CN104078230A - Intergranular insulated high-silicon electrical steel core and preparation method thereof - Google Patents
Intergranular insulated high-silicon electrical steel core and preparation method thereof Download PDFInfo
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- CN104078230A CN104078230A CN201410354648.9A CN201410354648A CN104078230A CN 104078230 A CN104078230 A CN 104078230A CN 201410354648 A CN201410354648 A CN 201410354648A CN 104078230 A CN104078230 A CN 104078230A
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Abstract
The invention relates to an intergranular insulated high-silicon electrical steel core and a preparation method thereof. According to the technical scheme, iron-silicon alloy powder, absolute ethyl alcohol, a silane coupling agent and distilled water are sequentially added into a reaction container according to the mass ratio of iron-silicon alloy powder, absolute ethyl alcohol, the silane coupling agent and distilled water of 1: (6-10): (0.04-0.1): (0.2-0.5) and then are stirred; tetraethoxysilane or tetramethoxysilane is added, ammonium hydroxide is added, and stirring is continuously performed; a mixture is washed, filtered and dried; the mixture is kept warm for 1-3 hours at the temperature of 600 DEG C to 800 DEG C and is cooled with a furnace and subjected to press forming; and a product is placed in a sintering furnace to be sintered for 1-10 hours at the temperature of 950 DEG C to 1,350 DEG C and is cooled with the furnace, and the intergranular insulated high-silicon electrical steel core is obtained. The intergranular insulated high-silicon electrical steel core and the preparation method have the characteristics of simple process, short period, high material utilization rate and low cost, and the prepared intergranular insulated high-silicon electrical steel core is low in loss, good in stability and long in service life.
Description
Technical field
The invention belongs to high-silicon electrical steel iron core technical field.Be specifically related to high-silicon electrical steel iron core of a kind of intergranular insulation and preparation method thereof.
Background technology
In recent years, along with the propelling of energy-saving and emission-reduction policy and applying of high efficiency motor, following middle and small motor and electrical micro-machine field will significantly increase the demand of high grade non-oriented electrical steel.In addition, along with the exploitation of the universal and high speed rotating motor of main flow motor frequency conversion control model, non-oriented electrical steel has been proposed to the requirement of high frequency, high magnetic strength and 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, Shi electricity – magnetic conversion equipment is realized the key of low energy consumption, low heating, microminaturization, low noise, high stable and environmental protection.
As everyone knows, because the eddy current loss of iron core is relevant with square forward of electrical sheet gauge of sheet, so to reduce electrical sheet gauge of sheet as far as possible, conventionally by milling method by its THICKNESS CONTROL below 1mm, to reduce eddy current loss.But, for high-silicon electrical steel, especially, in the time that silicone content exceedes 4.5wt%, in high-silicon electrical steel, be prone to B
2and DO
3ordered phase, causes its plasticity and toughness sharply to decline, and elongation is almost equal to zero, and rolling, moulding and punching are extremely difficult, produce with application be subject to serious restriction, so high-silicon electrical steel be difficult to by pair rolling method by its THICKNESS CONTROL in 1mm.
For high-silicon electrical steel plasticity and toughness sharply decline, the problem such as roll forming difficulty, a large amount of research has been carried out in reason that Chinese scholars increases in high-silicon electrical steel fragility, the aspect such as fragility that how to strengthen its plasticity and toughness and how to avoid electrical sheet, propose many new technology and methods, advanced effectively the development of high-silicon electrical steel.The object of technological innovation is intended to improve its plasticity and toughness and machinability by structure control, or avoids traditional rolling mill practice completely, adopts new method to prepare high-silicon electrical steel thin plate.As can be effectively suppressed or reduce the formation of ordered phase taking rapid solidification (cooling) technology as methods such as basic reaction-injection moulding and melt rapid quenching die castings (solidifying), to improve the machinability of high-silicon electrical steel.Also can be by adding trace alloying element and optimizing existing rolling technique, as " a kind of containing high silicon steel thin belt of chromium and preparation method thereof " (CN103276174A) patented technology and " a kind of high silicon steel thin belt and preparation method thereof " (CN101935800B) patented technology, adopt the cold rolling or Duan Zao – Re Zha – Wen Zha – cold-rolling process of the most conventional Re Zha –, progressively promote the ductility of high-silicon electrical steel, also can successfully obtain the ultra-thin high-silicon electrical steel thin plate of excellent performance.Another kind of Research Thinking is to avoid existing rolling technique, development is taking Chen Ji – diffusion method as basic correlation technique, as chemical vapour deposition (CVD), plasma activated chemical vapour deposition, the siliconising of hot dipping stain, embedding siliconising, magnetron sputtering, fused salt electro-deposition, electro beam physics vapour deposition, laser melting coating, the technology such as electrophoretic deposition, and for example " hot-dip silicon legal system is for method and the silicon strip continuous preparation device of high-silicon steel thin strip " (CN103320737A) patented technology and " by the suitability for industrialized production system of the high silicon strip of magnetron sputtering continuous two-sided codeposition technique system " (CN101319306A) patented technology, all can obtain the high-silicon electrical steel thin plate of excellent performance.
