CN112992517A - Preparation process of nano magnetic powder - Google Patents
Preparation process of nano magnetic powder Download PDFInfo
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- CN112992517A CN112992517A CN202110294650.1A CN202110294650A CN112992517A CN 112992517 A CN112992517 A CN 112992517A CN 202110294650 A CN202110294650 A CN 202110294650A CN 112992517 A CN112992517 A CN 112992517A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus 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
- H01F41/02—Apparatus 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 for manufacturing cores, coils, or magnets
Abstract
The invention relates to a nanometer magnetic powder, in particular to a preparation process of the nanometer magnetic powder, which comprises the following steps; step 1: mixing and stirring the magnetic metal ion solution and the network structure powder, and then drying to obtain a magnetic metal composition; step 2: putting the magnetic metal composition into an inorganic solvent, and uniformly adding an alcoholic solution of distilled water; and step 3: heating the hard gel precursor, introducing hydrogen, and spraying cold water mist to cool in 6-8min to obtain composite powder; and 4, step 4: adding a modifying active agent and an auxiliary agent into a metal solution containing an emulsifier, stirring, and drying to obtain alloy magnetic powder; and 5: heating the alloy magnetic powder, introducing hydrogen, and spraying cold water mist to cool the alloy magnetic powder within 6-8min to obtain nano magnetic powder; the invention synthesizes the nanometer magnetic powder by hydrogen reduction from the solid phase, and takes the network structure body as the carrier, so that the dispersion coefficient of the powder particle size is small, and the prepared nanometer magnetic powder has smaller particle size and is easier to process.
Description
Technical Field
The invention relates to nanometer magnetic powder, in particular to a preparation process of nanometer magnetic powder.
Background
An inductor is a component that can convert electrical energy into magnetic energy for storage. The inductor is similar in structure to a transformer, but has only one winding. The inductor has an inductance that only impedes the change in current. If the inductor is in a state where no current is passing, it will try to block the current from flowing through it when the circuit is on; if the inductor is in a current passing state, the inductor will try to keep the current unchanged when the circuit is opened. Inductors are also known as chokes, reactors, dynamic reactors. In order to improve the conductivity and the preparation precision of the inductor, the inductor is generally prepared by adopting nano-scale magnetic powder such as nano iron powder. However, due to the limitation of the nanometer preparation process, the prepared inductor has the defects of poor conductivity and the like due to reasons of non-ideal particle size, easy agglomeration and the like in the preparation process of the nanometer magnetic powder.
Disclosure of Invention
The invention aims to solve the defects in the background technology by providing a preparation process of nano magnetic powder.
The technical scheme adopted by the invention is as follows: the preparation method comprises the following steps;
step 1: mixing the magnetic metal ion solution and the network structure powder, stirring at 85-90 ℃ for 10-15min, and drying to obtain a magnetic metal composition;
step 2: putting the magnetic metal composition into an inorganic solvent, uniformly adding an alcoholic solution of distilled water while stirring, and controlling the pH value to be 6-7 to obtain a hard gel precursor;
and step 3: heating the hard gel precursor to 250-280 ℃, introducing hydrogen, continuing for 1-2h, and then spraying cold water mist to cool the hard gel precursor within 6-8min to obtain composite powder;
and 4, step 4: adding a modifying active agent and an auxiliary agent into a metal solution containing an emulsifier, stirring for 3-5min, and drying to obtain alloy magnetic powder;
and 5: heating the alloy magnetic powder to 250-280 ℃, introducing hydrogen, continuing for 1-2h, and then spraying cold water mist to cool the alloy magnetic powder within 6-8min to obtain the nano magnetic powder.
As a preferred technical scheme of the invention: the nanometer magnetic powder comprises the following raw materials in parts by weight:
75-90 parts of magnetic metal ion solution;
10-15 parts of network structure powder;
80-110 parts of an inorganic solvent;
20-35 parts of an alcohol solution of distilled water;
60-75 parts of metal solution containing an emulsifier;
3-5 parts of a modifying active agent;
4-9 parts of an auxiliary agent.
As a preferred technical scheme of the invention: the magnetic metal ion solution is any one of water solution of Fe, Co and Ni, and the mass fraction of solute is 10-13%.
As a preferred technical scheme of the invention: the network structure body is SiO2、AL2O3MgO, and polymethyl methacrylate.
As a preferred technical scheme of the invention: the inorganic solvent is one or a mixture of more of liquid sulfur dioxide, thionyl chloride (di) chloride (thionyl chloride) and sulfuryl chloride.
As a preferred technical scheme of the invention: the ratio of the emulsifier to the metal solution in the metal solution containing the emulsifier is 1:15-17, the emulsifier is fatty alcohol-polyoxyethylene ether or fatty amine-polyoxyethylene ether, the metal solution is an aqueous solution of any one of Fe, Co and Ni, and the mass fraction of the solute is 10% -13%.
As a preferred technical scheme of the invention: the preparation method of the modified active agent comprises the following steps:
weighing hydrogen-containing polysiloxane, octamethylcyclotetrasiloxane and end-capping reagent MM according to a certain proportion, placing the mixture into a three-neck flask, assembling an electric stirrer, a thermometer and a reflux condenser tube with the three-neck flask, then starting heating, and dropwise adding 3% concentrated H in a trickle shape when the temperature reaches 40 DEG C2SO4Maintaining the reaction temperature within 40-45 deg.C, mixing and reacting for 5-6h, pouring the crude product obtained after reaction into separating funnel, standing for separating liquid, collecting the upper layer liquid, adding NaHCO for several times3The powder is continuously stirred and fully reacted for 1 hour,and after an active agent with the pH value of 6-7 is obtained, carrying out suction filtration, and carrying out reduced pressure distillation to remove low-boiling-point substances, thus obtaining the required modified active agent.
As a preferred technical scheme of the invention: the ratio of the hydrogenpolysiloxane, the octamethylcyclotetrasiloxane and the end-capping reagent MM is 1:0.2-0.4: 0.5-0.7.
