of inert gas shielding, at 1200 ~ 1250 DEG C of bars
Sinter 3 ~ 5h under part, cool to room temperature with the furnace, obtain the high-silicon electrical steel iron core of intergranular insulation.
The high-silicon electrical steel iron core of the intergranular insulation prepared by the present embodiment is after testing: saturation induction density is 165 ~
167emu/g；Resistivity is insulation；Iron loss P5/50It is 0.27 ~ 0.28W/kg, P5/400It is 5.85 ~ 5.93W/kg, P5/1000For
20.93~21.22W/kg。
Embodiment 7
A kind of high-silicon electrical steel iron core of intergranular insulation and preparation method thereof.Comprising the concrete steps that of described preparation method:
The first step, ferro-silicium powder surface modifications
By the mass ratio of ferro-silicium powdered anhydrous ethanol silane coupler distilled water be 1 (8 ~ 8.5) (0.04 ~
0.07) (0.25 ~ 0.35), is sequentially added into reaction vessel by ferro-silicium powder, dehydrated alcohol, silane coupler and distilled water
In, under the conditions of 40 ~ 55 DEG C, stir 1 ~ 2h, obtain the mixed solution of ferro-silicium powder containing surface modification.
Second step, the preparation of nucleocapsid heterojunction structure composite powder
Under 40 ~ 55 DEG C and stirring condition, first in the mixed solution of the described ferro-silicium powder containing surface modification
Add tetraethyl orthosilicate, add ammonia, under the conditions of 40 ~ 55 DEG C, continue stirring 20 ~ 22h；With distilled water wash 2 ~ 3 times, use
Absolute ethanol washing 6 ~ 7 times, filters, and vacuum drying obtains nucleocapsid heterojunction structure composite powder.
Wherein: the mass ratio of ferro-silicium powder tetraethyl orthosilicate is 1:(1.6 ~ 1.8)；Ferro-silicium powder ammonia
Mass ratio is 1:(0.3 ~ 0.35).
3rd step, annealing heat treatment
Described nucleocapsid heterojunction structure composite powder is inserted in the annealing furnace of inert gas shielding, at 730 ~ 780 DEG C of bars
It is incubated 1 ~ 1.5h under part, cools to room temperature with the furnace, it is thus achieved that the nucleocapsid heterojunction structure composite powder annealing heat treated.
4th step, the preparation of high-silicon electrical steel powder compact
By compressing for the described nucleocapsid heterojunction structure composite powder made annealing treatment, compressing pressure is 400 ~
450Mpa, it is thus achieved that high-silicon electrical steel powder compact.
The preparation of the high-silicon electrical steel iron core of the 5th step, intergranular insulation
Described high-silicon electrical steel powder compact is inserted in the sintering furnace of vacuum protection, under the conditions of 1250 ~ 1300 DEG C
Sintering 5 ~ 7h, cools to room temperature with the furnace, obtains the high-silicon electrical steel iron core of intergranular insulation.
The high-silicon electrical steel iron core of the intergranular insulation prepared by the present embodiment is after testing: saturation induction density is 170 ~
172emu/g；Resistivity is 1.9 × 10-2~2.1×10-2Ω*m；Iron loss P5/50It is 0.49 ~ 0.50W/kg, P5/400Be 10.24 ~
10.32W/kg, P5/1000It is 36.64 ~ 36.92W/kg.
Embodiment 8
A kind of high-silicon electrical steel iron core of intergranular insulation and preparation method thereof.Comprising the concrete steps that of described preparation method:
The first step, ferro-silicium powder surface modifications
By the mass ratio of ferro-silicium powdered anhydrous ethanol silane coupler distilled water be 1 (8.5 ~ 10) (0.07 ~
0.1) (0.3 ~ 0.35), is sequentially added into ferro-silicium powder, dehydrated alcohol, silane coupler and distilled water in reaction vessel,
Under the conditions of 55 ~ 70 DEG C, stir 2 ~ 3h, obtain the mixed solution of ferro-silicium powder containing surface modification.
Second step, the preparation of nucleocapsid heterojunction structure composite powder
Under 55 ~ 70 DEG C and stirring condition, first in the mixed solution of the described ferro-silicium powder containing surface modification
Add tetraethyl orthosilicate, add ammonia, under the conditions of 55 ~ 70 DEG C, continue stirring 22 ~ 24h；With distilled water wash 2 ~ 3 times, use
Absolute ethanol washing 5 ~ 6 times, filters, and vacuum drying obtains nucleocapsid heterojunction structure composite powder.
