CN116178002A - Preparation process of strontium ferrite pre-sintering material - Google Patents
Preparation process of strontium ferrite pre-sintering material Download PDFInfo
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- CN116178002A CN116178002A CN202310223092.9A CN202310223092A CN116178002A CN 116178002 A CN116178002 A CN 116178002A CN 202310223092 A CN202310223092 A CN 202310223092A CN 116178002 A CN116178002 A CN 116178002A
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- strontium ferrite
- sintering
- strontium
- oxide
- ferrite pre
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- 229910052712 strontium Inorganic materials 0.000 title claims abstract description 110
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 109
- 239000000463 material Substances 0.000 title claims abstract description 79
- 238000005245 sintering Methods 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 68
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052729 chemical element Inorganic materials 0.000 claims abstract description 3
- 229910052742 iron Inorganic materials 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims description 55
- 239000002245 particle Substances 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 19
- 238000005496 tempering Methods 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- 238000005266 casting Methods 0.000 claims description 14
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 2
- -1 alicyclic amine Chemical class 0.000 claims description 2
- 150000004982 aromatic amines Chemical class 0.000 claims description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 2
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 229920002647 polyamide Polymers 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 2
- 150000003512 tertiary amines Chemical class 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims 1
- 239000006247 magnetic powder Substances 0.000 description 51
- 238000003723 Smelting Methods 0.000 description 25
- 238000000748 compression moulding Methods 0.000 description 12
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 12
- 238000002074 melt spinning Methods 0.000 description 12
- 238000003756 stirring Methods 0.000 description 11
- 229910017583 La2O Inorganic materials 0.000 description 10
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 10
- 229910052772 Samarium Inorganic materials 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention relates to a preparation process of a strontium ferrite pre-sintering material. The strontium ferrite pre-sintering material is formed by sintering iron oxide, strontium oxide and at least one chemical element of Ce, sm and Co; the permanent magnetic strontium ferrite powder comprises, by mass, 60-75% of iron-containing oxide, 15-23% of strontium-containing oxide, and at least one of Ce, sm and Co. The strontium ferrite pre-sintered material obtained by the invention has higher magnetic performance and high density.
Description
Technical Field
The invention belongs to the technical field of magnetic materials, and particularly relates to a preparation process of a strontium ferrite pre-sintering material.
Background
The permanent magnetic material is an ancient material with modern activity and has wide application field. The conversion of magnetic energy and acoustic energy can be used for manufacturing telephones, sound equipment, speakers and the like; the conversion of magnetic energy and mechanical energy can be used for manufacturing motors, motors and the like; the conversion of magnetic energy and electric energy can be used for manufacturing generators and the like. The device manufactured by the permanent magnetic material has the advantages of high efficiency, energy conservation, cleanness, no pollution, high reliability and the like. The strontium ferrite permanent magnet material is a permanent magnet material with larger demand in the current industrial production.
The production process of the permanent magnetic strontium ferrite material comprises two processes of pre-sintering material production and magnetic piece production. Presintering is one of the important procedures for producing permanent magnetic ferrite by an oxide method, plays an important role in the quality of products, and aims to keep the mixture at a certain temperature for a plurality of hours so as to lead the mixture particles to generate preliminary solid phase reaction and generate partial ferrite. The method has the main effects of reducing the non-uniformity of chemical activity, reducing the shrinkage of sintered products, improving the sintered density of the products, being easy to mold and the like.
Patent 201310233034.0 discloses a permanent magnetic ferrite low-temperature pre-sintering powder, which is sintered at a lower sintering temperature by adding a low-melting sintering aid favorable for improving the low-temperature pre-sintering effect, wherein the magnetic property of the prepared material reaches Br=410+/-10 mt and powder HcJ=320+/-15 kA/m.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and providing a preparation process of strontium ferrite pre-sintered material with excellent magnetic performance.