Although both at home and abroad researcher has carried out extensive and deep basic research work for the relevant variety of issue of high-silicon electrical steel, above-mentioned prior art or because cost is compared with high or because being subject to environmental constraints or further applying not or because stock utilization has restricted it compared with the problem such as low because of technical maturity.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art, and object is to provide that a kind of iron loss is low, steadiness good, the high-silicon electrical steel iron core of long service life, stock utilization is high and production cost is low intergranular insulation and preparation method thereof.
To achieve these goals, preparation method's of the present invention concrete steps are:
The first step, the modification of ferro-silicium powder surface
Be 1 ︰ (6 ~ 10) ︰ (0.04 ~ 0.1) ︰ (0.2 ~ 0.5) by ferro-silicium Fen Mo ︰ Wu the mass ratio of Shui Yi Chun ︰ Gui alkane Ou Lian Ji ︰ distilled water, ferro-silicium powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 40 ~ 70 DEG C of conditions, stir 1 ~ 3h, obtain the mixed solution containing the ferro-silicium powder of surface modification.
The preparation of second step, nucleocapsid heterostructure 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 tetraethoxysilane or methyl silicate, then add ammoniacal liquor, under 40 ~ 70 DEG C of conditions, continue to stir 8 ~ 24h; With distilled water washing 2 ~ 3 times, use absolute ethanol washing 5 ~ 8 times, to filter, vacuumize, obtains nucleocapsid heterostructure composite powder.
Wherein: the mass ratio of ferro-silicium Fen Mo ︰ tetraethoxysilane is 1:(0.1 ~ 2), the mass ratio of ferro-silicium Fen Mo ︰ methyl silicate is 1:(0.1 ~ 2); The mass ratio of ferro-silicium Fen Mo ︰ ammoniacal liquor is 1:(0.02 ~ 0.4).
The 3rd step, annealing heat treatment
Described nucleocapsid heterostructure composite powder is inserted in annealing furnace, under 600 ~ 800 DEG C of conditions, be incubated 1 ~ 3h, cool to room temperature with the furnace, obtain the heat treated nucleocapsid heterostructure composite powder of annealing.
The preparation of the 4th step, high-silicon electrical steel powder compact
The nucleocapsid heterostructure composite powder that described annealing in process is crossed is compressing, obtains 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, and sintering 1 ~ 10h under 950 DEG C ~ 1350 DEG C conditions, cools to room temperature with the furnace, obtains 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 the annealing furnace for inert gas shielding.
Described sintering furnace is the sintering furnace of vacuum protection or the sintering furnace for inert gas shielding.
Described compressing pressure is 100Mpa ~ 600Mpa.
Owing to adopting technique scheme, the present invention has the following advantages:
1) preparation method of the high-silicon electrical steel iron core of intergranular insulation disclosed by the invention, has avoided the bottleneck that existing high-silicon electrical steel is difficult to rolling, and a step sinter molding can obtain high-silicon electrical steel iron core, without rolling, compared with prior art technique is simple, and the cycle is short, and cost is low.
2) the present invention adopts surface coated method at ferro-silicium surface coated silica insulating barrier, realize the intergranular insulation of ferro-silicium, avoid the use of existing high-silicon electrical steel leaf insulator coating, improved the steadiness of high-silicon electrical steel iron core, extended useful 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 ferro-silicium in insulating wrapped district, and eddy current loss is little compared with existing high-silicon electrical steel iron core, and iron loss is low.
