CN110282964A - Mullite-cordierite matter anode material of lithium battery sintering saggar and preparation method thereof - Google Patents
Mullite-cordierite matter anode material of lithium battery sintering saggar and preparation method thereof Download PDFInfo
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- C04B35/16—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 silicates other than clay
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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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- F27D5/00—Supports, screens, or the like for the charge within the furnace
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
- C04B2235/3222—Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
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- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
- C04B2235/3481—Alkaline earth metal alumino-silicates other than clay, e.g. cordierite, beryl, micas such as margarite, plagioclase feldspars such as anorthite, zeolites such as chabazite
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Abstract
The present invention relates to a kind of mullite-cordierite matter anode material of lithium battery sintering saggars and preparation method thereof.Its technical solution is: the mullite particle of 30~35wt%, the mullite fine powder of 20~25wt%, the cordierite particle of 30~35wt%, the dextrin of 4~7wt% and the Guangxi 5~7wt% white clay being mixed, stirring obtains mixture A;The andalusite fine powder of the mullite fine powder of 30~35wt%, the magnesium aluminate spinel fine powder of 30~35wt% and 35~36wt% is stirred again, is dried, grinding obtains mixture B.Then mixture A is placed in mold, uniformly spills a layer mixture B on pressure head surface, the mechanical pressing in such a way that pot mouth is directed downwardly is dry, keeps the temperature 5~6 hours under the conditions of 1300~1400 DEG C, and mullite-cordierite matter anode material of lithium battery sintering saggar is made.Low in cost, simple process and high yield rate of the invention;The mullite-cordierite matter anode material of lithium battery sintering saggar bulk density of preparation is big, compressive resistance is high, thermal shock resistance is excellent and erosion-resisting characteristics is good.
Description
Technical field
The invention belongs to anode material of lithium battery sintering saggar technical fields.In particular to a kind of mullite-cordierite matter
Anode material of lithium battery sintering saggar and preparation method thereof.
Background technique
Saggar is sintered the carrier that must be used as anode material of lithium battery, with thermal shock resistance is good, intensity is high, anti-
The advantages that anode material of lithium battery erosion performance is good, therefore, hair of the research anode material of lithium battery sintering saggar to new energy
Exhibition has great meaning, in addition, saggar is difficult to recycle at this stage, the serious waste of resource is caused, when research can be long
Between had great importance using saggar to resource-effective.
" a kind of mullite foamed ceramics and preparation method thereof " (CN104311117A) patented technology, it is thin with sugar, alumina-silica
Powder is raw material, is fired at high temperature using foaming technique, although having lower cost and high added value, due to material
Formed in object it is mutually single, cause its thermal shock performance lower.
" a kind of cordierite honeycomb ceramic and preparation method " (CN101045629A) patented technology, with LiO2, talcum, calcining
Kaolin, aluminium oxide, aluminium hydroxide and silicon powder etc. are raw material, are cut by rear mixing, pugging, extrusion, wet base, is dry, dry
The techniques such as base cutting, firing obtain finished product, though there is higher intensity, cost of material is excessively high, it is difficult to large-scale application.
" a kind of lightweight dichroite-mullite composite ceramic material and preparation method thereof " (CN103922713A) patent skill
Art, diaspore, amorphous silica, talcum powder and clay are raw material, by stirring, molding, it is dry after be burnt under high temperature again,
Though intensity is preferable with thermal shock resistance, since cordierite is easily reacted with anode material of lithium battery, material is embodied anti-
Erosion performance is weaker low with service life.
Summary of the invention
The present invention is directed to overcome prior art defect, it is therefore an objective to provide a kind of mullite-low in cost and simple process
The preparation method of cordierite anode material of lithium battery sintering saggar, the mullite-cordierite matter lithium electricity prepared with this method
Pond positive electrode sintering saggar thermal shock resistance is good, erosion-resisting characteristics is excellent and long service life.
