CN102914165B - High-stability long-service-life sagger for roasting lithium battery anode material and manufacturing method - Google Patents
High-stability long-service-life sagger for roasting lithium battery anode material and manufacturing method Download PDFInfo
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- CN102914165B CN102914165B CN201210402437.9A CN201210402437A CN102914165B CN 102914165 B CN102914165 B CN 102914165B CN 201210402437 A CN201210402437 A CN 201210402437A CN 102914165 B CN102914165 B CN 102914165B
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Abstract
The invention relates to a high-stability long-service-life sagger for roasting a lithium battery anode material and belongs to the field of preparation of fire-resistant kiln furniture. The raw material comprises the following components: 50%-85% of 0-2mm aluminum oxide, 3%-30% of 0-0.2mm silicon dioxide, 1%-15% of 0-0.1mm magnesium oxide, 1%-15% of aluminum titanate being less than or equal to 200 meshes, and 1%-10% of calcium oxide being less than or equal to 200 meshes. The raw material component has an excellent function of improving the alkali resistance and increasing the thermal shock resistance of the sagger. A test proves that the effective service life of the sagger is 30%-100% longer than the service life of the present common sagger.
Description
Technical field
The present invention relates to a kind of saggar for anode material of lithium battery roasting and preparation method thereof, belong to the preparation field of refractory kiln, this anode material of lithium battery roasting saggar has high stable long-life feature.
Background technology
Anode material of lithium battery has to pass through the roasting of high temperature kiln, burn till and must adopt saggar to load, the raw material adopted due to anode material of lithium battery can decompose and produces penetrating power and the strong Lithium Oxide 98min of reactive behavior corrodes saggar in building-up process, easily to peel off, the problem such as efflorescence, the work-ing life of saggar is generally below 20 times.For erosion resistance and the work-ing life of saggar, research and development corrosion resistance is good, and long-life saggar has ten important effects for the production of anode material of lithium battery and technical progress.
Chinese patent application 200910146662.9 discloses one " saggar and manufacture method thereof for the manufacture of the positive active material of lithium ion battery ", containing aluminum oxide 46-68%, magnesium oxide 13-22%, silica 1 2-36% in composition, ferric oxide less than 0.5%.This with spinel, trichroite, mullite for raw material is formed aluminum oxide, magnesium oxide, silicon-dioxide are Chemical Composition compositing formula, there is good erosion resistance, but due to formula in spinel and magnesian quality comparation high, the polar expansion of material is more high than mullite, at the linear expansivity of 20-1500 DEG C, spinel is 9 × 10
-6/ DEG C
-1, magnesium oxide is 14.2 × 10
-6/ DEG C
-1, but mullite is only 5.3 × 10
-6/ DEG C
-1, when anode material of lithium battery high temperature process heat, there is cracking than being easier in the thermal shock performance relative mistake of saggar.
Chinese patent application 200910096395.9 disclosed " the making formula of baking sagger for lithium battery material ", each component weight percent is aluminum oxide 45-70%, magnesium oxide 10-20%, silica 1 5-35%, zirconium white 1-3%, metallic aluminium powder 1-5%.The deficiency existed is: aluminium is neutral material, the activity of metallic aluminium powder is also neutral comparatively speaking, anti-general alkaline material still can, but to decomposing the alkali corrosion of the ability of seeing through that produces and the strong Lithium Oxide 98min of reactive behavior, cobalt acid lithium during anode material of lithium battery high temperature process heat, corrosion resistance is relatively not strong, does not produce great active effect to the raising of the resistance to corrosion of saggar.
Summary of the invention
The object of this invention is to provide a kind of height for anode material of lithium battery roasting and stabilize long lifetime saggar, by formula and the improvement of manufacture method, improve corrosion resistance and the thermal shock performance of saggar, improve work-ing life of saggar, for anode material of lithium battery technical progress and reduce production cost and provide safeguard.
The object of the invention realizes, on the factor basis of fully having grasped restriction raising in work-ing life, main improvement in the aggregate of composition mullite phase adds aluminium titanates particulate, in substrate material, add calcium oxide particulate and zirconia particles simultaneously, thus overcome the deficiencies in the prior art, realize object of the present invention.
