CN108962531A - A kind of preparation method mixing manganese cluster molecule base magnetic material - Google Patents
A kind of preparation method mixing manganese cluster molecule base magnetic material Download PDFInfo
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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
- H01F1/42—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of organic or organo-metallic materials, e.g. graphene
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- H—ELECTRICITY
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- 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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Abstract
The invention discloses a kind of preparation methods for mixing manganese cluster molecule base magnetic material, the technique is by manganese cluster nano molecular alloy, silver-colored sulphur nano-cluster molecules, iron oxide, manganese oxide, the magnetic material and barium titanate of zirconium oxide combination, magnesia, magnesium silicate, apatite, the non-magnetic material of siliceous sandstone composition adds tetraethyleneglycol dimethyl ether after wet ball grinding and freeze-drying process respectively, benzyl dichlorosilane, sodium tartrate, calcium benzoate, tricarballylic acid, the raw materials such as stabilizer reaction, then pass through gradient smelting respectively, twin-screw extrusion, mold, liquid nitrogen rapid cooling, freezing solidification, it is dried with nitrogen, high-temperature vapor washing, naturally dry and etc. be prepared mixing manganese cluster molecule base magnetic material.The mixing manganese cluster molecule base magnetic material being prepared, electromagnetic performance is excellent, high frequency, flux density saturation, has preferable temperature stability and mechanical impact property, can satisfy a variety of demands in industry.
Description
Technical field
The present invention relates to this technical fields of electronics new material, are related specifically to a kind of mixing manganese cluster molecule base magnetic material
Preparation method.
Background technique
From 1963, Mclonnel proposes organic compound, and there may be ferromagnetic judgements, and give intermolecular
The mechanism of ferromagnetic exchange even summation from Wickmann in 1967 AT&T Labs synthesize first molecule ferromagnet since, molecule base
Magnet is quickly become the hot spot of research due to its unique property, and has thus opened the prelude of molecule based magnetic materials research.
In recent years, under the promotion of material science and life science, with the molecule containing unpaired electron and its magnetic of molecule aggregate
Property is that the one molecule magnetics of cross discipline of research object enters a booming brand-new period, is become across physics
One of the research frontier the most active of the subjects such as, material science, chemistry and life science.
Metal complex is that magnetic material studies another hot spot at this stage.It is by with coordination mode versatile and flexible
Organic ligand make bridging reagent around metal ion and a kind of compound for being formed.This kind of material has inorganic and organic simultaneously
Material characteristics, as long as our general MOLECULE DESIGNs are reasonable, by assembling different ligands, can regulate and control completely magnet structure and
Property.Research shows that the magnetism of complex mostlys come from the central metallic ions with larger spin S, it can be provided than pure
The magnetism that pure organic material is much better than, such material is the emphasis of molecule based magnetic materials research at this stage.Metal complex magnetic
Property material research field it is very extensive, at present it is known that typical single molecular magnets substantially contain Mn, Fe, V, Cr and one
The cluster compound of other a little metallic elements.The ion unpaired electron of Mn, Fe, V, Cr etc. are more in structure, while there are many different
Valence state can form two kinds of non-magnetic centers in same cluster compound intramolecular, and zero-field splitting effect is also relatively strong, is suitable for forming height certainly
Molecule is revolved, is intended to obtain stronger magnetism.Recently, research finds that four cores or six core manganese single molecular magnets can be used as magnetism
Material, this complex often have very big ground state spin values, make it possible to become a kind of potential molecular-based magnets, very
To may be a kind of nanometer of magneton.However, at present still without one kind all had in electromagnetic performance, stability and mechanical strength compared with
The magnetic material of high target.
