CN102360666A - Magnetically sensitive composite wire and preparation method thereof - Google Patents
Magnetically sensitive composite wire and preparation method thereof Download PDFInfo
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- CN102360666A CN102360666A CN2011103238639A CN201110323863A CN102360666A CN 102360666 A CN102360666 A CN 102360666A CN 2011103238639 A CN2011103238639 A CN 2011103238639A CN 201110323863 A CN201110323863 A CN 201110323863A CN 102360666 A CN102360666 A CN 102360666A
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Abstract
The invention discloses a magnetically sensitive composite wire and a preparation method thereof. The magnetic sensitive composite wire comprises nano-crystalline soft magnetic core and an organic and inorganic hybrid layer on the surface of the core. The nano-crystalline soft magnetic core comprises, by weight, 6% of Si4, 5-7% of Zr, 1-3% of Gd, 0.1-0.2% of Pr, 8% of B4, 3-6% of Nb, 1-3% of Ni, 1-2% of Co, and the balance Fe. The organic and inorganic hybrid layer is composed of TiO2, MgO, 3Al2O3-2SiO2, Y2O3 and ZrO2 according to the weight ratio of 1:1:1:0.03:0.5:3.5-4. The prepared magnetic sensitive composite wire is high in response speed, high in maximum impedance change rate, high in magnetic field sensitivity and fine in insulating performance.
Description
Technical field
The present invention relates to a kind of magnetosensitive composite filament and preparation method thereof, be specifically related to a kind of magnetosensitive composite filament with organic inorganic hybridization layer and nano-crystal soft-magnetic core.
Background technology
Patent CN200710301957.X relates to magnetic-sensitive material and preparation method thereof; This magnetic-sensitive material is to comprise metal-cored and composite material glassy layer; Wherein this glassy layer coats that this is metal-cored, and said metal-cored be that amorphous material and its composition comprise by mass percentage: the Fe of 1-15 quality %; The Si of 2-12 quality %; Total amount is among B, Nb, Cu, Mn, Mo, Ni, Cr and the Al one or more of being selected from of 2-25 quality %; And the Co of surplus.The SiO of glass tube 60-85 quality %
2The B that is not higher than 15 quality %
2O
3The Al that is not higher than 5 quality %
2O
3The Na that is not higher than 15 quality %
2O; Total amount is not higher than the K that is selected from of 20 quality %
2Among O, BaO, CaO and the MgO one or more.This invention is the heating foundry alloy, and the heat when making the foundry alloy fusing in the glass tube and relying on foundry alloy to melt makes the glass tube bottom softening; Pull out capillary glass tube from the glass tube bottom, filling the foundry alloy melt in this capillary; Capillary that cooling is pulled out and foundry alloy melt wherein, wherein this cooling is enough to make the foundry alloy melt to form amorphous state and makes the capillary glass tube sclerosis, obtains glass and coats amorphous wire.The response speed of this magnetic-sensitive material reaches 1 * 10
-7Second; Simultaneously, this magnetic-sensitive material keeps high impedance rate of change, and the maximum resistance variation rate reaches more than 200%; Magnetic field sensitivity reaches more than the 100%/Oe; This magnetic-sensitive material has the good mechanical performance, and its fracture strength reaches more than the 1GPa, helps the exploitation and the production of device; The glassy layer of this magnetic-sensitive material plays the effect of insulating barrier, and it still can keep insulation property more than 500 degrees centigrade.
But above-mentioned patent is to adopt glass to coat spin processes can between glassy layer and metal material, produce very big stress, the meeting raising of limiting material performance greatly; Glassy layer also receives the restriction of glassware material in addition, and the composition adjustability is poor.Core is a cobalt-base alloys, and cost is high.
Summary of the invention
To the objective of the invention is the defective that exists in the prior art in order solving, a kind of have superperformance, magnetosensitive composite filament that cost is low to be provided.