The high-silicon electrical steel iron core of the prepared intergranular of this embodiment insulation is after testing: saturation induction density is 158 ~ 186emu/g; Resistivity is 1.9 × 10
-2Ω * m ~ insulation; Iron loss P
5/50be 0.25 ~ 0.50W/kg, P
5/400be 5.85 ~ 10.32W/kg, P
5/1000be 20.93 ~ 36.92W/kg.
4) preparation method of the high-silicon electrical steel iron core that the present invention proposes, can directly prepare annular, E shape, back-shaped and fan-shaped and other Special-shaped iron core by the design of mould, and without punching process, stock utilization is high, and cost is low.
Therefore, the present invention has the advantages that technique is simple, the cycle is short, stock utilization is high and cost is low; The high-silicon electrical steel iron core iron loss of prepared intergranular insulation is low, and steadiness is good, long service life.
Brief description of the drawings
Fig. 1 is the section SEM figure of the high-silicon electrical steel iron core of the prepared a kind of intergranular insulation of the present invention;
Fig. 2 is iron loss spectrogram under the different frequency of high-silicon electrical steel iron core of intergranular shown in Fig. 1 insulation;
Fig. 3 is the pictorial diagram of the high-silicon electrical steel iron core of the intergranular insulation shown in Fig. 1.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention will be further described, not the restriction to its protection range.
The Si content of the powder of ferro-silicium described in this embodiment is 4.0 ~ 7.5wt%, in embodiment, repeats no more.
embodiment 1
High-silicon electrical steel iron core of a kind of intergranular insulation and preparation method thereof.Described preparation method's concrete steps are:
The first step, the modification of ferro-silicium powder surface
Be 1 ︰ (6 ~ 7) ︰ (0.04 ~ 0.05) ︰ (0.2 ~ 0.25) by ferro-silicium Fen Mo ︰ Wu the mass ratio of Shui Yi Chun ︰ Gui alkane Ou Lian Ji ︰ distilled water, ferro-silicium powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 40 ~ 45 DEG C of conditions, stir 1.5 ~ 2h, obtain the mixed solution containing the ferro-silicium powder of surface modification.
The preparation of second step, nucleocapsid heterostructure 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 tetraethoxysilane, then add ammoniacal liquor, under 40 ~ 45 DEG C of conditions, continue to stir 8 ~ 10h; With distilled water washing 2 ~ 3 times, use absolute ethanol washing 5 ~ 6 times, to filter, vacuumize, obtains nucleocapsid heterostructure composite powder.
Wherein: the mass ratio of ferro-silicium Fen Mo ︰ tetraethoxysilane is 1:(0.1 ~ 0.4); The mass ratio of ferro-silicium Fen Mo ︰ ammoniacal liquor is 1:(0.02 ~ 0.05).
The 3rd step, annealing heat treatment
Described nucleocapsid heterostructure composite powder is inserted in the annealing furnace of vacuum protection, under 600 ~ 650 DEG C of conditions, be incubated 1.5 ~ 2h, cool to room temperature with the furnace, obtain the heat treated nucleocapsid heterostructure composite powder of annealing.
The preparation of the 4th step, high-silicon electrical steel powder compact
The nucleocapsid heterostructure composite powder that described annealing in process is crossed is compressing, and compressing pressure is 100 ~ 200Mpa, obtains 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, and sintering 2 ~ 4h under 950 ~ 1000 DEG C of conditions, 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 prepared intergranular of the present embodiment insulation is after testing: saturation induction density is 184 ~ 186emu/g; Resistivity is 2.8 × 10
-2~ 3.0 × 10
-2Ω * m; Iron loss P
5/50be 0.42 ~ 0.43W/kg, P
5/400be 8.93 ~ 9.01W/kg, P
5/1000be 31.95 ~ 32.24W/kg.
embodiment 2
High-silicon electrical steel iron core of a kind of intergranular insulation and preparation method thereof.Described preparation method's concrete steps are:
The first step, the modification of ferro-silicium powder surface
Be 1 ︰ (7 ~ 8) ︰ (0.05 ~ 0.06) ︰ (0.25 ~ 0.3) by ferro-silicium Fen Mo ︰ Wu the mass ratio of Shui Yi Chun ︰ Gui alkane Ou Lian Ji ︰ distilled water, ferro-silicium powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 45 ~ 50 DEG C of conditions, stir 2.5 ~ 3h, obtain the mixed solution containing the ferro-silicium powder of surface modification.