As a preferred technical scheme of the invention: the auxiliary agent is graphite and Cu2A mixture of O.
As a preferred technical scheme of the invention: the graphite and Cu2The mixing ratio of O is 1: 1.3-1.5.
1. The invention can generate oxalate-bridged linear complex (such as FeC) in the preparation process by synthesizing nano magnetic powder from solid phase through hydrogen reduction and taking a network structure body as a solid phase carrier2O4·2H2O), because the negative divalent anions and the metal cations form a net structure through hydrogen bonds, the dispersion coefficient of the powder particle size is small, and the prepared nano magnetic powder has smaller particle size and is easier to process.
2. The invention modifies an activator by octamethylcyclotetrasiloxane and a blocking agent MM to concentrate H2SO4Consumption of CH as catalyst in the resulting polysiloxanes3The reduction of the hydrogen content and the active hydrogen in the nano magnetic powder is beneficial to reducing the distribution density of Si-H bonds in polysiloxane, the weaker the steric hindrance effect is, the smooth proceeding of the grafting reaction is facilitated, so that the active agent is wrapped around the initial particles, the particles are repelled due to the surface electrostatic effect, the aggregation and agglomeration of the particles can be prevented, and the prepared nano magnetic powder is not easy to agglomerate during drying.
3. The invention is characterized in that graphite and Cu are used2The conductive auxiliary mixed with O ensures that the conductivity of the nano magnetic powder is more excellent, and the prepared inductor has higher sensitivity and better conductivity.
Drawings
FIG. 1 is a schematic view showing an assembly of an electric stirrer, a thermometer and a reflux condenser with a three-necked flask in a preferred embodiment of the present invention.
Detailed Description
It should be noted that, in the present application, features of embodiments and embodiments may be combined with each other without conflict, and technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the preferred embodiment of the invention provides a preparation process of nanometer magnetic powder, which comprises the following steps;
step 1: mixing the magnetic metal ion solution with the network structure powder, stirring at 85 ℃ for 10min, and drying to obtain a magnetic metal composition;
step 2: putting the magnetic metal composition into an inorganic solvent, uniformly adding an alcoholic solution of distilled water while stirring, and controlling the pH value to be 6 to obtain a hard gel precursor;
and step 3: heating the hard gel precursor to 250 ℃, introducing hydrogen, continuing for 1h, and then spraying cold water mist to cool the hard gel precursor within 6min to obtain composite powder;
and 4, step 4: adding a modifying active agent and an auxiliary agent into a metal solution containing an emulsifier, stirring for 3min, and drying to obtain alloy magnetic powder;
and 5: heating the alloy magnetic powder to 250 ℃, introducing hydrogen, continuing for 1h, and then spraying cold water mist to cool the alloy magnetic powder within 6min to obtain the nano magnetic powder.
In this embodiment: the nanometer magnetic powder comprises the following raw materials in parts by weight:
75 parts of magnetic metal ion solution;
15 parts of network structure powder;
100 parts of an inorganic solvent;
20 parts of an alcoholic solution of distilled water;
75 parts of metal solution containing an emulsifier;
5 parts of a modifying active agent;
and 9 parts of an auxiliary agent.
In this embodiment: the magnetic metal ion solution is an Fe aqueous solution, and the mass fraction of the solute is 10%.
In this embodiment: the network structure body is SiO2。
In this embodiment: the inorganic solvent is liquid sulfur dioxide.
In this embodiment: the ratio of the emulsifier to the metal solution in the metal solution containing the emulsifier is 1:15, the emulsifier is fatty alcohol-polyoxyethylene ether, the metal solution is an Fe aqueous solution, and the mass fraction of the solute is 10.
In this embodiment: the preparation method of the modified active agent comprises the following steps:
weighing hydrogen-containing polysiloxane, octamethylcyclotetrasiloxane and end-capping reagent MM according to a certain proportion, placing the mixture into a three-neck flask, assembling an electric stirrer, a thermometer and a reflux condenser tube with the three-neck flask, then starting heating, and dropwise adding 3% concentrated H in a trickle shape when the temperature reaches 40 DEG C2SO4Maintaining the reaction temperature at 40 ℃, mixing and reacting for 5h, pouring the crude product obtained after the reaction into a separating funnel, standing and separating, taking the upper layer liquid, adding a small amount of NaHCO for multiple times3And (3) stirring the powder continuously, fully reacting for 1h to obtain an active agent with the pH value of 6, performing suction filtration, and performing reduced pressure distillation to remove low-boiling-point substances to obtain the required modified active agent.
In this embodiment: the ratio of the hydrogenpolysiloxane, the octamethylcyclotetrasiloxane and the end-capping reagent MM is 1:0.2: 0.7.
In this embodiment: the auxiliary agent is graphite and Cu2A mixture of O.
In this embodiment: the graphite and Cu2The mixing ratio of O is 1: 1.3.
Example 2:
the preferred embodiment of the invention provides a preparation process of nanometer magnetic powder, which comprises the following steps;
step 1: mixing the magnetic metal ion solution with the network structure powder, stirring at 88 ℃ for 12min, and drying to obtain a magnetic metal composition;
step 2: putting the magnetic metal composition into an inorganic solvent, uniformly adding an alcoholic solution of distilled water while stirring, and controlling the pH value to be 6 to obtain a hard gel precursor;
and step 3: heating the hard gel precursor to 275 ℃, introducing hydrogen, continuing for 1.5h, and then spraying cold water mist to cool the hard gel precursor in 7min to obtain composite powder;
and 4, step 4: adding a modifying active agent and an auxiliary agent into a metal solution containing an emulsifier, stirring for 4min, and drying to obtain alloy magnetic powder;
and 5: heating the alloy magnetic powder to 275 ℃, introducing hydrogen, continuing for 1.5h, and then spraying cold water mist to cool the alloy magnetic powder within 7min to obtain the nano magnetic powder.