In order to achieve the above object, the invention provides a kind of magnetosensitive composite filament, comprise the organic inorganic hybridization layer on nano-crystal soft-magnetic core and core surface; Said nano-crystal soft-magnetic core by following component by weight percentage composition form: Si 4～6%, and Zr 5～7%, and Gd 1～3%, and Pr 0.1～0.2%, and B 4～8%, and Nb 3～6%, and Ni 1～3%, and Co 1～2%, and all the other are Fe; Said organic inorganic hybridization layer is by TiO
2, MgO, 3Al
2O
32SiO
2, Y
2O
3, ZrO
2Form by weight 1:1:1:0.03:0.5:3.5～4 with colloidal sol.
Further improvement of the present invention is: above-mentioned colloidal sol prepares through following steps: in flask, add tetraethoxysilane, γ-methacryloxypropyl trimethoxy silane and ethanol, its mol ratio is 3:2:2.Under vigorous stirring, splash into acetic acid, addition is 5g/100mL, and mixing speed is 600-800 rev/min; Behind the room temperature reaction 3h, add methyl methacrylate and initator azodiisobutyronitrile, addition is respectively 10g/100mL and 5g/100mL, stirs 20min under the room temperature and obtains colloidal sol.
The diameter of above-mentioned nano-crystal soft-magnetic core is 7～10 microns, and the thickness of organic inorganic hybridization layer is the 0.5-0.9 micron.
The present invention also provides a kind of preparation method of magnetosensitive composite filament, may further comprise the steps:
(1) preparation nano-crystal soft-magnetic core: get and get following core raw material by weight percentage: Si 4～6%, and Zr 5～7%, and Gd 1～3%, and Pr 0.1～0.2%; B 4～8%, and Nb 3～6%, and Ni 1～3%; Co 1～2%, and all the other are prepared burden for Fe, and wherein B adds with the mode of iron boron intermediate alloy; The core raw material is put into the melting of vaccum sensitive stove stove; Smelting temperature is 1580～1610 ℃, obtains the core foundry alloy, and the remelting tubular type crucible of putting into the vacuum induction quick quenching furnace then carries out remelting; Remelting temperature is that the top of 1550～1570 ℃ of remelting tubular type crucibles places 2～4mm place under the quick quenching furnace runner wheel rim; Foundry alloy places fusing in the tubular type crucible, under ar gas acting, overflows and the runner EDGE CONTACT of rotating from the crucible top behind the alloy molten, forms the alloy silk; Then the alloy silk is obtained the nano-crystal soft-magnetic core 300～350 ℃ of insulations after 1～1.5 hour.Wherein, the rotational line speed of fast pure stove runner is 21～24m/s, and diameter of alloy wire is 7～10 microns.The weight percentage that iron boron intermediate alloy contains B is 20%.
(2) preparation colloidal sol: in flask, add tetraethoxysilane, γ-methacryloxypropyl trimethoxy silane and ethanol, its mol ratio is 3:2:2-2.2, preferred 3:2:2; Under vigorous stirring, splash into acetic acid, addition is 4.5～5.5g/100mL, preferred 5g/100mL, and mixing speed is 600-800 rev/min; Room temperature reaction 2.5～3.5h; Behind the preferred 3h, add methyl methacrylate and initator azodiisobutyronitrile, addition is respectively 9～11 g/100mL; Preferred 10g/100mL and 4.5～5.5g/100mL; Preferred 5g/100mL stirs 15～25min under the room temperature then, and preferred 20min obtains colloidal sol.Wherein flask is the there-necked flask of belt stirrer.