Summary of the invention
In order to solve the above-mentioned technical problem, the invention discloses a kind of preparation sides for mixing manganese cluster molecule base magnetic material
Manganese cluster nano molecular is closed the magnetic material that gold, silver sulphur nano-cluster molecules, iron oxide, manganese oxide, zirconium oxide combine by method, the technique
Material and barium titanate, magnesia, magnesium silicate, apatite, siliceous sandstone composition non-magnetic material pass through wet ball grinding and cold respectively
Freeze after being dried and adds tetraethyleneglycol dimethyl ether, benzyl dichlorosilane, sodium tartrate, calcium benzoate, tricarballylic acid, steady
The raw materials such as agent reaction are determined, then respectively by gradient smelting, twin-screw extrusion, mold, liquid nitrogen rapid cooling, freezing solidification, nitrogen
Air-blowing is dry, high-temperature vapor washing, naturally dry and etc. mixing manganese cluster molecule base magnetic material is prepared.It is prepared
Manganese cluster molecule base magnetic material is mixed, electromagnetic performance is excellent, high frequency, flux density saturation, has preferable temperature stability
And mechanical impact property, it can satisfy a variety of demands in industry.
Technical solution: to solve the above-mentioned problems, the invention discloses a kind of systems for mixing manganese cluster molecule base magnetic material
Preparation Method, comprising the following steps:
It (1) will be by 5-8 parts of manganese cluster nano molecular alloy, silver-colored 1-2 parts of sulphur nano-cluster molecules, 2-10 parts of iron oxide, oxidation
3-7 parts of manganese, 1-3 parts of zirconium oxide combination magnetic material mixtures and by 2-5 parts of barium titanate, 4-10 parts of magnesia, magnesium silicate 3-8
Part, 2-10 parts of apatite, 5-12 parts of the siliceous sandstone non-magnetic mixtures formed are uniformly mixed respectively, are separately added into wet type
It is ground in ball mill 10-24 hours, obtained Magnaglo and nonmagnetic powder mixture are sieved sorting respectively；
(2) Magnaglo mixture and nonmagnetic powder mixture that step (1) obtains are carried out at freeze-drying respectively
Reason, obtained magnetic product and non magnetic product are saved backup in -80 DEG C；
(3) by 5-8 parts of tetraethyleneglycol dimethyl ether, 3-8 parts of benzyl dichlorosilane, 5-10 parts of sodium tartrate, calcium benzoate
2-9 parts, 4-11 parts of tricarballylic acid, 2-5 parts of stabilizer, mixing are added to electric arc furnaces, carry out melting reaction, and temperature is increased to
200 DEG C, insulation reaction 30-90 minutes, it is naturally cooling to magnetic products being added after 150 DEG C or less in step (2) and non magnetic
Product is warming up to 220-225 DEG C after mixing evenly, while vacuumizing in electric arc furnaces, sustained response 2-5 hours, is then cooled to
80-85 DEG C, 24-36 hours are kept the temperature, it is spare；
(4) it will be melted, squeezed out to mold in the product injection parallel double-screw extruder of step (3)；
(5) liquid nitrogen is sprayed to the casting of step (4) in freezing chamber, makes its rapid cooling, is then freezed in freezing chamber
Solidification 5-10 hours；
(6) then the freezing casting for taking out step (5) is rinsed with high-temperature vapor then with being dried with nitrogen, is natural
It dries and then packs to get finished product.
Preferably, it is 98:1 that the parameter of wet ball-milling, which is ratio of grinding media to material, in the step (1), and ball-milling medium is ethylene glycol, ball
1500 revs/min of revolving speed of mill.
Preferably, freeze-drying parameter is -30 DEG C of cryogenic temperature in the step (2), freezes pressure 25Pa, cooling time
2 hours.
Preferably, the stabilizer in the step (3) is selected from cadmium 2-ethylhexoate, barium laurate, zinc naphthenate, two laurels
One or more of sour dibutyl tin.
Preferably, the vacuum pressure in the step (3) is 50Pa or less.
Preferably, it is 220-260 DEG C that the double screw extruder parameter in the step (4), which is extruder temperature, screw speed
It is 500 revs/min.
Preferably, the high-temperature vapor temperature in the step (6) is 280-300 DEG C.