In this embodiment: the nanometer magnetic powder comprises the following raw materials in parts by weight:
80 parts of magnetic metal ion solution;
10 parts of network structure powder;
90 parts of an inorganic solvent;
30 parts of an alcohol solution of distilled water;
65 parts of a metal solution containing an emulsifier;
3 parts of a modifying active agent;
and 5 parts of an auxiliary agent.
In this embodiment: the magnetic metal ion solution is a Co aqueous solution, and the mass fraction of the solute is 12%.
In this embodiment: the network structure is AL2O3。
In this embodiment: the inorganic solvent is a mixture of liquid sulfur dioxide and sulfuryl chloride.
In this embodiment: the ratio of the emulsifier to the metal solution in the metal solution containing the emulsifier is 1:16, the emulsifier is fatty amine polyoxyethylene ether, the metal solution is a Co aqueous solution, and the mass fraction of the solute is 12%.
In this embodiment: the preparation method of the modified active agent comprises the following steps:
weighing hydrogen-containing polysiloxane, octamethylcyclotetrasiloxane and end-capping reagent MM according to a certain proportion, placing the mixture into a three-neck flask, assembling an electric stirrer, a thermometer and a reflux condenser tube with the three-neck flask, then starting heating, and dropwise adding 3% concentrated H in a trickle shape when the temperature reaches 40 DEG C2SO4Keeping the reaction temperature within 42 ℃, mixing and reacting for 5.5h, pouring the crude product obtained after the reaction into a separating funnel, standing and separating, taking the upper layer liquid, adding a small amount of NaHCO for multiple times3And (3) stirring the powder continuously, fully reacting for 1h to obtain an active agent with the pH value of 7, performing suction filtration, and performing reduced pressure distillation to remove low-boiling-point substances to obtain the required modified active agent.
In this embodiment: the ratio of the hydrogenpolysiloxane, the octamethylcyclotetrasiloxane and the end-capping reagent MM is 1:0.3: 0.6.
In this embodiment: the auxiliary agent is graphite and Cu2A mixture of O.
In this embodiment: the graphite and Cu2The mixing ratio of O is 1: 1.4.
Example 3:
the preferred embodiment of the invention provides a preparation process of nanometer magnetic powder, which comprises the following steps;
step 1: mixing the magnetic metal ion solution with the network structure powder, stirring for 15min at 90 ℃, and then drying to obtain a magnetic metal composition;
step 2: putting the magnetic metal composition into an inorganic solvent, uniformly adding an alcoholic solution of distilled water while stirring, and controlling the pH value to be 7 to obtain a hard gel precursor;
and step 3: heating the hard gel precursor to 280 ℃, introducing hydrogen, continuing for 2 hours, and then spraying cold water mist to cool the hard gel precursor in 8min to obtain composite powder;
and 4, step 4: adding a modifying active agent and an auxiliary agent into a metal solution containing an emulsifier, stirring for 5min, and drying to obtain alloy magnetic powder;
and 5: heating the alloy magnetic powder to 280 ℃, introducing hydrogen, continuing for 2 hours, and then spraying cold water mist to cool the alloy magnetic powder in 8min to obtain the nano magnetic powder.
In this embodiment: the nanometer magnetic powder comprises the following raw materials in parts by weight:
90 parts of magnetic metal ion solution;
10 parts of network structure powder;
100 parts of an inorganic solvent;
35 parts of an alcoholic solution of distilled water;
75 parts of metal solution containing an emulsifier;
5 parts of a modifying active agent;
and 7 parts of an auxiliary agent.
In this embodiment: the magnetic metal ion solution is a Ni aqueous solution, and the mass fraction of the solute is 13%.
In this embodiment: the network structure is polymethyl methacrylate.
In this embodiment: the inorganic solvent is a mixture of liquid sulfur dioxide and thionyl chloride (thionyl chloride).
In this embodiment: the ratio of the emulsifier to the metal solution in the metal solution containing the emulsifier is 1:17, the emulsifier is fatty amine polyoxyethylene ether, the metal solution is Ni aqueous solution, and the mass fraction of the solute is 13%.
In this embodiment: the preparation method of the modified active agent comprises the following steps:
weighing hydrogen-containing polysiloxane, octamethylcyclotetrasiloxane and end-capping reagent MM in proportion, placing the mixture into a three-neck flask, assembling an electric stirrer, a thermometer and a reflux condenser pipe with the three-neck flask, heating, and heating when the temperature reaches3% concentrated H is added dropwise in a fine stream form after reaching 40 DEG C2SO4Maintaining the reaction temperature at 45 ℃, mixing and reacting for 6h, pouring the crude product obtained after the reaction into a separating funnel, standing and separating, taking the upper layer liquid, adding a small amount of NaHCO for multiple times3And (3) stirring the powder continuously, fully reacting for 1h to obtain an active agent with the pH value of 7, performing suction filtration, and performing reduced pressure distillation to remove low-boiling-point substances to obtain the required modified active agent.
In this embodiment: the ratio of the hydrogenpolysiloxane, the octamethylcyclotetrasiloxane and the end-capping reagent MM is 1:0.4: 0.5.
In this embodiment: the auxiliary agent is graphite and Cu2A mixture of O.
In this embodiment: the graphite and Cu2The mixing ratio of O is 1: 1.5.
Example 4:
the preferred embodiment of the invention provides a preparation process of nanometer magnetic powder, which comprises the following steps;
step 1: mixing the magnetic metal ion solution with the network structure powder, stirring at 85 ℃ for 10min, and drying to obtain a magnetic metal composition;
step 2: putting the magnetic metal composition into an inorganic solvent, uniformly adding an alcoholic solution of distilled water while stirring, and controlling the pH value to be 6 to obtain a hard gel precursor;
and step 3: heating the hard gel precursor to 250 ℃, introducing hydrogen, continuing for 1h, and then spraying cold water mist to cool the hard gel precursor within 6min to obtain composite powder;
and 4, step 4: adding a modifying active agent and an auxiliary agent into a metal solution containing an emulsifier, stirring for 3min, and drying to obtain alloy magnetic powder;
and 5: heating the alloy magnetic powder to 250 ℃, introducing hydrogen, continuing for 1h, and then spraying cold water mist to cool the alloy magnetic powder within 6min to obtain the nano magnetic powder.
