CN110451977A - A kind of anode material of lithium battery sintering saggar - Google Patents
A kind of anode material of lithium battery sintering saggar Download PDFInfo
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- CN110451977A CN110451977A CN201910425903.7A CN201910425903A CN110451977A CN 110451977 A CN110451977 A CN 110451977A CN 201910425903 A CN201910425903 A CN 201910425903A CN 110451977 A CN110451977 A CN 110451977A
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B35/64—Burning or sintering processes
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- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D5/00—Supports, screens, or the like for the charge within the furnace
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
- C04B2235/483—Si-containing organic compounds, e.g. silicone resins, (poly)silanes, (poly)siloxanes or (poly)silazanes
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- C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
Abstract
The invention discloses a kind of anode material of lithium battery sintering saggars, including saggar ontology (1), it is placed in the pressing plate (2) of saggar ontology (1) upper end and is placed in the idler wheel (3) of saggar ontology (1) lower end, the saggar ontology (1) is equipped with protrusion (11), clearance fit between the pressing plate (2) and the protrusion (11), the protrusion (11) are expander；Saggar structure of the invention is simple, and the quality for being sintered out is high；The advantages that saggar long service life, high temperature resistant, the thermal shock resistance prepared using method of the invention is good, anticorrosive.
Description
Technical field
The present invention relates to saggar field, in particular to a kind of anode material of lithium battery sintering saggar.
Background technique
Anode material of lithium battery has to pass through the roasting of high temperature kiln, and sintering process must be loaded using saggar, due to lithium
Raw material used by cell positive material can decompose in the synthesis process generates penetrating power and the strong lithia pair of reactivity
The problems such as saggar is corroded, and peeling, dusting easily occurs, the service life of saggar is generally at 16 times or less.For the anti-of saggar
Corrosivity and service life, research and development corrosion resistance is good, production and technology of the saggar of long-life for anode material of lithium battery
Progress has highly important effect.
Need for positive electrode to be fitted into anode material of lithium battery sintering process dedicated saggar push-in sintering furnace in into
Row sintering, saggar is laborious and inconvenient when promoting, and existing saggar connects positive electrode with the atmosphere in sintering furnace
Touching is also not enough, and the quality for the product for causing sintering to come out is not high or performance is uneven.
Summary of the invention
Invention is designed to provide a kind of anode material of lithium battery sintering saggar, solves corrosivity, service life
Problem short, saggar is inconvenient and product quality is not high.
The invention is realized in this way a kind of anode material of lithium battery sintering saggar, including saggar ontology, be placed in it is described
The pressing plate of saggar ontology upper end and the idler wheel for being placed in saggar ontology lower end, the saggar ontology is equipped with protrusion, described
Clearance fit between pressing plate and the protrusion, the protrusion are expander.
A further technical solution of the present invention is: the protrusion is four, the protrusion is evenly distributed in the saggar
On ontology.
A further technical solution of the present invention is: the preparation side of saggar ontology and pressing plate in the lithium battery anode saggar
Method are as follows: as mass fraction, raw material by 50~55% silicon carbide coarse powder, 20~25% carbide fine powders, 5~10% carbon
Powder powder, 10~15% silica powder, 5~8% adhesive polyethylene alcohol and 2%-3% waterborne organic silicon resin group
At the preparation method comprises the following steps:
Step 1: by silicon carbide coarse powder, carbide fine powder, carbon dust powder, silica powder, adhesive polyethylene alcohol and water
Property organic siliconresin add water in masticator kneading at water content be 7~15% plastic pug；
Step 2: by the plastic pug, punch forming is the wet base of required shape in impact molding machine, after drying
Obtain green compact；
Step 3: the raw embryo after drying is placed in sintering furnace, and 1400~1800 DEG C of carbon reductase 12~4 of heating under vacuum are small
When, after be heated to 2200~2800 DEG C of recrystallizations in the case where being passed through nitrogen atmosphere and handle 2~3 hours, obtain sintered body；
Step 4: sintered body is down to room temperature.
A further technical solution of the present invention is: the silicon carbide coarse powder purity is greater than 97%, powder particle size 50~100
Mesh, the carbide fine powder purity are greater than 97%, 350~500 mesh of powder particle size.