Wherein: the mass ratio of ferro-silicium powder tetraethyl orthosilicate is 1:(1.8 ~ 2)；The matter of ferro-silicium powder ammonia
Amount ratio is 1:(0.02 ~ 0.4).
3rd step, annealing heat treatment
Described nucleocapsid heterojunction structure composite powder is inserted in the annealing furnace of vacuum protection, under the conditions of 780 ~ 800 DEG C
Insulation 1.5 ~ 2h, cools to room temperature with the furnace, it is thus achieved that the nucleocapsid heterojunction structure composite powder annealing heat treated.
4th step, the preparation of high-silicon electrical steel powder compact
By compressing for the described nucleocapsid heterojunction structure composite powder made annealing treatment, compressing pressure is 450 ~
500Mpa, it is thus achieved that high-silicon electrical steel powder compact.
The preparation of the high-silicon electrical steel iron core of the 5th step, intergranular insulation
Described high-silicon electrical steel powder compact is inserted in the sintering furnace of inert gas shielding, at 1300 ~ 1350 DEG C of bars
Sinter 7 ~ 10h under part, cool to room temperature with the furnace, obtain the high-silicon electrical steel iron core of intergranular insulation.
The high-silicon electrical steel iron core of the intergranular insulation prepared by the present embodiment is after testing: saturation induction density is 158 ~
160emu/g；Resistivity is insulation；Iron loss P5/50It is 0.25 ~ 0.27W/kg, P5/400It is 5.87 ~ 5.95W/kg, P5/1000For
21.00~21.29W/kg。
This detailed description of the invention compared with prior art has a following good effect:
1) preparation method of the high-silicon electrical steel iron core of intergranular insulation disclosed in this detailed description of the invention, avoids existing height
Silicon electric steel is difficult to the bottleneck rolled, and a step sinter molding can obtain high-silicon electrical steel iron core, it is not necessary to rolling, with prior art
Comparing technique simple, the cycle is short, low cost.
2) the surface coated method of this detailed description of the invention employing is at ferro-silicium Surface coating silicon dioxide insulating layer, real
Show the intergranular insulation of ferro-silicium, it is to avoid the use of existing high-silicon electrical steel leaf insulator coating, improve high silicon electricity
The steadiness of work steel core, extends service life, and Fig. 1 is the high-silicon electrical steel implementing a kind of intergranular insulation prepared by row 4
The SEM figure of iron core, it can be seen that in the high-silicon electrical steel iron core of intergranular insulation, ferro-silicium powder is by SiO2Uniformly cladding, real
Show the intergranular insulation of ferro-silicium.
3) the high-silicon electrical steel iron core of the intergranular insulation that prepared by this detailed description of the invention, its eddy current is limited in insulating wrapped
In ferro-silicium in district, eddy-current loss is little compared with existing high-silicon electrical steel iron core, and iron loss is low, and Fig. 2 is the crystalline substance shown in Fig. 1
Between insulation high-silicon electrical steel iron core different frequency under iron loss spectrogram, it can be seen that its iron loss P5/50It is 0.25 ~ 0.27W/kg,
P5/400It is 5.87 ~ 5.95W/kg, P5/1000It is 21.00 ~ 21.29W/kg.
Prepared by this detailed description of the invention intergranular insulation high-silicon electrical steel iron core after testing: saturation induction density is
158~186emu/g；Resistivity is 1.9 × 10-2Ω * m ~ insulation；Iron loss P5/50It is 0.25 ~ 0.50W/kg, P5/400Be 5.85 ~
10.32W/kg, P5/1000It is 20.93 ~ 36.92W/kg.
4) preparation method of the high-silicon electrical steel iron core that this detailed description of the invention proposes, directly can be made by the design of mould
For going out annular, E shape, back-shaped and fan-shaped and other Special-shaped iron core, it is not necessary to punching process, stock utilization is high, low cost.Fig. 3 is
The material object of the high-silicon electrical steel iron core of the intergranular insulation shown in Fig. 1, it can be seen that directly prepare annular by the design of mould
Intergranular insulation high-silicon electrical steel iron core.
Therefore, this detailed description of the invention has that technique is simple, the cycle is short, stock utilization is high and the feature of low cost；Institute
The high-silicon electrical steel iron core iron loss of the intergranular insulation of preparation is low, and steadiness is good, and service life is long.
