CN105906330B - A kind of neodymium iron boron superfine powder sintering magazine and preparation method thereof - Google Patents
A kind of neodymium iron boron superfine powder sintering magazine and preparation method thereof Download PDFInfo
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- CN105906330B CN105906330B CN201610271944.1A CN201610271944A CN105906330B CN 105906330 B CN105906330 B CN 105906330B CN 201610271944 A CN201610271944 A CN 201610271944A CN 105906330 B CN105906330 B CN 105906330B
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
- C04B41/5031—Alumina
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3826—Silicon carbides
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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Abstract
A kind of neodymium iron boron superfine powder sintering magazine provided by the invention and production method, belong to injection molding applied technical field, which is made by raw material:Corundum, alumina, graphene, silicon carbide, amphene, liquid phenolic resin, silane coupling agent, antioxidant, absolute ethyl alcohol and release layer.The neodymium iron boron superfine powder sintering magazine that the present invention makes has the performance that high temperature resistant, cold-resistant thermal shock, impermeable, chemical property are stablized, simultaneously one layer of release layer is coated in the inner wall of the sintering magazine, so that in neodymium iron boron superfine powder removal process, release layer will not only penetrate into NdFeB material, but also superfine powder alloy can be made rapidly to be detached from sintering magazine;And the release layer may be reused, and save cost.
Description
Technical field
The invention belongs to injection molding applied technical field more particularly to a kind of neodymium iron boron superfine powder sintering magazine and its making sides
Method.
Background technology
Neodymium iron boron is world today's rare earth permanent-magnetic material with fastest developing speed.With internal and international to NdFeB material demand
Rapid growth, thereby produce the recycling problem of iron boron magnet waste material by the emperor himself.Do neodymium iron boron magnetic body waste material well to the maximum extent
Comprehensive utilization does environmental protection well, improves warp for saving resource, implementing scientific development view, construction economizing type harmonious society
It helps benefit, plays the role of very positive, be the new class that we should draw attention during doing circular economy well
Topic.
Neodymium iron boron magnetic body waste material and the composition of neodymium iron boron magnetic body device are almost the same, substantially by 30% or so rare earth (with
Based on neodymium, remaining is praseodymium, gadolinium, holmium, terbium, dysprosium etc.), 60% or more iron, remainder is micro- (boron, aluminium, copper, niobium etc.).And
The superfine powder Rare-Earth Content that airflow milling generates is up to 70% or more, and value is far above normal neodymium iron boron product.
Neodymium iron boron industry superfine powder ratio accounts for 1% of normal volume or more at present, and traditional recovery method needs will be ultra-fine
Powder completely burned in air, is collected by the waste recovery enterprise other than generation superfine powder, is detached by series of rare earth
Method be recycled, process flow is more, equipment input cost is high, the rate of recovery is low, cannot achieve ultra-fine to neodymium iron boron
Trace element (such as B, Cu, Al, Nb) in powder is efficiently used.For occurring converting neodymium iron boron superfine powder in the recent period
The method that superfine powder alloy recycles, in sintering process, using traditional irony sintering magazine be easy in the high temperature process with
Fusion, metaboly occur for superfine powder, cause superfine powder alloy to be sintered magazine with irony and are difficult to be detached from after the cooling period;And use stone
The sintering magazine of black material is easy to be permeated by superfine powder during sintering high temperature, and fusion phenomenon occurs, leads to superfine powder alloy
It is difficult to be detached from after the cooling period with graphite material sintering magazine, a large amount of carbons but will be brought into, be not easy to the sharp again of superfine powder alloy
With.
Invention content
In order to solve the above technical problems, the present invention provides a kind of neodymium iron boron superfine powders to be sintered magazine and preparation method thereof.
The present invention is achieved by the following technical programs.
A kind of neodymium iron boron superfine powder provided by the invention is sintered magazine, which is made by the raw material of following parts by weight
It forms:50~100 parts of corundum, 20~30 parts of alumina, 3~6 parts of graphene, 3~6 parts of silicon carbide, 1~3 part of amphene, liquid phenolic
5~15 parts of resin, 3~8 parts of silane coupling agent, antioxidant are 0.1~1 part, 15~30 parts of absolute ethyl alcohol.
Further, the silane coupling agent is in vinyl silanes, amino silane, methacryloxypropyl silane
It is at least one.
Further, the antioxidant 1010 and irgasfos 168 are according to 1:3 ratio mixes.
Further, 70 parts of corundum, 25 parts of alumina, 4 parts of graphene, 5 parts of silicon carbide, 2 parts of amphene, liquid phenolic resin 10
Part, 6 parts of silane coupling agent, antioxidant are 0.5 part, 25 parts of absolute ethyl alcohol.
Meanwhile the present invention also provides the production method that a kind of neodymium iron boron superfine powder is sintered magazine, including the following steps:
1) corundum, alumina are ground into 200~500 mesh powders, then proportionally weigh corundum jade, alumina, graphite
Alkene, silicon carbide, amphene, antioxidant are uniformly mixed, for use by 1800~2000r/min of high-speed mixer, 30~40min;
2) proportionally take absolute ethyl alcohol, liquid phenolic resin and silane coupling agent in reaction kettle, 70~80 DEG C of constant temperature,
150~250r/min stirs 25~30min;
3) mixture obtained step 1) is added in reaction kettle, and 70~80 DEG C of constant temperature, 150~250r/min stirrings 10~
15min;
4) mold being made according to the size of sintering magazine, the batch mixing that step 3) is obtained imports in mold, pressing mold molding,
It is conserved under 20~30 DEG C of dry environment more than for 24 hours;
5) the molding sintering magazine of step 4) is positioned in 50~65 DEG C of electric kiln dry 10~20h, then
It is positioned in 250~350 DEG C of electric kiln dry 20~40h, obtains sintering magazine.
Further, neodymium iron boron superfine powder sintering magazine inner wall also adheres to one layer of release layer, the release layer by with
The raw material of lower parts by weight is made:20~30 parts of calcium oxide, 3~8 parts of alchlor, 5~8 parts of calcium stearate, silicone oil 2~5
Part, 0.5~1 part of liquid phenolic resin, 10~15 parts of absolute ethyl alcohol;The grain size of the calcium oxide, alchlor, calcium stearate
No more than 0.05mm.
Further, the release layer is made by the raw material of following parts by weight:25 parts of calcium oxide, alchlor 6
Part, 7 parts of calcium stearate, 3 parts of silicone oil, 0.8 part of liquid phenolic resin, 12 parts of absolute ethyl alcohol.
Further, the demoulding layer thickness is no more than 1mm.
Meanwhile the present invention also provides the production method that a kind of neodymium iron boron superfine powder is sintered magazine, including the following steps:
1) corundum, alumina are ground into 200~500 mesh powders, then proportionally weigh corundum jade, alumina, graphite
Alkene, silicon carbide, amphene, antioxidant are uniformly mixed, for use by 1800~2000r/min of high-speed mixer, 30~40min;
2) proportionally take absolute ethyl alcohol, liquid phenolic resin and silane coupling agent in reaction kettle, 70~80 DEG C of constant temperature,
150~250r/min stirs 25~30min;
3) mixture obtained step 1) is added in reaction kettle, and 70~80 DEG C of constant temperature, 150~250r/min stirrings 10~
15min;
4) mold being made according to the size of sintering magazine, the batch mixing that step 3) is obtained imports in mold, pressing mold molding,
It is conserved under 20~30 DEG C of dry environment more than for 24 hours;
5) the molding sintering magazine of step 4) is positioned in 50~65 DEG C of electric kiln dry 10~20h, then
It is positioned in 250~350 DEG C of electric kiln dry 20~40h, obtains sintering magazine;
6) release layer mixes, and calcium oxide, alchlor, calcium stearate are ground into the powder that grain size is no more than 0.05mm,
Then calcium oxide, alchlor, calcium stearate, silicone oil, liquid phenolic resin, absolute ethyl alcohol are proportionally weighed and is put into reaction kettle
In, 70~80 DEG C of constant temperature, 150~250r/min stir 25~30min;
7) release layer sprays, and the batch mixing of slurry step 6) is put into flush coater, and release layer is sprayed to sintering magazine, release layer
Thickness is no more than 1mm;
8) the sintering magazine for being coated with release layer is positioned in 50~65 DEG C of electric kiln dry 10~20h, so
It is positioned in 250~350 DEG C of electric kiln dry 20~40h afterwards, obtains finished product.
The beneficial effects of the present invention are:Neodymium iron boron superfine powder that the present invention makes sintering magazine has high temperature resistant, cold-resistant
The performance that thermal shock, impermeable, chemical property are stablized, while being coated with one layer of release layer in the inner wall of the sintering magazine so that
In neodymium iron boron superfine powder removal process, release layer will not only penetrate into NdFeB material, but also superfine powder alloy can be made quick
Ground is detached from sintering magazine;And the release layer may be reused, and save cost.