A further technical solution of the present invention is: the carbon dust powder purity is not less than 95%, the carbon dust powder is to receive
Rice carbon black N330.
A further technical solution of the present invention is: the silica powder purity is greater than 98%, 150~200 mesh of powder particle size.
A further technical solution of the present invention is: the waterborne organic silicon resin is poly- alkyl organic resin, poly- aryl
Any one in organic siliconresin, polyoxyethylene alkyl aryl base organic siliconresin.
A further technical solution of the present invention is: briquetting pressure is 100~300MPa in the step 2.
A further technical solution of the present invention is: being heated to the heating of 1400~1800 DEG C of carbon thermal reductions in the step 3
Speed is 45~60 DEG C/min, and the heating rate for being heated to 2200~2800 DEG C of recrystallization processing is 70~90 DEG C/min, described
Nitrogen atmosphere is 0.5~1 atmospheric pressure.
A further technical solution of the present invention is: the cooling rate in the step 4 is 20~40 DEG C/min.
Beneficial effects of the present invention: saggar structure of the invention is simple, and the quality for being sintered out is high；Using side of the invention
The advantages that saggar long service life that method prepares, high temperature resistant, good, anticorrosive thermal shock resistance.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of anode material of lithium battery sintering saggar provided by the invention.
Appended drawing reference: 1. saggar ontologies, 2. pressing plates, 3. idler wheels, 11. protrusions.
Specific embodiment
Fig. 1 shows a kind of structural schematic diagram of anode material of lithium battery sintering saggar, including saggar ontology 1, is placed in
The pressing plate 2 of 1 upper end of saggar ontology and the idler wheel 3 for being placed in 1 lower end of saggar ontology, the saggar ontology 1 are equipped with
Protrusion 11, clearance fit between the pressing plate 2 and the protrusion 11, the protrusion 11 are expander；The protrusion 11 is four,
The protrusion 11 is evenly distributed on the saggar ontology 1.
Embodiment one:
In the lithium battery anode saggar saggar ontology 1 and pressing plate 2 the preparation method comprises the following steps: as mass fraction, it is former
Material by 50% silicon carbide coarse powder, 24% carbide fine powder, 6% carbon dust powder, 12% silica powder, 6% adhesive
Polyvinyl alcohol and 2% waterborne organic silicon resin composition, the preparation method comprises the following steps:
Step 1: by silicon carbide coarse powder, carbide fine powder, carbon dust powder, silica powder, adhesive polyethylene alcohol and water
Property organic siliconresin add water in masticator kneading at water content be 7% plastic pug；
Step 2: by the plastic pug, punch forming is the wet base of required shape in impact molding machine, after drying
Obtain green compact；
Step 3: the raw embryo after drying is placed in sintering furnace, 1400 DEG C of carbon reductase 12 hours of heating under vacuum, after logical
Enter to be heated to 2200 DEG C of recrystallizations under nitrogen atmosphere to handle 2 hours, obtains sintered body；
Step 4: sintered body is down to room temperature.
The silicon carbide coarse powder purity is greater than 97%, and 50 mesh of powder particle size, the carbide fine powder purity is greater than 97%, powder
Expect 350 mesh of partial size；The carbon dust powder purity is not less than 95%, and the carbon dust powder is nanometer carbon black N330；The silica
Powder purity is greater than 98%, 150 mesh of powder particle size；The waterborne organic silicon resin is poly- alkyl organic resin；The step 2
Middle briquetting pressure is 100MPa；The heating rate that 1400 DEG C of carbon thermal reductions are heated in the step 3 is 45 DEG C/min, heating
Heating rate to 2200 DEG C of recrystallization processing is 70 DEG C/min, and the nitrogen atmosphere is 0.5 atmospheric pressure；In the step 4
Cooling rate be 20 DEG C/min.
Saggar prepared by the present invention is after firing 523 ternary materials using 130 times, and surface is without peeling, scaling-off, artificial destruction
One layer of dense protective layer of observation side discovery saggar Surface Creation about 0.1mm thickness afterwards, is lithium carbonate, lithium metasilicate through elemental analysis
It is constituted with SiC compound.
Saggar prepared by the present invention is after firing 622 ternary materials using 80 times, and surface is without peeling, scaling-off, artificial destruction
One layer of dense protective layer of observation side discovery saggar Surface Creation about 0.1mm thickness afterwards, is lithium carbonate, lithium metasilicate through elemental analysis
It is constituted with SiC compound.
Saggar prepared by the present invention is after firing 811 ternary materials using 50 times, and surface is without peeling, scaling-off, artificial destruction
One layer of dense protective layer of observation side discovery saggar Surface Creation about 0.1mm thickness afterwards, is lithium carbonate, lithium metasilicate through elemental analysis
It is constituted with SiC compound.
The reason of formation is the lithium salts reaction lithium carbonate and lithium metasilicate due to SiC and alkalinity in longer service life,
Simultaneously because high-purity carborundum has many micropores, these lithium salts generated can penetrate into and firmly be adsorbed on saggar inner surface
On, play the role of preferable anticorrosive, in addition to this, cannot continue to corrode inner surface lower layer height in lithium carbonate and lithium metasilicate
Purity silicon carbide, Li is to saggar internal penetration which can inhibit to react very well again when, to play the role of erosion-resisting.
Embodiment two:
In the lithium battery anode saggar saggar ontology 1 and pressing plate 2 the preparation method comprises the following steps: as mass fraction, it is former
Material by 53% silicon carbide coarse powder, 25% carbide fine powder, 5% carbon dust powder, 10% silica powder, 5% adhesive
Polyvinyl alcohol and 2% waterborne organic silicon resin composition, the preparation method comprises the following steps:
Step 1: by silicon carbide coarse powder, carbide fine powder, carbon dust powder, silica powder, adhesive polyethylene alcohol and water
Property organic siliconresin add water in masticator kneading at water content be 10% plastic pug；
Step 2: by the plastic pug, punch forming is the wet base of required shape in impact molding machine, after drying
Obtain green compact；
Step 3: the raw embryo after drying is placed in sintering furnace, and 1600 DEG C of carbon of heating under vacuum restore 3 hours, after logical
Enter to be heated to 2500 DEG C of recrystallizations under nitrogen atmosphere to handle 2.5 hours, obtains sintered body；
Step 4: sintered body is down to room temperature；The silicon carbide coarse powder purity is greater than 97%, and 75 mesh of powder particle size is described
Carbide fine powder purity is greater than 97%, 400 mesh of powder particle size；The carbon dust powder purity is not less than 95%, the carbon dust powder
For nanometer carbon black N330；The silica powder purity is greater than 98%, 175 mesh of powder particle size；The waterborne organic silicon resin is poly-
Aryl organic siliconresin；Briquetting pressure is 200MPa in the step 2；1600 DEG C of carbon thermal reductions are heated in the step 3
Heating rate be 50 DEG C/min, be heated to 2500 DEG C recrystallization processing heating rate be 80 DEG C/min, the nitrogen atmosphere
For 0.8 atmospheric pressure；Cooling rate in the step 4 is 30 DEG C/min.
Saggar prepared by the present invention is after firing 523 ternary materials using 150 times, and surface is without peeling, scaling-off, artificial destruction
One layer of dense protective layer of observation side discovery saggar Surface Creation about 0.1mm thickness afterwards, is lithium carbonate, lithium metasilicate through elemental analysis
It is constituted with SiC compound.
Saggar prepared by the present invention is after firing 622 ternary materials using 100 times, and surface is without peeling, scaling-off, artificial destruction
One layer of dense protective layer of observation side discovery saggar Surface Creation about 0.1mm thickness afterwards, is lithium carbonate, lithium metasilicate through elemental analysis
It is constituted with SiC compound.
Saggar prepared by the present invention is after firing 811 ternary materials using 60 times, and surface is without peeling, scaling-off, artificial destruction
One layer of dense protective layer of observation side discovery saggar Surface Creation about 0.1mm thickness afterwards, is lithium carbonate, lithium metasilicate through elemental analysis
It is constituted with SiC compound.