In this embodiment: the nanometer magnetic powder comprises the following raw materials in parts by weight:
75 parts of magnetic metal ion solution;
15 parts of network structure powder;
100 parts of an inorganic solvent;
20 parts of an alcoholic solution of distilled water;
75 parts of metal solution containing an emulsifier;
5 parts of a modifying active agent;
and 9 parts of an auxiliary agent.
In this embodiment: the magnetic metal ion solution is an Fe aqueous solution, and the mass fraction of the solute is 6%.
In this embodiment: the network structure body is SiO2。
In this embodiment: the inorganic solvent is liquid sulfur dioxide.
In this embodiment: the ratio of the emulsifier to the metal solution in the metal solution containing the emulsifier is 1:15, the emulsifier is fatty alcohol-polyoxyethylene ether, the metal solution is an Fe aqueous solution, and the mass fraction of the solute is 10.
In this embodiment: the preparation method of the modified active agent comprises the following steps:
weighing hydrogen-containing polysiloxane, octamethylcyclotetrasiloxane and end-capping reagent MM according to a certain proportion, placing the mixture into a three-neck flask, assembling an electric stirrer, a thermometer and a reflux condenser tube with the three-neck flask, then starting heating, and dropwise adding 3% concentrated H in a trickle shape when the temperature reaches 40 DEG C2SO4Maintaining the reaction temperature at 40 ℃, mixing and reacting for 5h, pouring the crude product obtained after the reaction into a separating funnel, standing and separating, taking the upper layer liquid, adding a small amount of NaHCO for multiple times3And (3) stirring the powder continuously, fully reacting for 1h to obtain an active agent with the pH value of 6, performing suction filtration, and performing reduced pressure distillation to remove low-boiling-point substances to obtain the required modified active agent.
In this embodiment: the ratio of the hydrogenpolysiloxane, the octamethylcyclotetrasiloxane and the end-capping reagent MM is 1:0.2: 0.7.
In this embodiment: the auxiliary agent is graphite and Cu2A mixture of O.
In this embodiment: the graphite and Cu2The mixing ratio of O is 1: 1.3.
Example 5:
the preferred embodiment of the invention provides a preparation process of nanometer magnetic powder, which comprises the following steps;
step 1: mixing the magnetic metal ion solution with the network structure powder, stirring at 88 ℃ for 12min, and drying to obtain a magnetic metal composition;
step 2: putting the magnetic metal composition into an inorganic solvent, uniformly adding an alcoholic solution of distilled water while stirring, and controlling the pH value to be 6 to obtain a hard gel precursor;
and step 3: heating the hard gel precursor to 275 ℃, introducing hydrogen, continuing for 1.5h, and then spraying cold water mist to cool the hard gel precursor in 7min to obtain composite powder;
and 4, step 4: adding a modifying active agent and an auxiliary agent into a metal solution containing an emulsifier, stirring for 4min, and drying to obtain alloy magnetic powder;
and 5: heating the alloy magnetic powder to 275 ℃, introducing hydrogen, continuing for 1.5h, and then spraying cold water mist to cool the alloy magnetic powder within 7min to obtain the nano magnetic powder.
In this embodiment: the nanometer magnetic powder comprises the following raw materials in parts by weight:
80 parts of magnetic metal ion solution;
10 parts of network structure powder;
90 parts of an inorganic solvent;
30 parts of an alcohol solution of distilled water;
65 parts of a metal solution containing an emulsifier;
3 parts of a modifying active agent;
and 5 parts of an auxiliary agent.
In this embodiment: the magnetic metal ion solution is a Co aqueous solution, and the mass fraction of the solute is 12%.
In this embodiment: the network structure is epoxy resin.
In this embodiment: the inorganic solvent is a mixture of liquid sulfur dioxide and sulfuryl chloride.
In this embodiment: the ratio of the emulsifier to the metal solution in the metal solution containing the emulsifier is 1:16, the emulsifier is fatty amine polyoxyethylene ether, the metal solution is a Co aqueous solution, and the mass fraction of the solute is 12%.
In this embodiment: the preparation method of the modified active agent comprises the following steps:
weighing hydrogen-containing polysiloxane, octamethylcyclotetrasiloxane and end-capping reagent MM according to a certain proportion, placing the mixture into a three-neck flask, assembling an electric stirrer, a thermometer and a reflux condenser tube with the three-neck flask, then starting heating, and dropwise adding 3% concentrated H in a trickle shape when the temperature reaches 40 DEG C2SO4Keeping the reaction temperature within 42 ℃, mixing and reacting for 5.5h, pouring the crude product obtained after the reaction into a separating funnel, standing and separating, taking the upper layer liquid, adding a small amount of NaHCO for multiple times3And (3) stirring the powder continuously, fully reacting for 1h to obtain an active agent with the pH value of 7, performing suction filtration, and performing reduced pressure distillation to remove low-boiling-point substances to obtain the required modified active agent.
In this embodiment: the ratio of the hydrogenpolysiloxane, the octamethylcyclotetrasiloxane and the end-capping reagent MM is 1:0.3: 0.6.
In this embodiment: the auxiliary agent is graphite and Cu2A mixture of O.
In this embodiment: the graphite and Cu2The mixing ratio of O is 1: 1.4.