Specifically implement like this: a kind of height for anode material of lithium battery roasting stabilizes long lifetime saggar, it is characterized in that the weight proportion of material component is:
Aluminum oxide 0 ~ 2 ㎜ 50% ~ 85%
Silicon-dioxide 0 ~ 0.2 ㎜ 3% ~ 30%
Magnesium oxide 0 ~ 0.1 ㎜ 1% ~ 15%
Aluminium titanates≤200 order 1% ~ 15%
Calcium oxide≤200 order 1% ~ 10%
Zirconium white≤200 order 1% ~ 10%.
In this formula, add in aggregate and have aluminium titanates particulate, the aluminium titanates added is a kind of type material collecting low thermal coefficient of expansion and high melting-point, thermal expansivity is little, even negative expansion can be there is, it is the one that in low-expansion material, resistance to elevated temperatures is best, from microstructure and state, there are crystal and pore in inside, determining it, to have the thermal conductivity that metal and other macromolecular material do not possess low, anti-slag, alkaline-resisting, anti-corrosion, widely use under environment that is wear-resistant, high temperature resistant, that do alkali, the condition harshness such as corrosion-resistant, the especially occasion of highly heatproof and shockproof.
In this formula, in substrate material, add calcium oxide particulate and zirconia particles.Add the acid-basicity that calcium oxide regulates material, it at high temperature reacts with magnesium oxide, zirconium white in material the compound phase being formed and have and protest alkalescence.Add zirconium white, negative expansion mechanism is introduced by the martensitic transformation of zirconium dioxide, the thermal expansivity of matrix is reduced, produce tiny crack, enable the energy receiving part thermal expansion to produce, reduce thermal stresses, improve the thermal shock resistance of saggar, the unreactiveness of zirconium dioxide produces certain active effect for the raising of the resistance to corrosion of saggar simultaneously.The present invention's formula produces good effect for the improvement alkali-resistivity of saggar and the raising of thermal shock resistance, on probation through testing, and acceptable life is than the saggar life 30% ~ 100% generally used at present.
The screening formulation that this height for anode material of lithium battery roasting stabilizes long lifetime saggar is: the weight proportion of material component is:
Aluminum oxide is 0 ~ 2 ㎜ 60% ~ 80%
Silicon-dioxide 0 ~ 0.2 ㎜ 8% ~ 20%
Magnesium oxide 0 ~ 0.1 ㎜ 4% ~ 10%
Aluminium titanates≤200 order 3% ~ 8%
Calcium oxide≤200 order 2% ~ 5%
Zirconium white≤200 order 2% ~ 4%.
The manufacture method that this height for anode material of lithium battery roasting stabilizes long lifetime saggar is: mixed by proportioning by each raw material, undertaken full and uniform mixed by the equipment of mixing, make pug and carry out becoming blank for subsequent use after ageing mixture processes for 8 ~ 48 hours, blank makes blank by compression moulding technique, blank sinters by oxidizing atmosphere after drying room drying, sintering temperature 1300 ~ 1550 DEG C, firing period is 36 ~ 60 hours, prepares finished product saggar.
The saggar prepared by aforesaid method is for the production of anode material of lithium battery, and have high stable, long lifetime feature, acceptable life is than the saggar life 30% ~ 100% generally used at present.
Embodiment
Embodiment 1
Adopt the raw material through selected process, each component mass percent is: aluminum oxide is 50%, and silicon-dioxide is 30%, and magnesium oxide is 10%, aluminium titanates 5%, calcium oxide 3%, zirconium white 2%.Each raw material is undertaken full and uniform mixed by the equipment of mixing, make pug and carry out becoming blank for subsequent use after ageing mixture processes for 8 hours, blank makes blank by compression moulding technique, blank sinters by oxidizing atmosphere after drying room drying, sintering temperature 1300 DEG C, firing period is 50 hours, prepares finished product saggar.Saggar qualified after testing drops on probation.Through anode material of lithium battery 21 times on probation, peeling off does not appear in saggar internal surface, pulverization situation, then 10 times on probation, there is fine cracks.
Embodiment 2
Adopt the raw material through selected process, each component mass percent is: aluminum oxide is 55%, and silicon-dioxide is 13%, and magnesium oxide is 4%, aluminium titanates 15%, calcium oxide 10%, zirconium white 3%.Each raw material is undertaken full and uniform mixed by the equipment of mixing, make pug and carry out becoming blank for subsequent use after ageing mixture processes for 24 hours, blank makes blank by compression moulding technique, blank sinters by oxidizing atmosphere after drying room drying, sintering temperature 1380 DEG C, firing period is 36 hours, prepares finished product saggar.Saggar qualified after testing drops on probation.Try 18 times through anode material of lithium battery, peeling off do not appear in saggar internal surface, pulverization situation, there is fine cracks then for 8 times on probation.