The preparation of second step, nucleocapsid heterostructure 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, then add ammoniacal liquor, under 45 ~ 50 DEG C of conditions, continue to stir 10 ~ 12h; With distilled water washing 2 ~ 3 times, use absolute ethanol washing 6 ~ 7 times, to filter, vacuumize, obtains nucleocapsid heterostructure composite powder.
Wherein: the mass ratio of ferro-silicium Fen Mo ︰ methyl silicate is 1:(0.4 ~ 0.6); The mass ratio of ferro-silicium Fen Mo ︰ ammoniacal liquor is 1:(0.05 ~ 0.1).
The 3rd step, annealing heat treatment
Described nucleocapsid heterostructure composite powder is inserted in the annealing furnace of vacuum protection, under 650 ~ 700 DEG C of conditions, be incubated 2 ~ 2.5h, cool to room temperature with the furnace, obtain the heat treated nucleocapsid heterostructure composite powder of annealing.
The preparation of the 4th step, high-silicon electrical steel powder compact
The nucleocapsid heterostructure composite powder that described annealing in process is crossed is compressing, and compressing pressure is 200 ~ 300Mpa, obtains 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, and sintering 4 ~ 6h under 1000 ~ 1050 DEG C of conditions, 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 prepared intergranular of the present embodiment insulation is after testing: saturation induction density is 180 ~ 182emu/g; Resistivity is 1.4 × 10
-2~ 1.6 × 10
-2Ω * m; Iron loss P
5/50be 0.36 ~ 0.37W/kg, P
5/400be 7.66 ~ 7.74W/kg, P
5/1000be 27.41 ~ 27.69W/kg.
embodiment 3
High-silicon electrical steel iron core of a kind of intergranular insulation and preparation method thereof.Described preparation method's concrete steps are:
The first step, the modification of ferro-silicium powder surface
Be 1 ︰ (8 ~ 9) ︰ (0.06 ~ 0.07) ︰ (0.3 ~ 0.35) by ferro-silicium Fen Mo ︰ Wu the mass ratio of Shui Yi Chun ︰ Gui alkane Ou Lian Ji ︰ distilled water, ferro-silicium powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 50 ~ 55 DEG C of conditions, stir 1 ~ 1.5h, obtain the mixed solution containing the ferro-silicium powder of surface modification.
The preparation of second step, nucleocapsid heterostructure 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 tetraethoxysilane, then add ammoniacal liquor, under 50 ~ 55 DEG C of conditions, continue to stir 12 ~ 14h; With distilled water washing 2 ~ 3 times, use absolute ethanol washing 7 ~ 8 times, to filter, vacuumize, obtains nucleocapsid heterostructure composite powder.
Wherein: the mass ratio of ferro-silicium Fen Mo ︰ tetraethoxysilane is 1:(0.6 ~ 1); The mass ratio of ferro-silicium Fen Mo ︰ ammoniacal liquor is 1:(0.1 ~ 0.15).
The 3rd step, annealing heat treatment
Described nucleocapsid heterostructure composite powder is inserted in the annealing furnace of vacuum protection, under 700 ~ 750 DEG C of conditions, be incubated 2.5 ~ 3h, cool to room temperature with the furnace, obtain the heat treated nucleocapsid heterostructure composite powder of annealing.
The preparation of the 4th step, high-silicon electrical steel powder compact
The nucleocapsid heterostructure composite powder that described annealing in process is crossed is compressing, and compressing pressure is 300 ~ 400Mpa, obtains 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, and sintering 6 ~ 8h under 1050 ~ 1100 DEG C of conditions, 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 prepared intergranular of the present embodiment insulation is after testing: saturation induction density is 176 ~ 178emu/g; Resistivity is 8.0 × 10
-1~ 8.2 × 10
-1Ω * m; Iron loss P
5/50be 0.33 ~ 0.34W/kg, P
5/400be 7.14 ~ 7.22W/kg, P
5/1000be 25.55 ~ 25.83W/kg.
embodiment 4
High-silicon electrical steel iron core of a kind of intergranular insulation and preparation method thereof.Described preparation method's concrete steps are:
The first step, the modification of ferro-silicium powder surface
Be 1 ︰ (9 ~ 10) ︰ (0.07 ~ 0.08) ︰ (0.35 ~ 0.40) by ferro-silicium Fen Mo ︰ Wu the mass ratio of Shui Yi Chun ︰ Gui alkane Ou Lian Ji ︰ distilled water, ferro-silicium powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 55 ~ 60 DEG C of conditions, stir 2 ~ 2.5h, obtain the mixed solution containing the ferro-silicium powder of surface modification.