Example 6:
the preferred embodiment of the invention provides a preparation process of nanometer magnetic powder, which comprises the following steps;
step 1: mixing the magnetic metal ion solution with the network structure powder, stirring for 15min at 90 ℃, and then drying to obtain a magnetic metal composition;
step 2: putting the magnetic metal composition into an inorganic solvent, uniformly adding an alcoholic solution of distilled water while stirring, and controlling the pH value to be 7 to obtain a hard gel precursor;
and step 3: heating the hard gel precursor to 280 ℃, introducing hydrogen, continuing for 2 hours, and then spraying cold water mist to cool the hard gel precursor in 8min to obtain composite powder;
and 4, step 4: adding a modifying active agent and an auxiliary agent into a metal solution containing an emulsifier, stirring for 5min, and drying to obtain alloy magnetic powder;
and 5: heating the alloy magnetic powder to 280 ℃, introducing hydrogen, continuing for 2 hours, and then spraying cold water mist to cool the alloy magnetic powder in 8min to obtain the nano magnetic powder.
In this embodiment: the nanometer magnetic powder comprises the following raw materials in parts by weight:
90 parts of magnetic metal ion solution;
10 parts of network structure powder;
100 parts of an inorganic solvent;
35 parts of an alcoholic solution of distilled water;
75 parts of metal solution containing an emulsifier;
5 parts of a modifying active agent;
and 7 parts of an auxiliary agent.
In this embodiment: the magnetic metal ion solution is a Ni aqueous solution, and the mass fraction of the solute is 13%.
In this embodiment: the network structure is polymethyl methacrylate.
In this embodiment: the inorganic solvent is liquid ammonia.
In this embodiment: the ratio of the emulsifier to the metal solution in the metal solution containing the emulsifier is 1:17, the emulsifier is fatty amine polyoxyethylene ether, the metal solution is Ni aqueous solution, and the mass fraction of the solute is 13%.
In this embodiment: the preparation method of the modified active agent comprises the following steps:
weighing hydrogen-containing polysiloxane and octal according to the proportionPutting cyclotetrasiloxane and end-capping reagent MM in a three-neck flask, assembling an electric stirrer, a thermometer and a reflux condenser tube with the three-neck flask, then starting heating, and dropwise adding 3% concentrated H in a thin stream shape when the temperature reaches 40 DEG C2SO4Maintaining the reaction temperature at 45 ℃, mixing and reacting for 6h, pouring the crude product obtained after the reaction into a separating funnel, standing and separating, taking the upper layer liquid, adding a small amount of NaHCO for multiple times3And (3) stirring the powder continuously, fully reacting for 1h to obtain an active agent with the pH value of 7, performing suction filtration, and performing reduced pressure distillation to remove low-boiling-point substances to obtain the required modified active agent.
In this embodiment: the ratio of the hydrogenpolysiloxane, the octamethylcyclotetrasiloxane and the end-capping reagent MM is 1:0.4: 0.5.
In this embodiment: the auxiliary agent is graphite and Cu2A mixture of O.
In this embodiment: the graphite and Cu2The mixing ratio of O is 1: 1.5.
Example 7:
the preferred embodiment of the invention provides a preparation process of nanometer magnetic powder, which comprises the following steps;
step 1: mixing the magnetic metal ion solution with the network structure powder, stirring at 85 ℃ for 10min, and drying to obtain a magnetic metal composition;
step 2: putting the magnetic metal composition into an inorganic solvent, uniformly adding an alcoholic solution of distilled water while stirring, and controlling the pH value to be 6 to obtain a hard gel precursor;
and step 3: heating the hard gel precursor to 250 ℃, introducing hydrogen, continuing for 1h, and then spraying cold water mist to cool the hard gel precursor within 6min to obtain composite powder;
and 4, step 4: adding a modifying active agent and an auxiliary agent into a metal solution containing an emulsifier, stirring for 3min, and drying to obtain alloy magnetic powder;
and 5: heating the alloy magnetic powder to 250 ℃, introducing hydrogen, continuing for 1h, and then spraying cold water mist to cool the alloy magnetic powder within 6min to obtain the nano magnetic powder.
In this embodiment: the nanometer magnetic powder comprises the following raw materials in parts by weight:
75 parts of magnetic metal ion solution;
15 parts of network structure powder;
100 parts of an inorganic solvent;
20 parts of an alcoholic solution of distilled water;
75 parts of metal solution containing an emulsifier;
5 parts of a modifying active agent;
and 9 parts of an auxiliary agent.
In this embodiment: the magnetic metal ion solution is an Fe aqueous solution, and the mass fraction of the solute is 10%.
In this embodiment: the network structure body is SiO2。
In this embodiment: the inorganic solvent is liquid sulfur dioxide.
In this embodiment: the ratio of the emulsifier to the metal solution in the metal solution containing the emulsifier is 1:3, the emulsifier is fatty alcohol-polyoxyethylene ether, the metal solution is an Fe aqueous solution, and the mass fraction of the solute is 10.
In this embodiment: the preparation method of the modified active agent comprises the following steps:
weighing hydrogen-containing polysiloxane, octamethylcyclotetrasiloxane and end-capping reagent MM according to a certain proportion, placing the mixture into a three-neck flask, assembling an electric stirrer, a thermometer and a reflux condenser tube with the three-neck flask, then starting heating, and dropwise adding 3% concentrated H in a trickle shape when the temperature reaches 40 DEG C2SO4Maintaining the reaction temperature at 40 ℃, mixing and reacting for 5h, pouring the crude product obtained after the reaction into a separating funnel, standing and separating, taking the upper layer liquid, adding a small amount of NaHCO for multiple times3And (3) stirring the powder continuously, fully reacting for 1h to obtain an active agent with the pH value of 6, performing suction filtration, and performing reduced pressure distillation to remove low-boiling-point substances to obtain the required modified active agent.
In this embodiment: the ratio of the hydrogenpolysiloxane, the octamethylcyclotetrasiloxane and the end-capping reagent MM is 1:0.2: 0.7.
In this embodiment: the auxiliary agent is graphite and Cu2A mixture of O.
In this embodiment: the graphite and Cu2The mixing ratio of O is 1: 1.3.