Embodiment 3
Adopt the raw material through selected process, each component mass percent is: aluminum oxide is 60%, and silicon-dioxide is 20%, and magnesium oxide is 15%, aluminium titanates 3%, calcium oxide 1%, zirconium white 1%.Each raw material is undertaken full and uniform mixed by the equipment of mixing, make pug and carry out becoming blank for subsequent use after ageing mixture processes for 20 hours, blank makes blank by compression moulding technique, blank sinters by oxidizing atmosphere after drying room drying, sintering temperature 1450 DEG C, firing period is 48 hours, prepares finished product saggar.Saggar qualified after testing drops on probation.Saggar qualified after testing drops on probation.Through anode material of lithium battery 25 times on probation, peeling off does not appear in saggar internal surface, pulverization situation, then 15 times on probation, there is fine cracks.
Embodiment 4
Adopt the raw material through selected process, each component mass percent is: aluminum oxide is 65%, and silicon-dioxide is 14%, and magnesium oxide is 1%, aluminium titanates 8%, calcium oxide 2%, zirconium white 10%.Each raw material is undertaken full and uniform mixed by the equipment of mixing, make pug and carry out becoming blank for subsequent use after ageing mixture processes for 36 hours, blank makes blank by compression moulding technique, blank sinters by oxidizing atmosphere after drying room drying, sintering temperature 1450 DEG C, firing period is 50 hours, prepares finished product saggar.Saggar qualified after testing drops on probation.Saggar qualified after testing drops on probation.Through anode material of lithium battery 16 times on probation, peeling off does not appear in saggar internal surface, pulverization situation, then 18 times on probation, there is fine cracks.
Embodiment 5
Adopt the raw material through selected process, each component mass percent is: aluminum oxide is 80%, and silicon-dioxide is 8%, and magnesium oxide is 5%, aluminium titanates 1%, calcium oxide 5%, zirconium white 1%.Each raw material is undertaken full and uniform mixed by the equipment of mixing, make pug and carry out becoming blank for subsequent use after ageing mixture processes for 48 hours, blank makes blank by compression moulding technique, blank sinters by oxidizing atmosphere after drying room drying, sintering temperature 1520 DEG C, firing period is 60 hours, prepares finished product saggar.Saggar qualified after testing drops on probation.Saggar qualified after testing drops on probation.Through anode material of lithium battery 23 times on probation, peeling off does not appear in saggar internal surface, pulverization situation, then 15 times on probation, there is fine cracks.
Embodiment 6
Adopt the raw material through selected process, each component mass percent is: aluminum oxide is 85%, and silicon-dioxide is 3%, and magnesium oxide is 1%, aluminium titanates 6%, calcium oxide 1%, zirconium white 4%.Each raw material is undertaken full and uniform mixed by the equipment of mixing, make pug and carry out becoming blank for subsequent use after ageing mixture processes for 48 hours, blank makes blank by compression moulding technique, blank sinters by oxidizing atmosphere after drying room drying, sintering temperature 1550 DEG C, firing period is 60 hours, prepares finished product saggar.Saggar qualified after testing drops on probation.Saggar qualified after testing drops on probation.Through anode material of lithium battery 22 times on probation, peeling off does not appear in saggar internal surface, pulverization situation, then 14 times on probation, there is fine cracks.
Claims (3)
1. the height for anode material of lithium battery roasting stabilizes a long lifetime saggar, it is characterized in that the weight proportion of material component is:
Aluminum oxide 0 ~ 2 ㎜ 50% ~ 85%
Silicon-dioxide 0 ~ 0.2 ㎜ 3% ~ 30%
Magnesium oxide 0 ~ 0.1 ㎜ 1% ~ 15%
Aluminium titanates≤200 order 1% ~ 15%
Calcium oxide≤200 order 1% ~ 10%
Zirconium white≤200 order 1% ~ 10%.