The preparation of second step, nucleocapsid heterostructure 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, then add ammoniacal liquor, under 55 ~ 60 DEG C of conditions, continue to stir 14 ~ 16h; With distilled water washing 2 ~ 3 times, use absolute ethanol washing 5 ~ 6 times, to filter, vacuumize, obtains nucleocapsid heterostructure composite powder.
Wherein: the mass ratio of ferro-silicium Fen Mo ︰ methyl silicate is 1:(1 ~ 1.2); The mass ratio of ferro-silicium Fen Mo ︰ ammoniacal liquor is 1:(0.15 ~ 0.2).
The 3rd step, annealing heat treatment
Described nucleocapsid heterostructure composite powder is inserted in the annealing furnace of vacuum protection, under 750 ~ 800 DEG C of conditions, be incubated 1 ~ 1.5h, cool to room temperature with the furnace, obtain the heat treated nucleocapsid heterostructure composite powder of annealing.
The preparation of the 4th step, high-silicon electrical steel powder compact
The nucleocapsid heterostructure composite powder that described annealing in process is crossed is compressing, and compressing pressure is 400 ~ 500Mpa, obtains 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, and sintering 8 ~ 10h under 1100 ~ 1150 DEG C of conditions, 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 prepared intergranular of the present embodiment insulation is after testing: saturation induction density is 175 ~ 177emu/g; Resistivity is insulation; Iron loss P
5/50be 0.29 ~ 0.30W/kg, P
5/400be 6.11 ~ 6.19W/kg, P
5/1000be 21.86 ~ 22.14W/kg.
embodiment 5
High-silicon electrical steel iron core of a kind of intergranular insulation and preparation method thereof.Described preparation method's concrete steps are:
The first step, the modification of ferro-silicium powder surface
Be 1 ︰ (6 ~ 6.5) ︰ (0.08 ~ 0.09) ︰ (0.4 ~ 0.45) by ferro-silicium Fen Mo ︰ Wu the mass ratio of Shui Yi Chun ︰ Gui alkane Ou Lian Ji ︰ distilled water, ferro-silicium powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 60 ~ 65 DEG C of conditions, stir 1.5 ~ 2h, obtain the mixed solution containing the ferro-silicium powder of surface modification.
The preparation of second step, nucleocapsid heterostructure 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, then add ammoniacal liquor, under 60 ~ 65 DEG C of conditions, continue to stir 16 ~ 18h; With distilled water washing 2 ~ 3 times, use absolute ethanol washing 7 ~ 8 times, to filter, vacuumize, obtains nucleocapsid heterostructure composite powder.
Wherein: the mass ratio of ferro-silicium Fen Mo ︰ methyl silicate is 1:(1.2 ~ 1.4); The mass ratio of ferro-silicium Fen Mo ︰ ammoniacal liquor is 1:(0.2 ~ 0.25).
The 3rd step, annealing heat treatment
Described nucleocapsid heterostructure composite powder is inserted in the annealing furnace of inert gas shielding, under 600 ~ 700 DEG C of conditions, be incubated 1 ~ 2h, cool to room temperature with the furnace, obtain the heat treated nucleocapsid heterostructure composite powder of annealing.