(3) preparation magnetosensitive composite filament: with granularity is the TiO of 50～100nm
2, MgO, 3Al
2O
32SiO
2, Y
2O
3, ZrO
2And the colloidal sol that makes in the step (2) mixes and to obtain coating, wherein, and TiO
2, MgO, 3Al
2O
32SiO
2, Y
2O
3, ZrO
2With the weight ratio of colloidal sol be 1:1:1:0.03:0.5:3.5～4; Coating is applied to forms the organic inorganic hybridization layer on the nano-crystal soft-magnetic core that step (1) makes; Through 15～25min; Obtain organic inorganic hybridization layer nano-crystal soft-magnetic core magnetosensitive composite wire material behind the preferred 20min baking-curing, baking temperature is 130～150 ℃, preferred 140 ℃.Wherein the thickness of organic inorganic hybridization layer is the 0.5-0.9 micron.
The present invention compares prior art and has the following advantages: nano-crystal soft-magnetic core of the present invention adopts Si, Zr, B, Co, Nb to be used and guarantees that ferrous alloy is decrystallized easily; But Gd and Pr are used reinforced alloys simultaneously, guarantee that alloy core material has enough intensity, and element Ni and Pr are used and guarantee that alloy is in the nanoscale yardstick after being heated, and prevent growing up of crystal grain.TiO in the organic inorganic hybridization layer
2, MgO, mullite (3Al
2O
32SiO
2), Y
2O
3, ZrO
2Has good insulating properties.Adopt colloidal sol can guarantee that the inorganic powder in the organic inorganic hybridization layer firmly is attached to soft magnetism core surface.The present invention forms the cold inorganic material layer that is coated with in silk back at the soft magnetism core; Can between two kinds of materials, not produce very big stress; The response speed of magnetic-sensitive material is high, and the maximum resistance variation rate is high, and magnetic field sensitivity is high; Still insulation property can be kept more than 530 degrees centigrade, therefore material property can be improved to greatest extent; And can assign to optimize the performance of material through the one-tenth of regulating the inorganic powder in the organic inorganic hybridization layer.Core is a ferrous alloy, and institute's cost of material of getting is low, with short production cycle, and production technology is easy, and forming inorganic material layer does not need thermal energy consumption, low cost of manufacture.Be convenient to very much suitability for industrialized production.
Description of drawings
Fig. 1 is the organization chart of organic inorganic hybridization layer in the magnetosensitive composite filament of the present invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment magnetosensitive composite filament of the present invention is elaborated.
Embodiment one
1, preparation nano-crystal soft-magnetic core: get and get following core raw material by weight percentage: Si 4%, and Zr 5%, and Gd 1%, and Pr 0.1%, and B 4%, and Nb 3%, and Ni 1%, and Co 1%, and all the other are prepared burden for Fe, and wherein B adds with the mode of iron boron intermediate alloy; The core raw material is put into the melting of vaccum sensitive stove stove; Smelting temperature is 1580～1610 ℃, obtains the core foundry alloy, and the remelting tubular type crucible of putting into the vacuum induction quick quenching furnace then carries out remelting; Remelting temperature is that the top of 1550～1570 ℃ of remelting tubular type crucibles places 2～4mm place under the quick quenching furnace runner wheel rim; Foundry alloy places fusing in the tubular type crucible, under ar gas acting, overflows and the runner EDGE CONTACT of rotating from the crucible top behind the alloy molten, forms the alloy silk; Then the alloy silk is obtained the nano-crystal soft-magnetic core 300～350 ℃ of insulations after 1～1.5 hour.Wherein, the rotational line speed of fast pure stove runner is 24m/s, and diameter of alloy wire is 7 microns.The weight percentage that iron boron intermediate alloy contains B is 20%.
2, preparation colloidal sol: in the there-necked flask of belt stirrer, add tetraethoxysilane, γ-methacryloxypropyl trimethoxy silane and ethanol, its mol ratio is 3:2:2; Under vigorous stirring, splash into acetic acid, addition is 5g/100mL, and mixing speed is 600 rev/mins; Behind the room temperature reaction 3h, add methyl methacrylate and initator azodiisobutyronitrile, addition is respectively 10g/100mL and 5g/100mL, stirs 20min then under the room temperature and obtains colloidal sol.