Claims (6)
1. the preparation method of the high-silicon electrical steel iron core of an intergranular insulation, it is characterised in that the concrete steps of described preparation method
It is:
The first step, ferro-silicium powder surface modifications
By ferro-silicium powder: dehydrated alcohol: silane coupler: the mass ratio of distilled water is 1:(6 ~ 10): (0.04 ~ 0.1):
(0.2 ~ 0.5), is sequentially added into ferro-silicium powder, dehydrated alcohol, silane coupler and distilled water in reaction vessel, 40 ~
Stir 1 ~ 3h under the conditions of 70 DEG C, obtain the mixed solution of ferro-silicium powder containing surface modification；
Second step, the preparation of nucleocapsid heterojunction structure composite powder
Under 40 ~ 70 DEG C and stirring condition, first add in the mixed solution of the described ferro-silicium powder containing surface modification
Tetraethyl orthosilicate or methyl silicate, add ammonia, continues stirring 8 ~ 24h under the conditions of 40 ~ 70 DEG C；With distilled water wash 2 ~
3 times, with absolute ethanol washing 5 ~ 8 times, filter, vacuum drying, obtain nucleocapsid heterojunction structure composite powder；
Wherein: ferro-silicium powder: the mass ratio of tetraethyl orthosilicate is 1:(0.1 ~ 2), ferro-silicium powder: methyl silicate
Mass ratio is 1:(0.1 ~ 2)；Ferro-silicium powder: the mass ratio of ammonia is 1:(0.02 ~ 0.4)；
3rd step, annealing heat treatment
Described nucleocapsid heterojunction structure composite powder is inserted in annealing furnace, under the conditions of 600 ~ 800 DEG C, is incubated 1 ~ 3h, cold with stove
But to room temperature, it is thus achieved that the nucleocapsid heterojunction structure composite powder annealing heat treated；
4th step, the preparation of high-silicon electrical steel powder compact
By compressing for the described nucleocapsid heterojunction structure composite powder made annealing treatment, it is thus achieved that high-silicon electrical steel powder compact；
The preparation of the high-silicon electrical steel iron core of the 5th step, intergranular insulation
Described high-silicon electrical steel powder compact is inserted in sintering furnace, under the conditions of 950 ~ 1350 DEG C, sinters 1 ~ 10h, cold with stove
But to room temperature, the high-silicon electrical steel iron core of intergranular insulation is obtained.
2. the preparation method of the high-silicon electrical steel iron core insulated according to intergranular described in claim 1, it is characterised in that described ferrum
The Si content of silicon alloy powder is 4.0 ~ 7.5wt%.
3. according to the preparation method of high-silicon electrical steel iron core of the insulation of intergranular described in claim 1, it is characterised in that described in move back
Stove is the annealing furnace of vacuum protection or for the annealing furnace of inert gas shielding.
4. the preparation method of the high-silicon electrical steel iron core insulated according to intergranular described in claim 1, it is characterised in that described burning
Freezing of a furnace is the sintering furnace of vacuum protection or for the sintering furnace of inert gas shielding.
5. the preparation method of the high-silicon electrical steel iron core insulated according to intergranular described in claim 1, it is characterised in that described pressure
The pressure making type is 100 ~ 600Mpa.
6. the high-silicon electrical steel iron core of an intergranular insulation, it is characterised in that the high-silicon electrical steel iron core of described intergranular insulation is root
Exhausted according to the intergranular prepared by the preparation method of the high-silicon electrical steel iron core of the intergranular insulation according to any one of claim 1 ~ 5
The high-silicon electrical steel iron core of edge.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410354648.9A CN104078230B (en) | 2014-07-24 | 2014-07-24 | A kind of high-silicon electrical steel iron core of intergranular insulation and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410354648.9A CN104078230B (en) | 2014-07-24 | 2014-07-24 | A kind of high-silicon electrical steel iron core of intergranular insulation and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104078230A CN104078230A (en) | 2014-10-01 |
| CN104078230B true CN104078230B (en) | 2016-09-14 |
Family
ID=51599430
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410354648.9A Active CN104078230B (en) | 2014-07-24 | 2014-07-24 | A kind of high-silicon electrical steel iron core of intergranular insulation and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104078230B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106825551A (en) * | 2016-12-26 | 2017-06-13 | 安徽工业大学 | Silicon steel soft magnet core high based on laser sintered 3D printing and preparation method thereof |