In order to solve the technical problems, the invention adopts the following technical scheme:
firstly, providing a strontium ferrite pre-sintering material, which is formed by sintering iron oxide, strontium oxide and at least one chemical element of Ce, sm and Co; the strontium ferrite pre-sintering material comprises, by mass, 60-75% of iron-containing oxide, 1-5% of strontium-containing oxide, and at least one of Ce, sm and Co as the rest.
Further, the permanent magnetic strontium ferrite powder comprises, by mass, 60-75% of iron oxide, 15-23% of strontium oxide, 1-5% of Ce or Co and 0.5-2% of Sm.
Further, the iron oxide is one of iron oxide, ferrous oxide and ferroferric oxide, preferably iron oxide.
Further, the oxide of strontium is strontium oxide or strontium carbonate.
The invention also provides a preparation process of the strontium ferrite pre-sintering material, which comprises the following steps:
(1) Uniformly mixing the strontium ferrite pre-sintering material according to the mass ratio, adding lanthanum oxide or aluminum oxide for vacuum smelting, and cooling to obtain a casting sheet;
(2) Grinding the cast sheet into micron-sized fine powder, mixing with a curing agent, pressing for molding, sintering, tempering and cooling.
Further, the temperature is 1400-1600 ℃ and the time is 10-25 min.
Further, the particle size of the fine powder is 0.3 to 0.5 μm.
Further, the curing agent is one selected from aliphatic amine, alicyclic amine, aromatic amine, polyamide, tertiary amine and dicyandiamide.
Further, the sintering mode is as follows: heating the rotary kiln to 1000-1300 ℃ for sintering for 2-3.5 hours, and after quick cooling and air cooling, sintering for 1-2.5 hours at 1100-1350 ℃.
Further, the tempering treatment conditions are as follows: tempering at 1000-1300 deg.c for 0.5-1.5 hr.
The beneficial effects of the invention are as follows: according to the invention, the strontium ferrite pre-sintered material obtained by secondary sintering of the raw materials such as the iron oxide, the strontium oxide and the like has excellent magnetic performance on the premise of meeting the density requirement, so that the market competitiveness of the existing strontium ferrite material is improved.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The point value in the technical scope of the invention is not exhaustive, and the new technical proposal formed by equivalent substitution of single or multiple technical characteristics in the technical proposal of the embodiment is also within the scope of the invention; meanwhile, in all the listed or unrecited embodiments of the present invention, each parameter in the same embodiment represents only one example of the technical scheme (i.e. a feasibility scheme), and no strict coordination and limitation relation exists between each parameter, wherein each parameter can be replaced with each other without violating axiom and the requirement of the present invention, except what is specifically stated.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
It should be noted that the experimental methods used in the following examples are conventional methods unless otherwise specified, and the materials, reagents, etc. used in the following examples are commercially available unless otherwise specified.
Example 1
A preparation process of the strontium ferrite pre-sintering material comprises the following steps:
s1, preparing strontium ferrite magnetic powder, namely Fe2O3 and SrCO 3 The Ce and Sm materials are uniformly mixed in a clean mixer according to the weight percentage of 75 percent to 20 percent to 3 percent to 2 percent to obtain the strontium ferrite magnetic powder.
S2, adding a proper amount of La2O3 material into the strontium ferrite magnetic powder according to the weight percentage ratio of the strontium ferrite magnetic powder to the La2O 3=90:10, and uniformly stirring.
S3, placing the powder into a vacuum rapid hardening melt-spinning furnace for smelting for 15min, wherein the smelting temperature is 1480 ℃, casting and rapidly cooling to obtain cast sheets, processing the cast sheets at 1000 ℃ for 10h to prepare coarse powder, and grinding the coarse powder into fine powder with the average particle size of 0.3-0.5 mu m.
