WO2019029145A1 - Silicone resin - Google Patents

Silicone resin Download PDF

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Publication number
WO2019029145A1
WO2019029145A1 PCT/CN2018/076090 CN2018076090W WO2019029145A1 WO 2019029145 A1 WO2019029145 A1 WO 2019029145A1 CN 2018076090 W CN2018076090 W CN 2018076090W WO 2019029145 A1 WO2019029145 A1 WO 2019029145A1
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WO
WIPO (PCT)
Prior art keywords
silicone resin
parts
soft magnetic
heat treatment
magnetic powder
Prior art date
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PCT/CN2018/076090
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French (fr)
Chinese (zh)
Inventor
郭雄志
张云帆
肖强
徐方胜
周金
刘欢
何恺
Original Assignee
深圳市铂科新材料股份有限公司
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Publication of WO2019029145A1 publication Critical patent/WO2019029145A1/en

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
    • H01F1/22—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
    • H01F1/24—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
    • H01F1/26—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated by macromolecular organic substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/49—Phosphorus-containing compounds
    • C08K5/5399—Phosphorus bound to nitrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C08K5/548—Silicon-containing compounds containing sulfur

Definitions

  • the invention belongs to the field of chemistry, and in particular relates to a silicone resin.
  • a soft magnetic material is a kind of magnetic material having low coercive force and high magnetic permeability. Soft magnetic materials are easy to magnetize and easy to demagnetize, and are widely used in electrical equipment and electronic equipment. In recent years, power electronic equipment has been moving toward high frequency, miniaturization, and high efficiency, and higher requirements have been placed on the performance of magnetic materials.
  • Common soft magnetic materials include metal soft magnetic materials and ferrite soft magnetic materials.
  • the metal soft magnetic material includes a strip represented by a silicon steel sheet and a metal soft magnetic powder core. Due to the low electrical resistivity of materials, strips such as silicon steel sheets have gradually failed to keep up with the high frequency development of power electronic equipment. When used above 30 kHz, the loss of silicon steel sheet is greatly increased, which generates huge heat and threatens the normal operation of electronic equipment.
  • the metal soft magnetic powder core is a soft magnetic material prepared by a series of processes such as insulating coating, press forming and high temperature heat treatment of the metal soft magnetic powder. Since the surface of the powder is coated with an insulating material, the eddy current between the particles is hindered, and the eddy current loss is effectively reduced. Compared with ferrite soft magnetic materials, the metal soft magnetic powder core has a high saturation magnetic flux density, which is more advantageous for miniaturization of components. At the same time, the metal soft magnetic powder core has the characteristics of distributed air gap, which can avoid ferrite materials. Noise problems due to open air gaps and other unstable factors.
  • the metal soft magnetic powder core Compared with ferrite, the metal soft magnetic powder core has a high saturation magnetic flux density, which is advantageous for miniaturization. In addition, due to its uniform distribution of air gap, it can avoid the noise problem caused by the open air gap, and can be greatly reduced. Small copper loss due to magnetic flux cut copper wire.
  • the loss of a metal soft magnetic powder core usually includes hysteresis loss and eddy current loss.
  • the hysteresis loss is proportional to the frequency
  • the eddy current loss is proportional to the square of the frequency. In order to ensure normal use under high frequency conditions, it is necessary to effectively reduce hysteresis loss and eddy current loss.
  • Press forming introduces stress into the core, resulting in increased hysteresis loss; therefore, high temperature heat treatment is required to release the internal stress of the core.
  • Heat treatment at 600 ° C or even 700 ° C or higher is usually required.
  • Eddy current losses can be controlled by insulation cladding. By coating the surface of the metal powder with an insulating layer, the eddy current between the powders can be suppressed, and the eddy current is confined inside the powder, which can greatly reduce the eddy current loss of the magnetic core.
  • the high temperature heat treatment tends to damage the insulating layer, the insulation effect is deteriorated, the eddy current loss is rapidly increased, and the total loss is also increased.
  • Chinese Patent No. CN101089108A discloses "an inorganic insulating binder for a metal soft magnetic powder core and a preparation method thereof", characterized in that the inorganic insulating binder is mixed with SiO 2 , Al 2 O 3 , ZrO 2 , mica powder and water. In this method, the organic matter is not used, and the aging problem caused by the heat generation of the powder core during use can be avoided, and the mechanical strength of the powder core can be improved.
  • the inorganic insulating binder adheres to the surface of the powder only by physical adsorption, and in the process of press molding or the like, the uneven distribution of the insulating agent on the surface of the powder is easily generated, and the contact resistance between the surfaces of the powder is lowered, and the insulating effect is affected. influences.
  • Chinese patent CN104376949A discloses "an organic-inorganic composite insulating coated Fe-Si-Al magnetic powder core" characterized in that a mixed solution of mica powder, epoxy resin, absolute ethanol and tetraethyl orthosilicate is used as an insulating agent.
  • the Fe-Si-Al magnetic powder core produced has a minimum loss of about 275 mW/cm 3 .
  • the heat treatment temperature of the invention is between 500 and 700 ° C. Although it is higher than the heat resistance of the conventional organic material, it is not conducive to the complete release of the internal stress of the core.
  • Chinese Patent No. CN104759619A discloses "a method for preparing metal magnetic powder insulation treatment and preparing metal magnetic powder core", which is characterized in that surface passivation of metal powder is carried out by using phosphoric acid and boric acid, and then diffusion of B and P elements is carried out in a vacuum atmosphere. Increase the electrical resistivity of the metal powder itself and reduce the eddy current loss.
  • the diffusion reaction needs to be carried out in a high-temperature vacuum environment, and the temperature is kept for 24 hours, which is disadvantageous in that it takes a long time and a high cost.
  • Chinese patent CN105798284A discloses a "inorganic binder for metal soft magnetic powder core, metal soft magnetic powder core", which is characterized in that the provided binder satisfies all inorganic, heat treatment does not decompose, low temperature solidification, anti-aging, and conforms to ROSH. Standard.
  • the invention also needs to use phosphoric acid to achieve surface insulation and passivation of the powder, the phosphate formed on the surface is brittle, and is prone to cracking during press forming; at the same time, phosphate decomposes above 600 ° C, resulting in coating defect. , insulation performance is reduced.
  • the present invention proposes a silicone resin.
  • a silicone resin consisting of the following components by weight: 30-50 parts of MQ silicone resin, 30-60 parts of precipitated silica, and 2-6 parts of propyl propyl methyldimethoxysilane. 5 to 10 parts with HMPA.
  • the silicone resin is composed of the following components by weight: 30 to 35 parts of MQ silicone resin, 50 to 60 parts of precipitated silica, 2 to 6 parts of propyl propyl methyldimethoxysilane, and HMPA 5 ⁇ 10 copies.
  • the ratio of the M chain and the Q link in the MQ silicone resin is 0.4 to 0.5.
  • the MQ silicone resin has a hydrogen content of 0.05 to 0.1 mmol/g, and the MQ silicone resin has a viscosity of 10 to 50 mPa ⁇ s.
  • the preparation method of the silicone resin is to put MQ silicone resin, precipitated white carbon black, propyl propyl methyl dimethoxy silane and HMPA into a kneading machine, knead for 2 hours, and then put into a vacuum internal mixer to heat up the heat. Refining, heating to 130 ⁇ 160 ° C, vacuum heat treatment 2 ⁇ 3h, after temperature measurement, secondary heating to 160 ⁇ 190 ° C, vacuum heat treatment 3.5 ⁇ 4h; discharge, placed 12 ⁇ 24h to obtain silicone resin.
  • the invention also provides a metal soft magnetic powder core which is resistant to high temperature heat treatment, and is composed of a metal soft magnetic powder and a silicone resin, and the mass ratio of the metal soft magnetic powder to the silicone resin is 0.5 to 5:100.
  • the metal soft magnetic powder is at least one of iron powder, iron silicon powder, iron silicon aluminum powder, iron nickel powder, and iron nickel molybdenum powder, and the powder has a particle diameter of 25 ⁇ m to 250 ⁇ m.
  • the silicone resin is a white powder having a powder particle size of less than 50 ⁇ m.
  • the invention also provides a preparation method of a metal soft magnetic powder core resistant to high temperature heat treatment, comprising the following steps:
  • a) preparing a metal soft magnetic powder using a gas atomization method, a water atomization method or a mechanical crushing method to prepare a metal soft magnetic powder having a powder particle size of 25 ⁇ m to 250 ⁇ m;
  • Insulation coating treatment mixing the silicone resin, the metal soft magnetic powder and the releasing agent in a mass ratio of 0.5 to 5:100:0.2 to 1 to obtain a mixed powder;
  • step c) press molding press-molding the mixed powder obtained in step b) to obtain a molded body
  • step d) primary heat treatment: the shaped body obtained in step c) is kept at 200 ⁇ 500 ° C for 1 ⁇ 2h;
  • the molded body treated by the step d) is kept at 700 to 900 ° C for 1 to 2 hours to obtain a metal soft magnetic powder core which is resistant to high temperature heat treatment.
  • the release agent is a stearate such as zinc stearate.
  • the insulating coating treatment is carried out by using a V-shaped mixer, a kneading machine, a ball mill, a sand mill or a kneader.
  • step c) the press molding is performed by press molding using a hydraulic press, and the pressing pressure is 10 to 20 T/cm 2 .