3, preparation magnetosensitive composite filament: with granularity is the TiO of 50nm
2, MgO, 3Al
2O
32SiO
2, Y
2O
3, ZrO
2And the colloidal sol that makes in the step (2) mixes and to obtain coating, wherein, and TiO
2, MgO, 3Al
2O
32SiO
2, Y
2O
3, ZrO
2With the weight ratio of colloidal sol be 1:1:1:0.03:0.5:3.5; Coating is applied to forms the organic inorganic hybridization layer on the nano-crystal soft-magnetic core that step (1) makes, through preferably obtaining organic inorganic hybridization layer nano-crystal soft-magnetic core magnetosensitive composite wire material behind the 20min baking-curing, baking temperature is 140 ℃.Wherein the thickness of organic inorganic hybridization layer is the 0.5-0.9 micron.
Embodiment two
1, preparation nano-crystal soft-magnetic core: get and get following core raw material by weight percentage: Si 6%, and Zr 7%, and Gd 3%, and Pr 0.2%, and B 8%, and Nb 6%, and Ni 3%, and Co 2%, and all the other are prepared burden for Fe, and wherein B adds with the mode of iron boron intermediate alloy; The core raw material is put into the melting of vaccum sensitive stove stove; Smelting temperature is 1580～1610 ℃, obtains the core foundry alloy, and the remelting tubular type crucible of putting into the vacuum induction quick quenching furnace then carries out remelting; Remelting temperature is that the top of 1550～1570 ℃ of remelting tubular type crucibles places 2～4mm place under the quick quenching furnace runner wheel rim; Foundry alloy places fusing in the tubular type crucible, under ar gas acting, overflows and the runner EDGE CONTACT of rotating from the crucible top behind the alloy molten, forms the alloy silk; Then the alloy silk is obtained the nano-crystal soft-magnetic core 300～350 ℃ of insulations after 1～1.5 hour.Wherein, the rotational line speed of fast pure stove runner is 21m/s, and diameter of alloy wire is 10 microns.The weight percentage that iron boron intermediate alloy contains B is 20%.
2, preparation colloidal sol: in the there-necked flask of belt stirrer, add tetraethoxysilane, γ-methacryloxypropyl trimethoxy silane and ethanol, its mol ratio is 3:2:2; Under vigorous stirring, splash into acetic acid, addition is 5g/100mL, and mixing speed is 800 rev/mins; Behind the room temperature reaction 3h, add methyl methacrylate and initator azodiisobutyronitrile, addition is respectively 10g/100mL and 5g/100mL, stirs 20min then under the room temperature and obtains colloidal sol.
3, preparation magnetosensitive composite filament: with granularity is the TiO of 100nm
2, MgO, 3Al
2O
32SiO
2, Y
2O
3, ZrO
2And the colloidal sol that makes in the step (2) mixes and to obtain coating, wherein, and TiO
2, MgO, 3Al
2O
32SiO
2, Y
2O
3, ZrO
2With the weight ratio of colloidal sol be 1:1:1:0.03:0.5:4; Coating is applied to forms the organic inorganic hybridization layer on the nano-crystal soft-magnetic core that step (1) makes, through preferably obtaining organic inorganic hybridization layer nano-crystal soft-magnetic core magnetosensitive composite wire material behind the 20min baking-curing, baking temperature is 140 ℃.Wherein the thickness of organic inorganic hybridization layer is the 0.5-0.9 micron.
