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CN110273189B - Continuous silicon steel long fiber electrical magnetic material and preparation method thereof - Google Patents

Continuous silicon steel long fiber electrical magnetic material and preparation method thereof Download PDF

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Publication number
CN110273189B
CN110273189B CN201910540795.8A CN201910540795A CN110273189B CN 110273189 B CN110273189 B CN 110273189B CN 201910540795 A CN201910540795 A CN 201910540795A CN 110273189 B CN110273189 B CN 110273189B
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silicon steel
temperature
mixed
gel
iron
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CN110273189A (en
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娄建勇
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Wuxi Shenwanghe Electronic Technology Co ltd
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Wuxi Shenwanghe Electronic Technology Co ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/02Heat treatment
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0015Electro-spinning characterised by the initial state of the material
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/44Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/48Oxides or hydroxides of chromium, molybdenum or tungsten; Chromates; Dichromates; Molybdates; Tungstates
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Power Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Fibers (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

In order to solve the defects of the prior art, the invention provides a preparation method of a continuous silicon steel long fiber electrical magnetic material, which comprises the following steps: s1, mixing an organic solvent, manganese hydroxide and deionized water, wherein the molar ratio of the organic solvent to the manganese oxide is 1:0.5-20, and the pH value is kept at 5.6-8.5; s2, adding a metal iron salt into the mixed solvent, wherein the mass ratio of the metal iron salt to the mixed solvent is as follows: 1: 5-20; s3, dehydrating the mixed solution at the temperature of 60-80 ℃ in vacuum to a gel state to obtain iron gel; s4, adding silicon tetrachloride at the temperature of 15-20 ℃ of the iron gel, and stirring until a preset ratio of silicon element to iron element is achieved; s5, spinning the mixed gel by adopting a high-voltage electrostatic spinning method; s6, obtaining the continuous silicon steel magnetic long fiber after heat treatment operation. The invention finally spins the continuous silicon steel long fiber with the length-diameter ratio of more than 4000:1, but not short fiber.

Description

Continuous silicon steel long fiber electrical magnetic material and preparation method thereof
Technical Field
The invention belongs to the technical field of magnetic materials, and particularly relates to a continuous silicon steel long fiber electrical magnetic material.
Background
Soft magnetic materials used in low-frequency magnetic fields are required to have high magnetic permeability, low coercive force, and other properties. The magnetic conductivity is high, and when the number of turns of the coil is fixed, high magnetic induction intensity can be generated by passing small excitation current, so that high output voltage is obtained. The coercive force of the material is low, the area of a magnetic hysteresis loop is small, and the iron loss is also small. Therefore, the iron core made of the material with high magnetic permeability and low coercive force is beneficial to reducing the size of a product and improving the sensitivity.
The low-frequency soft magnetic material is mainly silicon steel sheets. Adding 0.8-4.5% of silicon into iron containing a small amount of carbon to obtain the silicon steel. Compared with pure iron for electricians, the silicon steel has higher resistivity and low iron loss, and the magnetic aging is basically eliminated. At present, silicon steel sheets are widely used for iron cores of products such as motors, transformers, relays, mutual inductors, switches and the like. Although the saturation magnetic induction of the silicon steel sheet is high, the silicon steel sheet contains silicon element, so that the heat conductivity of the silicon steel sheet is reduced, the hardness is improved, and the brittleness is increased. For this reason, the magnetic properties of the high-performance cold-rolled silicon steel sheet are sensitive to the influence of stress, and stress is generated during punching, stacking, or winding of the iron core, thereby deteriorating the magnetic properties. This drawback greatly limits the application of silicon steel sheets to equipment of various specific configurations and dimensions.
Focusing on the fact that the production and application of magnetic fiber materials are mature day by day, the production of continuous silicon steel long fiber electrical materials for low-frequency magnetic fields becomes possible. The continuous silicon steel long fiber can be regarded as one-dimensional embodiment of a silicon steel sheet, and is required to be in a filiform shape, the width is in a nanometer or micrometer level, and the length-diameter ratio is higher. The continuous silicon steel long fiber electrical material changes a silicon steel sheet from a three-dimensional structure to a one-dimensional structure of silicon steel fibers, and can further improve the magnetic conductivity and greatly reduce the coercive force under the nanometer and micrometer scales.