| CN107186211B (en) * | 2017-05-18 | 2018-06-19 | 中国人民解放军陆军工程大学 | Method for coating atomized spherical aluminum-magnesium alloy powder with silane coupling agent |
| CN107999765A (en) * | 2017-12-18 | 2018-05-08 | 中南大学 | A kind of method that powder warm-rolling prepares Fe-6.5%Si soft magnetic materials thin strips |
| CN107900355A (en) * | 2017-12-18 | 2018-04-13 | 中南大学 | A kind of method that powder warm-rolling prepares high silicon steel thin belt material |
| CN107914017A (en) * | 2017-12-18 | 2018-04-17 | 中南大学 | A kind of powder warm-rolling preparation method of Fe 6.5%Si soft magnetic materials thin strips |
| CN107900351A (en) * | 2017-12-18 | 2018-04-13 | 中南大学 | A kind of powder rolling manufacture method of high silicon steel thin belt material |
| CN108677185B (en) * | 2018-05-29 | 2020-05-15 | 昆明理工大学 | Preparation method of high-silicon high-niobium coating |
| CN109014177A (en) * | 2018-08-31 | 2018-12-18 | 国网江苏省电力有限公司泰州供电分公司 | A kind of preparation method of insulating wrapped composite powder and transformer core |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101933103A (en) * | 2007-11-02 | 2010-12-29 | 丰田自动车株式会社 | Powder for magnetic core, powder magnetic core, and their production methods |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001267113A (en) * | 2000-03-16 | 2001-09-28 | Yaskawa Electric Corp | Method of manufacturing soft magnetic material |
-
2014
- 2014-07-24 CN CN201410354648.9A patent/CN104078230B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101933103A (en) * | 2007-11-02 | 2010-12-29 | 丰田自动车株式会社 | Powder for magnetic core, powder magnetic core, and their production methods |
Non-Patent Citations (3)
| Title |
|---|
| 《6.5wt%Si高硅钢冷轧薄板制备工艺、结构和性能》;林均品等;《前言科学》;20070630;全文 * |
| 《Si02绝缘包覆制备高频低损耗铁基软磁复合材料》;李爱坤;《中国优秀硕士论文全文数据库》;20140615;第20-40页 * |
| 《含核壳异质结构6．5%Si 高硅钢铁芯的制备与磁性能》;吴朝阳等;《功能材料》;20130710;全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104078230A (en) | 2014-10-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104078230B (en) | A kind of high-silicon electrical steel iron core of intergranular insulation and preparation method thereof | |
| CN104078182B (en) | A kind of iron-based soft magnetic composite magnetic powder core and preparation method thereof | |
| CN106041061B (en) | A kind of preparation method of the low-loss composite magnetic powder core of high-performance | |
| CN101935800B (en) | High-silicon-steel thin belt and preparation method thereof | |
| CN103093916B (en) | Neodymium iron boron magnetic materials and preparation method of the same | |
| CN102071339A (en) | Samarium-cobalt permanent magnet material and preparation method thereof | |
| CN103060822A (en) | Blueing treatment process for semi-processed electrical steel rotor or stator | |
| CN105063473B (en) | Method for manufacturing non-oriented high-silicon steel cold-rolled sheet based on strip cast rolling and DID (deformation induced disordering) | |
| CN109108238B (en) | Preparation method of high-resistivity iron-based nanocrystalline alloy thin strip | |
| CN104347218A (en) | Novel sintered ndfeb permanent magnet and preparation method thereof | |
| CN103820741B (en) | A kind of mu-metal material for energy-saving electric machine and preparation method thereof | |
| CN102274937B (en) | Method for preparing ferrite stainless steel thin tape containing inversion segregation stannum | |
| CN105154775B (en) | A kind of fusion reactor is used can low temperature generation α-Al2O3The base steel structural material of hydrogen permeation barrier | |
| CN102818454A (en) | Composite crucible with advantages of energy saving, low cost and capability of being alloyed | |
| CN103834862A (en) | Iron-cobalt alloy and preparation method of magnetizing pole head of iron-cobalt alloy | |
| CN103469069B (en) | Austenite low-permeability steel with lower yield strength not less than 810MPa and production method | |
| CN106270425B (en) | A kind of magnetic refrigerating material mass production preparation method | |
| CN104087840A (en) | Preparation method of iron-based soft magnetic material | |
| Wang et al. | Development of the new energy-efficient amorphous iron based electrical motor | |
| CN103495725B (en) | A kind of iron-silicon-aluminum soft magnetic powder granule-morphology treatment process | |
| CN107354401B (en) | A kind of amorphous alloy magnetism band vacuum heat treatment process | |
| CN107502775A (en) | It is a kind of to be used to manufacture alloy material of rotor and preparation method thereof | |
| CN109778082A (en) | A kind of Fe-based amorphous alloy and its preparation method and application of high/low temperature annealing toughness | |
| CN105118600A (en) | Magnetic powder alloy material | |
| CN1331168C (en) | Heat treatment of soft magnetic components |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |