CN102914165A - 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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- CN102914165A CN102914165A CN2012104024379A CN201210402437A CN102914165A CN 102914165 A CN102914165 A CN 102914165A CN 2012104024379 A CN2012104024379 A CN 2012104024379A CN 201210402437 A CN201210402437 A CN 201210402437A CN 102914165 A CN102914165 A CN 102914165A
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- saggar
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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 the 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 has high stable long-life characteristics with saggar.
Background technology
Anode material of lithium battery must be through the roasting of high temperature kiln, burn till and to adopt saggar to load, because the raw material that anode material of lithium battery adopts can decompose the generation penetrating power in building-up process and the strong lithia of reactivity corrodes saggar, easily peel off, the problem such as efflorescence, the service life of saggar is generally below 20 times.For corrosion resistance and the service life of saggar, the research and development corrosion resistance is good, and long-life saggar has ten important effects for production and the technological progress of anode material of lithium battery.
That Chinese patent application 200910146662.9 discloses is a kind of " for the manufacture of saggar and the manufacture method thereof of the positive active material of lithium ion battery ", contain aluminium oxide 46-68%, magnesia 13-22%, silica 1 2-36% in the composition, di-iron trioxide is below 0.5%.Thisly consist of aluminium oxide, magnesia, silica take spinelle, cordierite, mullite as raw material and be the compositing formula of chemical analysis, preferably corrosion resistance is arranged, but because spinelle and magnesian mass ratio in the prescription are higher, the line expansion ratio mullite of material is high, at 20-1500 ℃ linear expansion coefficient, spinelle is 9 * 10
-6/ ℃
-1, magnesia is 14.2 * 10
-6/ ℃
-1, but mullite only is 5.3 * 10
-6/ ℃
-1, when the anode material of lithium battery high temperature solid-state was synthetic, the thermal shock performance relative mistake of saggar was than being easier to occur cracking.
Chinese patent application 200910096395.9 disclosed " the making prescription of baking sagger for lithium battery material ", the each component percentage by weight is aluminium oxide 45-70%, magnesia 10-20%, silica 1 5-35%, zirconia 1-3%, metallic aluminium powder 1-5%.The deficiency that exists is: aluminium is neutral material, the activity of metallic aluminium powder also is neutral comparatively speaking, anti-general alkaline material still can, but the alkali corrosion of the lithia that the ability of seeing through that decomposition produces when synthetic to the anode material of lithium battery high temperature solid-state and reactivity are strong, cobalt acid lithium, corrosion resistance is relatively not strong, and the raising of the resistance to corrosion of saggar is not produced great positive role.
Summary of the invention
The purpose of this invention is to provide the stable long-life saggar of a kind of height for the anode material of lithium battery roasting, improvement by prescription and manufacture method, improve corrosion resistance and the thermal shock performance of saggar, improve the service life of saggar, for the technological progress of anode material of lithium battery and reduce production costs and provide safeguard.
The object of the invention realizes, on the factor basis of fully having grasped restriction raising in service life, the main improvement adds the aluminium titanates particulate in the aggregate that forms the mullite phase, in substrate material, add simultaneously calcium oxide particulate and zirconia particulate, thereby overcome the deficiencies in the prior art, realize purpose of the present invention.
Specifically implement like this: the stable long-life saggar of a kind of height for the anode material of lithium battery roasting is characterized in that the weight proportion of material component is:
Aluminium oxide 0 ~ 2 ㎜ 50% ~ 85%
Silica 0 ~ 0.2 ㎜ 3% ~ 30%
Magnesia 0 ~ 0.1 ㎜ 1% ~ 15%
Aluminium titanates≤200 orders 1% ~ 15%
Calcium oxide≤200 orders 1% ~ 10%
Zirconia≤200 orders 1% ~ 10%.
In this prescription, add in the aggregate aluminium titanates particulate is arranged, the aluminium titanates that adds is a kind of new material that collects low thermal coefficient of expansion and high melting-point, thermal coefficient of expansion is little, even negative expansion can appear, best a kind of of resistance to elevated temperatures in the low-expansion material, from microstructure and state, there are crystal and pore in inside, it is low to have determined that it has a thermal conductivity factor that metal and other macromolecular material do not possess, anti-slag, alkaline-resisting, anti-corrosion is widely used under wear-resistant, high temperature resistant, as to do alkali, the condition harshness such as corrosion-resistant environment, especially the occasion of highly heatproof and shockproof.
In this prescription, add calcium oxide particulate and zirconia particulate in the substrate material.Add calcium oxide and regulate the Acidity of Aikalinity of material, it at high temperature with material in magnesia, zirconia reaction form the compound phase with protest alkalescence.Add zirconia, introduce negative expansion mechanism by the martensite phase transformation of zirconium dioxide, the thermal coefficient of expansion of matrix is reduced, produce micro-crack, enable to receive the energy of part thermal expansion generation, reduce thermal stress, improve the thermal shock resistance of saggar, the chemical inertness of zirconium dioxide produces certain positive role for the raising of the resistance to corrosion of saggar simultaneously.The present invention's prescription produces good effect for the raising of the alkali resistance of improving saggar and thermal shock resistance, and is on probation through testing, and Acceptable life is than the saggar life 30% ~ 100% that generally uses at present.
The optimization formula that this height for the anode material of lithium battery roasting is stabilized the long-life saggar is: the weight proportion of material component is:
Aluminium oxide is 0 ~ 2 ㎜ 60% ~ 80%
Silica 0 ~ 0.2 ㎜ 8% ~ 20%
Magnesia 0 ~ 0.1 ㎜ 4% ~ 10%
Aluminium titanates≤200 orders 3% ~ 8%
Calcium oxide≤200 orders 2% ~ 5%
Zirconia≤200 orders 2% ~ 4%.
The manufacture method that this height for the anode material of lithium battery roasting is stabilized the long-life saggar is: each raw material is mixed by proportioning, undertaken full and uniform mixed by the equipment of mixing, the one-tenth blank is for subsequent use after making pug and carrying out ageing mixture processing in 8～48 hours, blank is made blank by compressing technique, use the oxidizing atmosphere sintering after the blank process drying room drying, 1300～1550 ℃ of sintering temperatures, firing period is 36～60 hours, prepares the finished product saggar.
Be used for the production of anode material of lithium battery by the saggar of said method preparation, have high stable, long-life characteristics, Acceptable life is than the saggar life 30% ~ 100% that generally uses at present.
The specific embodiment
Embodiment 1
Adopt the raw material through selected processing, the each component mass percent is: aluminium oxide is 50%, and silica is 30%, and magnesia is 10%, aluminium titanates 5%, calcium oxide 3%, zirconia 2%.Each raw material is undertaken full and uniform mixed by the equipment of mixing, the one-tenth blank is for subsequent use after making pug and carrying out ageing mixture processing in 8 hours, blank is made blank by compressing technique, use the oxidizing atmosphere sintering after the blank process drying room drying, 1300 ℃ of sintering temperatures, firing period is 50 hours, prepares the finished product saggar.Qualified saggar drops on probation after testing.Try out 21 times through anode material of lithium battery, peeling off does not appear in the saggar inner surface, the efflorescence situation, 10 times on probation again, fine cracks occurs.
Embodiment 2
Adopt the raw material through selected processing, the each component mass percent is: aluminium oxide is 55%, and silica is 13%, and magnesia is 4%, aluminium titanates 15%, calcium oxide 10%, zirconia 3%.Each raw material is undertaken full and uniform mixed by the equipment of mixing, the one-tenth blank is for subsequent use after making pug and carrying out ageing mixture processing in 24 hours, blank is made blank by compressing technique, use the oxidizing atmosphere sintering after the blank process drying room drying, 1380 ℃ of sintering temperatures, firing period is 36 hours, prepares the finished product saggar.Qualified saggar drops on probation after testing.Through anode material of lithium battery examination 18 times, peeling off does not appear in the saggar inner surface, the efflorescence situation, 8 times on probation again, fine cracks occurs.