At present, most of the related patents of the magnetic fibers relate to the preparation method of the short magnetic fibers, and the related aspects of the silicon steel fibers are rarely related. The patent "Mn-Zn ferrite fiber and its preparation method" (see patent publication No. CN 101104556A) specifically describes the specific preparation method of Mn-Zn ferrite fiber. The patent mainly discloses that the prepared ferrite fiber is mainly used in the field of high-frequency magnetic fields. Meanwhile, the fiber is obtained by filament picking, filament drawing or filament throwing, and the diameter of the obtained fiber is 0.2-100 mu m and does not reach the nanometer size. The patent of a shell-core structure magnetic fibrous silicon dioxide nanoparticle and a preparation method and application thereof (see patent publication No. CN 107362775A) concretely describes a shell-core structure magnetic fibrous silicon dioxide nanoparticle and a preparation method thereof. The outer layer is fibrous silicon dioxide, and the inner core is hollow ferroferric oxide. The patent results in short fibers or nanoparticles with short aspect ratios. And meanwhile, the nano particles are finally obtained only by alternately cleaning distilled water and absolute ethyl alcohol and then drying, and the efficiency is low. The invention relates to a far infrared flat ECDP magnetic fiber and a preparation method thereof (see patent publication No. CN 102011210A), and discloses a flat magnetic fiber with antibacterial, anti-ultraviolet and far infrared health care functions. The patent adopts a melt spinning method, a non-sol-gel method and a high-voltage electrostatic spinning method are combined, and the whole process is more complex. In the patent of a magnetic fiber and a manufacturing method thereof (see patent publication No. CN 101649503A), a double-screw extruder is adopted for extrusion and granulation to obtain a magnetic fiber core layer material. And spinning the skin layer material and the core layer material in proportion by using a skin-core spinning machine to form a wound filament. Different from the above patents, the invention mainly provides a preparation method of silicon steel fibers, which combines a sol-gel method and a high-voltage electrostatic spinning method, and adopts special process flow and proportion to finally obtain the continuous magnetic long fibers.
Disclosure of Invention
The invention provides a preparation method of a continuous silicon steel long fiber electrical magnetic material aiming at the problems in the prior art, which comprises the following steps:
s1, mixing an organic solvent, manganese hydroxide and deionized water, wherein the molar ratio of the organic solvent to the manganese oxide is 1:0.5-20, adding the deionized water to keep the pH value of the solution at 5.6-8.5, and uniformly stirring to obtain a mixed solvent;
s2, adding a metal iron salt into the mixed solvent, wherein the mass ratio of the metal iron salt to the mixed solvent is as follows: 1:5-20, and uniformly stirring to obtain a mixed solution;
s3, dehydrating the mixed solution at the temperature of 60-80 ℃ in vacuum to a gel state to obtain iron gel;
s4, dropwise adding silicon tetrachloride at the temperature of 15-20 ℃ of the iron gel, and stirring until a preset ratio of silicon element to iron element is achieved to obtain mixed gel;
s5, spinning the mixed gel by adopting a high-voltage electrostatic spinning method, and collecting the obtained long fibrous cellulose filaments;
s6, placing the long fibrous long fiber obtained in the step S5 in a heating device, and performing heat treatment operation to obtain the continuous silicon steel magnetic long fiber.
Further, in step S1, the organic solvent is: one or both of polyvinyl alcohol and citric acid.
Further, in step S2, the metallic iron salt is: one or both of ferric nitrate and ferric chloride.
Further, the molar mass of the silicon element is A, and the molar mass of the iron element is B; step S4, the predetermined ratio of si to fe is: a: b is 1-10: 90-99.
Further, the molar mass A of the silicon element satisfies the following condition: a/(a + B) ═ C; the value range of C is as follows: 0.01-0.1.
Further, in step S5, the control parameters of the high voltage electrostatic spinning are as follows: the flow rate is 0.5-1.2ml/h, the voltage is 15-25kV, and the distance between the two electrodes is 12-16 cm.
Further, the heat treatment operation of step S6 includes:
(1) filling nitrogen-hydrogen mixed gas into a heating device with long fibrous cellulose filaments, gradually raising the temperature of the heating device, and finally stabilizing at the temperature of 730-;
(2) controlling the temperature of the heating device to be 380-420 ℃, and calcining for 4-5 hours in an air environment;
(3) filling hydrogen, gradually raising the temperature of the heating device, and finally stabilizing at the temperature of 730-.