Embodiment three
1, preparation nano-crystal soft-magnetic core: get and get following core raw material: Si5% by weight percentage, Zr 6%, and Gd 2%, and Pr 0.15%, and B 6%, and Nb 4%, and Ni 2%, and Co 1.5%, and all the other are prepared burden for Fe, and wherein B adds with the mode of iron boron intermediate alloy; The core raw material is put into the melting of vaccum sensitive stove stove; Smelting temperature is 1580～1610 ℃, obtains the core foundry alloy, and the remelting tubular type crucible of putting into the vacuum induction quick quenching furnace then carries out remelting; Remelting temperature is that the top of 1550～1570 ℃ of remelting tubular type crucibles places 2～4mm place under the quick quenching furnace runner wheel rim; Foundry alloy places fusing in the tubular type crucible, under ar gas acting, overflows and the runner EDGE CONTACT of rotating from the crucible top behind the alloy molten, forms the alloy silk; Then the alloy silk is obtained the nano-crystal soft-magnetic core 300～350 ℃ of insulations after 1～1.5 hour.Wherein, the rotational line speed of fast pure stove runner is 22m/s, and diameter of alloy wire is 9 microns.The weight percentage that iron boron intermediate alloy contains B is 20%.
2, preparation colloidal sol: in the there-necked flask of belt stirrer, add tetraethoxysilane, γ-methacryloxypropyl trimethoxy silane and ethanol, its mol ratio is 3:2:2; Under vigorous stirring, splash into acetic acid, addition is 5g/100mL, and mixing speed is 700 rev/mins; Behind the room temperature reaction 3h, add methyl methacrylate and initator azodiisobutyronitrile, addition is respectively 10g/100mL and 5g/100mL, stirs 20min then under the room temperature and obtains colloidal sol.
3, preparation magnetosensitive composite filament: with granularity is the TiO of 70nm
2, MgO, 3Al
2O
32SiO
2, Y
2O
3, ZrO
2And the colloidal sol that makes in the step (2) mixes and to obtain coating, wherein, and TiO
2, MgO, 3Al
2O
32SiO
2, Y
2O
3, ZrO
2With the weight ratio of colloidal sol be 1:1:1:0.03:0.5:3.8; Coating is applied to forms the organic inorganic hybridization layer on the nano-crystal soft-magnetic core that step (1) makes, through preferably obtaining organic inorganic hybridization layer nano-crystal soft-magnetic core magnetosensitive composite wire material behind the 20min baking-curing, baking temperature is 140 ℃.Wherein the thickness of organic inorganic hybridization layer is the 0.5-0.9 micron.
Embodiment four (proportioning components is instance in this case scope of design not)
1, get and get following core raw material by weight percentage: Si 3%, and Zr 3%, and Gd 0.9%, and Pr 0.05%, and B 3%, and Nb 2%, and Ni 0.8%, and Co 0.5%, and all the other are prepared burden for Fe, and wherein B adds with the mode of iron boron intermediate alloy; The core raw material is put into the melting of vaccum sensitive stove stove; Smelting temperature is 1580～1610 ℃, obtains the core foundry alloy, and the remelting tubular type crucible of putting into the vacuum induction quick quenching furnace then carries out remelting; Remelting temperature is that the top of 1550～1570 ℃ of remelting tubular type crucibles places 2～4mm place under the quick quenching furnace runner wheel rim; Foundry alloy places fusing in the tubular type crucible, under ar gas acting, overflows and the runner EDGE CONTACT of rotating from the crucible top behind the alloy molten, forms the alloy silk; Then the alloy silk is obtained the nano-crystal soft-magnetic core 300～350 ℃ of insulations after 1～1.5 hour.Wherein, the rotational line speed of fast pure stove runner is 21～24m/s, and diameter of alloy wire is 7～10 microns.The weight percentage that iron boron intermediate alloy contains B is 20%.
2, preparation colloidal sol: in the there-necked flask of belt stirrer, add tetraethoxysilane, γ-methacryloxypropyl trimethoxy silane and ethanol, its mol ratio is 3:2:2; Under vigorous stirring, splash into acetic acid, addition is 5g/100mL, and mixing speed is 600 rev/mins; Behind the room temperature reaction 3h, add methyl methacrylate and initator azodiisobutyronitrile, addition is respectively 10g/100mL and 5g/100mL, stirs 20min then under the room temperature and obtains colloidal sol.