Example 8:
the preferred embodiment of the invention provides a preparation process of nanometer magnetic powder, which comprises the following steps;
step 1: mixing the magnetic metal ion solution with the network structure powder, stirring at 88 ℃ for 12min, and drying to obtain a magnetic metal composition;
step 2: putting the magnetic metal composition into an inorganic solvent, uniformly adding an alcoholic solution of distilled water while stirring, and controlling the pH value to be 6 to obtain a hard gel precursor;
and step 3: heating the hard gel precursor to 275 ℃, introducing hydrogen, continuing for 1.5h, and then spraying cold water mist to cool the hard gel precursor in 7min to obtain composite powder;
and 4, step 4: adding a modifying active agent and an auxiliary agent into a metal solution containing an emulsifier, stirring for 4min, and drying to obtain alloy magnetic powder;
and 5: heating the alloy magnetic powder to 275 ℃, introducing hydrogen, continuing for 1.5h, and then spraying cold water mist to cool the alloy magnetic powder within 7min to obtain the nano magnetic powder.
In this embodiment: the nanometer magnetic powder comprises the following raw materials in parts by weight:
80 parts of magnetic metal ion solution;
10 parts of network structure powder;
90 parts of an inorganic solvent;
30 parts of an alcohol solution of distilled water;
65 parts of a metal solution containing an emulsifier;
3 parts of a modifying active agent;
and 5 parts of an auxiliary agent.
In this embodiment: the magnetic metal ion solution is a Co aqueous solution, and the mass fraction of the solute is 12%.
In this embodiment: the network structure is AL2O3。
In this embodiment: the inorganic solvent is a mixture of liquid sulfur dioxide and sulfuryl chloride.
In this embodiment: the ratio of the emulsifier to the metal solution in the metal solution containing the emulsifier is 1:16, the emulsifier is fatty amine polyoxyethylene ether, the metal solution is a Co aqueous solution, and the mass fraction of the solute is 12%.
In this embodiment: the preparation method of the modified active agent comprises the following steps:
weighing hydrogen-containing polysiloxane, octamethylcyclotetrasiloxane and end-capping reagent MM according to a proportion, placing the hydrogen-containing polysiloxane, octamethylcyclotetrasiloxane and end-capping reagent MM into a three-neck flask, assembling an electric stirrer, a thermometer and a reflux condenser tube with the three-neck flask, then starting heating, maintaining the reaction temperature within 42 ℃, mixing and reacting for 5.5 hours, pouring a crude product obtained after reaction into a separating funnel, standing and separating, taking an upper layer of liquid, adding a small amount of NaHCO for multiple times, and adding a small amount of NaHCO into the3And (3) stirring the powder continuously, fully reacting for 1h to obtain an active agent with the pH value of 7, performing suction filtration, and performing reduced pressure distillation to remove low-boiling-point substances to obtain the required modified active agent.
In this embodiment: the ratio of the hydrogenpolysiloxane, the octamethylcyclotetrasiloxane and the end-capping reagent MM is 1:0.3: 0.6.
In this embodiment: the auxiliary agent is graphite and Cu2A mixture of O.
In this embodiment: the graphite and Cu2The mixing ratio of O is 1: 1.4.
Example 9:
the preferred embodiment of the invention provides a preparation process of nanometer magnetic powder, which comprises the following steps;
step 1: mixing the magnetic metal ion solution with the network structure powder, stirring for 15min at 90 ℃, and then drying to obtain a magnetic metal composition;
step 2: putting the magnetic metal composition into an inorganic solvent, uniformly adding an alcoholic solution of distilled water while stirring, and controlling the pH value to be 7 to obtain a hard gel precursor;
and step 3: heating the hard gel precursor to 280 ℃, introducing hydrogen, continuing for 2 hours, and then spraying cold water mist to cool the hard gel precursor in 8min to obtain composite powder;
and 4, step 4: adding a modifying active agent and an auxiliary agent into a metal solution containing an emulsifier, stirring for 5min, and drying to obtain alloy magnetic powder;
and 5: heating the alloy magnetic powder to 280 ℃, introducing hydrogen, continuing for 2 hours, and then spraying cold water mist to cool the alloy magnetic powder in 8min to obtain the nano magnetic powder.
In this embodiment: the nanometer magnetic powder comprises the following raw materials in parts by weight:
90 parts of magnetic metal ion solution;
10 parts of network structure powder;
100 parts of an inorganic solvent;
35 parts of an alcoholic solution of distilled water;
75 parts of metal solution containing an emulsifier;
5 parts of a modifying active agent;
and 7 parts of an auxiliary agent.
In this embodiment: the magnetic metal ion solution is a Ni aqueous solution, and the mass fraction of the solute is 13%.
In this embodiment: the network structure is polymethyl methacrylate.
In this embodiment: the inorganic solvent is a mixture of liquid sulfur dioxide and thionyl chloride (thionyl chloride).
In this embodiment: the ratio of the emulsifier to the metal solution in the metal solution containing the emulsifier is 1:17, the emulsifier is fatty amine polyoxyethylene ether, the metal solution is Ni aqueous solution, and the mass fraction of the solute is 13%.
In this embodiment: the preparation method of the modified active agent comprises the following steps:
weighing hydrogen-containing polysiloxane, octamethylcyclotetrasiloxane and end-capping reagent MM according to a certain proportion, placing the mixture into a three-neck flask, assembling an electric stirrer, a thermometer and a reflux condenser tube with the three-neck flask, then starting heating, and dropwise adding 3% concentrated H in a trickle shape when the temperature reaches 40 DEG C2SO4Maintaining the reaction temperature at 45 ℃, mixing and reacting for 6h, pouring the crude product obtained after the reaction into a separating funnel, standing and separating, taking the upper layer liquid, adding a small amount of NaHCO for multiple times3And (3) stirring the powder continuously, fully reacting for 1h to obtain an active agent with the pH value of 7, performing suction filtration, and performing reduced pressure distillation to remove low-boiling-point substances to obtain the required modified active agent.