Further, in the nitrogen-hydrogen mixed gas in the step (1), the ratio of nitrogen: hydrogen is 1: 5-20;
further, the temperature of the heating device is gradually increased in the step (1) and the step (3), and the temperature rising speed is 5-30 ℃/min.
Further, magnesium oxide or chromium oxide coating materials are adopted to perform spray coating on the continuous silicon steel magnetic long fibers obtained in the step S6.
In addition, the invention also provides a continuous silicon steel long fiber electrical magnetic material which is prepared by the preparation method of the continuous silicon steel long fiber electrical magnetic material.
The invention has at least one of the following advantages:
the invention provides a preparation method of a continuous silicon steel long fiber electrical material. It has at least the following advantages.
1. The invention combines two technologies of a sol-gel method and a high-voltage electrostatic spinning method to obtain a proper spinnable precursor according to different proportions. By controlling the parameters of a proper high-voltage electrostatic spinning machine and combining a drum type collector, continuous silicon steel long fibers with the length-diameter ratio of more than 4000:1 are finally spun instead of short fibers. The manufacturing process of the silicon steel long magnetic fiber provided by the invention is completely different from the cold rolling or hot rolling process of the existing silicon steel sheet.
2. From the aspect of magnetization characteristics, the one-dimensional continuous silicon steel long fiber under the nanoscale obtained by the invention is closer to the scale level of the iron simple substance, so that the obtained magnetic permeability is higher, and the coercive force is reduced. The electrical magnetic material of continuous silicon steel long fiber utilizes the advantages of nanotechnology, greatly improves the magnetic property of the material from the source, and leads the equipment to obtain larger magnetic field intensity under the same volume. Therefore, the size of the electrical and electronic equipment can be reduced by one step, and the consumption of resources is saved.
3. The continuous silicon steel long fiber obtained by the invention has the advantage of one-dimensional structure, and is beneficial to constructing advanced product equipment structure, so that the continuous silicon steel long fiber is really developed towards flattening and microminiaturization. Through a special process, the fibers with one-dimensional structures can be woven into a two-dimensional planar membrane. This advantage is particularly advantageous for the development of a flat device. Through the process transformation, the magnetic core can be even directly constructed in the electrical chip, the new chip manufacturing process is promoted, and new industry and business opportunities are inoculated. Through the 3D printing technology, a three-dimensional structure can be directly obtained, the processes of riveting, welding and the like in the traditional process manufacturing are omitted, and the production and delivery speed of the product is greatly improved. And 4.0 industry of flexible manufacturing and personalized customization, and basic technical innovation support is provided.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A continuous silicon steel long fiber electrical magnetic material is prepared by the following method:
s1, mixing an organic solvent, manganese hydroxide and deionized water, wherein the molar ratio of the organic solvent to the manganese oxide is 1:10, adding the deionized water to keep the pH value of the solution at 7.2, and uniformly stirring to obtain a mixed solvent; step S1 the organic solvent is: polyvinyl alcohol.
S2, adding a metal iron salt into the mixed solvent, wherein the mass ratio of the metal iron salt to the mixed solvent is as follows: 1:10, and uniformly stirring to obtain a mixed solution; the metallic iron salt in the step S2 is: ferric nitrate.
S3, dehydrating the mixed solution at 70 ℃ in vacuum to a gel state to obtain iron gel;
s4, adding silicon tetrachloride dropwise at the iron gel temperature of 18 ℃, and stirring until a preset ratio of silicon element to iron element is achieved to obtain mixed gel; the molar mass of the silicon element is A, and the molar mass of the iron element is B; step S4, the predetermined ratio of si to fe is: a: and B is 2: 98.
S5, spinning the mixed gel by adopting a high-voltage electrostatic spinning method, and collecting the obtained long fibrous cellulose filaments;
the control parameters of the high-voltage electrostatic spinning in the step S5 are as follows: the flow rate was 0.8ml/h, the voltage was 20kV, and the distance between the electrodes was 14 cm.
S6, placing the long fibrous long fiber obtained in the step S5 in a heating device, and performing heat treatment operation to obtain the continuous silicon steel magnetic long fiber.
Example 2
A continuous silicon steel long fiber electrical magnetic material is prepared by the following method:
s1, mixing an organic solvent, manganese hydroxide and deionized water, wherein the molar ratio of the organic solvent to the manganese oxide is 1:20, adding the deionized water to keep the pH value of the solution at 5.6, and uniformly stirring to obtain a mixed solvent; step S1 the organic solvent is: and (4) citric acid.