The preparation of the 4th step, high-silicon electrical steel powder compact
The nucleocapsid heterostructure composite powder that described annealing in process is crossed is compressing, and compressing pressure is 500 ~ 600Mpa, obtains 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, and sintering 1 ~ 3h under 1150 ~ 1200 DEG C of conditions, 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 prepared intergranular of the present embodiment insulation is after testing: saturation induction density is 168 ~ 170emu/g; Resistivity is insulation; Iron loss P
5/50be 0.28 ~ 0.30W/kg, P
5/400be 6.04 ~ 6.12W/kg, P
5/1000be 21.61 ~ 21.90W/kg.
embodiment 6
High-silicon electrical steel iron core of a kind of intergranular insulation and preparation method thereof.Described preparation method's concrete steps are:
The first step, the modification of ferro-silicium powder surface
Be 1 ︰ (6.5 ~ 8) ︰ (0.09 ~ 0.1) ︰ (0.45 ~ 0.5) by ferro-silicium Fen Mo ︰ Wu the mass ratio of Shui Yi Chun ︰ Gui alkane Ou Lian Ji ︰ distilled water, ferro-silicium powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 65 ~ 70 DEG C of conditions, stir 2.5 ~ 3h, obtain the mixed solution containing the ferro-silicium powder of surface modification.
The preparation of second step, nucleocapsid heterostructure 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, then add ammoniacal liquor, under 65 ~ 70 DEG C of conditions, continue to stir 18 ~ 20h; With distilled water washing 2 ~ 3 times, use absolute ethanol washing 7 ~ 8 times, to filter, vacuumize, obtains nucleocapsid heterostructure composite powder.
Wherein: the mass ratio of ferro-silicium Fen Mo ︰ methyl silicate is 1:(1.4 ~ 1.6); The mass ratio of ferro-silicium Fen Mo ︰ ammoniacal liquor is 1:(0.25 ~ 0.3).
The 3rd step, annealing heat treatment
Described nucleocapsid heterostructure composite powder is inserted in the annealing furnace of inert gas shielding, under 700 ~ 800 DEG C of conditions, be incubated 2 ~ 3h, cool to room temperature with the furnace, obtain the heat treated nucleocapsid heterostructure composite powder of annealing.
The preparation of the 4th step, high-silicon electrical steel powder compact
The nucleocapsid heterostructure composite powder that described annealing in process is crossed is compressing, and compressing pressure is 350 ~ 400Mpa, obtains 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, and sintering 3 ~ 5h under 1200 ~ 1250 DEG C of conditions, 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 prepared intergranular of the present embodiment insulation is after testing: saturation induction density is 165 ~ 167emu/g; Resistivity is insulation; Iron loss P
5/50be 0.27 ~ 0.28W/kg, P
5/400be 5.85 ~ 5.93W/kg, P
5/1000be 20.93 ~ 21.22W/kg.
embodiment 7
High-silicon electrical steel iron core of a kind of intergranular insulation and preparation method thereof.Described preparation method's concrete steps are:
The first step, the modification of ferro-silicium powder surface
Be 1 ︰ (8 ~ 8.5) ︰ (0.04 ~ 0.07) ︰ (0.25 ~ 0.35) by ferro-silicium Fen Mo ︰ Wu the mass ratio of Shui Yi Chun ︰ Gui alkane Ou Lian Ji ︰ distilled water, ferro-silicium powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 40 ~ 55 DEG C of conditions, stir 1 ~ 2h, obtain the mixed solution containing the ferro-silicium powder of surface modification.
The preparation of second step, nucleocapsid heterostructure 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 tetraethoxysilane, then add ammoniacal liquor, under 40 ~ 55 DEG C of conditions, continue to stir 20 ~ 22h; With distilled water washing 2 ~ 3 times, use absolute ethanol washing 6 ~ 7 times, to filter, vacuumize, obtains nucleocapsid heterostructure composite powder.
Wherein: the mass ratio of ferro-silicium Fen Mo ︰ tetraethoxysilane is 1:(1.6 ~ 1.8); The mass ratio of ferro-silicium Fen Mo ︰ ammoniacal liquor is 1:(0.3 ~ 0.35).
The 3rd step, annealing heat treatment
Described nucleocapsid heterostructure composite powder is inserted in the annealing furnace of inert gas shielding, under 730 ~ 780 DEG C of conditions, be incubated 1 ~ 1.5h, cool to room temperature with the furnace, obtain the heat treated nucleocapsid heterostructure composite powder of annealing.