In this embodiment: the ratio of the hydrogen-containing polysiloxane, the octamethylcyclotetrasiloxane and the end-capping reagent MM is 1:1: 1.
In this embodiment: the auxiliary agent is graphite and Cu2A mixture of O.
In this embodiment: the graphite and Cu2The mixing ratio of O is 1: 1.5.
Example 10:
the preferred embodiment of the invention provides a preparation process of nanometer magnetic powder, which comprises the following steps;
step 1: mixing the magnetic metal ion solution with the network structure powder, stirring at 85 ℃ for 10min, and drying to obtain a magnetic metal composition;
step 2: putting the magnetic metal composition into an inorganic solvent, uniformly adding an alcoholic solution of distilled water while stirring, and controlling the pH value to be 6 to obtain a hard gel precursor;
and step 3: heating the hard gel precursor to 250 ℃, introducing hydrogen, continuing for 1h, and then spraying cold water mist to cool the hard gel precursor within 6min to obtain composite powder;
and 4, step 4: adding a modifying active agent and an auxiliary agent into a metal solution containing an emulsifier, stirring for 3min, and drying to obtain alloy magnetic powder;
and 5: heating the alloy magnetic powder to 250 ℃, introducing hydrogen, continuing for 1h, and then spraying cold water mist to cool the alloy magnetic powder within 6min to obtain the nano magnetic powder.
In this embodiment: the nanometer magnetic powder comprises the following raw materials in parts by weight:
75 parts of magnetic metal ion solution;
15 parts of network structure powder;
100 parts of an inorganic solvent;
20 parts of an alcoholic solution of distilled water;
75 parts of metal solution containing an emulsifier;
5 parts of a modifying active agent;
and 9 parts of an auxiliary agent.
In this embodiment: the magnetic metal ion solution is an Fe aqueous solution, and the mass fraction of the solute is 10%.
In this embodiment: the network structure body is SiO2。
In this embodiment: the inorganic solvent is liquid sulfur dioxide.
In this embodiment: the ratio of the emulsifier to the metal solution in the metal solution containing the emulsifier is 1:15, the emulsifier is fatty alcohol-polyoxyethylene ether, the metal solution is an Fe aqueous solution, and the mass fraction of the solute is 10.
In this embodiment: the preparation method of the modified active agent comprises the following steps:
weighing hydrogen-containing polysiloxane, octamethylcyclotetrasiloxane and end-capping reagent MM according to a certain proportion, placing the mixture into a three-neck flask, assembling an electric stirrer, a thermometer and a reflux condenser tube with the three-neck flask, then starting heating, and dropwise adding 3% concentrated H in a trickle shape when the temperature reaches 40 DEG C2SO4Maintaining the reaction temperature at 40 ℃, mixing and reacting for 5h, pouring the crude product obtained after the reaction into a separating funnel, standing and separating, taking the upper layer liquid, adding a small amount of NaHCO for multiple times3Stirring the powder continuously, reacting for 1 hr to obtain pH 6 activator, vacuum filtering, and distilling under reduced pressure to remove low-boiling-point substancesObtaining the required modified active agent.
In this embodiment: the ratio of the hydrogenpolysiloxane, the octamethylcyclotetrasiloxane and the end-capping reagent MM is 1:0.2: 0.7.
In this embodiment: the auxiliary agent is Cu2O。
In this embodiment: the graphite and Cu2The mixing ratio of O is 1: 1.3.
Example 11:
the preferred embodiment of the invention provides a preparation process of nanometer magnetic powder, which comprises the following steps;
step 1: mixing the magnetic metal ion solution with the network structure powder, stirring at 88 ℃ for 12min, and drying to obtain a magnetic metal composition;
step 2: putting the magnetic metal composition into an inorganic solvent, uniformly adding an alcoholic solution of distilled water while stirring, and controlling the pH value to be 6 to obtain a hard gel precursor;
and step 3: heating the hard gel precursor to 275 ℃, introducing hydrogen, continuing for 1.5h, and then spraying cold water mist to cool the hard gel precursor in 7min to obtain composite powder;
and 4, step 4: adding a modifying active agent and an auxiliary agent into a metal solution containing an emulsifier, stirring for 4min, and drying to obtain alloy magnetic powder;
and 5: heating the alloy magnetic powder to 275 ℃, introducing hydrogen, continuing for 1.5h, and then spraying cold water mist to cool the alloy magnetic powder within 7min to obtain the nano magnetic powder.
In this embodiment: the nanometer magnetic powder comprises the following raw materials in parts by weight:
80 parts of magnetic metal ion solution;
10 parts of network structure powder;
90 parts of an inorganic solvent;
30 parts of an alcohol solution of distilled water;
65 parts of a metal solution containing an emulsifier;
3 parts of a modifying active agent;
and 5 parts of an auxiliary agent.
In this embodiment: the magnetic metal ion solution is a Co aqueous solution, and the mass fraction of the solute is 12%.
In this embodiment: the network structure is AL2O3。
In this embodiment: the inorganic solvent is a mixture of liquid sulfur dioxide and sulfuryl chloride.
In this embodiment: the ratio of the emulsifier to the metal solution in the metal solution containing the emulsifier is 1:16, the emulsifier is fatty amine polyoxyethylene ether, the metal solution is a Co aqueous solution, and the mass fraction of the solute is 12%.
In this embodiment: the preparation method of the modified active agent comprises the following steps:
weighing hydrogen-containing polysiloxane, octamethylcyclotetrasiloxane and end-capping reagent MM according to a certain proportion, placing the mixture into a three-neck flask, assembling an electric stirrer, a thermometer and a reflux condenser tube with the three-neck flask, then starting heating, and dropwise adding 3% concentrated H in a trickle shape when the temperature reaches 40 DEG C2SO4Keeping the reaction temperature within 42 ℃, mixing and reacting for 5.5h, pouring the crude product obtained after the reaction into a separating funnel, standing and separating, taking the upper layer liquid, adding a small amount of NaHCO for multiple times3And (3) stirring the powder continuously, fully reacting for 1h to obtain an active agent with the pH value of 7, performing suction filtration, and performing reduced pressure distillation to remove low-boiling-point substances to obtain the required modified active agent.