Description of the drawings
Fig. 1 is the dimensional structure diagram of the neodymium iron boron superfine powder sintering magazine of the embodiment of the present invention;
Specific implementation mode
Be described further below technical scheme of the present invention, but claimed range be not limited to it is described.
Embodiment one
Present embodiments provide a kind of neodymium iron boron superfine powder sintering magazine, the sintering magazine made by raw material below and
At:Corundum 50kg, alumina 20kg, graphene 3kg, silicon carbide 3kg, amphene 1kg, liquid phenolic resin 5kg, silane coupling agent
3kg, antioxidant 0.1kg, absolute ethyl alcohol 15kg.The silane coupling agent is vinyl silanes, amino silane, metering system
At least one of acyloxy silane;The antioxidant 1010 and irgasfos 168 is according to 1:3 ratio mixes.
The production method of the sintering magazine is:
1) corundum, alumina are ground into 200 mesh powders, then proportionally weigh corundum jade, alumina, graphene, carbon
SiClx, amphene, antioxidant are uniformly mixed, for use by high-speed mixer 1800r/min, 30min;
2) proportionally take absolute ethyl alcohol, liquid phenolic resin and silane coupling agent in reaction kettle, 70 DEG C of constant temperature,
150r/min stirs 25min;
3) mixture for obtaining step 1) is added in reaction kettle, and 70 DEG C of constant temperature, 150r/min stir 10min;
4) mold being made according to the size of sintering magazine, the batch mixing that step 3) is obtained imports in mold, pressing mold molding,
It is conserved under 20 DEG C of dry environment more than for 24 hours;
5) the molding sintering magazine of step 4) is positioned in 50 DEG C of electric kiln dry 10h, is then placed into 250
DEG C electric kiln in dry 20h, obtain sintering magazine.As shown in Figure 1, the size of the sintering magazine be respectively L30cm,
H15cm、W20cm、D1.5cm。
Embodiment two
Present embodiments provide a kind of neodymium iron boron superfine powder sintering magazine, the sintering magazine made by raw material below and
At:Corundum 100kg, alumina 30kg, graphene 6kg, silicon carbide 6kg, amphene 3kg, liquid phenolic resin 15kg, silane coupling agent
8kg, antioxidant 1kg, absolute ethyl alcohol 30kg.The silane coupling agent is vinyl silanes, amino silane, methacryl
At least one of oxysilane;The antioxidant 1010 and irgasfos 168 is according to 1:3 ratio mixes.
The production method of the sintering magazine is:
1) corundum, alumina are ground into 500 mesh powders, then proportionally weigh corundum jade, alumina, graphene, carbon
SiClx, amphene, antioxidant are uniformly mixed, for use by high-speed mixer 2000r/min, 40min;
2) proportionally take absolute ethyl alcohol, liquid phenolic resin and silane coupling agent in reaction kettle, 80 DEG C of constant temperature,
250r/min stirs 30min;
3) mixture for obtaining step 1) is added in reaction kettle, and 80 DEG C of constant temperature, 250r/min stir 15min;
4) mold being made according to the size of sintering magazine, the batch mixing that step 3) is obtained imports in mold, pressing mold molding,
It is conserved under 30 DEG C of dry environment more than for 24 hours;
5) the molding sintering magazine of step 4) is positioned in 65 DEG C of electric kiln dry 20h, is then placed into 350
DEG C electric kiln in dry 40h, obtain sintering magazine.As shown in Figure 1, the size of the sintering magazine be respectively L30cm,
H15cm、W20cm、D1.5cm。
Embodiment three
Present embodiments provide a kind of neodymium iron boron superfine powder sintering magazine, the sintering magazine made by raw material below and
At:Corundum 70kg, alumina 25kg, graphene 4kg, silicon carbide 5kg, amphene 2kg, liquid phenolic resin 10kg, silane coupling agent
6kg, antioxidant 0.5kg, absolute ethyl alcohol 25kg.The silane coupling agent is vinyl silanes, amino silane, metering system
At least one of acyloxy silane;The antioxidant 1010 and irgasfos 168 is according to 1:3 ratio mixes.
The production method of the sintering magazine is:
1) corundum, alumina are ground into 400 mesh powders, then proportionally weigh corundum jade, alumina, graphene, carbon
SiClx, amphene, antioxidant are uniformly mixed, for use by high-speed mixer 1900r/min, 35min;
2) proportionally take absolute ethyl alcohol, liquid phenolic resin and silane coupling agent in reaction kettle, 75 DEG C of constant temperature,
200r/min stirs 28min;
3) mixture for obtaining step 1) is added in reaction kettle, and 75 DEG C of constant temperature, 200r/min stir 12min;
4) mold being made according to the size of sintering magazine, the batch mixing that step 3) is obtained imports in mold, pressing mold molding,
It is conserved under 25 DEG C of dry environment more than for 24 hours;
5) the molding sintering magazine of step 4) is positioned in 55 DEG C of electric kiln dry 15h, is then placed into 300
DEG C electric kiln in dry 30h, obtain sintering magazine.As shown in Figure 1, the size of the sintering magazine be respectively L30cm,
H15cm、W20cm、D1.5cm。
Example IV
Provided in this embodiment, neodymium iron boron superfine powder sintering magazine inner wall also adheres to one layer of release layer, the release layer
It is made by following raw material:Calcium oxide 20kg, alchlor 3kg, calcium stearate 5kg, silicone oil 2kg, liquid phenolic resin
0.5kg, absolute ethyl alcohol 10kg;The calcium oxide, alchlor, calcium stearate grain size be no more than 0.05mm;Other raw materials
With embodiment three.
Its production method be embodiment three step 5) afterwards also have following steps:
6) release layer mixes, and calcium oxide, alchlor, calcium stearate are ground into the powder that grain size is no more than 0.05mm,
Then calcium oxide, alchlor, calcium stearate, silicone oil, liquid phenolic resin, absolute ethyl alcohol are proportionally weighed and is put into reaction kettle
In, 70 DEG C of constant temperature, 150r/min stir 25min;
7) release layer sprays, and the batch mixing of slurry step 6) is put into flush coater, and release layer is sprayed to sintering magazine, release layer
Thickness is no more than 1mm;
8) the sintering magazine for being coated with release layer is positioned in 50 DEG C of electric kiln dry 10h, be then placed into
Dry 20h, obtains finished product in 250 DEG C of electric kiln.
Embodiment five
Provided in this embodiment, neodymium iron boron superfine powder sintering magazine inner wall also adheres to one layer of release layer, the release layer
It is made by following raw material:Calcium oxide 30kg, alchlor 8kg, calcium stearate 8kg, silicone oil 5kg, liquid phenolic resin
1kg, absolute ethyl alcohol 15kg;The calcium oxide, alchlor, calcium stearate grain size be no more than 0.05mm;Other raw materials are same
Embodiment three.
Its production method be embodiment three step 5) afterwards also have following steps:
6) release layer mixes, and calcium oxide, alchlor, calcium stearate are ground into the powder that grain size is no more than 0.05mm,
Then calcium oxide, alchlor, calcium stearate, silicone oil, liquid phenolic resin, absolute ethyl alcohol are proportionally weighed and is put into reaction kettle
In, 80 DEG C of constant temperature, 250r/min stir 30min;
7) release layer sprays, and the batch mixing of slurry step 6) is put into flush coater, and release layer is sprayed to sintering magazine, release layer
Thickness is no more than 1mm;
8) the sintering magazine for being coated with release layer is positioned in 65 DEG C of electric kiln dry 20h, be then placed into
Dry 40h, obtains finished product in 350 DEG C of electric kiln.
Embodiment six
Provided in this embodiment, neodymium iron boron superfine powder sintering magazine inner wall also adheres to one layer of release layer, the release layer
It is made by following raw material:Calcium oxide 25kg, alchlor 6kg, calcium stearate 7kg, silicone oil 3kg, liquid phenolic resin
0.8kg, absolute ethyl alcohol 12kg;Other raw materials are the same as embodiment three.
Its production method be embodiment three step 5) afterwards also have following steps:
6) release layer mixes, and calcium oxide, alchlor, calcium stearate are ground into the powder that grain size is no more than 0.05mm,
Then calcium oxide, alchlor, calcium stearate, silicone oil, liquid phenolic resin, absolute ethyl alcohol are proportionally weighed and is put into reaction kettle
In, 75 DEG C of constant temperature, 290r/min stir 28min;
7) release layer sprays, and the batch mixing of slurry step 6) is put into flush coater, and release layer is sprayed to sintering magazine, release layer
Thickness is no more than 1mm;
8) the sintering magazine for being coated with release layer is positioned in 55 DEG C of electric kiln dry 15h, be then placed into
Dry 30h, obtains finished product in 300 DEG C of electric kiln.