  • step d) one heat treatment is performed in an air atmosphere.
  • the secondary heat treatment is performed in a non-oxidizing gas, a reducing gas or a vacuum atmosphere; for example, an inert gas such as Ar, N 2 or He, a reducing gas such as H 2 or a vacuum.
  • a non-oxidizing gas for example, an inert gas such as Ar, N 2 or He, a reducing gas such as H 2 or a vacuum.
  • the invention Compared with the prior art, the invention has the following beneficial effects: the invention effectively reduces the hysteresis loss without increasing the eddy current loss, thereby reducing the loss of the magnetic core.
  • the silicone resin of the invention has high decomposition temperature and can improve the heat resistance of the insulating powder; the insulating operation is simple, no additional passivating agent or binder is added, the cost is reduced, the man-hour is saved, and the film formed on the surface of the metal powder after one heat treatment is formed.
  • the insulation layer with good uniformity and high heat resistance can make the metal soft magnetic powder core can be heat treated at 900 °C, which greatly reduces the The loss of the metal soft magnetic powder core in high frequency application; in addition, the silicone resin of the invention has a bonding effect, can effectively improve the mechanical strength of the metal soft magnetic powder core, and reduce the yield rate due to product defects in the production process.
  • silicone resin 30 parts of MQ silicone resin having a ratio of M chain link and Q chain link of 0.4, a hydrogen content of 0.05 mmol/g, a viscosity of 10 mPa ⁇ s, and 30 parts of precipitated white carbon black, ⁇ 2 parts of propylmethyldimethoxysilane, 5 parts of HMPA, put into a kneader, kneaded for 2 hours, then put into a vacuum internal mixer to heat and knead, heat up to 130 ° C, vacuum heat treatment for 2 h, after temperature measurement, twice The temperature was raised to 160 ° C, vacuum heat treatment for 3.5 h; the material was discharged, and the silicone resin was placed for 12 hours; and the silicone resin powder having an average particle diameter of 25 ⁇ m was screened;
  • Insulation coating treatment a silicone resin powder having an average particle diameter of 25 ⁇ m, a -150 mesh FeSiAl metal soft magnetic powder, and zinc stearate were mixed at a mass ratio of 0.5:100:0.2, and uniformly stirred using a V-shaped mixer to obtain a mixture. powder;
  • Press molding The mixed powder obtained by the insulating coating treatment is press-formed using a hydraulic press at a pressing pressure of 10 T/cm 2 to obtain a molded body;
  • One heat treatment the molded body obtained by press molding is kept at 500 ° C for 1 hour in an air atmosphere;
  • Secondary heat treatment The molded body subjected to primary heat treatment was kept in an argon atmosphere at 900 ° C for 1 hour to obtain a metal soft magnetic powder core resistant to high temperature heat treatment.
  • Preparation of soft magnetic powder of metal Preparation of -150 mesh FeSiAl metal soft magnetic powder by water atomization method
  • silicone resin 35 parts of MQ silicone resin having a ratio of M chain link and Q chain link of 0.45, a hydrogen content of 0.08 mmol/g, a viscosity of 30 mPa.s, and 40 parts of precipitated white carbon black, ⁇ 3 parts of propylmethyldimethoxysilane, 6 parts of HMPA, put into a kneader, kneaded for 2 hours, then put into a vacuum mixer to heat and knead, heat up to 140 ° C, vacuum heat treatment for 2.5 h, after temperature measurement, two The temperature was raised to 170 ° C, vacuum heat treatment for 3.6 h; the material was discharged, and the silicone resin was placed for 18 hours; and the silicone resin powder having an average particle diameter of 20 ⁇ m was screened;
  • Insulation coating treatment a silicone resin having an average particle diameter of 20 ⁇ m, a -150 mesh FeSiAl metal soft magnetic powder and calcium stearate were mixed at a mass ratio of 2:100:0.5, and uniformly stirred using a crucible machine to obtain a mixed powder. ;
  • Press molding the mixed powder obtained by the insulating coating treatment is press-formed using a hydraulic press, and the pressing pressure is 15 T/cm 2 to obtain a molded body;
  • One heat treatment the molded body obtained by press molding is kept at 400 ° C for 1.5 hours in an air atmosphere;
  • Secondary heat treatment The molded body subjected to the primary heat treatment was kept at 900 ° C for 1.5 hours under nitrogen to obtain a metal soft magnetic powder core which was heat-resistant to a high temperature.
  • Preparation of soft magnetic powder of metal Preparation of -150 mesh FeSiAl metal soft magnetic powder by mechanical crushing method
  • silicone resin 40 parts of MQ silicone resin having a ratio of M chain link and Q chain link of 0.5, a hydrogen content of 0.1 mmol/g, a viscosity of 50 mPa ⁇ s, and 50 parts of precipitated white carbon black, ⁇ 4 parts of propylmethyldimethoxysilane and 7 parts of HMPA, put into a kneader, kneaded for 2 hours, and then put into a vacuum internal mixer to heat and knead, heat up to 150 ° C, vacuum heat treatment for 3 h, after temperature measurement, twice The temperature was raised to 180 ° C, vacuum heat treatment for 4 h; the material was discharged, and the silicone resin was placed for 24 hours; and the silicone resin powder having an average particle diameter of 15 ⁇ m was screened;
  • Insulation coating treatment a silicone resin powder silicone resin having an average particle diameter of 15 ⁇ m, a -150 mesh FeSiAl metal soft magnetic powder and calcium stearate were mixed at a mass ratio of 5:100:1, and uniformly stirred using a ball mill to obtain a mixture. powder;
  • Press molding the mixed powder obtained by the insulating coating treatment is press-formed using a hydraulic press, and the pressing pressure is 20 T/cm 2 to obtain a molded body;
  • One heat treatment the molded body obtained by press molding is kept at 300 ° C for 2 hours in an air atmosphere;
  • Secondary heat treatment The molded body subjected to the primary heat treatment was kept at a temperature of 900 ° C for 1 hour in a helium gas to obtain a metal soft magnetic powder core resistant to high temperature heat treatment.
  • Preparation of soft magnetic powder of metal Preparation of -150 mesh FeSiAl metal soft magnetic powder by gas atomization;
  • silicone resin 4 parts of MQ silicone resin having a ratio of M chain link and Q chain link of 0.4, a hydrogen content of 0.1 mmol/g, a viscosity of 10 mPa ⁇ s, and 60 parts of precipitated white carbon black, ⁇ 5 parts of propylmethyldimethoxysilane, 8 parts of HMPA, put into a kneader, kneaded for 2 hours, then put into a vacuum internal mixer to heat and knead, heat up to 160 ° C, vacuum heat treatment for 2 h, after temperature measurement, twice The temperature was raised to 190 ° C, vacuum heat treatment for 4 h; discharged, placed for 12 h to obtain a silicone resin; and a silicone resin powder having an average particle diameter of 15 ⁇ m was screened;
  • Insulation coating treatment a silicone resin having an average particle diameter of 15 ⁇ m, a -150 mesh FeSiAl metal soft magnetic powder and zinc stearate are mixed at a mass ratio of 2:100:0.5, and uniformly stirred using a sand mill to obtain a mixed powder. ;
  • Press molding the mixed powder obtained by the insulating coating treatment is press-formed using a hydraulic press, and the pressing pressure is 20 T/cm 2 to obtain a molded body;
  • One heat treatment the molded body obtained by press molding is kept at 200 ° C for 2 hours in an air atmosphere;
  • Secondary heat treatment The molded body subjected to the primary heat treatment was kept in a hydrogen atmosphere at 900 ° C for 2 hours to obtain a metal soft magnetic powder core resistant to high temperature heat treatment.
  • Preparation of soft magnetic powder of metal Preparation of -300 mesh FeSiAl metal soft magnetic powder by gas atomization method
  • silicone resin 50 parts of MQ silicone resin having a ratio of M chain link and Q chain link of 0.45, a hydrogen content of 0.08 mmol/g, a viscosity of 50 mPa ⁇ s, and 30 parts of precipitated white carbon black, ⁇ 6 parts of propylmethyldimethoxysilane, 9 parts of HMPA, put into a kneader, kneaded for 2 hours, and then put into a vacuum internal mixer to heat and knead, heat up to 150 ° C, vacuum heat treatment for 2 h, after temperature measurement, twice The temperature was raised to 190 ° C, vacuum heat treatment for 3.5 h; discharged, placed for 24 h to obtain a silicone resin; and a silicone resin powder having an average particle diameter of 15 ⁇ m was screened;
  • Insulation coating treatment a silicone resin having an average particle diameter of 15 ⁇ m, a -300 mesh FeSiAl metal soft magnetic powder and zinc stearate are mixed at a mass ratio of 2:100:0.5, and uniformly stirred using a kneader to obtain a mixed powder;
  • Press molding the mixed powder obtained by the insulating coating treatment is press-formed using a hydraulic press, and the pressing pressure is 20 T/cm 2 to obtain a molded body;
  • One heat treatment the molded body obtained by press molding is kept at 500 ° C for 2 hours in an air atmosphere;
  • Secondary heat treatment The molded body subjected to primary heat treatment was kept in a vacuum at 900 ° C for 2 hours to obtain a metal soft magnetic powder core resistant to high temperature heat treatment.
  • Preparation of metal soft magnetic powder Preparation of -100 mesh FeSiAl metal soft magnetic powder by gas atomization method
  • silicone resin 50 parts of MQ silicone resin with a ratio of M chain link and Q chain link of 0.5, a hydrogen content of 0.05 mmol/g, a viscosity of 30 mPa ⁇ s, and 30 parts of precipitated white carbon black, ⁇ 2 parts of propylmethyldimethoxysilane, 10 parts of HMPA, put into a kneader, kneaded for 2 hours, then put into a vacuum mixer to heat and heat the mixture, heat up to 150 ° C, vacuum heat treatment for 3 h, after temperature measurement, twice The temperature was raised to 190 ° C, vacuum heat treatment for 4 h; the material was discharged, and the silicone resin was placed for 24 hours; and the silicone resin powder having an average particle diameter of 15 ⁇ m was screened;
  • Insulation coating treatment a silicone resin having an average particle diameter of 15 ⁇ m, a -100 mesh FeSiAl metal soft magnetic powder and zinc stearate are mixed at a mass ratio of 2:100:0.5, and uniformly stirred using a kneader to obtain a mixed powder;
  • Press molding the mixed powder obtained by the insulating coating treatment is press-formed using a hydraulic press, and the pressing pressure is 20 T/cm 2 to obtain a molded body;
  • One heat treatment the molded body obtained by press molding is kept at 500 ° C for 2 hours in an air atmosphere;
  • Secondary heat treatment The molded body subjected to primary heat treatment was kept in a vacuum at 900 ° C for 2 hours to obtain a metal soft magnetic powder core resistant to high temperature heat treatment.
  • Preparation of soft magnetic powder of metal Preparation of -150 mesh FeSi metal soft magnetic powder by gas atomization;
  • silicone resin 50 parts of MQ silicone resin with a ratio of M chain link and Q chain link of 0.5, a hydrogen content of 0.05 mmol/g, a viscosity of 30 mPa ⁇ s, and 30 parts of precipitated white carbon black, ⁇ 2 parts of propylmethyldimethoxysilane, 10 parts of HMPA, put into a kneader, kneaded for 2 hours, then put into a vacuum mixer to heat and heat the mixture, heat up to 150 ° C, vacuum heat treatment for 3 h, after temperature measurement, twice The temperature was raised to 190 ° C, vacuum heat treatment for 4 h; the material was discharged, and the silicone resin was placed for 24 hours; and the silicone resin powder having an average particle diameter of 15 ⁇ m was screened;
  • Insulation coating treatment a silicone resin having an average particle diameter of 15 ⁇ m, a -150 mesh FeSi metal soft magnetic powder and zinc stearate are mixed at a mass ratio of 2:100:0.5, and uniformly stirred using a kneader to obtain a mixed powder;
  • Press molding the mixed powder obtained by the insulating coating treatment is press-formed using a hydraulic press, and the pressing pressure is 20 T/cm 2 to obtain a molded body;
  • One heat treatment the molded body obtained by press molding is kept at 500 ° C for 2 hours in an air atmosphere;
  • Secondary heat treatment The molded body subjected to primary heat treatment was kept in a vacuum at 900 ° C for 2 hours to obtain a metal soft magnetic powder core resistant to high temperature heat treatment.
  • Preparation of soft magnetic powder of metal Preparation of -100 mesh FeNi metal soft magnetic powder by gas atomization;
  • silicone resin 50 parts of MQ silicone resin with a ratio of M chain link and Q chain link of 0.5, a hydrogen content of 0.05 mmol/g, a viscosity of 30 mPa ⁇ s, and 30 parts of precipitated white carbon black, ⁇ 2 parts of propylmethyldimethoxysilane, 10 parts of HMPA, put into a kneader, kneaded for 2 hours, then put into a vacuum mixer to heat and heat the mixture, heat up to 150 ° C, vacuum heat treatment for 3 h, after temperature measurement, twice The temperature was raised to 190 ° C, vacuum heat treatment for 4 h; the material was discharged, and the silicone resin was placed for 24 hours; and the silicone resin powder having an average particle diameter of 15 ⁇ m was screened;
  • Insulation coating treatment a silicone resin having an average particle diameter of 15 ⁇ m, a -300 mesh FeNi metal soft magnetic powder and zinc stearate are mixed at a mass ratio of 2:100:0.5, and uniformly stirred using a kneader to obtain a mixed powder;
  • Press molding The mixed powder obtained by the insulating coating treatment is press-formed using a hydraulic press at a pressing pressure of 20 T/cm 2 to obtain a molded body;
  • One heat treatment the molded body obtained by press molding is kept at 500 ° C for 2 hours in an air atmosphere;
  • Secondary heat treatment The molded body subjected to primary heat treatment was kept in a vacuum at 900 ° C for 2 hours to obtain a metal soft magnetic powder core resistant to high temperature heat treatment.
  • Preparation of metal soft magnetic powder Preparation of -300 mesh FeNiMo metal soft magnetic powder by gas atomization method;
  • silicone resin 50 parts of MQ silicone resin with a ratio of M chain link and Q chain link of 0.5, a hydrogen content of 0.05 mmol/g, a viscosity of 30 mPa ⁇ s, and 30 parts of precipitated white carbon black, ⁇ 2 parts of propylmethyldimethoxysilane, 10 parts of HMPA, put into a kneader, kneaded for 2 hours, then put into a vacuum mixer to heat and heat the mixture, heat up to 150 ° C, vacuum heat treatment for 3 h, after temperature measurement, twice The temperature was raised to 190 ° C, vacuum heat treatment for 4 h; the material was discharged, and the silicone resin was placed for 24 hours; and the silicone resin powder having an average particle diameter of 15 ⁇ m was screened;
  • Insulation coating treatment a silicone resin having an average particle diameter of 15 ⁇ m, a -300 mesh FeNiMo metal soft magnetic powder and zinc stearate are mixed at a mass ratio of 2:100:0.5, and uniformly stirred using a kneader to obtain a mixed powder;
  • Press molding the mixed powder obtained by the insulating coating treatment is press-formed using a hydraulic press, and the pressing pressure is 20 T/cm 2 to obtain a molded body;
  • One heat treatment the molded body obtained by press molding is kept at 500 ° C for 2 hours in an air atmosphere;
  • Secondary heat treatment The molded body subjected to primary heat treatment was kept in a vacuum at 900 ° C for 2 hours to obtain a metal soft magnetic powder core resistant to high temperature heat treatment.

Abstract

Provided in the present invention is a silicone resin, comprising the following components in parts by weight: 30-50 parts of MQ silicone resin, 30-60 parts of precipitated white carbon black, 2-6 parts of mercaptopropylmethdimethoxysilane and 5-10 parts of HMPA. Compared to existing technology, the present invention has the following beneficial effects: the silicone resin disclosed in the present invention has a high decomposition temperature and may improve the heat resistance of insulating powder, so that a metal soft magnetic powder core may be subjected to heat treatment at 900°C, and the loss of the metal soft magnetic powder core under high-frequency application is greatly reduced. After high-temperature heat treatment, the film formed on the surface of the metal powder has good compactness, is uniform and produces good insulation effects. In addition, the silicone resin according to the present invention has a bonding effect, may effectively improve the mechanical strength of the metal soft magnetic powder core and reduce yields brought about by product defects in a production process.

Description

一种硅树脂Silicone resin 技术领域Technical field
本发明属于化学领域，具体涉及一种硅树脂。The invention belongs to the field of chemistry, and in particular relates to a silicone resin.
背景技术Background technique
软磁材料作为磁性材料的一种，具有低矫顽力和高磁导率。软磁材料易于磁化，也易于退磁，广泛用于电工设备和电子设备中。近年来，电力电子设备一直朝着高频化、小型化、高效率的方向发展，对磁性材料的性能也提出了更高的要求。A soft magnetic material is a kind of magnetic material having low coercive force and high magnetic permeability. Soft magnetic materials are easy to magnetize and easy to demagnetize, and are widely used in electrical equipment and electronic equipment. In recent years, power electronic equipment has been moving toward high frequency, miniaturization, and high efficiency, and higher requirements have been placed on the performance of magnetic materials.
常见的软磁材料包括，金属软磁材料和铁氧体软磁材料。Common soft magnetic materials include metal soft magnetic materials and ferrite soft magnetic materials.
金属软磁材料包括以硅钢片为代表的带材和金属软磁粉芯。由于材料电阻率较低，硅钢片等带材已逐渐跟不上电力电子设备的高频化发展。在高于30kHz的条件下使用，由于硅钢片损耗大幅增长，会产生巨大的热量，威胁电子设备的正常运行。The metal soft magnetic material includes a strip represented by a silicon steel sheet and a metal soft magnetic powder core. Due to the low electrical resistivity of materials, strips such as silicon steel sheets have gradually failed to keep up with the high frequency development of power electronic equipment. When used above 30 kHz, the loss of silicon steel sheet is greatly increased, which generates huge heat and threatens the normal operation of electronic equipment.
金属软磁粉芯是金属软磁粉末经过绝缘包覆、压制成型、高温热处理等一系列工艺制作而成的软磁材料。由于粉末表面包覆了绝缘物质，阻碍粉末了颗粒间的涡流，有效地降低了涡流损耗。与铁氧体软磁材料相比，金属软磁粉芯的饱和磁通密度高，更有利于实现元件的小型化；同时，金属软磁粉芯具有分布式气隙的特点，可以避免铁氧体材料因开气隙产生的噪音问题及其他不稳定因素。The metal soft magnetic powder core is a soft magnetic material prepared by a series of processes such as insulating coating, press forming and high temperature heat treatment of the metal soft magnetic powder. Since the surface of the powder is coated with an insulating material, the eddy current between the particles is hindered, and the eddy current loss is effectively reduced. Compared with ferrite soft magnetic materials, the metal soft magnetic powder core has a high saturation magnetic flux density, which is more advantageous for miniaturization of components. At the same time, the metal soft magnetic powder core has the characteristics of distributed air gap, which can avoid ferrite materials. Noise problems due to open air gaps and other unstable factors.
与铁氧体相比，金属软磁粉芯的饱和磁通密度高，有利于实现小型化；另外由于其具有均匀分布气隙的特点，可以避免因开气隙产生的噪音问题，同时可以大幅减小因漏磁切割铜线产生的铜损。Compared with ferrite, the metal soft magnetic powder core has a high saturation magnetic flux density, which is advantageous for miniaturization. In addition, due to its uniform distribution of air gap, it can avoid the noise problem caused by the open air gap, and can be greatly reduced. Small copper loss due to magnetic flux cut copper wire.
为了更好的适应高频化、小型化和高效率的要求，需要提高金属 软磁粉芯的密度并降低磁芯损耗。In order to better meet the requirements of high frequency, miniaturization and high efficiency, it is necessary to increase the density of the metal soft magnetic powder core and reduce the core loss.
金属软磁粉芯的损耗通常包括磁滞损耗和涡流损耗。磁滞损耗与频率成正比，涡流损耗与频率的平方成正比。为了保证在高频条件下正常使用，需要有效的降低磁滞损耗和涡流损耗。The loss of a metal soft magnetic powder core usually includes hysteresis loss and eddy current loss. The hysteresis loss is proportional to the frequency, and the eddy current loss is proportional to the square of the frequency. In order to ensure normal use under high frequency conditions, it is necessary to effectively reduce hysteresis loss and eddy current loss.
压制成型会向磁芯内部引入应力，导致磁滞损耗增大；所以需要进行高温热处理，释放磁芯内部应力。通常需要进行600℃甚至700℃以上的热处理。涡流损耗可以由绝缘包覆控制。通过对金属粉末表面包覆绝缘层，可以抑制粉末之间的涡流，将涡流限制在粉末内部，这样可以大大降低磁芯的涡流损耗。但高温热处理容易破坏绝缘层，使绝缘效果变差，涡流损耗急速增大，总损耗也增大。Press forming introduces stress into the core, resulting in increased hysteresis loss; therefore, high temperature heat treatment is required to release the internal stress of the core. Heat treatment at 600 ° C or even 700 ° C or higher is usually required. Eddy current losses can be controlled by insulation cladding. By coating the surface of the metal powder with an insulating layer, the eddy current between the powders can be suppressed, and the eddy current is confined inside the powder, which can greatly reduce the eddy current loss of the magnetic core. However, the high temperature heat treatment tends to damage the insulating layer, the insulation effect is deteriorated, the eddy current loss is rapidly increased, and the total loss is also increased.
所以，需要在确保粉末绝缘性的前提下，实现高温热处理。Therefore, it is necessary to realize high-temperature heat treatment under the premise of ensuring powder insulation.
中国专利CN101089108A公开了“一种金属软磁粉芯用无机绝缘粘结剂及其制备方法”，其特征在于无机绝缘粘结剂由SiO 2、Al 2O 3、ZrO 2、云母粉及水混合而成，该方法不使用有机物，可以避免粉芯在使用过程中因发热导致的老化问题，同时可以提高粉芯的机械强度。但是该无机绝缘粘结剂仅以物理吸附的方式附着于粉末表面，在压制成型等过程中，容易产生绝缘剂在粉末表面分布不均匀的现象，降低粉末表面之间的接触电阻，绝缘效果受到影响。 Chinese Patent No. CN101089108A discloses "an inorganic insulating binder for a metal soft magnetic powder core and a preparation method thereof", characterized in that the inorganic insulating binder is mixed with SiO 2 , Al 2 O 3 , ZrO 2 , mica powder and water. In this method, the organic matter is not used, and the aging problem caused by the heat generation of the powder core during use can be avoided, and the mechanical strength of the powder core can be improved. However, the inorganic insulating binder adheres to the surface of the powder only by physical adsorption, and in the process of press molding or the like, the uneven distribution of the insulating agent on the surface of the powder is easily generated, and the contact resistance between the surfaces of the powder is lowered, and the insulating effect is affected. influences.
中国专利CN104376949A公开了“一种有机-无机复合绝缘包覆Fe-Si-Al磁粉芯”，其特征在于使用云母粉末、环氧树脂、无水乙醇、正硅酸乙酯的混合溶液作为绝缘剂，制作的Fe-Si-Al磁粉芯损耗最低在275mW/cm 3左右。该发明的热处理温度在500～700℃之间，虽然 比传统的有机物耐热温度高，但还是不利于磁芯内部应力的完全释放。 Chinese patent CN104376949A discloses "an organic-inorganic composite insulating coated Fe-Si-Al magnetic powder core" characterized in that a mixed solution of mica powder, epoxy resin, absolute ethanol and tetraethyl orthosilicate is used as an insulating agent. The Fe-Si-Al magnetic powder core produced has a minimum loss of about 275 mW/cm 3 . The heat treatment temperature of the invention is between 500 and 700 ° C. Although it is higher than the heat resistance of the conventional organic material, it is not conducive to the complete release of the internal stress of the core.
中国专利CN104759619A公开了“一种金属磁粉绝缘处理及制备金属磁粉芯的制备方法”，其特征在于采用磷酸和硼酸对金属粉末进行表面钝化，然后在真空气氛中进行B、P元素的扩散，提高金属粉末本身的电阻率，降低涡流损耗。但是该扩散反应需要在高温真空环境下进行，且保温24小时，存在耗时长、成本较高的不足。Chinese Patent No. CN104759619A discloses "a method for preparing metal magnetic powder insulation treatment and preparing metal magnetic powder core", which is characterized in that surface passivation of metal powder is carried out by using phosphoric acid and boric acid, and then diffusion of B and P elements is carried out in a vacuum atmosphere. Increase the electrical resistivity of the metal powder itself and reduce the eddy current loss. However, the diffusion reaction needs to be carried out in a high-temperature vacuum environment, and the temperature is kept for 24 hours, which is disadvantageous in that it takes a long time and a high cost.
中国专利CN105798284A公开了一种“用于金属软磁粉芯的无机粘结剂、金属软磁粉芯”，其特征在于提供的粘结剂满足全无机、热处理不分解、低温固化、抗老化、符合ROSH的标准。但是该发明还需采用磷酸对粉体实现表面的绝缘和钝化，表面生成的磷酸盐具有脆性，压制成型过程中容易发生破裂；同时磷酸盐在600℃以上会发生分解，导致包覆层缺损，绝缘性能降低。Chinese patent CN105798284A discloses a "inorganic binder for metal soft magnetic powder core, metal soft magnetic powder core", which is characterized in that the provided binder satisfies all inorganic, heat treatment does not decompose, low temperature solidification, anti-aging, and conforms to ROSH. Standard. However, the invention also needs to use phosphoric acid to achieve surface insulation and passivation of the powder, the phosphate formed on the surface is brittle, and is prone to cracking during press forming; at the same time, phosphate decomposes above 600 ° C, resulting in coating defect. , insulation performance is reduced.
技术问题technical problem
为解决现有技术中金属软磁粉芯不耐高温热处理、损耗较大的问题，本发明提出一种硅树脂。In order to solve the problem that the metal soft magnetic powder core is not resistant to high temperature heat treatment and has large loss in the prior art, the present invention proposes a silicone resin.
技术解决方案Technical solution
本发明技术方案如下：一种硅树脂，由如下重量份组分组成：MQ硅树脂30～50份、沉淀白炭黑30～60份、巯丙基甲基二甲氧基硅烷2～6份和HMPA 5～10份。The technical scheme of the present invention is as follows: a silicone resin consisting of the following components by weight: 30-50 parts of MQ silicone resin, 30-60 parts of precipitated silica, and 2-6 parts of propyl propyl methyldimethoxysilane. 5 to 10 parts with HMPA.
进一步的，所述硅树脂是由如下重量份组分组成：MQ硅树脂30～35份、沉淀白炭黑50～60份、巯丙基甲基二甲氧基硅烷2～6份和HMPA 5～10份。Further, the silicone resin is composed of the following components by weight: 30 to 35 parts of MQ silicone resin, 50 to 60 parts of precipitated silica, 2 to 6 parts of propyl propyl methyldimethoxysilane, and HMPA 5 ~10 copies.
进一步的，所述的MQ硅树脂中M链节和Q链节的比为0.4～ 0.5。Further, the ratio of the M chain and the Q link in the MQ silicone resin is 0.4 to 0.5.
进一步的，所述的MQ硅树脂的含氢量为0.05～0.1mmol/g，所述的MQ硅树脂的粘度为10～50mPa.s。Further, the MQ silicone resin has a hydrogen content of 0.05 to 0.1 mmol/g, and the MQ silicone resin has a viscosity of 10 to 50 mPa·s.
进一步的，所述硅树脂的制备方法，是将MQ硅树脂、沉淀白炭黑、巯丙基甲基二甲氧基硅烷和HMPA投入捏合机，捏合2小时后投入真空密炼机中升温密炼，升温到130～160℃，抽真空热处理2～3h，测温后，二次升温到160～190℃，抽真空热处理3.5～4h；出料，放置12～24h得硅树脂。Further, the preparation method of the silicone resin is to put MQ silicone resin, precipitated white carbon black, propyl propyl methyl dimethoxy silane and HMPA into a kneading machine, knead for 2 hours, and then put into a vacuum internal mixer to heat up the heat. Refining, heating to 130 ~ 160 ° C, vacuum heat treatment 2 ~ 3h, after temperature measurement, secondary heating to 160 ~ 190 ° C, vacuum heat treatment 3.5 ~ 4h; discharge, placed 12 ~ 24h to obtain silicone resin.
本发明还提供一种耐高温热处理的金属软磁粉芯，由金属软磁粉末和硅树脂组成，所述金属软磁粉末和硅树脂的质量比为0.5～5：100。The invention also provides a metal soft magnetic powder core which is resistant to high temperature heat treatment, and is composed of a metal soft magnetic powder and a silicone resin, and the mass ratio of the metal soft magnetic powder to the silicone resin is 0.5 to 5:100.
进一步的，所述的金属软磁粉末为铁粉、铁硅粉、铁硅铝粉、铁镍粉、铁镍钼粉中的至少一种，粉末粒径为25μm～250μm。Further, the metal soft magnetic powder is at least one of iron powder, iron silicon powder, iron silicon aluminum powder, iron nickel powder, and iron nickel molybdenum powder, and the powder has a particle diameter of 25 μm to 250 μm.
进一步的，所述硅树脂为白色粉末，粉末粒径小于50μm。Further, the silicone resin is a white powder having a powder particle size of less than 50 μm.
本发明还提供一种耐高温热处理的金属软磁粉芯的制备方法，包括如下步骤：The invention also provides a preparation method of a metal soft magnetic powder core resistant to high temperature heat treatment, comprising the following steps:
a)制备金属软磁粉末：采用气雾化法、水雾化法或机械破碎法制备得到粉末粒径为25μm～250μm的金属软磁粉末；a) preparing a metal soft magnetic powder: using a gas atomization method, a water atomization method or a mechanical crushing method to prepare a metal soft magnetic powder having a powder particle size of 25 μm to 250 μm;
b)绝缘包覆处理：将硅树脂、金属软磁粉末和脱模剂按质量比为0.5～5：100：0.2～1混合搅拌均匀，得混合粉末；b) Insulation coating treatment: mixing the silicone resin, the metal soft magnetic powder and the releasing agent in a mass ratio of 0.5 to 5:100:0.2 to 1 to obtain a mixed powder;
c)压制成型：将步骤b)得到的混合粉末压制成型，得成型体；c) press molding: press-molding the mixed powder obtained in step b) to obtain a molded body;
d)一次热处理：将步骤c)得到的成型体在200～500℃的条件下保温1～2h；d) primary heat treatment: the shaped body obtained in step c) is kept at 200 ~ 500 ° C for 1 ~ 2h;
e)二次热处理：将经过步骤d)处理的成型体在700～900℃的条件下保温1～2h，得耐高温热处理的金属软磁粉芯。e) Secondary heat treatment: The molded body treated by the step d) is kept at 700 to 900 ° C for 1 to 2 hours to obtain a metal soft magnetic powder core which is resistant to high temperature heat treatment.
进一步的，所述脱模剂为硬脂酸锌等硬脂酸盐。Further, the release agent is a stearate such as zinc stearate.
进一步的，步骤b)绝缘包覆处理中采用V形搅拌机、擂溃机、球磨机、砂磨机或混捏机进行搅拌。Further, in step b), the insulating coating treatment is carried out by using a V-shaped mixer, a kneading machine, a ball mill, a sand mill or a kneader.
进一步的，步骤c)压制成型中使用液压机压制成型，压制压力为10～20T/cm 2。 Further, in step c), the press molding is performed by press molding using a hydraulic press, and the pressing pressure is 10 to 20 T/cm 2 .
进一步的，步骤d)一次热处理在空气氛围中进行。Further, step d) one heat treatment is performed in an air atmosphere.
进一步的，步骤e)二次热处理在非氧化性气体、还原气体或真空氛围中进行；例如Ar、N 2、He等惰性气体，H 2等还原气体或者真空。 Further, the step e) the secondary heat treatment is performed in a non-oxidizing gas, a reducing gas or a vacuum atmosphere; for example, an inert gas such as Ar, N 2 or He, a reducing gas such as H 2 or a vacuum.
有益效果Beneficial effect
与现有技术相比，本发明具有如下有益效果：本发明在不增大涡流损耗的前提下，有效降低了磁滞损耗，从而降低了磁芯的损耗。本发明的硅树脂分解温度高，可以提高绝缘粉末耐热性能；绝缘操作简便，无需添加其他钝化剂或者粘结剂，降低成本、节省工时；经过一次热处理后，在金属粉末表面形成的膜，没有裂纹，致密性好、均匀一致，可以起到很好的绝缘效果；均匀性好、耐热性高的绝缘层，使得金属软磁粉芯可以在900℃的条件下进行热处理，大大降低了金属软磁粉芯在高频应用下的损耗；另外，本发明的硅树脂具有粘接效果，可以有效提高金属软磁粉芯的机械强度，降低生产过程中因产品缺损导致的良品率。Compared with the prior art, the invention has the following beneficial effects: the invention effectively reduces the hysteresis loss without increasing the eddy current loss, thereby reducing the loss of the magnetic core. The silicone resin of the invention has high decomposition temperature and can improve the heat resistance of the insulating powder; the insulating operation is simple, no additional passivating agent or binder is added, the cost is reduced, the man-hour is saved, and the film formed on the surface of the metal powder after one heat treatment is formed. No crack, good compactness and uniformity, can play a good insulation effect; the insulation layer with good uniformity and high heat resistance can make the metal soft magnetic powder core can be heat treated at 900 °C, which greatly reduces the The loss of the metal soft magnetic powder core in high frequency application; in addition, the silicone resin of the invention has a bonding effect, can effectively improve the mechanical strength of the metal soft magnetic powder core, and reduce the yield rate due to product defects in the production process.
本发明的最佳实施方式BEST MODE FOR CARRYING OUT THE INVENTION
为进一步阐释本发明为实现预定目的而采取的技术手段及功效，以下结合具体实施例，对本发明的具体实施方式、结构、特征及功效，详细说明如下；The specific embodiments, structures, features and functions of the present invention are described in detail below with reference to the specific embodiments in the accompanying drawings.
实施例1Example 1
制备金属软磁粉末：采用气雾化法-150目的FeSiAl金属软磁粉末；Preparation of soft magnetic powder of metal: using a gas atomization method - 150 mesh FeSiAl metal soft magnetic powder;
制备硅树脂：按重量份秤取M链节和Q链节的比为0.4、含氢量为0.05mmol/g、粘度为10mPa.s的MQ硅树脂30份，沉淀白炭黑30份，巯丙基甲基二甲氧基硅烷2份，HMPA 5份，投入捏合机，捏合2小时后投入真空密炼机中升温密炼，升温到130℃，抽真空热处理2h，测温后，二次升温到160℃，抽真空热处理3.5h；出料，放置12h得硅树脂；并筛选出平均粒径为25μm的硅树脂粉末；Preparation of silicone resin: 30 parts of MQ silicone resin having a ratio of M chain link and Q chain link of 0.4, a hydrogen content of 0.05 mmol/g, a viscosity of 10 mPa·s, and 30 parts of precipitated white carbon black, 巯2 parts of propylmethyldimethoxysilane, 5 parts of HMPA, put into a kneader, kneaded for 2 hours, then put into a vacuum internal mixer to heat and knead, heat up to 130 ° C, vacuum heat treatment for 2 h, after temperature measurement, twice The temperature was raised to 160 ° C, vacuum heat treatment for 3.5 h; the material was discharged, and the silicone resin was placed for 12 hours; and the silicone resin powder having an average particle diameter of 25 μm was screened;
绝缘包覆处理：将平均粒径为25μm的硅树脂粉末、-150目的FeSiAl金属软磁粉末和硬脂酸锌按质量比为0.5：100：0.2混合，使用V形搅拌机进行搅拌均匀，得混合粉末；Insulation coating treatment: a silicone resin powder having an average particle diameter of 25 μm, a -150 mesh FeSiAl metal soft magnetic powder, and zinc stearate were mixed at a mass ratio of 0.5:100:0.2, and uniformly stirred using a V-shaped mixer to obtain a mixture. powder;
压制成型：将经绝缘包覆处理得到的混合粉末使用液压机压制成型，压制压力为10T/cm 2，得成型体；。 Press molding: The mixed powder obtained by the insulating coating treatment is press-formed using a hydraulic press at a pressing pressure of 10 T/cm 2 to obtain a molded body;
一次热处理：将压制成型得到的成型体在500℃的条件下在空气氛围中保温1小时；One heat treatment: the molded body obtained by press molding is kept at 500 ° C for 1 hour in an air atmosphere;
二次热处理：将经过一次热处理的成型体在900℃的条件下在氩气中保温1小时，得耐高温热处理的金属软磁粉芯。Secondary heat treatment: The molded body subjected to primary heat treatment was kept in an argon atmosphere at 900 ° C for 1 hour to obtain a metal soft magnetic powder core resistant to high temperature heat treatment.
实施例2Example 2
制备金属软磁粉末：采用水雾化法制备-150目的FeSiAl金属软磁粉末；Preparation of soft magnetic powder of metal: Preparation of -150 mesh FeSiAl metal soft magnetic powder by water atomization method;
制备硅树脂：按重量份秤取M链节和Q链节的比为0.45、含氢量为0.08mmol/g、粘度为30mPa.s的MQ硅树脂35份，沉淀白炭黑40份，巯丙基甲基二甲氧基硅烷3份，HMPA 6份，投入捏合机，捏合2小时后投入真空密炼机中升温密炼，升温到140℃，抽真空热处理2.5h，测温后，二次升温到170℃，抽真空热处理3.6h；出料，放置18h得硅树脂；并筛选出平均粒径为20μm的硅树脂粉末；Preparation of silicone resin: 35 parts of MQ silicone resin having a ratio of M chain link and Q chain link of 0.45, a hydrogen content of 0.08 mmol/g, a viscosity of 30 mPa.s, and 40 parts of precipitated white carbon black, 巯3 parts of propylmethyldimethoxysilane, 6 parts of HMPA, put into a kneader, kneaded for 2 hours, then put into a vacuum mixer to heat and knead, heat up to 140 ° C, vacuum heat treatment for 2.5 h, after temperature measurement, two The temperature was raised to 170 ° C, vacuum heat treatment for 3.6 h; the material was discharged, and the silicone resin was placed for 18 hours; and the silicone resin powder having an average particle diameter of 20 μm was screened;
绝缘包覆处理：将平均粒径为20μm的硅树脂、-150目的FeSiAl金属软磁粉末和硬脂酸钙按质量比为2：100：0.5混合，使用擂溃机进行搅拌均匀，得混合粉末；Insulation coating treatment: a silicone resin having an average particle diameter of 20 μm, a -150 mesh FeSiAl metal soft magnetic powder and calcium stearate were mixed at a mass ratio of 2:100:0.5, and uniformly stirred using a crucible machine to obtain a mixed powder. ;
压制成型：将经绝缘包覆处理得到的混合粉末使用液压机压制成型，压制压力为15T/cm 2，得成型体； Press molding: the mixed powder obtained by the insulating coating treatment is press-formed using a hydraulic press, and the pressing pressure is 15 T/cm 2 to obtain a molded body;
一次热处理：将压制成型得到的成型体在400℃的条件下在空气氛围中保温1.5小时；One heat treatment: the molded body obtained by press molding is kept at 400 ° C for 1.5 hours in an air atmosphere;
二次热处理：将经过一次热处理的成型体在900℃的条件下在氮气中保温1.5小时，得耐高温热处理的金属软磁粉芯。Secondary heat treatment: The molded body subjected to the primary heat treatment was kept at 900 ° C for 1.5 hours under nitrogen to obtain a metal soft magnetic powder core which was heat-resistant to a high temperature.
实施例3Example 3
制备金属软磁粉末：采用机械破碎法制备-150目的FeSiAl金属软磁粉末；Preparation of soft magnetic powder of metal: Preparation of -150 mesh FeSiAl metal soft magnetic powder by mechanical crushing method;
制备硅树脂：按重量份秤取M链节和Q链节的比为0.5、含氢量 为0.1mmol/g、粘度为50mPa.s的MQ硅树脂40份，沉淀白炭黑50份，巯丙基甲基二甲氧基硅烷4份，HMPA 7份，投入捏合机，捏合2小时后投入真空密炼机中升温密炼，升温到150℃，抽真空热处理3h，测温后，二次升温到180℃，抽真空热处理4h；出料，放置24h得硅树脂；并筛选出平均粒径为15μm的硅树脂粉末；Preparation of silicone resin: 40 parts of MQ silicone resin having a ratio of M chain link and Q chain link of 0.5, a hydrogen content of 0.1 mmol/g, a viscosity of 50 mPa·s, and 50 parts of precipitated white carbon black, 巯4 parts of propylmethyldimethoxysilane and 7 parts of HMPA, put into a kneader, kneaded for 2 hours, and then put into a vacuum internal mixer to heat and knead, heat up to 150 ° C, vacuum heat treatment for 3 h, after temperature measurement, twice The temperature was raised to 180 ° C, vacuum heat treatment for 4 h; the material was discharged, and the silicone resin was placed for 24 hours; and the silicone resin powder having an average particle diameter of 15 μm was screened;
绝缘包覆处理：将平均粒径为15μm的硅树脂粉硅树脂、-150目的FeSiAl金属软磁粉末和硬脂酸钙按质量比为5：100：1混合，使用球磨机进行搅拌均匀，得混合粉末；Insulation coating treatment: a silicone resin powder silicone resin having an average particle diameter of 15 μm, a -150 mesh FeSiAl metal soft magnetic powder and calcium stearate were mixed at a mass ratio of 5:100:1, and uniformly stirred using a ball mill to obtain a mixture. powder;
压制成型：将经绝缘包覆处理得到的混合粉末使用液压机压制成型，压制压力为20T/cm 2，得成型体； Press molding: the mixed powder obtained by the insulating coating treatment is press-formed using a hydraulic press, and the pressing pressure is 20 T/cm 2 to obtain a molded body;
一次热处理：将压制成型得到的成型体在300℃的条件下在空气氛围中保温2小时；One heat treatment: the molded body obtained by press molding is kept at 300 ° C for 2 hours in an air atmosphere;
二次热处理：将经过一次热处理的成型体在900℃的条件下在氦气中保温1小时，得耐高温热处理的金属软磁粉芯。Secondary heat treatment: The molded body subjected to the primary heat treatment was kept at a temperature of 900 ° C for 1 hour in a helium gas to obtain a metal soft magnetic powder core resistant to high temperature heat treatment.
实施例4Example 4
制备金属软磁粉末：采用气雾化法制备-150目的FeSiAl金属软磁粉末；Preparation of soft magnetic powder of metal: Preparation of -150 mesh FeSiAl metal soft magnetic powder by gas atomization;
制备硅树脂：按重量份秤取M链节和Q链节的比为0.4、含氢量为0.1mmol/g、粘度为10mPa.s的MQ硅树脂45份，沉淀白炭黑60份，巯丙基甲基二甲氧基硅烷5份，HMPA 8份，投入捏合机，捏合2小时后投入真空密炼机中升温密炼，升温到160℃，抽真空热处理2h，测温后，二次升温到190℃，抽真空热处理4h；出料，放置12h 得硅树脂；并筛选出平均粒径为15μm的硅树脂粉末；Preparation of silicone resin: 4 parts of MQ silicone resin having a ratio of M chain link and Q chain link of 0.4, a hydrogen content of 0.1 mmol/g, a viscosity of 10 mPa·s, and 60 parts of precipitated white carbon black, 巯5 parts of propylmethyldimethoxysilane, 8 parts of HMPA, put into a kneader, kneaded for 2 hours, then put into a vacuum internal mixer to heat and knead, heat up to 160 ° C, vacuum heat treatment for 2 h, after temperature measurement, twice The temperature was raised to 190 ° C, vacuum heat treatment for 4 h; discharged, placed for 12 h to obtain a silicone resin; and a silicone resin powder having an average particle diameter of 15 μm was screened;
绝缘包覆处理：将平均粒径为15μm的硅树脂、-150目的FeSiAl金属软磁粉末和硬脂酸锌按质量比为2：100：0.5混合，使用砂磨机进行搅拌均匀，得混合粉末；Insulation coating treatment: a silicone resin having an average particle diameter of 15 μm, a -150 mesh FeSiAl metal soft magnetic powder and zinc stearate are mixed at a mass ratio of 2:100:0.5, and uniformly stirred using a sand mill to obtain a mixed powder. ;
压制成型：将经绝缘包覆处理得到的混合粉末使用液压机压制成型，压制压力为20T/cm 2，得成型体； Press molding: the mixed powder obtained by the insulating coating treatment is press-formed using a hydraulic press, and the pressing pressure is 20 T/cm 2 to obtain a molded body;
一次热处理：将压制成型得到的成型体在200℃的条件下在空气氛围中保温2小时；One heat treatment: the molded body obtained by press molding is kept at 200 ° C for 2 hours in an air atmosphere;
二次热处理：将经过一次热处理的成型体在900℃的条件下在氢气中保温2小时，得耐高温热处理的金属软磁粉芯。Secondary heat treatment: The molded body subjected to the primary heat treatment was kept in a hydrogen atmosphere at 900 ° C for 2 hours to obtain a metal soft magnetic powder core resistant to high temperature heat treatment.