In this embodiment: the ratio of the hydrogenpolysiloxane, the octamethylcyclotetrasiloxane and the end-capping reagent MM is 1:0.3: 0.6.
In this embodiment: the auxiliary agent is graphite and Cu2A mixture of O.
In this embodiment: the graphite and Cu2The mixing ratio of O is 1: 0.8.
Comparative example 1:
compared with example 1, the nano-magnetic powder in comparative example 1 does not contain a modifying active agent under the condition that other conditions are not changed.
Comparative example 2:
compared with example 1, the nano-magnetic powder in comparative example 1 contains no auxiliary agent under otherwise unchanged conditions.
The inventors conducted a particle size test using a laser particle sizer on the nano-magnetic powders of examples 1 to 11 and comparative examples 1 to 2, and conducted a polarization performance test using the respective inductors, and the test results are as follows:
| particle size (nm) | Polarization current (mA cm-2) | |
| Example 1 | 45 | 150 |
| Example 2 | 48 | 156 |
| Example 3 | 47 | 151 |
| Example 4 | 80 | 133 |
| Example 5 | 150 | 130 |
| Example 6 | 123 | 140 |
| Example 7 | 96 | 115 |
| Example 8 | 136 | 134 |
| Example 9 | 130 | 145 |
| Example 10 | 159 | 124 |
| Example 11 | 253 | 136 |
| Comparative example 1 | 458 | 98 |
| Comparative example 2 | 189 | 73 |
As can be seen from the data in the above table, the nano-magnetic powders prepared in examples 1 to 11 provided by the present invention are superior to those prepared in comparative examples 1 to 2 in terms of particle size and electrical conductivity, particularly, superior in examples 1 to 3.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. A preparation process of nanometer magnetic powder is characterized in that: the preparation method comprises the following steps;
step 1: mixing the magnetic metal ion solution and the network structure powder, stirring at 85-90 ℃ for 10-15min, and drying to obtain a magnetic metal composition;
step 2: putting the magnetic metal composition into an inorganic solvent, uniformly adding an alcoholic solution of distilled water while stirring, and controlling the pH value to be 6-7 to obtain a hard gel precursor;
and step 3: heating the hard gel precursor to 250-280 ℃, introducing hydrogen, continuing for 1-2h, and then spraying cold water mist to cool the hard gel precursor within 6-8min to obtain composite powder;
and 4, step 4: adding a modifying active agent and an auxiliary agent into a metal solution containing an emulsifier, stirring for 3-5min, and drying to obtain alloy magnetic powder;
and 5: heating the alloy magnetic powder to 250-280 ℃, introducing hydrogen, continuing for 1-2h, and then spraying cold water mist to cool the alloy magnetic powder within 6-8min to obtain the nano magnetic powder.
2. The process for preparing nano-magnetic powder according to claim 1, wherein: the nanometer magnetic powder comprises the following raw materials in parts by weight:
75-90 parts of magnetic metal ion solution;
10-15 parts of network structure powder;
80-110 parts of an inorganic solvent;
20-35 parts of an alcohol solution of distilled water;
60-75 parts of metal solution containing an emulsifier;
3-5 parts of a modifying active agent;
4-9 parts of an auxiliary agent.
3. The process for preparing nano-magnetic powder according to claim 1, wherein: the magnetic metal ion solution is any one of water solution of Fe, Co and Ni, and the mass fraction of solute is 10-13%.
4. The process for preparing nano-magnetic powder according to claim 1, wherein: the network structure body is SiO2、AL2O3MgO, and polymethyl methacrylate.
5. The process for preparing nano-magnetic powder according to claim 1, wherein: the inorganic solvent is one or a mixture of more of liquid sulfur dioxide, thionyl chloride (di) chloride (thionyl chloride) and sulfuryl chloride.
6. The process for preparing nano-magnetic powder according to claim 1, wherein: the ratio of the emulsifier to the metal solution in the metal solution containing the emulsifier is 1:15-17, the emulsifier is fatty alcohol-polyoxyethylene ether or fatty amine-polyoxyethylene ether, the metal solution is an aqueous solution of any one of Fe, Co and Ni, and the mass fraction of the solute is 10% -13%.
7. The process for preparing nano-magnetic powder according to claim 1, wherein: the preparation method of the modified active agent comprises the following steps:
weighing hydrogen-containing polysiloxane, octamethylcyclotetrasiloxane and end-capping reagent MM according to a certain proportion, placing the mixture into a three-neck flask, assembling an electric stirrer, a thermometer and a reflux condenser tube with the three-neck flask, then starting heating, and dropwise adding 3% concentrated H in a trickle shape when the temperature reaches 40 DEG C2SO4Maintaining the reaction temperature within 40-45 deg.C, mixing and reacting for 5-6h, pouring the crude product obtained after reaction into separating funnel, standing for separating liquid, collecting the upper layer liquid, adding NaHCO for several times3And (3) stirring the powder continuously, fully reacting for 1h to obtain an active agent with the pH value of 6-7, performing suction filtration, and performing reduced pressure distillation to remove low-boiling-point substances to obtain the required modified active agent.
8. The process for preparing nano-magnetic powder according to claim 7, wherein: the ratio of the hydrogenpolysiloxane, the octamethylcyclotetrasiloxane and the end-capping reagent MM is 1:0.2-0.4: 0.5-0.7.
9. The process for preparing nano-magnetic powder according to claim 1, wherein: the auxiliary agent is graphite and Cu2A mixture of O.
10. The process for preparing nano-magnetic powder according to claim 9, characterized in that: the graphite and Cu2The mixing ratio of O is 1: 1.3-1.5.
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