S2, adding a metal iron salt into the mixed solvent, wherein the mass ratio of the metal iron salt to the mixed solvent is as follows: 1:20, and uniformly stirring to obtain a mixed solution; the metallic iron salt in the step S2 is: ferric chloride.
S3, dehydrating the mixed solution at the temperature of 80 ℃ in vacuum to a gel state to obtain iron gel;
s4, adding silicon tetrachloride dropwise at the temperature of 20 ℃ of the iron gel, and stirring until a preset ratio of silicon element to iron element is achieved to obtain mixed gel; the molar mass of the silicon element is A, and the molar mass of the iron element is B; step S4, the predetermined ratio of si to fe is: a: and B is 10: 99.
S5, spinning the mixed gel by adopting a high-voltage electrostatic spinning method, and collecting the obtained long fibrous cellulose filaments;
the control parameters of the high-voltage electrostatic spinning in the step S5 are as follows: the flow rate was 1.2ml/h, the voltage was 25kV, and the distance between the electrodes was 16 cm.
S6, placing the long fibrous long fiber obtained in the step S5 in a heating device, and performing heat treatment operation to obtain the continuous silicon steel magnetic long fiber.
Example 3
A continuous silicon steel long fiber electrical magnetic material is prepared by the following method:
s1, mixing an organic solvent, manganese hydroxide and deionized water, wherein the molar ratio of the organic solvent to the manganese oxide is 1:0.5, adding the deionized water to keep the pH value of the solution at 8.5, and uniformly stirring to obtain a mixed solvent; step S1 the organic solvent is: polyvinyl alcohol and citric acid are mixed in equal proportion.
S2, adding a metal iron salt into the mixed solvent, wherein the mass ratio of the metal iron salt to the mixed solvent is as follows: 1:5, and uniformly stirring to obtain a mixed solution; the metallic iron salt in the step S2 is: mixing ferric nitrate and ferric chloride in equal proportion.
S3, dehydrating the mixed solution at the temperature of 60 ℃ in vacuum to a gel state to obtain iron gel;
s4, adding silicon tetrachloride dropwise at the temperature of 15 ℃ of the iron gel, and stirring until a preset ratio of silicon element to iron element is achieved to obtain mixed gel; the molar mass of the silicon element is A, and the molar mass of the iron element is B; step S4, the predetermined ratio of si to fe is: a: and B is 1: 90.
S5, spinning the mixed gel by adopting a high-voltage electrostatic spinning method, and collecting the obtained long fibrous cellulose filaments;
the control parameters of the high-voltage electrostatic spinning in the step S5 are as follows: the flow rate was 0.5ml/h, the voltage was 15kV, and the distance between the two electrodes was 12 cm.
S6, placing the long fibrous long fiber obtained in the step S5 in a heating device, and performing heat treatment operation to obtain the continuous silicon steel magnetic long fiber.
Example 4
A continuous silicon steel long fiber electrical magnetic material is prepared by the following method:
s1, mixing an organic solvent, manganese hydroxide and deionized water, wherein the molar ratio of the organic solvent to the manganese oxide is 1:3, adding the deionized water to keep the pH value of the solution at 6.8, and uniformly stirring to obtain a mixed solvent; step S1 the organic solvent is: polyvinyl alcohol and citric acid are mixed in equal proportion.
S2, adding a metal iron salt into the mixed solvent, wherein the mass ratio of the metal iron salt to the mixed solvent is as follows: 1:12, and uniformly stirring to obtain a mixed solution; the metallic iron salt in the step S2 is: mixing ferric nitrate and ferric chloride in equal proportion.
S3, dehydrating the mixed solution at 70 ℃ in vacuum to a gel state to obtain iron gel;
s4, adding silicon tetrachloride dropwise at the iron gel temperature of 18 ℃, and stirring until a preset ratio of silicon element to iron element is achieved to obtain mixed gel; the molar mass of the silicon element is A, and the molar mass of the iron element is B; step S4, the predetermined ratio of si to fe is: a: and B is 5: 98.
S5, spinning the mixed gel by adopting a high-voltage electrostatic spinning method, and collecting the obtained long fibrous cellulose filaments;
the control parameters of the high-voltage electrostatic spinning in the step S5 are as follows: the flow rate was 0.8ml/h, the voltage was 18kV, and the distance between the electrodes was 13 cm.