S4, mixing fine powder with the average particle size of 0.3-0.5 mu m with 0.1% dicyandiamide curing agent, carrying out orientation compression molding in a magnetic field with the strength of 3T, heating up a rotary kiln to 1000 ℃ for sintering for 3 hours, carrying out quick cooling air cooling, carrying out secondary sintering at 1300 ℃ for 2 hours, carrying out tempering treatment at 1200 ℃ for 1 hour, and finally cooling to room temperature to obtain the strontium ferrite pre-sintered material.
Example 2
A preparation process of the strontium ferrite pre-sintering material comprises the following steps:
s1, preparing strontium ferrite magnetic powder, namely Fe2O3 and SrCO 3 The Ce and Sm materials are uniformly mixed in a clean mixer according to the weight percentage of 73 to 23 to 3 to 1 to obtain the strontium ferrite magnetic powder.
S2, adding a proper amount of La2O3 material into the strontium ferrite magnetic powder according to the weight percentage ratio of the strontium ferrite magnetic powder to the La2O 3=90:10, and uniformly stirring.
S3, placing the powder into a vacuum rapid hardening melt-spinning furnace for smelting for 15min, wherein the smelting temperature is 1480 ℃, casting and rapidly cooling to obtain cast sheets, processing the cast sheets at 1000 ℃ for 10h to prepare coarse powder, and grinding the coarse powder into fine powder with the average particle size of 0.3-0.5 mu m.
S4, mixing fine powder with the average particle size of 0.3-0.5 mu m with 0.1% dicyandiamide curing agent, carrying out orientation compression molding in a magnetic field with the strength of 3T, heating up a rotary kiln to 1000 ℃ for sintering for 3 hours, carrying out quick cooling air cooling, carrying out secondary sintering at 1300 ℃ for 2 hours, carrying out tempering treatment at 1200 ℃ for 1 hour, and finally cooling to room temperature to obtain the strontium ferrite pre-sintered material.
Example 3
A preparation process of the strontium ferrite pre-sintering material comprises the following steps:
s1, preparing strontium ferrite magnetic powder, namely Fe2O3 and SrCO 3 The Ce and Sm materials are uniformly mixed in a clean mixer according to the weight percentage of 70 to 23 to 5 to 2 percent, so as to obtain the strontium ferrite magnetic powder.
S2, adding a proper amount of La2O3 material into the strontium ferrite magnetic powder according to the weight percentage ratio of the strontium ferrite magnetic powder to the La2O 3=90:10, and uniformly stirring.
S3, placing the powder into a vacuum rapid hardening melt-spinning furnace for smelting for 15min, wherein the smelting temperature is 1480 ℃, casting and rapidly cooling to obtain cast sheets, processing the cast sheets at 1000 ℃ for 10h to prepare coarse powder, and grinding the coarse powder into fine powder with the average particle size of 0.3-0.5 mu m.
S4, mixing fine powder with the average particle size of 0.3-0.5 mu m with 0.1% dicyandiamide curing agent, carrying out orientation compression molding in a magnetic field with the strength of 3T, heating the rotary kiln to 1200 ℃ for sintering for 2.5 hours, carrying out quick cooling air cooling, carrying out secondary sintering for 2 hours at 1300 ℃, carrying out tempering treatment for 1 hour at 1000 ℃, and finally cooling to room temperature to obtain the strontium ferrite pre-sintered material.
Example 4
A preparation process of the strontium ferrite pre-sintering material comprises the following steps:
s1, preparing strontium ferrite magnetic powder, namely Fe2O3 and SrCO 3 The strontium ferrite magnetic powder is obtained by uniformly mixing Co and Sm materials in a clean mixer according to the weight percentage of 75 to 20 to 3 to 2 percent.
S2, adding a proper amount of La2O3 material into the strontium ferrite magnetic powder according to the weight percentage ratio of the strontium ferrite magnetic powder to the La2O 3=90:10, and uniformly stirring.
S3, placing the powder into a vacuum rapid hardening melt-spinning furnace for smelting for 15min, wherein the smelting temperature is 1480 ℃, casting and rapidly cooling to obtain cast sheets, processing the cast sheets at 1000 ℃ for 10h to prepare coarse powder, and grinding the coarse powder into fine powder with the average particle size of 0.3-0.5 mu m.