The preparation of the 4th step, high-silicon electrical steel powder compact
The nucleocapsid heterostructure composite powder that described annealing in process is crossed is compressing, and compressing pressure is 400 ~ 450Mpa, obtains 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, and sintering 5 ~ 7h under 1250 ~ 1300 DEG C of conditions, 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 prepared intergranular of the present embodiment insulation is after testing: saturation induction density is 170 ~ 172emu/g; Resistivity is 1.9 × 10
-2~ 2.1 × 10
-2Ω * m; Iron loss P
5/50be 0.49 ~ 0.50W/kg, P
5/400be 10.24 ~ 10.32W/kg, P
5/1000be 36.64 ~ 36.92W/kg.
embodiment 8
High-silicon electrical steel iron core of a kind of intergranular insulation and preparation method thereof.Described preparation method's concrete steps are:
The first step, the modification of ferro-silicium powder surface
Be 1 ︰ (8.5 ~ 10) ︰ (0.07 ~ 0.1) ︰ (0.3 ~ 0.35) by ferro-silicium Fen Mo ︰ Wu the mass ratio of Shui Yi Chun ︰ Gui alkane Ou Lian Ji ︰ distilled water, ferro-silicium powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 55 ~ 70 DEG C of conditions, stir 2 ~ 3h, obtain the mixed solution containing the ferro-silicium powder of surface modification.
The preparation of second step, nucleocapsid heterostructure 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 tetraethoxysilane, then add ammoniacal liquor, under 55 ~ 70 DEG C of conditions, continue to stir 22 ~ 24h; With distilled water washing 2 ~ 3 times, use absolute ethanol washing 5 ~ 6 times, to filter, vacuumize, obtains nucleocapsid heterostructure composite powder.
Wherein: the mass ratio of ferro-silicium Fen Mo ︰ tetraethoxysilane is 1:(1.8 ~ 2); The mass ratio of ferro-silicium Fen Mo ︰ ammoniacal liquor is 1:(0.02 ~ 0.4).
The 3rd step, annealing heat treatment
Described nucleocapsid heterostructure composite powder is inserted in the annealing furnace of vacuum protection, under 780 ~ 800 DEG C of conditions, be incubated 1.5 ~ 2h, cool to room temperature with the furnace, obtain the heat treated nucleocapsid heterostructure composite powder of annealing.
The preparation of the 4th step, high-silicon electrical steel powder compact
The nucleocapsid heterostructure composite powder that described annealing in process is crossed is compressing, and compressing pressure is 450 ~ 500Mpa, obtains 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, and sintering 7 ~ 10h under 1300 ~ 1350 DEG C of conditions, 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 prepared intergranular of the present embodiment insulation is after testing: saturation induction density is 158 ~ 160emu/g; Resistivity is insulation; Iron loss P
5/50be 0.25 ~ 0.27W/kg, P
5/400be 5.87 ~ 5.95W/kg, P
5/1000be 21.00 ~ 21.29W/kg.
This embodiment compared with prior art has following good effect:
1) preparation method of the high-silicon electrical steel iron core of the disclosed intergranular insulation of this embodiment, has avoided the bottleneck that existing high-silicon electrical steel is difficult to rolling, and a step sinter molding can obtain high-silicon electrical steel iron core, without rolling, compared with prior art technique is simple, and the cycle is short, and cost is low.
2) this embodiment adopts surface coated method at ferro-silicium surface coated silica insulating barrier, realize the intergranular insulation of ferro-silicium, avoid the use of existing high-silicon electrical steel leaf insulator coating, improve the steadiness of high-silicon electrical steel iron core, extend useful life, Fig. 1 is the SEM figure of the high-silicon electrical steel iron core of the prepared a kind of intergranular insulation of implementation column 4, can find out, in the high-silicon electrical steel iron core of intergranular insulation, ferro-silicium powder is by SiO
2evenly coated, realize the intergranular insulation of ferro-silicium.
3) the high-silicon electrical steel iron core of the intergranular insulation that prepared by this embodiment, its eddy current is limited in the ferro-silicium in insulating wrapped district, eddy current loss is little compared with existing high-silicon electrical steel iron core, iron loss is low, Fig. 2 is iron loss spectrogram under the different frequency of high-silicon electrical steel iron core of intergranular shown in Fig. 1 insulation, can find out its iron loss P
5/50be 0.25 ~ 0.27W/kg, P
5/400be 5.87 ~ 5.95W/kg, P
5/1000be 21.00 ~ 21.29W/kg.