S6, placing the long fibrous long fiber obtained in the step S5 in a heating device, and performing heat treatment operation to obtain the continuous silicon steel magnetic long fiber.
Example 5
Based on any one of embodiments 1 to 4, the molar mass A of the silicon element satisfies the following condition: a/(a + B) ═ C; the value range of C is as follows: 0.01-0.1. Compared with the fiber length of the final product under the condition of the rest silicon element proportion, the fiber length of the final product can be obviously improved by controlling the molar mass of the silicon element within the range, and the fiber length is increased by 15-20 percent compared with the fiber length of the final product.
Example 6
In any of embodiments 1-4, the heat treatment of step S6 includes:
(1) filling nitrogen-hydrogen mixed gas into a heating device with long fibrous cellulose filaments, gradually raising the temperature of the heating device, and finally stabilizing at 770 ℃ of 730 and preferably 750 ℃, and heating for 3-4 hours, preferably 3.5 hours;
(2) controlling the temperature of the heating device to be 380-420 ℃, preferably 400 ℃, and calcining for 4-5 hours, preferably 4.5 hours in an air environment;
(3) filling hydrogen and gradually raising the temperature of the heating device, and finally stabilizing at 770 ℃ of 730 and preferably 750 ℃, and heating for 4-6 hours, preferably 5 hours.
In the nitrogen-hydrogen mixed gas in the step (1), the ratio of nitrogen: hydrogen is 1:5-20, preferably 1: 10; and (3) gradually raising the temperature of the heating device in the steps (1) and (3), wherein the temperature raising speed is 5-30 ℃/min, and preferably 15 ℃/min. The operation can remove the redundant oxygen element in the silicon steel long fiber.
Based on 1 embodiment of the invention, magnesium oxide or chromium oxide coating materials are adopted to perform spray coating on the continuous silicon steel magnetic long fiber obtained in the step S6, so that a good anti-corrosion effect can be achieved.
The invention has at least one of the following advantages:
the invention provides a preparation method of a continuous silicon steel long fiber electrical material. It has at least the following advantages.
1. The invention combines two technologies of a sol-gel method and a high-voltage electrostatic spinning method to obtain a proper spinnable precursor according to different proportions. By controlling the parameters of a proper high-voltage electrostatic spinning machine and combining a drum type collector, continuous silicon steel long fibers with the length-diameter ratio of more than 4000:1 are finally spun instead of short fibers. The manufacturing process of the silicon steel long magnetic fiber provided by the invention is completely different from the cold rolling or hot rolling process of the existing silicon steel sheet.
2. From the aspect of magnetization characteristics, the one-dimensional continuous silicon steel long fiber under the nanoscale obtained by the invention is closer to the scale level of the iron simple substance, so that the obtained magnetic permeability is higher, and the coercive force is reduced. The electrical magnetic material of continuous silicon steel long fiber utilizes the advantages of nanotechnology, greatly improves the magnetic property of the material from the source, and leads the equipment to obtain larger magnetic field intensity under the same volume. Therefore, the size of the electrical and electronic equipment can be reduced by one step, and the consumption of resources is saved.
3. The continuous silicon steel long fiber obtained by the invention has the advantage of one-dimensional structure, and is beneficial to constructing advanced product equipment structure, so that the continuous silicon steel long fiber is really developed towards flattening and microminiaturization. Through a special process, the fibers with one-dimensional structures can be woven into a two-dimensional planar membrane. This advantage is particularly advantageous for the development of a flat device. Through the process transformation, the magnetic core can be even directly constructed in the electrical chip, the new chip manufacturing process is promoted, and new industry and business opportunities are inoculated. Through the 3D printing technology, a three-dimensional structure can be directly obtained, the processes of riveting, welding and the like in the traditional process manufacturing are omitted, and the production and delivery speed of the product is greatly improved. And 4.0 industry of flexible manufacturing and personalized customization, and basic technical innovation support is provided.
It is to be noted and understood that various modifications and improvements can be made to the invention described in detail above without departing from the spirit and scope of the invention as claimed. Accordingly, the scope of the claimed subject matter is not limited by any of the specific exemplary teachings provided.