3, preparation magnetosensitive composite filament: with granularity is the TiO of 50～100nm
2, MgO, 3Al
2O
32SiO
2, Y
2O
3, ZrO
2And the colloidal sol that makes in the step (2) mixes and to obtain coating, wherein, and TiO
2, MgO, 3Al
2O
32SiO
2, Y
2O
3, ZrO
2With the weight ratio of colloidal sol be 1:1:1:0.03:0.5:3; Coating is applied to forms the organic inorganic hybridization layer on the nano-crystal soft-magnetic core that step (1) makes, through preferably obtaining organic inorganic hybridization layer nano-crystal soft-magnetic core magnetosensitive composite wire material behind the 20min baking-curing, baking temperature is 140 ℃.Wherein the thickness of organic inorganic hybridization layer is 0.7 micron.
Embodiment five (proportioning components is instance in this case scope of design not)
1, preparation nano-crystal soft-magnetic core: get and get following core raw material by weight percentage: Si 7%, and Zr 8%, and Gd 5%, and Pr 0.4%, and B 9%, and Nb 8%, and Ni 4%, and Co 3%, and all the other are prepared burden for Fe, and wherein B adds with the mode of iron boron intermediate alloy; The core raw material is put into the melting of vaccum sensitive stove stove; Smelting temperature is 1580～1610 ℃, obtains the core foundry alloy, and the remelting tubular type crucible of putting into the vacuum induction quick quenching furnace then carries out remelting; Remelting temperature is that the top of 1550～1570 ℃ of remelting tubular type crucibles places 2～4mm place under the quick quenching furnace runner wheel rim; Foundry alloy places fusing in the tubular type crucible, under ar gas acting, overflows and the runner EDGE CONTACT of rotating from the crucible top behind the alloy molten, forms the alloy silk; Then the alloy silk is obtained the nano-crystal soft-magnetic core 300～350 ℃ of insulations after 1～1.5 hour.Wherein, the rotational line speed of fast pure stove runner is 21～24m/s, and diameter of alloy wire is 7～10 microns.The weight percentage that iron boron intermediate alloy contains B is 20%.
2, preparation colloidal sol: in the there-necked flask of belt stirrer, add tetraethoxysilane, γ-methacryloxypropyl trimethoxy silane and ethanol, its mol ratio is 3:2:2; Under vigorous stirring, splash into acetic acid, addition is 5g/100mL, and mixing speed is 600 rev/mins; Behind the room temperature reaction 3h, add methyl methacrylate and initator azodiisobutyronitrile, addition is respectively 10g/100mL and 5g/100mL, stirs 20min then under the room temperature and obtains colloidal sol.
3, preparation magnetosensitive composite filament: with granularity is the TiO of 50～100nm
2, MgO, 3Al
2O
32SiO
2, Y
2O
3, ZrO
2And the colloidal sol that makes in the step (2) mixes and to obtain coating, wherein, and TiO
2, MgO, 3Al
2O
32SiO
2, Y
2O
3, ZrO
2With the weight ratio of colloidal sol be 1:1:1:0.03:0.5:5; Coating is applied to forms the organic inorganic hybridization layer on the nano-crystal soft-magnetic core that step (1) makes, through preferably obtaining organic inorganic hybridization layer nano-crystal soft-magnetic core magnetosensitive composite wire material behind the 20min baking-curing, baking temperature is 140 ℃.Wherein the thickness of organic inorganic hybridization layer is the 0.5-0.9 micron.
Effect embodiment
Be illustrated in figure 1 as the organization chart of organic inorganic hybridization layer in the magnetosensitive composite wire material that embodiment two makes.
Can find out this dense structure and evenly by Fig. 1.
In conjunction with each performance of products parameter in the following table:
Each particular product performance parameters of table 1
By last Biao Kede, the product two, product three and product four response speeds that make through the present invention are high, and the maximum resistance variation rate is high, and magnetic field sensitivity is high, good insulation preformance.