S4, mixing fine powder with the average particle size of 0.3-0.5 mu m with 0.1% dicyandiamide curing agent, carrying out orientation compression molding in a magnetic field with the strength of 3T, heating up a rotary kiln to 1000 ℃ for sintering for 3 hours, carrying out quick cooling air cooling, carrying out secondary sintering at 1100 ℃ for 2 hours, carrying out tempering treatment at 1000 ℃ for 1 hour, and finally cooling to room temperature to obtain the strontium ferrite pre-sintered material.
Example 5
A preparation process of the strontium ferrite pre-sintering material comprises the following steps:
s1, preparing strontium ferrite magnetic powder, namely Fe2O3 and SrCO 3 The materials Ce and Sm are as followsThe strontium ferrite magnetic powder is obtained by uniformly mixing 75 percent to 20 percent to 3 percent to 2 percent of the components in a clean stirrer.
S2, according to the ratio of strontium ferrite magnetic powder to Al 2 O 3 An appropriate amount of Al is added in a weight percentage ratio of =90:10 2 O 3 The material is added into strontium ferrite magnetic powder and stirred uniformly.
S3, placing the powder into a vacuum rapid hardening melt-spinning furnace for smelting for 15min, wherein the smelting temperature is 1480 ℃, casting and rapidly cooling to obtain cast sheets, processing the cast sheets at 1000 ℃ for 10h to prepare coarse powder, and grinding the coarse powder into fine powder with the average particle size of 0.3-0.5 mu m.
S4, mixing fine powder with the average particle size of 0.3-0.5 mu m with 0.1% dicyandiamide curing agent, carrying out orientation compression molding in a magnetic field with the strength of 3T, heating up a rotary kiln to 1000 ℃ for sintering for 3 hours, carrying out quick cooling air cooling, carrying out secondary sintering at 1300 ℃ for 2 hours, carrying out tempering treatment at 1200 ℃ for 1 hour, and finally cooling to room temperature to obtain the strontium ferrite pre-sintered material.
Example 6
A preparation process of the strontium ferrite pre-sintering material comprises the following steps:
s1, preparing strontium ferrite magnetic powder, namely Fe2O3 and SrCO 3 The Ce and Sm materials are uniformly mixed in a clean mixer according to the weight percentage of 75 percent to 23 percent to 1.5 percent to 0.5 percent, and the strontium ferrite magnetic powder is obtained.
S2, adding a proper amount of La2O3 material into the strontium ferrite magnetic powder according to the weight percentage ratio of the strontium ferrite magnetic powder to the La2O 3=90:10, and uniformly stirring.
S3, placing the powder into a vacuum rapid hardening melt-spinning furnace for smelting for 15min, wherein the smelting temperature is 1480 ℃, casting and rapidly cooling to obtain cast sheets, processing the cast sheets at 1000 ℃ for 10h to prepare coarse powder, and grinding the coarse powder into fine powder with the average particle size of 0.3-0.5 mu m.
S4, mixing fine powder with the average particle size of 0.3-0.5 mu m with 0.1% dicyandiamide curing agent, carrying out orientation compression molding in a magnetic field with the strength of 3T, heating up a rotary kiln to 1000 ℃ for sintering for 3 hours, carrying out quick cooling air cooling, carrying out secondary sintering at 1300 ℃ for 2 hours, carrying out tempering treatment at 1200 ℃ for 1 hour, and finally cooling to room temperature to obtain the strontium ferrite pre-sintered material.
Comparative example 1
The strontium ferrite magnetic powder composition was different compared to example 1.
A preparation process of the strontium ferrite pre-sintering material comprises the following steps:
s1, preparing strontium ferrite magnetic powder, namely Fe2O3 and SrCO 3 、SiO 2 The BaO materials are uniformly mixed in a clean mixer according to the weight percentage of 75 percent to 20 percent to 3 percent to 2 percent to obtain the strontium ferrite magnetic powder.