The reason of formation is the lithium salts reaction lithium carbonate and lithium metasilicate due to SiC and alkalinity in longer service life,
Simultaneously because high-purity carborundum has many micropores, these lithium salts generated can penetrate into and firmly be adsorbed on saggar inner surface
On, play the role of preferable anticorrosive, in addition to this, cannot continue to corrode inner surface lower layer height in lithium carbonate and lithium metasilicate
Purity silicon carbide, Li is to saggar internal penetration which can inhibit to react very well again when, to play the role of erosion-resisting.
Embodiment three:
In the lithium battery anode saggar saggar ontology 1 and pressing plate 2 the preparation method comprises the following steps: as mass fraction, it is former
Material by 55% silicon carbide coarse powder, 20% carbide fine powder, 6% carbon dust powder, 10% silica powder, 6% adhesive
Polyvinyl alcohol and 3% waterborne organic silicon resin composition, the preparation method comprises the following steps:
Step 1: by silicon carbide coarse powder, carbide fine powder, carbon dust powder, silica powder, adhesive polyethylene alcohol and water
Property organic siliconresin add water in masticator kneading at water content be 15% plastic pug；
Step 2: by the plastic pug, punch forming is the wet base of required shape in impact molding machine, after drying
Obtain green compact；
Step 3: the raw embryo after drying is placed in sintering furnace, 1800 DEG C of heating under vacuum carbon reductase 12 4 hours, after logical
Enter to be heated to 2800 DEG C of recrystallizations under nitrogen atmosphere to handle 3 hours, obtains sintered body；
Step 4: sintered body is down to room temperature.
The silicon carbide coarse powder purity is greater than 97%, and 100 mesh of powder particle size, the carbide fine powder purity is greater than 97%,
500 mesh of powder particle size；The carbon dust powder purity is not less than 95%, and the carbon dust powder is nanometer carbon black N330；The oxidation
Silicon powder purity is greater than 98%, 200 mesh of powder particle size；The waterborne organic silicon resin is polyoxyethylene alkyl aryl base organic siliconresin；It is described
Briquetting pressure is 300MPa in step 2；Be heated in the step 3 1800 DEG C of carbon thermal reductions heating rate be 60 DEG C/
Min, the heating rate for being heated to 2800 DEG C of recrystallization processing is 90 DEG C/min, and the nitrogen atmosphere is 1 atmospheric pressure；The step
Cooling rate in rapid four is 40 DEG C/min.
Saggar prepared by the present invention is after firing 523 ternary materials using 140 times, and surface is without peeling, scaling-off, artificial destruction
One layer of dense protective layer of observation side discovery saggar Surface Creation about 0.1mm thickness afterwards, is lithium carbonate, lithium metasilicate through elemental analysis
It is constituted with SiC compound.
Saggar prepared by the present invention is after firing 622 ternary materials using 90 times, and surface is without peeling, scaling-off, artificial destruction
One layer of dense protective layer of observation side discovery saggar Surface Creation about 0.1mm thickness afterwards, is lithium carbonate, lithium metasilicate through elemental analysis
It is constituted with SiC compound.
Saggar prepared by the present invention is after firing 811 ternary materials using 55 times, and surface is without peeling, scaling-off, artificial destruction
One layer of dense protective layer of observation side discovery saggar Surface Creation about 0.1mm thickness afterwards, is lithium carbonate, lithium metasilicate through elemental analysis
It is constituted with SiC compound.
The reason of formation is the lithium salts reaction lithium carbonate and lithium metasilicate due to SiC and alkalinity in longer service life,
Simultaneously because high-purity carborundum has many micropores, these lithium salts generated can penetrate into and firmly be adsorbed on saggar inner surface
On, play the role of preferable anticorrosive, in addition to this, cannot continue to corrode inner surface lower layer height in lithium carbonate and lithium metasilicate
Purity silicon carbide, Li is to saggar internal penetration which can inhibit to react very well again when, to play the role of erosion-resisting.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of anode material of lithium battery sintering saggar, it is characterised in that: including saggar ontology (1), be placed in the saggar sheet
The pressing plate (2) of body (1) upper end and the idler wheel (3) for being placed in saggar ontology (1) lower end, the saggar ontology (1) are equipped with
Protrusion (11), clearance fit between the pressing plate (2) and the protrusion (11), the protrusion (11) are expander.