The performance specification of product five and product six, the constituent element composition of the composition of soft magnetic core and coating can comprise that insulating properties exerts an influence to material maximum resistance variation rate height, magnetic field sensitivity not in the composition range of design.Reason is that the constituent element composition is not enough, and the effect of the constituent element of soft magnetic core alloying element and coating is not enough; The constituent element composition is too much, can in magnetic core alloy and coating, all form unnecessary compound, and, magnetic field sensitivity high to the maximum resistance variation rate has a negative impact.
Claims (8)
1. a magnetosensitive composite filament is characterized in that: the organic inorganic hybridization layer that comprises nano-crystal soft-magnetic core and core surface; Said nano-crystal soft-magnetic core by following component by weight percentage composition form: Si 4～6%, and Zr 5～7%, and Gd 1～3%, and Pr 0.1～0.2%, and B 4～8%, and Nb 3～6%, and Ni 1～3%, and Co 1～2%, and all the other are Fe; Said organic inorganic hybridization layer is by TiO
2, MgO, 3Al
2O
32SiO
2, Y
2O
3, ZrO
2Form by weight 1:1:1:0.03:0.5:3.5～4 with colloidal sol.
2. magnetosensitive composite filament according to claim 1; It is characterized in that: said colloidal sol prepares through following steps: in flask, add tetraethoxysilane, γ-methacryloxypropyl trimethoxy silane and ethanol; Its mol ratio is 3:2:2-2.2; Under agitation splash into acetic acid, addition is 5g/100mL, and mixing speed is 600-800 rev/min; Behind the room temperature reaction 3h, add methyl methacrylate and initator azodiisobutyronitrile, addition is respectively 10g/100mL and 5g/100mL, stirs 20min under the room temperature and obtains colloidal sol.
3. magnetosensitive composite filament according to claim 1 and 2 is characterized in that: the diameter of said nano-crystal soft-magnetic core is 7～10 microns, and the thickness of organic inorganic hybridization layer is the 0.5-0.9 micron.
4. the preparation method of a magnetosensitive composite filament is characterized in that: may further comprise the steps:
(1) preparation nano-crystal soft-magnetic core: get and get following core raw material by weight percentage: Si 4～6%, and Zr 5～7%, and Gd 1～3%, and Pr 0.1～0.2%; B 4～8%, and Nb 3～6%, and Ni 1～3%; Co 1～2%, and all the other are prepared burden for Fe, and wherein B adds with the mode of iron boron intermediate alloy; The core raw material is put into the melting of vaccum sensitive stove stove; Smelting temperature is 1580～1610 ℃; Obtain the core foundry alloy; The remelting tubular type crucible of putting into the vacuum induction quick quenching furnace then carries out remelting, and remelting temperature is top layout 2～4mm place under quick quenching furnace runner wheel rim of 1550～1570 ℃ of remelting tubular type crucibles, and foundry alloy places fusing in the remelting tubular type crucible; Under ar gas acting, overflow and the runner EDGE CONTACT of rotating from the crucible top behind the alloy molten, the formation diameter is 7～10 microns an alloy silk; Then the alloy silk is obtained the nano-crystal soft-magnetic core 300～350 ℃ of insulations after 1～1.5 hour;
(2) preparation colloidal sol: in flask, add tetraethoxysilane, γ-methacryloxypropyl trimethoxy silane and ethanol, its mol ratio is 3:2:2-2.2; Under agitation splash into acetic acid, addition is 4.5～5.5g/100mL, and mixing speed is 600-800 rev/min; Behind room temperature reaction 2.5～3.5 h, add methyl methacrylate and initator azodiisobutyronitrile, addition is respectively 9～11 g/100mL and 4.5～5.5g/100mL, stirs 15～25min under the room temperature then, obtains colloidal sol;
(3) preparation magnetosensitive composite filament: with granularity is the TiO of 50～100nm
2, MgO, 3Al
2O
32SiO
2, Y
2O
3, ZrO
2And the colloidal sol that makes in the step (2) mixes and to obtain coating, wherein, and TiO
2, MgO, 3Al
2O
32SiO
2, Y
2O
3, ZrO
2With the weight ratio of colloidal sol be 1:1:1:0.03:0.5:3.5～4; Coating is applied to forms the organic inorganic hybridization layer on the nano-crystal soft-magnetic core that step (1) makes, behind 15～25min baking-curing, obtain organic inorganic hybridization layer nano-crystal soft-magnetic core magnetosensitive composite wire material, baking temperature is 130～150 ℃.