S2, adding a proper amount of La2O3 material into the strontium ferrite magnetic powder according to the weight percentage ratio of the strontium ferrite magnetic powder to the La2O 3=90:10, and uniformly stirring.
S3, placing the powder into a vacuum rapid hardening melt-spinning furnace for smelting for 15min, wherein the smelting temperature is 1480 ℃, casting and rapidly cooling to obtain cast sheets, processing the cast sheets at 1000 ℃ for 10h to prepare coarse powder, and grinding the coarse powder into fine powder with the average particle size of 0.3-0.5 mu m.
S4, mixing fine powder with the average particle size of 0.3-0.5 mu m with 0.1% dicyandiamide curing agent, carrying out orientation compression molding in a magnetic field with the strength of 3T, heating up a rotary kiln to 1000 ℃ for sintering for 3 hours, carrying out quick cooling air cooling, carrying out secondary sintering at 1300 ℃ for 2 hours, carrying out tempering treatment at 1200 ℃ for 1 hour, and finally cooling to room temperature to obtain the strontium ferrite pre-sintered material.
Comparative example 2
The strontium ferrite magnetic powder composition was different compared to example 1.
A preparation process of the strontium ferrite pre-sintering material comprises the following steps:
s1, preparing strontium ferrite magnetic powder, namely Fe2O3 and SrCO 3 The strontium ferrite magnetic powder is obtained by uniformly mixing the BaO and CaO materials in a clean mixer according to the weight percentage of 75 to 20 to 3 to 2 percent.
S2, adding a proper amount of La2O3 material into the strontium ferrite magnetic powder according to the weight percentage ratio of the strontium ferrite magnetic powder to the La2O 3=90:10, and uniformly stirring.
S3, placing the powder into a vacuum rapid hardening melt-spinning furnace for smelting for 15min, wherein the smelting temperature is 1480 ℃, casting and rapidly cooling to obtain cast sheets, processing the cast sheets at 1000 ℃ for 10h to prepare coarse powder, and grinding the coarse powder into fine powder with the average particle size of 0.3-0.5 mu m.
S4, mixing fine powder with the average particle size of 0.3-0.5 mu m with 0.1% dicyandiamide curing agent, carrying out orientation compression molding in a magnetic field with the strength of 3T, heating up a rotary kiln to 1000 ℃ for sintering for 3 hours, carrying out quick cooling air cooling, carrying out secondary sintering at 1300 ℃ for 2 hours, carrying out tempering treatment at 1200 ℃ for 1 hour, and finally cooling to room temperature to obtain the strontium ferrite pre-sintered material.
Comparative example 3
In step (2) the oxide is different compared to example 1.
A preparation process of the strontium ferrite pre-sintering material comprises the following steps:
s1, preparing strontium ferrite magnetic powder, namely Fe2O3 and SrCO 3 The Ce and Sm materials are uniformly mixed in a clean mixer according to the weight percentage of 75 percent to 20 percent to 3 percent to 2 percent to obtain the strontium ferrite magnetic powder.
S2, adding a proper amount of neodymium oxide material into the strontium ferrite magnetic powder according to the weight percentage ratio of the strontium ferrite magnetic powder to the neodymium oxide=90:10, and uniformly stirring.
S3, placing the powder into a vacuum rapid hardening melt-spinning furnace for smelting for 15min, wherein the smelting temperature is 1480 ℃, casting and rapidly cooling to obtain cast sheets, processing the cast sheets at 1000 ℃ for 10h to prepare coarse powder, and grinding the coarse powder into fine powder with the average particle size of 0.3-0.5 mu m.