Claims (2)

1. A method for preparing a continuous silicon steel long fiber electrical magnetic material is characterized by comprising the following steps:
s1, mixing an organic solvent, manganese hydroxide and deionized water, wherein the molar ratio of the organic solvent to the manganese hydroxide is 1:0.5-20, adding the deionized water to keep the pH value of the solution at 5.6-8.5, and uniformly stirring to obtain a mixed solvent;
s2, adding a metal iron salt into the mixed solvent, wherein the mass ratio of the metal iron salt to the mixed solvent is as follows: 1:5-20, and uniformly stirring to obtain a mixed solution;
s3, dehydrating the mixed solution at the temperature of 60-80 ℃ in vacuum to a gel state to obtain iron gel;
s4, dropwise adding silicon tetrachloride at the temperature of 15-20 ℃ of the iron gel, and stirring until a predetermined ratio of silicon element to iron element is achieved to obtain mixed gel;
s5, spinning the mixed gel by adopting a high-voltage electrostatic spinning method, and collecting the obtained long fibrous cellulose filaments;
s6, placing the long filamentous vegetarian fiber obtained in the step S5 into a heating device, and performing heat treatment to obtain continuous silicon steel magnetic long fibers;
step S1 the organic solvent is: one or two of polyvinyl alcohol or citric acid are mixed;
the metallic iron salt in the step S2 is: mixing one or both of ferric nitrate and ferric chloride;
the molar mass of the silicon element is A, and the molar mass of the iron element is B; step S4, the predetermined ratio of si to fe is: a: b is 1-10: 90-99;
the molar mass A of the silicon element meets the following conditions: a/(a + B) ═ C; the value range of C is as follows: 0.01-0.1;
the control parameters of the high-voltage electrostatic spinning in the step S5 are as follows: the flow rate is 0.5-1.2ml/h, the voltage is 15-25kV, and the distance between the two electrodes is 12-16 cm;
step S6 the heat treatment operation includes:
(1) filling nitrogen-hydrogen mixed gas into a heating device with long fibrous cellulose filaments, gradually raising the temperature of the heating device, and finally stabilizing at the temperature of 730-;
(2) controlling the temperature of the heating device to be 380-420 ℃, and calcining for 4-5 hours in an air environment;
(3) filling hydrogen, gradually raising the temperature of the heating device, and finally stabilizing at the temperature of 730-;
in the nitrogen-hydrogen mixed gas in the step (1), the ratio of nitrogen: hydrogen is 1: 5-20;
gradually raising the temperature of the heating device in the steps (1) and (3), wherein the temperature raising speed is 5-30 ℃/min;
and (4) adopting a magnesium oxide or chromium oxide coating material to perform spray coating on the continuous silicon steel magnetic long fiber obtained in the step S6.
2. A continuous long silicon steel fiber electrical magnetic material, which is prepared by the method of claim 1.
CN201910540795.8A 2019-06-21 2019-06-21 Continuous silicon steel long fiber electrical magnetic material and preparation method thereof Expired - Fee Related CN110273189B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1759964A (en) * 2005-10-27 2006-04-19 江苏大学 Method for preparing superfine metal fibers through method of organogel-thermal reduction process
CN101914821A (en) * 2010-05-14 2010-12-15 江苏大学 Ni-Zn ferrite/SiO2 composite nanofiber and its preparation method
CN103498285A (en) * 2013-10-18 2014-01-08 苏州大学 Method using electrospinning technique to prepare ordered nanometer magnetic composite material
CN105386158A (en) * 2015-11-03 2016-03-09 浙江大学 Preparation method for porous hollow bismuth ferrite nano fibers

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* Cited by examiner, † Cited by third party
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JP2015513007A (en) * 2012-02-16 2015-04-30 コーネル・ユニバーシティーCornell University Ordered porous nanofibers, production method and application thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1759964A (en) * 2005-10-27 2006-04-19 江苏大学 Method for preparing superfine metal fibers through method of organogel-thermal reduction process
CN101914821A (en) * 2010-05-14 2010-12-15 江苏大学 Ni-Zn ferrite/SiO2 composite nanofiber and its preparation method
CN103498285A (en) * 2013-10-18 2014-01-08 苏州大学 Method using electrospinning technique to prepare ordered nanometer magnetic composite material
CN105386158A (en) * 2015-11-03 2016-03-09 浙江大学 Preparation method for porous hollow bismuth ferrite nano fibers

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