实施例5Example 5
制备金属软磁粉末：采用气雾化法制备-300目的FeSiAl金属软磁粉末；Preparation of soft magnetic powder of metal: Preparation of -300 mesh FeSiAl metal soft magnetic powder by gas atomization method;
制备硅树脂：按重量份秤取M链节和Q链节的比为0.45、含氢量为0.08mmol/g、粘度为50mPa.s的MQ硅树脂50份，沉淀白炭黑30份，巯丙基甲基二甲氧基硅烷6份，HMPA 9份，投入捏合机，捏合2小时后投入真空密炼机中升温密炼，升温到150℃，抽真空热处理2h，测温后，二次升温到190℃，抽真空热处理3.5h；出料，放置24h得硅树脂；并筛选出平均粒径为15μm的硅树脂粉末；Preparation of silicone resin: 50 parts of MQ silicone resin having a ratio of M chain link and Q chain link of 0.45, a hydrogen content of 0.08 mmol/g, a viscosity of 50 mPa·s, and 30 parts of precipitated white carbon black, 巯6 parts of propylmethyldimethoxysilane, 9 parts of HMPA, put into a kneader, kneaded for 2 hours, and then put into a vacuum internal mixer to heat and knead, heat up to 150 ° C, vacuum heat treatment for 2 h, after temperature measurement, twice The temperature was raised to 190 ° C, vacuum heat treatment for 3.5 h; discharged, placed for 24 h to obtain a silicone resin; and a silicone resin powder having an average particle diameter of 15 μm was screened;
绝缘包覆处理：将平均粒径为15μm的硅树脂、-300目的FeSiAl金属软磁粉末和硬脂酸锌按质量比为2：100：0.5混合，使用混捏机进行搅拌均匀，得混合粉末；Insulation coating treatment: a silicone resin having an average particle diameter of 15 μm, a -300 mesh FeSiAl metal soft magnetic powder and zinc stearate are mixed at a mass ratio of 2:100:0.5, and uniformly stirred using a kneader to obtain a mixed powder;
压制成型：将经绝缘包覆处理得到的混合粉末使用液压机压制成型，压制压力为20T/cm 2，得成型体； Press molding: the mixed powder obtained by the insulating coating treatment is press-formed using a hydraulic press, and the pressing pressure is 20 T/cm 2 to obtain a molded body;
一次热处理：将压制成型得到的成型体在500℃的条件下在空气氛围中保温2小时；One heat treatment: the molded body obtained by press molding is kept at 500 ° C for 2 hours in an air atmosphere;
二次热处理：将经过一次热处理的成型体在900℃的条件下在真空中保温2小时，得耐高温热处理的金属软磁粉芯。Secondary heat treatment: The molded body subjected to primary heat treatment was kept in a vacuum at 900 ° C for 2 hours to obtain a metal soft magnetic powder core resistant to high temperature heat treatment.
实施例6Example 6
制备金属软磁粉末：采用气雾化法制备-100目的FeSiAl金属软磁粉末；Preparation of metal soft magnetic powder: Preparation of -100 mesh FeSiAl metal soft magnetic powder by gas atomization method;
制备硅树脂：按重量份秤取M链节和Q链节的比为0.5、含氢量为0.05mmol/g、粘度为30mPa.s的MQ硅树脂50份，沉淀白炭黑30份，巯丙基甲基二甲氧基硅烷2份，HMPA 10份，投入捏合机，捏合2小时后投入真空密炼机中升温密炼，升温到150℃，抽真空热处理3h，测温后，二次升温到190℃，抽真空热处理4h；出料，放置24h得硅树脂；并筛选出平均粒径为15μm的硅树脂粉末；Preparation of silicone resin: 50 parts of MQ silicone resin with a ratio of M chain link and Q chain link of 0.5, a hydrogen content of 0.05 mmol/g, a viscosity of 30 mPa·s, and 30 parts of precipitated white carbon black, 巯2 parts of propylmethyldimethoxysilane, 10 parts of HMPA, put into a kneader, kneaded for 2 hours, then put into a vacuum mixer to heat and heat the mixture, heat up to 150 ° C, vacuum heat treatment for 3 h, after temperature measurement, twice The temperature was raised to 190 ° C, vacuum heat treatment for 4 h; the material was discharged, and the silicone resin was placed for 24 hours; and the silicone resin powder having an average particle diameter of 15 μm was screened;
绝缘包覆处理：将平均粒径为15μm的硅树脂、-100目的FeSiAl金属软磁粉末和硬脂酸锌按质量比为2：100：0.5混合，使用混捏机进行搅拌均匀，得混合粉末；Insulation coating treatment: a silicone resin having an average particle diameter of 15 μm, a -100 mesh FeSiAl metal soft magnetic powder and zinc stearate are mixed at a mass ratio of 2:100:0.5, and uniformly stirred using a kneader to obtain a mixed powder;
压制成型：将经绝缘包覆处理得到的混合粉末使用液压机压制成型，压制压力为20T/cm 2，得成型体； Press molding: the mixed powder obtained by the insulating coating treatment is press-formed using a hydraulic press, and the pressing pressure is 20 T/cm 2 to obtain a molded body;
一次热处理：将压制成型得到的成型体在500℃的条件下在空气氛围中保温2小时；One heat treatment: the molded body obtained by press molding is kept at 500 ° C for 2 hours in an air atmosphere;
二次热处理：将经过一次热处理的成型体在900℃的条件下在真空中保温2小时，得耐高温热处理的金属软磁粉芯。Secondary heat treatment: The molded body subjected to primary heat treatment was kept in a vacuum at 900 ° C for 2 hours to obtain a metal soft magnetic powder core resistant to high temperature heat treatment.
实施例7Example 7
制备金属软磁粉末：采用气雾化法制备-150目的FeSi金属软磁粉末；Preparation of soft magnetic powder of metal: Preparation of -150 mesh FeSi metal soft magnetic powder by gas atomization;
制备硅树脂：按重量份秤取M链节和Q链节的比为0.5、含氢量为0.05mmol/g、粘度为30mPa.s的MQ硅树脂50份，沉淀白炭黑30份，巯丙基甲基二甲氧基硅烷2份，HMPA 10份，投入捏合机，捏合2小时后投入真空密炼机中升温密炼，升温到150℃，抽真空热处理3h，测温后，二次升温到190℃，抽真空热处理4h；出料，放置24h得硅树脂；并筛选出平均粒径为15μm的硅树脂粉末；Preparation of silicone resin: 50 parts of MQ silicone resin with a ratio of M chain link and Q chain link of 0.5, a hydrogen content of 0.05 mmol/g, a viscosity of 30 mPa·s, and 30 parts of precipitated white carbon black, 巯2 parts of propylmethyldimethoxysilane, 10 parts of HMPA, put into a kneader, kneaded for 2 hours, then put into a vacuum mixer to heat and heat the mixture, heat up to 150 ° C, vacuum heat treatment for 3 h, after temperature measurement, twice The temperature was raised to 190 ° C, vacuum heat treatment for 4 h; the material was discharged, and the silicone resin was placed for 24 hours; and the silicone resin powder having an average particle diameter of 15 μm was screened;
绝缘包覆处理：将平均粒径为15μm的硅树脂、-150目的FeSi金属软磁粉末和硬脂酸锌按质量比为2：100：0.5混合，使用混捏机进行搅拌均匀，得混合粉末；Insulation coating treatment: a silicone resin having an average particle diameter of 15 μm, a -150 mesh FeSi metal soft magnetic powder and zinc stearate are mixed at a mass ratio of 2:100:0.5, and uniformly stirred using a kneader to obtain a mixed powder;
压制成型：将经绝缘包覆处理得到的混合粉末使用液压机压制成型，压制压力为20T/cm 2，得成型体； Press molding: the mixed powder obtained by the insulating coating treatment is press-formed using a hydraulic press, and the pressing pressure is 20 T/cm 2 to obtain a molded body;
一次热处理：将压制成型得到的成型体在500℃的条件下在空气氛围中保温2小时；One heat treatment: the molded body obtained by press molding is kept at 500 ° C for 2 hours in an air atmosphere;
二次热处理：将经过一次热处理的成型体在900℃的条件下在真空中保温2小时，得耐高温热处理的金属软磁粉芯。Secondary heat treatment: The molded body subjected to primary heat treatment was kept in a vacuum at 900 ° C for 2 hours to obtain a metal soft magnetic powder core resistant to high temperature heat treatment.