By operation, recycled sinter magnet can easily be split away off from sintering magazine, be sintered de- on magazine
The outer wall of the phenomenon that mold layer falls off without damage, recycled sinter magnet is smooth, no release layer infiltration;The sintering magazine is also undeformed,
Cracking, the generation of metachromatism.
Claims (5)
1. a kind of production method of neodymium iron boron superfine powder sintering magazine, which is characterized in that include the following steps:
1) corundum, alumina are ground into 200~500 mesh powders, then proportionally weigh corundum, alumina, graphene, carbonization
Silicon, amphene, antioxidant are uniformly mixed, for use by 1800~2000r/min of high-speed mixer, 30~40min;
2) proportionally take absolute ethyl alcohol, liquid phenolic resin and silane coupling agent in reaction kettle, 70~80 DEG C of constant temperature, 150
~250r/min stirs 25~30min;
3) mixture obtained step 1) is added in reaction kettle, and 70~80 DEG C of constant temperature, 150~250r/min stirrings 10~
15min;
4) mold being made according to the size of sintering magazine, the batch mixing that step 3) is obtained imports in mold, pressing mold molding, 20~
It is conserved under 30 DEG C of dry environment more than for 24 hours;
5) the molding sintering magazine of step 4) is positioned in 50~65 DEG C of electric kiln dry 10~20h, then placed
Dry 20~40h in 250~350 DEG C of electric kiln, obtains sintering magazine;
6) release layer mixes, and calcium oxide, alundum (Al2O3), calcium stearate is ground into the powder that grain size is no more than 0.05mm, so
Calcium oxide, alundum (Al2O3), calcium stearate, silicone oil, liquid phenolic resin, absolute ethyl alcohol are proportionally weighed afterwards is put into reaction kettle
In, 70~80 DEG C of constant temperature, 150~250r/min stir 25~30min;
7) release layer sprays, and the batch mixing of slurry step 6) is put into flush coater, and release layer, the thickness of release layer are sprayed to sintering magazine
No more than 1mm;
8) the sintering magazine for being coated with release layer is positioned in 50~65 DEG C of electric kiln dry 10~20h, then put
It is placed in 250~350 DEG C of electric kiln dry 20~40h, obtains finished product;
The neodymium iron boron superfine powder is sintered magazine, is made by the raw material of following parts by weight:50~100 parts of corundum, alumina 20
~30 parts, 3~6 parts of graphene, 3~6 parts of silicon carbide, 1~3 part of amphene, 5~15 parts of liquid phenolic resin, silane coupling agent 3~
8 parts, antioxidant be 0.1~1 part, 15~30 parts of absolute ethyl alcohol;
Neodymium iron boron superfine powder sintering magazine inner wall also adheres to one layer of release layer, the release layer by following parts by weight original
Material is made:20~30 parts of calcium oxide, 3~8 parts of alundum (Al2O3), 5~8 parts of calcium stearate, 2~5 parts of silicone oil, liquid phenolic
0.5~1 part of resin, 10~15 parts of absolute ethyl alcohol;The calcium oxide, alundum (Al2O3), calcium stearate grain size be no more than
0.05mm。
2. the production method of neodymium iron boron superfine powder sintering magazine as described in claim 1, it is characterised in that:The silane is even
Connection agent is at least one of vinyl silanes, amino silane, methacryloxypropyl silane.
3. the production method of neodymium iron boron superfine powder sintering magazine as described in claim 1, it is characterised in that:The antioxidant
By antioxidant 1010 and irgasfos 168 according to 1:3 ratio mixes.
4. the production method of neodymium iron boron superfine powder sintering magazine as described in claim 1, which is characterized in that by following parts by weight
Raw material be made:70 parts of corundum, 25 parts of alumina, 4 parts of graphene, 5 parts of silicon carbide, 2 parts of amphene, liquid phenolic resin 10
Part, 6 parts of silane coupling agent, antioxidant are 0.5 part, 25 parts of absolute ethyl alcohol.
5. the production method of neodymium iron boron superfine powder sintering magazine as described in claim 1, it is characterised in that:The release layer
It is made by the raw material of following parts by weight:25 parts of calcium oxide, 6 parts of alundum (Al2O3), 7 parts of calcium stearate, 3 parts of silicone oil, liquid
0.8 part of phenolic resin, 12 parts of absolute ethyl alcohol.
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