2. the height for anode material of lithium battery roasting according to claim 1 stabilizes long lifetime saggar, it is characterized in that the weight proportion of material component is:
Aluminum oxide is 0 ~ 2 ㎜ 60% ~ 80%
Silicon-dioxide 0 ~ 0.2 ㎜ 8% ~ 20%
Magnesium oxide 0 ~ 0.1 ㎜ 4% ~ 10%
Aluminium titanates≤200 order 3% ~ 8%
Calcium oxide≤200 order 2% ~ 5%
Zirconium white≤200 order 2% ~ 4%.
3. the height for anode material of lithium battery roasting according to claim 1 and 2 stabilizes long lifetime saggar, it is characterized in that manufacture method is: mixed by proportioning by each raw material, undertaken full and uniform mixed by the equipment of mixing, make pug and carry out becoming blank for subsequent use after ageing mixture processes for 8 ~ 48 hours, blank makes blank by compression moulding technique, blank sinters by oxidizing atmosphere after drying room drying, sintering temperature 1300 ~ 1550 DEG C, firing period is 36 ~ 60 hours, prepares finished product saggar.
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| CN102914165B true CN102914165B (en) | 2015-05-27 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024036648A1 (en) | 2022-08-15 | 2024-02-22 | 天津巴莫科技有限责任公司 | Sagger and preparation method therefor |
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| CN104030700A (en) * | 2014-05-26 | 2014-09-10 | 浙江立鑫高温耐火材料有限公司 | Zircon mullite saggar |
| CN106630977A (en) * | 2016-11-29 | 2017-05-10 | 湖南省新化县长江电子有限责任公司 | Sintering sagger for electronic ceramics of new energy automobile and production method of sintering sagger |
| CN107903041B (en) * | 2017-10-25 | 2021-01-26 | 湖北亿佳欧电子陶瓷股份有限公司 | Casket-like bowl and preparation method thereof |
| CN108101558B (en) * | 2017-12-25 | 2021-03-23 | 浙江大学 | Composite sagger, preparation method and application thereof |
| CN109467422B (en) * | 2018-04-20 | 2021-07-02 | 湖南德景源科技有限公司 | Special high-cycle special ceramic crucible for lithium battery and preparation method thereof |
| CN110550941B (en) * | 2019-08-23 | 2022-05-03 | 许行彪 | High-temperature-resistant non-oxidized graphite ceramic material |
| CN110540418A (en) * | 2019-09-20 | 2019-12-06 | 湖南金铠新材料科技有限公司 | Sagger special for sintering lithium battery positive electrode material and preparation method thereof |
| CN112028650A (en) * | 2020-09-03 | 2020-12-04 | 深圳市飞粤新材料科技有限公司 | Sagger for lithium ion battery anode material |
| CN113603469B (en) * | 2021-08-04 | 2022-12-16 | 江苏晶邦新型材料有限公司 | Composite spinel-mullite ceramic refractory material and preparation method thereof |
| CN114031380A (en) * | 2021-10-29 | 2022-02-11 | 洛阳索莱特材料科技有限公司 | Preparation method of alumina-zirconia ceramic sagger |
| CN114105630A (en) * | 2021-12-08 | 2022-03-01 | 湖南仁海科技材料发展有限公司 | Petalite combined calcium hexaluminate sagger and preparation method thereof |
| CN114907110B (en) * | 2022-05-26 | 2023-11-14 | 胡勇波 | Synthetic composite spinel Dan Xiabo and manufacturing method thereof |
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| CN101486586A (en) * | 2009-02-26 | 2009-07-22 | 冯维银 | Formula for manufacturing lithium battery material calcination sagger |
| CN102531552A (en) * | 2010-12-14 | 2012-07-04 | 淄博高新区联创科技服务中心 | Aluminum oxide/silicon dioxide/aluminum titanate porous ceramic and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05170518A (en) * | 1991-11-06 | 1993-07-09 | Shinagawa Refract Co Ltd | Furnace material for furnace for burning electronic ceramics |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486586A (en) * | 2009-02-26 | 2009-07-22 | 冯维银 | Formula for manufacturing lithium battery material calcination sagger |
| CN102531552A (en) * | 2010-12-14 | 2012-07-04 | 淄博高新区联创科技服务中心 | Aluminum oxide/silicon dioxide/aluminum titanate porous ceramic and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024036648A1 (en) | 2022-08-15 | 2024-02-22 | 天津巴莫科技有限责任公司 | Sagger and preparation method therefor |
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