实施例8Example 8
制备金属软磁粉末：采用气雾化法制备-100目的FeNi金属软磁 粉末；Preparation of soft magnetic powder of metal: Preparation of -100 mesh FeNi metal soft magnetic powder by gas atomization;
制备硅树脂：按重量份秤取M链节和Q链节的比为0.5、含氢量为0.05mmol/g、粘度为30mPa.s的MQ硅树脂50份，沉淀白炭黑30份，巯丙基甲基二甲氧基硅烷2份，HMPA 10份，投入捏合机，捏合2小时后投入真空密炼机中升温密炼，升温到150℃，抽真空热处理3h，测温后，二次升温到190℃，抽真空热处理4h；出料，放置24h得硅树脂；并筛选出平均粒径为15μm的硅树脂粉末；Preparation of silicone resin: 50 parts of MQ silicone resin with a ratio of M chain link and Q chain link of 0.5, a hydrogen content of 0.05 mmol/g, a viscosity of 30 mPa·s, and 30 parts of precipitated white carbon black, 巯2 parts of propylmethyldimethoxysilane, 10 parts of HMPA, put into a kneader, kneaded for 2 hours, then put into a vacuum mixer to heat and heat the mixture, heat up to 150 ° C, vacuum heat treatment for 3 h, after temperature measurement, twice The temperature was raised to 190 ° C, vacuum heat treatment for 4 h; the material was discharged, and the silicone resin was placed for 24 hours; and the silicone resin powder having an average particle diameter of 15 μm was screened;
绝缘包覆处理：将平均粒径为15μm的硅树脂、-300目的FeNi金属软磁粉末和硬脂酸锌按质量比为2：100：0.5混合，使用混捏机进行搅拌均匀，得混合粉末；Insulation coating treatment: a silicone resin having an average particle diameter of 15 μm, a -300 mesh FeNi metal soft magnetic powder and zinc stearate are mixed at a mass ratio of 2:100:0.5, and uniformly stirred using a kneader to obtain a mixed powder;
压制成型：将经绝缘包覆处理得到的混合粉末使用液压机压制成型，压制压力为20T/cm 2，得成型体；。 Press molding: The mixed powder obtained by the insulating coating treatment is press-formed using a hydraulic press at a pressing pressure of 20 T/cm 2 to obtain a molded body;
一次热处理：将压制成型得到的成型体在500℃的条件下在空气氛围中保温2小时；One heat treatment: the molded body obtained by press molding is kept at 500 ° C for 2 hours in an air atmosphere;
二次热处理：将经过一次热处理的成型体在900℃的条件下在真空中保温2小时，得耐高温热处理的金属软磁粉芯。Secondary heat treatment: The molded body subjected to primary heat treatment was kept in a vacuum at 900 ° C for 2 hours to obtain a metal soft magnetic powder core resistant to high temperature heat treatment.
实施例9Example 9
制备金属软磁粉末：采用气雾化法制备-300目的FeNiMo金属软磁粉末；Preparation of metal soft magnetic powder: Preparation of -300 mesh FeNiMo metal soft magnetic powder by gas atomization method;
制备硅树脂：按重量份秤取M链节和Q链节的比为0.5、含氢量为0.05mmol/g、粘度为30mPa.s的MQ硅树脂50份，沉淀白炭黑30份，巯丙基甲基二甲氧基硅烷2份，HMPA 10份，投入捏合机，捏 合2小时后投入真空密炼机中升温密炼，升温到150℃，抽真空热处理3h，测温后，二次升温到190℃，抽真空热处理4h；出料，放置24h得硅树脂；并筛选出平均粒径为15μm的硅树脂粉末；Preparation of silicone resin: 50 parts of MQ silicone resin with a ratio of M chain link and Q chain link of 0.5, a hydrogen content of 0.05 mmol/g, a viscosity of 30 mPa·s, and 30 parts of precipitated white carbon black, 巯2 parts of propylmethyldimethoxysilane, 10 parts of HMPA, put into a kneader, kneaded for 2 hours, then put into a vacuum mixer to heat and heat the mixture, heat up to 150 ° C, vacuum heat treatment for 3 h, after temperature measurement, twice The temperature was raised to 190 ° C, vacuum heat treatment for 4 h; the material was discharged, and the silicone resin was placed for 24 hours; and the silicone resin powder having an average particle diameter of 15 μm was screened;
绝缘包覆处理：将平均粒径为15μm的硅树脂、-300目的FeNiMo金属软磁粉末和硬脂酸锌按质量比为2：100：0.5混合，使用混捏机进行搅拌均匀，得混合粉末；Insulation coating treatment: a silicone resin having an average particle diameter of 15 μm, a -300 mesh FeNiMo metal soft magnetic powder and zinc stearate are mixed at a mass ratio of 2:100:0.5, and uniformly stirred using a kneader to obtain a mixed powder;
压制成型：将经绝缘包覆处理得到的混合粉末使用液压机压制成型，压制压力为20T/cm 2，得成型体； Press molding: the mixed powder obtained by the insulating coating treatment is press-formed using a hydraulic press, and the pressing pressure is 20 T/cm 2 to obtain a molded body;
一次热处理：将压制成型得到的成型体在500℃的条件下在空气氛围中保温2小时；One heat treatment: the molded body obtained by press molding is kept at 500 ° C for 2 hours in an air atmosphere;
二次热处理：将经过一次热处理的成型体在900℃的条件下在真空中保温2小时，得耐高温热处理的金属软磁粉芯。Secondary heat treatment: The molded body subjected to primary heat treatment was kept in a vacuum at 900 ° C for 2 hours to obtain a metal soft magnetic powder core resistant to high temperature heat treatment.
对现有技术金属软磁粉芯和实施例1-10进行对比测试，其中损耗测试条件为50kHz,100mT，测试设备为Iwatsu SY-8219；得到下表数据：A comparison test was performed on the prior art metal soft magnetic powder core and Examples 1-10, wherein the loss test condition was 50 kHz, 100 mT, and the test equipment was Iwatsu SY-8219; the following data was obtained:
  磁滞损耗(mW/cm 3) Hysteresis loss (mW/cm 3 ) 涡流损耗(mW/cm 3) Eddy current loss (mW/cm 3 ) 总损耗(mW/cm 3) Total loss (mW/cm 3 )
现有金属软磁粉芯Existing metal soft magnetic powder core 210210 6464 274274
实施例1Example 1 193193 3737 230230
实施例2Example 2 184184 3838 222222
实施例3Example 3 195195 3838 233233
实施例4Example 4 182182 4242 224224
实施例5Example 5 204204 3232 236236
实施例6Example 6 178178 4747 225225
实施例7Example 7 380380 7070 450450
实施例8Example 8 169169 7878 247247
实施例9Example 9 162162 6464 226226
对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其他的具体形式实现本发明。因此，无论从哪一点来看，均应将实施例看作是示范性的，而且是非限为性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。It is apparent to those skilled in the art that the present invention is not limited to the details of the above-described exemplary embodiments, and the present invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the invention is defined by the appended claims instead All changes in the meaning and scope of the claimed equivalents are included in the present invention.
此外，应当理解，虽然本说明书按照实施方式加以描述，但并非每个实施方式仅包含一个独立的技术方案，说明书的这种叙述方式仅仅是为清楚起见，本领域技术人员应当将说明书作为一个整体，各实施例中的技术方案也可以经适当组合，形成本领域技术人员可以理解的其他实施方式。In addition, it should be understood that although the description is described in terms of embodiments, not every embodiment includes only one independent technical solution. The description of the specification is merely for the sake of clarity, and those skilled in the art should The technical solutions in the respective embodiments may also be combined as appropriate to form other embodiments that can be understood by those skilled in the art.

Claims (5)

  1. 一种硅树脂，其特征在于，由如下重量份组分组成：MQ硅树脂30～50份、沉淀白炭黑30～60份、巯丙基甲基二甲氧基硅烷2～6份和HMPA5～10份。A silicone resin characterized by being composed of the following components by weight: 30 to 50 parts of MQ silicone resin, 30 to 60 parts of precipitated white carbon black, 2 to 6 parts of fluorenylmethyldimethoxysilane, and HMPA 5 ~10 copies.
  2. 根据权利要求1所述的硅树脂，其特征在于，所述硅树脂是由如下重量份组分组成：MQ硅树脂30～35份、沉淀白炭黑50～60份、巯丙基甲基二甲氧基硅烷2～6份和HMPA5～10份。The silicone resin according to claim 1, wherein the silicone resin is composed of the following components by weight: 30 to 35 parts of MQ silicone resin, 50 to 60 parts of precipitated silica, and propylmethyl group II. 2 to 6 parts of methoxysilane and 5 to 10 parts of HMPA.
  3. 根据权利要求1所述的硅树脂，其特征在于，所述的MQ硅树脂中M链节和Q链节的比为0.4～0.5。The silicone resin according to claim 1, wherein the ratio of the M chain link to the Q chain link in the MQ silicone resin is from 0.4 to 0.5.
  4. 根据权利要求1所述的硅树脂，其特征在于，所述的MQ硅树脂的含氢量为0.05～0.1mmol/g，所述的MQ硅树脂的粘度为10～50mPa.s。The silicone resin according to claim 1, wherein the MQ silicone resin has a hydrogen content of 0.05 to 0.1 mmol/g, and the MQ silicone resin has a viscosity of 10 to 50 mPa·s.
  5. 一种硅树脂的制备方法，其特征在于，将MQ硅树脂30～50份、沉淀白炭黑30～60份、巯丙基甲基二甲氧基硅烷2～6份和HMPA5～10份投入捏合机，捏合2小时后投入真空密炼机中升温密炼，升温到130～160℃，抽真空热处理2～3h，测温后，二次升温到160～190℃，抽真空热处理3.5～4h；出料，放置12～24h得硅树脂。A method for preparing a silicone resin, comprising: 30 to 50 parts of MQ silicone resin, 30 to 60 parts of precipitated white carbon black, 2 to 6 parts of propyl propyl methyl dimethoxy silane, and 5 to 10 parts of HMPA Kneading machine, kneading for 2 hours, then put into a vacuum mixer to heat and mix, heat up to 130 ~ 160 ° C, vacuum heat treatment 2 ~ 3h, after temperature measurement, secondary temperature rise to 160 ~ 190 ° C, vacuum heat treatment 3.5 ~ 4h ; discharge, placed 12 ~ 24h to obtain silicone resin.
PCT/CN2018/076090 2017-08-10 2018-02-09 Silicone resin WO2019029145A1 (en)

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