The high-silicon electrical steel iron core of the prepared intergranular of this embodiment insulation is after testing: saturation induction density is 158 ~ 186emu/g; Resistivity is 1.9 × 10
-2Ω * m ~ insulation; Iron loss P
5/50be 0.25 ~ 0.50W/kg, P
5/400be 5.85 ~ 10.32W/kg, P
5/1000be 20.93 ~ 36.92W/kg.
4) preparation method of the high-silicon electrical steel iron core that this embodiment proposes, can directly prepare annular, E shape, back-shaped and fan-shaped and other Special-shaped iron core by the design of mould, and without punching process, stock utilization is high, and cost is low.Fig. 3 is the material object of the high-silicon electrical steel iron core of the intergranular insulation shown in Fig. 1, can find out, directly prepares the high-silicon electrical steel iron core of annular intergranular insulation by the design of mould.
Therefore, this embodiment has the advantages that technique is simple, the cycle is short, stock utilization is high and cost is low; The high-silicon electrical steel iron core iron loss of prepared intergranular insulation is low, and steadiness is good, long service life.
Claims (6)
1. a preparation method for the high-silicon electrical steel iron core of intergranular insulation, is characterized in that described preparation method's concrete steps are:
The first step, the modification of ferro-silicium powder surface
Be 1 ︰ (6 ~ 10) ︰ (0.04 ~ 0.1) ︰ (0.2 ~ 0.5) by ferro-silicium Fen Mo ︰ Wu the mass ratio of Shui Yi Chun ︰ Gui alkane Ou Lian Ji ︰ distilled water, ferro-silicium powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 40 ~ 70 DEG C of conditions, stir 1 ~ 3h, obtain the mixed solution containing the ferro-silicium powder of surface modification;
The preparation of second step, nucleocapsid heterostructure 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 tetraethoxysilane or methyl silicate, then add ammoniacal liquor, under 40 ~ 70 DEG C of conditions, continue to stir 8 ~ 24h; With distilled water washing 2 ~ 3 times, use absolute ethanol washing 5 ~ 8 times, to filter, vacuumize, obtains nucleocapsid heterostructure composite powder;
Wherein: the mass ratio of ferro-silicium Fen Mo ︰ tetraethoxysilane is 1:(0.1 ~ 2), the mass ratio of ferro-silicium Fen Mo ︰ methyl silicate is 1:(0.1 ~ 2); The mass ratio of ferro-silicium Fen Mo ︰ ammoniacal liquor is 1:(0.02 ~ 0.4);
The 3rd step, annealing heat treatment
Described nucleocapsid heterostructure composite powder is inserted in annealing furnace, under 600 ~ 800 DEG C of conditions, be incubated 1 ~ 3h, cool to room temperature with the furnace, obtain the heat treated nucleocapsid heterostructure composite powder of annealing;
The preparation of the 4th step, high-silicon electrical steel powder compact
The nucleocapsid heterostructure composite powder that described annealing in process is crossed is compressing, obtains 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, and sintering 1 ~ 10h under 950 ~ 1350 DEG C of conditions, cools to room temperature with the furnace, obtains the high-silicon electrical steel iron core of intergranular insulation.
2. according to the preparation method of the high-silicon electrical steel iron core of the insulation of intergranular described in claim 1, the Si content that it is characterized in that described ferro-silicium powder is 4.0 ~ 7.5wt%.
3. according to the preparation method of the high-silicon electrical steel iron core of the insulation of intergranular described in claim 1, it is characterized in that described annealing furnace is the annealing furnace of vacuum protection or the annealing furnace for inert gas shielding.
4. according to the preparation method of the high-silicon electrical steel iron core of the insulation of intergranular described in claim 1, it is characterized in that described sintering furnace is the sintering furnace of vacuum protection or the sintering furnace for inert gas shielding.
5. according to the preparation method of the high-silicon electrical steel iron core of the insulation of intergranular described in claim 1, it is characterized in that described compressing pressure is 100 ~ 600Mpa.
6. a high-silicon electrical steel iron core for intergranular insulation, the high-silicon electrical steel iron core that it is characterized in that described intergranular insulation is the high-silicon electrical steel iron core of the intergranular insulation prepared according to the preparation method of the high-silicon electrical steel iron core of the intergranular insulation described in any one in claim 1 ~ 5.
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