5. the preparation method of magnetosensitive composite filament according to claim 4 is characterized in that: the rotational line speed of the fast pure stove runner in the said step (1) is 21～24m/s.
6. the preparation method of magnetosensitive composite filament according to claim 4 is characterized in that: the weight percentage that the middle iron boron intermediate alloy of said step (1) contains B is 20%.
7. according to the preparation method of claims 4 described magnetosensitive composite filaments, it is characterized in that: tetraethoxysilane, γ-methacryloxypropyl trimethoxy silane and ethanol mol ratio are 3:2:2 in the said step (2); The addition of said acetic acid is 5g/100mL, and the methyl methacrylate addition is 10g/100mL, and the azodiisobutyronitrile addition is 5g/100mL.
8. the preparation method of magnetosensitive composite filament according to claim 4 is characterized in that: flask is the there-necked flask that blender is housed in the said step (2).
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103021616A (en) * | 2012-12-04 | 2013-04-03 | 江苏亚威变压器有限公司 | Sealed amorphous alloy power transformer |
| CN103695813A (en) * | 2013-12-19 | 2014-04-02 | 南京信息工程大学 | Amorphous alloy material with high saturation magnetization and preparation method thereof |
| CN105671462A (en) * | 2016-04-15 | 2016-06-15 | 苏州思创源博电子科技有限公司 | Method for preparing zr-based amorphous alloy with coating |
| CN105695901A (en) * | 2016-04-13 | 2016-06-22 | 苏州思创源博电子科技有限公司 | Preparation method for titanium, zirconium and aluminum based metal glass |
| CN110767399A (en) * | 2019-10-25 | 2020-02-07 | 中磁电科有限公司 | Composite magnetic material and manufacturing method thereof |
| CN112366056A (en) * | 2020-10-23 | 2021-02-12 | 浙江工业大学 | High-frequency low-loss soft magnetic composite material and preparation method thereof |
| CN112366057A (en) * | 2020-10-23 | 2021-02-12 | 浙江工业大学 | Organic-inorganic hybrid nano titanate coated metal soft magnetic composite material and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103021616A (en) * | 2012-12-04 | 2013-04-03 | 江苏亚威变压器有限公司 | Sealed amorphous alloy power transformer |
| CN103695813A (en) * | 2013-12-19 | 2014-04-02 | 南京信息工程大学 | Amorphous alloy material with high saturation magnetization and preparation method thereof |
| CN103695813B (en) * | 2013-12-19 | 2015-08-19 | 南京信息工程大学 | A kind of high saturation and magnetic intensity amorphous alloy material and preparation method thereof |
| CN105695901A (en) * | 2016-04-13 | 2016-06-22 | 苏州思创源博电子科技有限公司 | Preparation method for titanium, zirconium and aluminum based metal glass |
| CN105671462A (en) * | 2016-04-15 | 2016-06-15 | 苏州思创源博电子科技有限公司 | Method for preparing zr-based amorphous alloy with coating |
| CN110767399A (en) * | 2019-10-25 | 2020-02-07 | 中磁电科有限公司 | Composite magnetic material and manufacturing method thereof |
| CN112366056A (en) * | 2020-10-23 | 2021-02-12 | 浙江工业大学 | High-frequency low-loss soft magnetic composite material and preparation method thereof |
| CN112366057A (en) * | 2020-10-23 | 2021-02-12 | 浙江工业大学 | Organic-inorganic hybrid nano titanate coated metal soft magnetic composite material and preparation method thereof |
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