2. a kind of anode material of lithium battery sintering saggar according to claim 1, it is characterised in that: the protrusion (11)
It is four, the protrusion (11) is evenly distributed on the saggar ontology (1).
3. a kind of anode material of lithium battery sintering saggar according to claim 1, it is characterised in that: the lithium battery is just
In the saggar of pole saggar ontology (1) and pressing plate (2) the preparation method comprises the following steps: as mass fraction, raw material by 50~55% carbon
SiClx coarse powder, 20~25% carbide fine powders, 5~10% carbon dust powder, 10~15% silica powder, 5~8% bonding
Agent polyvinyl alcohol and 2%-3% waterborne organic silicon resin composition, the preparation method comprises the following steps:
Step 1: by silicon carbide coarse powder, carbide fine powder, carbon dust powder, silica powder, adhesive polyethylene alcohol and aqueous have
Machine silicone resin adds the water plastic pug that kneading is 7~15% at water content in masticator；
Step 2: by the plastic pug in impact molding machine punch forming be required shape wet base, after drying it is raw
Base；
Step 3: the raw embryo after drying is placed in sintering furnace, 1400~1800 DEG C of carbon reductase 12~4 hour of heating under vacuum, after
It is heated to 2200~2800 DEG C of recrystallizations in the case where being passed through nitrogen atmosphere to handle 2~3 hours, obtains sintered body；
Step 4: sintered body is down to room temperature.
4. a kind of anode material of lithium battery sintering saggar according to claim 3, it is characterised in that: the silicon carbide is thick
Powder purity is greater than 97%, and 50~100 mesh of powder particle size, the carbide fine powder purity is greater than 97%, powder particle size 350~500
Mesh.
5. a kind of anode material of lithium battery sintering saggar according to claim 3, it is characterised in that: the carbon dust powder
Purity is not less than 95%, and the carbon dust powder is nanometer carbon black N330.
6. a kind of anode material of lithium battery sintering saggar according to claim 3, it is characterised in that: the silica powder
Purity is greater than 98%, 150~200 mesh of powder particle size.
7. a kind of anode material of lithium battery sintering saggar according to claim 3, it is characterised in that: described aqueous organic
Silicone resin is poly- alkyl organic resin, poly- aryl organic siliconresin, any one in polyoxyethylene alkyl aryl base organic siliconresin.
8. a kind of anode material of lithium battery sintering saggar according to claim 3, it is characterised in that: in the step 2
Briquetting pressure is 100~300MPa.
9. a kind of anode material of lithium battery sintering saggar according to claim 3, it is characterised in that: in the step 3
The heating rate for being heated to 1400~1800 DEG C of carbon thermal reductions is 45~60 DEG C/min, is heated at 2200~2800 DEG C of recrystallizations
The heating rate of reason is 70~90 DEG C/min, and the nitrogen atmosphere is 0.5~1 atmospheric pressure.
10. a kind of anode material of lithium battery sintering saggar according to claim 3, it is characterised in that: the step 4
In cooling rate be 20~40 DEG C/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110759736A (en) * | 2019-11-28 | 2020-02-07 | 沈洋 | Recrystallized silicon carbide sagger and application thereof to burning of lithium battery anode material |
| CN111102844A (en) * | 2019-12-12 | 2020-05-05 | 湖南太子新材料科技有限公司 | Preparation method of sagger for sintering lithium battery positive electrode material |
| CN114161547A (en) * | 2021-12-13 | 2022-03-11 | 湖南太子新材料科技有限公司 | Forming method of sagger for lithium battery positive electrode material |
-
2019
- 2019-05-21 CN CN201910425903.7A patent/CN110451977A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110759736A (en) * | 2019-11-28 | 2020-02-07 | 沈洋 | Recrystallized silicon carbide sagger and application thereof to burning of lithium battery anode material |
| CN111102844A (en) * | 2019-12-12 | 2020-05-05 | 湖南太子新材料科技有限公司 | Preparation method of sagger for sintering lithium battery positive electrode material |
| CN114161547A (en) * | 2021-12-13 | 2022-03-11 | 湖南太子新材料科技有限公司 | Forming method of sagger for lithium battery positive electrode material |
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