S4, mixing fine powder with the average particle size of 0.3-0.5 mu m with 0.1% dicyandiamide curing agent, carrying out orientation compression molding in a magnetic field with the strength of 3T, heating up a rotary kiln to 1000 ℃ for sintering for 3 hours, carrying out quick cooling air cooling, carrying out secondary sintering at 1300 ℃ for 2 hours, carrying out tempering treatment at 1200 ℃ for 1 hour, and finally cooling to room temperature to obtain the strontium ferrite pre-sintered material.
Comparative example 4
In comparison with example 1, only one sintering is carried out.
A preparation process of the strontium ferrite pre-sintering material comprises the following steps:
s1, preparing strontium ferrite magnetic powder, namely Fe2O3 and SrCO 3 The Ce and Sm materials are uniformly mixed in a clean mixer according to the weight percentage of 75 percent to 20 percent to 3 percent to 2 percent to obtain the strontium ferrite magnetic powder.
S2, adding a proper amount of La2O3 material into the strontium ferrite magnetic powder according to the weight percentage ratio of the strontium ferrite magnetic powder to the La2O 3=90:10, and uniformly stirring.
S3, placing the powder into a vacuum rapid hardening melt-spinning furnace for smelting for 15min, wherein the smelting temperature is 1480 ℃, casting and rapidly cooling to obtain cast sheets, processing the cast sheets at 1000 ℃ for 10h to prepare coarse powder, and grinding the coarse powder into fine powder with the average particle size of 0.3-0.5 mu m.
S4, mixing fine powder with the average particle size of 0.3-0.5 mu m with 0.1% dicyandiamide curing agent, carrying out orientation compression molding in a magnetic field with the strength of 3T, heating the rotary kiln to 1000 ℃ for sintering for 3 hours, rapidly cooling, carrying out tempering treatment at 1200 ℃ for 1 hour, and finally cooling to room temperature to obtain the strontium ferrite pre-sintered material.
Comparative example 5
The sintering temperature was too low compared to example 1.
A preparation process of the strontium ferrite pre-sintering material comprises the following steps:
s1, preparing strontium ferrite magnetic powder, namely Fe2O3 and SrCO 3 The Ce and Sm materials are uniformly mixed in a clean mixer according to the weight percentage of 75 percent to 20 percent to 3 percent to 2 percent to obtain the strontium ferrite magnetic powder.
S2, adding a proper amount of La2O3 material into the strontium ferrite magnetic powder according to the weight percentage ratio of the strontium ferrite magnetic powder to the La2O 3=90:10, and uniformly stirring.
S3, placing the powder into a vacuum rapid hardening melt-spinning furnace for smelting for 15min, wherein the smelting temperature is 1480 ℃, casting and rapidly cooling to obtain cast sheets, processing the cast sheets at 1000 ℃ for 10h to prepare coarse powder, and grinding the coarse powder into fine powder with the average particle size of 0.3-0.5 mu m.
S4, mixing fine powder with the average particle size of 0.3-0.5 mu m with 0.1% dicyandiamide curing agent, carrying out orientation compression molding in a magnetic field with the strength of 3T, heating up a rotary kiln to 850 ℃ for sintering for 3 hours, carrying out quick cooling air cooling, carrying out secondary sintering at 960 ℃ for 2 hours, carrying out tempering treatment at 1200 ℃ for 1 hour, and finally cooling to room temperature to obtain the strontium ferrite pre-sintered material.
Comparative example 6
In comparison with example 1, the strontium ferrite magnetic powder lacks Sm.
A preparation process of the strontium ferrite pre-sintering material comprises the following steps:
s1, preparing strontium ferrite magnetic powder, namely Fe2O3 and SrCO 3 The Ce materials are uniformly mixed in a clean mixer according to the weight percentage of 75 to 23 to 2 percent, and the strontium ferrite magnetic powder is obtained.
S2, adding a proper amount of La2O3 material into the strontium ferrite magnetic powder according to the weight percentage ratio of the strontium ferrite magnetic powder to the La2O 3=90:10, and uniformly stirring.