Compared with prior art, the present invention has the advantages that:
(1) preparation method of mixing manganese cluster molecule base magnetic material of the invention receives manganese cluster nano molecular conjunction gold, silver sulphur
The magnetic material and barium titanate, magnesia, magnesium silicate, apatite, silicon that rice cluster molecule, iron oxide, manganese oxide, zirconium oxide combine
The non-magnetic material of matter sandstone composition adds tetraethyleneglycol dimethyl ether, benzene after wet ball grinding and freeze-drying process respectively
The raw materials such as dimethyl dichlorosilane (DMCS), sodium tartrate, calcium benzoate, tricarballylic acid, stabilizer reaction, it is then molten by gradient respectively
Refining, twin-screw extrusion, mold, liquid nitrogen rapid cooling, freezing solidify, be dried with nitrogen, high-temperature vapor washing, naturally dry etc. walk
Suddenly mixing manganese cluster molecule base magnetic material is prepared.The mixing manganese cluster molecule base magnetic material being prepared, electromagnetic performance
Excellent, high frequency, has preferable temperature stability and mechanical impact property at flux density saturation, can satisfy a variety of in industry
Demand.
(2) mixing manganese cluster molecule base magnetic material raw material of the invention be easy to get, simple process, be suitable for heavy industrialization transport
With practical.
Specific embodiment
Embodiment 1
It (1) will be by 5 parts of manganese cluster nano molecular alloy, silver-colored 1 part of sulphur nano-cluster molecules, 2 parts of iron oxide, 3 parts of manganese oxide, oxygen
Change the magnetic material mixture of 1 part of zirconium combination and by 2 parts of barium titanate, 4 parts of magnesia, 3 parts of magnesium silicate, 2 parts of apatite, siliceous sand
The non-magnetic mixtures of 5 parts of rock compositions are uniformly mixed respectively, are separately added into wet ball mill and are ground 10 hours, obtain
Magnaglo and nonmagnetic powder mixture are sieved sorting respectively, and it is 98:1, ball milling that wherein the parameter of wet ball-milling, which is ratio of grinding media to material,
Medium is ethylene glycol, 1500 revs/min of rotational speed of ball-mill；
(2) Magnaglo mixture and nonmagnetic powder mixture that step (1) obtains are carried out at freeze-drying respectively
Reason, obtained magnetic product and non magnetic product are saved backup in -80 DEG C, wherein freeze-drying parameter is -30 DEG C of cryogenic temperature,
Freeze pressure 25Pa, cooling time 2 hours；
(3) by 5 parts of tetraethyleneglycol dimethyl ether, 3 parts of benzyl dichlorosilane, 5 parts of sodium tartrate, 2 parts of calcium benzoate, the third three
4 parts of carboxylic acid, 2 parts of cadmium 2-ethylhexoate, mixing are added to electric arc furnaces, carry out melting reaction, and temperature is increased to 200 DEG C, heat preservation
Reaction 30 minutes is added magnetic product and non magnetic product in step (2), stirs evenly after being naturally cooling to 150 DEG C or less
After be warming up to 220-225 DEG C, while being vacuumized in electric arc furnaces, vacuum pressure is 50Pa hereinafter, sustained response 2 hours, is then dropped
Temperature keeps the temperature 24 hours to 80-85 DEG C, spare；
(4) it will be melted, squeezed out to mold in the product injection parallel double-screw extruder of step (3), wherein double spiral shells
Bar extruder parameter is that extruder temperature is 220 DEG C, and screw speed is 500 revs/min；
(5) liquid nitrogen is sprayed to the casting of step (4) in freezing chamber, makes its rapid cooling, is then freezed in freezing chamber
Solidification 5 hours；
(6) then the freezing casting for taking out step (5) is rinsed then with being dried with nitrogen with high-temperature vapor, high temperature
Steam temperature is 280-300 DEG C, and then then naturally dry is packed to get finished product.
Embodiment 2
It (1) will be by 6 parts of manganese cluster nano molecular alloy, silver-colored 1 part of sulphur nano-cluster molecules, 5 parts of iron oxide, 4 parts of manganese oxide, oxygen
Change the magnetic material mixture of 2 parts of zirconium combinations and by 3 parts of barium titanate, 6 parts of magnesia, 5 parts of magnesium silicate, 4 parts of apatite, siliceous sand
The non-magnetic mixtures of 7 parts of rock compositions are uniformly mixed respectively, are separately added into wet ball mill and are ground 15 hours, obtain
Magnaglo and nonmagnetic powder mixture are sieved sorting respectively, and it is 98:1, ball milling that wherein the parameter of wet ball-milling, which is ratio of grinding media to material,
Medium is ethylene glycol, 1500 revs/min of rotational speed of ball-mill；
(2) Magnaglo mixture and nonmagnetic powder mixture that step (1) obtains are carried out at freeze-drying respectively
Reason, obtained magnetic product and non magnetic product are saved backup in -80 DEG C, wherein freeze-drying parameter is -30 DEG C of cryogenic temperature,
Freeze pressure 25Pa, cooling time 2 hours；
(3) by 6 parts of tetraethyleneglycol dimethyl ether, 5 parts of benzyl dichlorosilane, 7 parts of sodium tartrate, 5 parts of calcium benzoate, the third three
6 parts of carboxylic acid, 3 parts of barium laurate, mixing are added to electric arc furnaces, carry out melting reaction, and temperature is increased to 200 DEG C, insulation reaction
50 minutes, magnetic product and non magnetic product in step (2) are added after being naturally cooling to 150 DEG C or less, rises after mixing evenly
Temperature is vacuumized to 220-225 DEG C, while in electric arc furnaces, and vacuum pressure is 50Pa hereinafter, sustained response 3 hours, is then cooled to
80-85 DEG C, 28 hours are kept the temperature, it is spare；
(4) it will be melted, squeezed out to mold in the product injection parallel double-screw extruder of step (3), wherein double spiral shells
Bar extruder parameter is that extruder temperature is 230 DEG C, and screw speed is 500 revs/min；
(5) liquid nitrogen is sprayed to the casting of step (4) in freezing chamber, makes its rapid cooling, is then freezed in freezing chamber
Solidification 6 hours；
(6) then the freezing casting for taking out step (5) is rinsed then with being dried with nitrogen with high-temperature vapor, high temperature
Steam temperature is 280-300 DEG C, and then then naturally dry is packed to get finished product.
Embodiment 3
It (1) will be by 7 parts of manganese cluster nano molecular alloy, silver-colored 2 parts of sulphur nano-cluster molecules, 8 parts of iron oxide, 6 parts of manganese oxide, oxygen
Change the magnetic material mixture of 2 parts of zirconium combinations and by 4 parts of barium titanate, 8 parts of magnesia, 7 parts of magnesium silicate, 9 parts of apatite, siliceous sand
The non-magnetic mixtures of 10 parts of rock compositions are uniformly mixed respectively, are separately added into wet ball mill and are ground 20 hours, obtain
Magnaglo and nonmagnetic powder mixture be sieved respectively sorting, it is 98:1, ball that wherein the parameter of wet ball-milling, which is ratio of grinding media to material,
Grinding media is ethylene glycol, 1500 revs/min of rotational speed of ball-mill；
(2) Magnaglo mixture and nonmagnetic powder mixture that step (1) obtains are carried out at freeze-drying respectively
Reason, obtained magnetic product and non magnetic product are saved backup in -80 DEG C, wherein freeze-drying parameter is -30 DEG C of cryogenic temperature,
Freeze pressure 25Pa, cooling time 2 hours；
(3) by 7 parts of tetraethyleneglycol dimethyl ether, 7 parts of benzyl dichlorosilane, 9 parts of sodium tartrate, 8 parts of calcium benzoate, the third three
9 parts of carboxylic acid, 4 parts of zinc naphthenate, mixing are added to electric arc furnaces, carry out melting reaction, and temperature is increased to 200 DEG C, insulation reaction
70 minutes, magnetic product and non magnetic product in step (2) are added after being naturally cooling to 150 DEG C or less, rises after mixing evenly
Temperature is vacuumized to 220-225 DEG C, while in electric arc furnaces, and vacuum pressure is 50Pa hereinafter, sustained response 4 hours, is then cooled to
80-85 DEG C, 32 hours are kept the temperature, it is spare；
(4) it will be melted, squeezed out to mold in the product injection parallel double-screw extruder of step (3), wherein double spiral shells
Bar extruder parameter is that extruder temperature is 240 DEG C, and screw speed is 500 revs/min；
(5) liquid nitrogen is sprayed to the casting of step (4) in freezing chamber, makes its rapid cooling, is then freezed in freezing chamber
Solidification 8 hours；
(6) then the freezing casting for taking out step (5) is rinsed then with being dried with nitrogen with high-temperature vapor, high temperature
Steam temperature is 280-300 DEG C, and then then naturally dry is packed to get finished product.
Embodiment 4
(1) will by 8 parts of manganese cluster nano molecular alloy, silver-colored 2 parts of sulphur nano-cluster molecules, 10 parts of iron oxide, 7 parts of manganese oxide,
3 parts of zirconium oxide combination magnetic material mixtures and by 5 parts of barium titanate, 10 parts of magnesia, 8 parts of magnesium silicate, 10 parts of apatite, silicon
The non-magnetic mixtures of 12 parts of matter sandstone compositions are uniformly mixed respectively, are separately added into wet ball mill and are ground 24 hours,
Obtained Magnaglo and nonmagnetic powder mixture is sieved sorting respectively, and it is 98 that wherein the parameter of wet ball-milling, which is ratio of grinding media to material:
1, ball-milling medium is ethylene glycol, 1500 revs/min of rotational speed of ball-mill；
(2) Magnaglo mixture and nonmagnetic powder mixture that step (1) obtains are carried out at freeze-drying respectively
Reason, obtained magnetic product and non magnetic product are saved backup in -80 DEG C, wherein freeze-drying parameter is -30 DEG C of cryogenic temperature,
Freeze pressure 25Pa, cooling time 2 hours；
(3) by 8 parts of tetraethyleneglycol dimethyl ether, 8 parts of benzyl dichlorosilane, 10 parts of sodium tartrate, 9 parts of calcium benzoate, third
11 parts of tricarboxylic acids, 5 parts of dibutyl tin dilaurate, mixing are added to electric arc furnaces, carry out melting reaction, and temperature is increased to 200
DEG C, insulation reaction 90 minutes, magnetic product and non magnetic product in step (2) are added after being naturally cooling to 150 DEG C or less, stirs
It is warming up to 220-225 DEG C after mixing uniformly, while being vacuumized in electric arc furnaces, vacuum pressure is 50Pa hereinafter, sustained response 5 hours,
Then it is cooled to 80-85 DEG C, keeps the temperature 36 hours, it is spare；
(4) it will be melted, squeezed out to mold in the product injection parallel double-screw extruder of step (3), wherein double spiral shells
Bar extruder parameter is that extruder temperature is 260 DEG C, and screw speed is 500 revs/min；
(5) liquid nitrogen is sprayed to the casting of step (4) in freezing chamber, makes its rapid cooling, is then freezed in freezing chamber
Solidification 10 hours；
(6) then the freezing casting for taking out step (5) is rinsed then with being dried with nitrogen with high-temperature vapor, high temperature
Steam temperature is 280-300 DEG C, and then then naturally dry is packed to get finished product.
Comparative example 1
It (1) will be by 5 parts of manganese cluster nano molecular alloy, silver-colored 1 part of sulphur nano-cluster molecules, 2 parts of iron oxide, 3 parts of manganese oxide, oxygen
Change the magnetic material mixture of 1 part of zirconium combination and by 2 parts of barium titanate, 4 parts of magnesia, 3 parts of magnesium silicate, 2 parts of apatite, siliceous sand
The non-magnetic mixtures of 5 parts of rock compositions are uniformly mixed respectively, are separately added into wet ball mill and are ground 10 hours, obtain
Magnaglo and nonmagnetic powder mixture are sieved sorting respectively, and it is 98:1, ball milling that wherein the parameter of wet ball-milling, which is ratio of grinding media to material,
Medium is ethylene glycol, 1500 revs/min of rotational speed of ball-mill；
(2) by 5 parts of tetraethyleneglycol dimethyl ether, 3 parts of benzyl dichlorosilane, 5 parts of sodium tartrate, 2 parts of calcium benzoate, the third three
4 parts of carboxylic acid, 2 parts of cadmium 2-ethylhexoate, mixing are added to electric arc furnaces, carry out melting reaction, and temperature is increased to 200 DEG C, heat preservation
Reaction 30 minutes is added magnetic product and non magnetic product in step (1), stirs evenly after being naturally cooling to 150 DEG C or less
After be warming up to 220-225 DEG C, while being vacuumized in electric arc furnaces, vacuum pressure is 50Pa hereinafter, sustained response 2 hours, is then dropped
Temperature keeps the temperature 24 hours to 80-85 DEG C, spare；
(3) it will be melted, squeezed out to mold in the product injection parallel double-screw extruder of step (2), wherein double spiral shells
Bar extruder parameter is that extruder temperature is 220 DEG C, and screw speed is 500 revs/min；
(4) liquid nitrogen is sprayed to the casting of step (3) in freezing chamber, makes its rapid cooling, is then freezed in freezing chamber
Solidification 5 hours；
(5) then the freezing casting for taking out step (4) is rinsed then with being dried with nitrogen with high-temperature vapor, high temperature
Steam temperature is 280-300 DEG C, and then then naturally dry is packed to get finished product.
Comparative example 2
(1) will by 8 parts of manganese cluster nano molecular alloy, silver-colored 2 parts of sulphur nano-cluster molecules, 10 parts of iron oxide, 7 parts of manganese oxide,
3 parts of zirconium oxide combination magnetic material mixtures and by 5 parts of barium titanate, 10 parts of magnesia, 8 parts of magnesium silicate, 10 parts of apatite, silicon
The non-magnetic mixtures of 12 parts of matter sandstone compositions are uniformly mixed respectively, are separately added into wet ball mill and are ground 24 hours,
Obtained Magnaglo and nonmagnetic powder mixture is sieved sorting respectively, and it is 98 that wherein the parameter of wet ball-milling, which is ratio of grinding media to material:
1, ball-milling medium is ethylene glycol, 1500 revs/min of rotational speed of ball-mill；
(2) Magnaglo mixture and nonmagnetic powder mixture that step (1) obtains are carried out at freeze-drying respectively
Reason, obtained magnetic product and non magnetic product are saved backup in -80 DEG C, wherein freeze-drying parameter is -30 DEG C of cryogenic temperature,
Freeze pressure 25Pa, cooling time 2 hours；
(3) by 8 parts of tetraethyleneglycol dimethyl ether, 8 parts of benzyl dichlorosilane, 10 parts of sodium tartrate, 9 parts of calcium benzoate, third
11 parts of tricarboxylic acids, 5 parts of dibutyl tin dilaurate, mixing are added to electric arc furnaces, carry out melting reaction, and temperature is increased to 200
DEG C, insulation reaction 90 minutes, magnetic product and non magnetic product in step (2) are added after being naturally cooling to 150 DEG C or less, stirs
It is warming up to 220-225 DEG C after mixing uniformly, while being vacuumized in electric arc furnaces, vacuum pressure is 50Pa hereinafter, sustained response 5 hours,
Then it is cooled to 80-85 DEG C, keeps the temperature 36 hours, it is spare；
(4) it will be melted, squeezed out to mold in the product injection parallel double-screw extruder of step (3), wherein double spiral shells
Bar extruder parameter is that extruder temperature is 260 DEG C, and screw speed is 500 revs/min；
(5) by the casting of step (4) at room temperature spontaneous curing 10 hours；
(6) it to the casting of step (5), then with being dried with nitrogen, is then rinsed with high-temperature vapor, high-temperature vapor
Temperature is 280-300 DEG C, and then then naturally dry is packed to get finished product.
By the mixing manganese cluster molecule base magnetic material obtained of embodiment 1-4 and comparative example 1-2 carry out respectively magnetic flux density,
Initial permeability, magnetic core consume this several performance tests, and test result is shown in Table 1.
Table 1
| Magnetic flux density gauss | Initial permeability μ i | Magnetic core consumes 25 DEG C | |
| Embodiment 1 | 13700 | 2070 | 360 |
| Embodiment 2 | 13500 | 2160 | 320 |
| Embodiment 3 | 13800 | 2250 | 370 |
| Embodiment 4 | 13700 | 2070 | 340 |
| Comparative example 1 | 6800 | 1260 | 560 |
| Comparative example 2 | 7300 | 1170 | 620 |
Manganese cluster nano molecular is closed gold, silver sulphur nanoclusters by the preparation method of mixing manganese cluster molecule base magnetic material of the invention
The magnetic material and barium titanate, magnesia, magnesium silicate, apatite, siliceous sand that cluster molecule, iron oxide, manganese oxide, zirconium oxide combine
The non-magnetic material of rock composition adds tetraethyleneglycol dimethyl ether, benzyl after wet ball grinding and freeze-drying process respectively
The raw materials such as dichlorosilane, sodium tartrate, calcium benzoate, tricarballylic acid, stabilizer reaction, then respectively by gradient smelting, double
Screw Extrusion, mold, liquid nitrogen rapid cooling, freezing solidify, be dried with nitrogen, high-temperature vapor wash, naturally dry and etc. system
It is standby to obtain mixing manganese cluster molecule base magnetic material.The mixing manganese cluster molecule base magnetic material being prepared, electromagnetic performance is excellent,
High frequency, has preferable temperature stability and mechanical impact property at flux density saturation, can satisfy a variety of demands in industry.
Mixing manganese cluster molecule base magnetic material raw material of the invention is easy to get, simple process, is suitable for heavy industrialization and uses, practicability
By force.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (7)
1. a kind of preparation method for mixing manganese cluster molecule base magnetic material, which comprises the following steps:
It (1) will be by 5-8 parts of manganese cluster nano molecular alloy, silver-colored 1-2 parts of sulphur nano-cluster molecules, 2-10 parts of iron oxide, manganese oxide 3-7
Part, 1-3 part of zirconium oxide combine magnetic material mixtures and by 2-5 parts of barium titanate, 4-10 parts of magnesia, 3-8 parts of magnesium silicate, phosphorus
2-10 parts of lime stone, 5-12 parts of the siliceous sandstone non-magnetic mixtures formed are uniformly mixed respectively, are separately added into wet ball-milling
It is ground in machine 10-24 hours, obtained Magnaglo and nonmagnetic powder mixture are sieved sorting respectively；
(2) Magnaglo mixture and nonmagnetic powder mixture that step (1) obtains are subjected to freeze-drying process respectively, obtained
To magnetic product and non magnetic product save backup in -80 DEG C；
(3) by 5-8 parts of tetraethyleneglycol dimethyl ether, 3-8 parts of benzyl dichlorosilane, 5-10 parts of sodium tartrate, calcium benzoate 2-9
Part, 4-11 parts of tricarballylic acid, 2-5 parts of stabilizer, mixing are added to electric arc furnaces, carry out melting reaction, and temperature is increased to 200
DEG C, insulation reaction 30-90 minutes, magnetic product and non magnetic production in step (2) are added after being naturally cooling to 150 DEG C or less
Object is warming up to 220-225 DEG C after mixing evenly, while vacuumizing in electric arc furnaces, sustained response 2-5 hours, is then cooled to 80-
85 DEG C, 24-36 hours are kept the temperature, it is spare；
(4) it will be melted, squeezed out to mold in the product injection parallel double-screw extruder of step (3)；
(5) liquid nitrogen is sprayed to the casting of step (4) in freezing chamber, makes its rapid cooling, solidification is then freezed in freezing chamber
5-10 hours；
(6) then the freezing casting for taking out step (5) is rinsed, naturally dry then with being dried with nitrogen with high-temperature vapor
Then it packs to get finished product.
2. a kind of preparation method for mixing manganese cluster molecule base magnetic material according to claim 1, which is characterized in that described
It is 98:1 that the parameter of wet ball-milling, which is ratio of grinding media to material, in step (1), and ball-milling medium is ethylene glycol, 1500 revs/min of rotational speed of ball-mill.
3. a kind of preparation method for mixing manganese cluster molecule base magnetic material according to claim 1, which is characterized in that described
Freeze-drying parameter is -30 DEG C of cryogenic temperature in step (2), freezes pressure 25Pa, cooling time 2 hours.
4. a kind of preparation method for mixing manganese cluster molecule base magnetic material according to claim 1, which is characterized in that described
Stabilizer in step (3) is selected from one of cadmium 2-ethylhexoate, barium laurate, zinc naphthenate, dibutyl tin dilaurate
Or it is several.
5. a kind of preparation method for mixing manganese cluster molecule base magnetic material according to claim 1, which is characterized in that described
Vacuum pressure in step (3) is 50Pa or less.
6. a kind of preparation method for mixing manganese cluster molecule base magnetic material according to claim 1, which is characterized in that described
It is 220-260 DEG C that double screw extruder parameter in step (4), which is extruder temperature, and screw speed is 500 revs/min.
7. a kind of preparation method for mixing manganese cluster molecule base magnetic material according to claim 1, which is characterized in that described
High-temperature vapor temperature in step (6) is 280-300 DEG C.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1325901A1 (en) * | 2002-01-04 | 2003-07-09 | Council of Scientific and Industrial Research | An improved process for the preparation of adipic acid |
| CN101591359A (en) * | 2009-04-30 | 2009-12-02 | 广西师范大学 | The synthetic method of basic acetate microporous coordination polymer material |
| CN104086595A (en) * | 2013-04-02 | 2014-10-08 | 西北大学 | Ferromagnetic heptanuclear manganese magnetic cluster compound and preparation method thereof |
| CN106935351A (en) * | 2017-01-17 | 2017-07-07 | 江西伟普科技有限公司 | Nano modification injection molding adhesion magnetic material and preparation method thereof |
| CN107011386A (en) * | 2017-05-19 | 2017-08-04 | 广西师范大学 | A kind of 16 core manganese cluster compounds and its synthetic method and application |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1325901A1 (en) * | 2002-01-04 | 2003-07-09 | Council of Scientific and Industrial Research | An improved process for the preparation of adipic acid |
| CN101591359A (en) * | 2009-04-30 | 2009-12-02 | 广西师范大学 | The synthetic method of basic acetate microporous coordination polymer material |
| CN104086595A (en) * | 2013-04-02 | 2014-10-08 | 西北大学 | Ferromagnetic heptanuclear manganese magnetic cluster compound and preparation method thereof |
| CN106935351A (en) * | 2017-01-17 | 2017-07-07 | 江西伟普科技有限公司 | Nano modification injection molding adhesion magnetic material and preparation method thereof |
| CN107011386A (en) * | 2017-05-19 | 2017-08-04 | 广西师范大学 | A kind of 16 core manganese cluster compounds and its synthetic method and application |
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