Embodiment 3
Adopt the raw material through selected processing, the each component mass percent is: aluminium oxide is 60%, and silica is 20%, and magnesia is 15%, aluminium titanates 3%, calcium oxide 1%, zirconia 1%.Each raw material is undertaken full and uniform mixed by the equipment of mixing, the one-tenth blank is for subsequent use after making pug and carrying out ageing mixture processing in 20 hours, blank is made blank by compressing technique, use the oxidizing atmosphere sintering after the blank process drying room drying, 1450 ℃ of sintering temperatures, firing period is 48 hours, prepares the finished product saggar.Qualified saggar drops on probation after testing.Qualified saggar drops on probation after testing.Try out 25 times through anode material of lithium battery, peeling off does not appear in the saggar inner surface, the efflorescence situation, 15 times on probation again, fine cracks occurs.
Embodiment 4
Adopt the raw material through selected processing, the each component mass percent is: aluminium oxide is 65%, and silica is 14%, and magnesia is 1%, aluminium titanates 8%, calcium oxide 2%, zirconia 10%.Each raw material is undertaken full and uniform mixed by the equipment of mixing, the one-tenth blank is for subsequent use after making pug and carrying out ageing mixture processing in 36 hours, blank is made blank by compressing technique, use the oxidizing atmosphere sintering after the blank process drying room drying, 1450 ℃ of sintering temperatures, firing period is 50 hours, prepares the finished product saggar.Qualified saggar drops on probation after testing.Qualified saggar drops on probation after testing.Try out 16 times through anode material of lithium battery, peeling off does not appear in the saggar inner surface, the efflorescence situation, 18 times on probation again, fine cracks occurs.
Embodiment 5
Adopt the raw material through selected processing, the each component mass percent is: aluminium oxide is 80%, and silica is 8%, and magnesia is 5%, aluminium titanates 1%, calcium oxide 5%, zirconia 1%.Each raw material is undertaken full and uniform mixed by the equipment of mixing, the one-tenth blank is for subsequent use after making pug and carrying out ageing mixture processing in 48 hours, blank is made blank by compressing technique, use the oxidizing atmosphere sintering after the blank process drying room drying, 1520 ℃ of sintering temperatures, firing period is 60 hours, prepares the finished product saggar.Qualified saggar drops on probation after testing.Qualified saggar drops on probation after testing.Try out 23 times through anode material of lithium battery, peeling off does not appear in the saggar inner surface, the efflorescence situation, 15 times on probation again, fine cracks occurs.
Embodiment 6
Adopt the raw material through selected processing, the each component mass percent is: aluminium oxide is 85%, and silica is 3%, and magnesia is 1%, aluminium titanates 6%, calcium oxide 1%, zirconia 4%.Each raw material is undertaken full and uniform mixed by the equipment of mixing, the one-tenth blank is for subsequent use after making pug and carrying out ageing mixture processing in 48 hours, blank is made blank by compressing technique, use the oxidizing atmosphere sintering after the blank process drying room drying, 1550 ℃ of sintering temperatures, firing period is 60 hours, prepares the finished product saggar.Qualified saggar drops on probation after testing.Qualified saggar drops on probation after testing.Try out 22 times through anode material of lithium battery, peeling off does not appear in the saggar inner surface, the efflorescence situation, 14 times on probation again, fine cracks occurs.
Claims (3)
1. a height that is used for the anode material of lithium battery roasting is stabilized the long-life saggar, it is characterized in that the weight proportion of material component is:
Aluminium oxide 0 ~ 2 ㎜ 50% ~ 85%
Silica 0 ~ 0.2 ㎜ 3% ~ 30%
Magnesia 0 ~ 0.1 ㎜ 1% ~ 15%
Aluminium titanates≤200 orders 1% ~ 15%
Calcium oxide≤200 orders 1% ~ 10%
Zirconia≤200 orders 1% ~ 10%.
2. the height for the anode material of lithium battery roasting according to claim 1 is stabilized the long-life saggar, it is characterized in that the weight proportion of material component is:
Aluminium oxide is 0 ~ 2 ㎜ 60% ~ 80%
Silica 0 ~ 0.2 ㎜ 8% ~ 20%
Magnesia 0 ~ 0.1 ㎜ 4% ~ 10%
Aluminium titanates≤200 orders 3% ~ 8%
Calcium oxide≤200 orders 2% ~ 5%
Zirconia≤200 orders 2% ~ 4%.
3. the height for the anode material of lithium battery roasting according to claim 1 and 2 is stabilized the long-life saggar, it is characterized in that manufacture method is: each raw material is mixed by proportioning, undertaken full and uniform mixed by the equipment of mixing, the one-tenth blank is for subsequent use after making pug and carrying out ageing mixture processing in 8～48 hours, blank is made blank by compressing technique, use the oxidizing atmosphere sintering after the blank process drying room drying, 1300～1550 ℃ of sintering temperatures, firing period is 36～60 hours, prepares the finished product saggar.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107903041A (en) * | 2017-10-25 | 2018-04-13 | 湖北亿佳欧电子陶瓷股份有限公司 | A kind of saggar and preparation method thereof |
| CN108101558A (en) * | 2017-12-25 | 2018-06-01 | 浙江大学 | Compound saggar, preparation method and applications |
| CN109467422A (en) * | 2018-04-20 | 2019-03-15 | 湖南德景源科技有限公司 | Dedicated high circulation special cermacis crucible of a kind of lithium electricity and preparation method thereof |
| 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 |
| CN110550941A (en) * | 2019-08-23 | 2019-12-10 | 许行彪 | High-temperature-resistant non-oxidized graphite ceramic material |
| 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 |
| CN113603469A (en) * | 2021-08-04 | 2021-11-05 | 浙江吉昌新材料有限公司 | 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 |
| CN114907110A (en) * | 2022-05-26 | 2022-08-16 | 胡勇波 | Synthetic composite spinel sagger and manufacturing method thereof |
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| CN115043650B (en) | 2022-08-15 | 2022-11-15 | 天津巴莫科技有限责任公司 | Casket-like bowl and preparation method thereof |
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| 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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| JPH05170518A (en) * | 1991-11-06 | 1993-07-09 | Shinagawa Refract Co Ltd | Furnace material for furnace for burning electronic ceramics |
| 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 (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107903041A (en) * | 2017-10-25 | 2018-04-13 | 湖北亿佳欧电子陶瓷股份有限公司 | A kind of saggar and preparation method thereof |
| CN108101558A (en) * | 2017-12-25 | 2018-06-01 | 浙江大学 | Compound saggar, preparation method and applications |
| CN108101558B (en) * | 2017-12-25 | 2021-03-23 | 浙江大学 | Composite sagger, preparation method and application thereof |
| CN109467422A (en) * | 2018-04-20 | 2019-03-15 | 湖南德景源科技有限公司 | Dedicated high circulation special cermacis crucible of a kind of lithium electricity and preparation method thereof |
| CN110550941A (en) * | 2019-08-23 | 2019-12-10 | 许行彪 | High-temperature-resistant non-oxidized graphite ceramic material |
| 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 |
| CN113603469A (en) * | 2021-08-04 | 2021-11-05 | 浙江吉昌新材料有限公司 | 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 |
| CN114907110A (en) * | 2022-05-26 | 2022-08-16 | 胡勇波 | Synthetic composite spinel sagger and manufacturing 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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