S3, placing the powder into a vacuum rapid hardening melt-spinning furnace for smelting for 15min, wherein the smelting temperature is 1480 ℃, casting and rapidly cooling to obtain cast sheets, processing the cast sheets at 1000 ℃ for 10h to prepare coarse powder, and grinding the coarse powder into fine powder with the average particle size of 0.3-0.5 mu m.
S4, mixing fine powder with the average particle size of 0.3-0.5 mu m with 0.1% dicyandiamide curing agent, carrying out orientation compression molding in a magnetic field with the strength of 3T, heating up a rotary kiln to 1000 ℃ for sintering for 3 hours, carrying out quick cooling air cooling, carrying out secondary sintering at 1300 ℃ for 2 hours, carrying out tempering treatment at 1200 ℃ for 1 hour, and finally cooling to room temperature to obtain the strontium ferrite pre-sintered material.
< Performance detection >)
The strontium ferrite pre-sintered materials obtained in the treatment modes of examples 1 to 6 and comparative examples 1 to 5 were subjected to performance detection by using a NIM-10000 type magnetic performance tester in the mode of patent CN103626485B, and the results are shown in the following table:
the foregoing examples are illustrative only and serve to explain some features of the method of the invention. The appended claims are intended to claim the broadest possible scope and the embodiments presented herein are merely illustrative of selected implementations based on combinations of all possible embodiments. It is, therefore, not the intention of the applicant that the appended claims be limited by the choice of examples illustrating the features of the invention. Some numerical ranges used in the claims also include sub-ranges within which variations in these ranges should also be construed as being covered by the appended claims where possible.
Claims (10)
1. A strontium ferrite pre-sintering material is characterized by being formed by sintering iron oxide, strontium oxide and at least one chemical element of Ce, sm and Co; the strontium ferrite pre-sintering material comprises, by mass, 60-75% of iron-containing oxide, 15-23% of strontium-containing oxide, and at least one of Ce, sm and Co as the rest.
2. The strontium ferrite pre-sintering material according to claim 1, wherein the components and mass percentages of the strontium ferrite pre-sintering material are 60-75% of iron oxide, 15-23% of strontium oxide, 1-5% of Ce or Co and 0.5-2% of Sm.
3. Strontium ferrite pre-sinter according to claim 1 or 2, wherein the iron oxide is one of iron oxide, ferrous oxide, and ferric oxide, preferably iron oxide.
4. A strontium ferrite pre-sinter as claimed in claim 1 or 2, wherein the strontium oxide is strontium oxide or strontium carbonate.
5. The preparation process of the strontium ferrite pre-sintering material is characterized by comprising the following steps of:
(1) Uniformly mixing the strontium ferrite pre-sintering material according to the mass ratio, adding lanthanum oxide or aluminum oxide for vacuum melting, and cooling to obtain a casting sheet;
(2) Grinding the cast sheet into micron-sized fine powder, mixing with a curing agent, pressing for molding, sintering, tempering and cooling.
6. The strontium ferrite pre-sintering process according to claim 1, wherein the vacuum melting conditions are as follows: the temperature is 1400-1600 ℃ and the time is 10-25 min.
7. The process for preparing a strontium ferrite pre-sintering material as set forth in claim 1, wherein the micron-sized fine powder has a particle size of 0.3 to 0.5 μm.
8. The process for preparing a strontium ferrite pre-sintering material as set forth in claim 1, wherein the curing agent is one selected from the group consisting of aliphatic amine, alicyclic amine, aromatic amine, polyamide, tertiary amine and dicyandiamide.
9. The process for preparing a strontium ferrite pre-sintering material according to claim 1, wherein the sintering method comprises the following steps: heating the rotary kiln to 1000-1300 ℃ for sintering for 2-3.5 hours, and after quick cooling and air cooling, sintering for 1-2.5 hours at 1100-1350 ℃.
10. The process for preparing a strontium ferrite pre-sintering material as set forth in claim 1, wherein the tempering treatment conditions are as follows: tempering at 1000-1300 deg.c for 0.5-1.5 hr.
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