To achieve the above object, the step of the technical solution adopted by the present invention is:
Step 1: by the mullite particle of 30~35wt%, the mullite fine powder of 20~25wt%, 30~35wt% violet
The Guangxi white clay of bluestone particle, the dextrin of 4~7wt% and 5~7wt% is placed in batch mixer, is stirred 1~1.2h, is obtained mixture
A。
Step 2: by the mullite fine powder of 30~35wt%, the magnesium aluminate spinel fine powder of 30~35wt% and 35~
The andalusite fine powder of 36wt% is placed in batch mixer, stirs 1~1.2h, and 1~2h is dried under the conditions of 100~110 DEG C, is ground to
Granularity≤0.048mm obtains mixture B.
Step 3: first the mixture A is placed in mold, one layer of mixture B is uniformly spilt then at pressure head surface, with pot mouth
Mode directed downwardly mechanical pressing under conditions of 120~160MPa, then dry 20 under the conditions of 100~110 DEG C~for 24 hours, in
5~6 hours are kept the temperature under the conditions of 1300~1400 DEG C, mullite-cordierite matter anode material of lithium battery sintering saggar is made.
The chemical component of the mullite particle is: Al2O3>=67.3wt%, SiO2>=30.4wt%, Fe2O3≥
0.92wt%;The density of the mullite particle is 2.82~2.97g/cm3, granularity≤3mm of mullite particle.
The mullite fine powder includes mullite fine powder described in mullite fine powder and step 2 described in step 1.It is described not come
The chemical component of stone fine powder is: Al2O3>=67.3wt%, SiO2>=30.4wt%, Fe2O3>=0.92wt%;The mullite is thin
The density of powder is 2.82~2.97g/cm3, granularity≤0.088mm of mullite fine powder.
The chemical component of the cordierite particle is: Al2O3>=34.1wt%, SiO2>=42.2wt%, MgO >=
14.3wt%;The density of the cordierite particle is 2.67~2.79g/cm3, granularity≤3mm of cordierite particle.
Granularity≤0.088mm of the dextrin.
The chemical component of the Guangxi white clay is: Al2O3>=35.2wt%, SiO2Containing >=48.1wt%, K2O≥
2.1wt%;Granularity≤0.088mm of the Guangxi white clay.
The chemical component of the magnesium aluminate spinel fine powder: content of MgO >=46.3wt%, Al2O3Content >=46.2wt%;Institute
State granularity≤0.088mm of magnesium aluminate spinel fine powder.
The chemical component of the andalusite fine powder is: Al2O3>=61.8wt%, SiO2≥29.7;The andalusite fine powder
Granularity≤0.088mm.
Due to the adoption of the above technical scheme, compared with the prior art, the present invention has the following advantages:
1, prepared mixture A is placed in mold by the present invention, spills the mixture B of one layer of preparation in pressure head surface,
Mullite-cordierite matter anode material of lithium battery sintering casket is made through dry and firing in pot mouth mode mechanical pressing directed downwardly
Alms bowl (hereinafter referred to as " saggar "), therefore simple process;Dense protective layer is formed in the inner surface of saggar in sintering process, is increased
The erosion-resisting characteristics of saggar improves the service life of saggar.
2, the present invention is using cordierite particle as aggregate, since the crystal structure of cordierite particle makes its good thermal shock, because
This, prepared saggar has excellent thermal shock resistance.
3 raw material sources of the invention are abundant and low in cost, without especial equipment requirements, preparation during preparing saggar
It is short with firing time, thus it is at low cost and easy to industrialized production.
Mullite-cordierite matter anode material of lithium battery sintering saggar is through detecting prepared by the present invention: yield rate is
99.6~99.9%;Apparent porosity is 8.4~10.4gcm3;Bulk density is 2.86~3.26gcm3;Flexural strength is
10.2~13.2MPa;Compressive resistance is 42.42~48.47MPa;900 DEG C of Static crucible method anti-slag experiment erosion index are 2.2
~3.7%.
Therefore, the present invention has the characteristics that low in cost, simple process and high yield rate;Prepared mullite-violet is green
Stone matter anode material of lithium battery sintering saggar bulk density is big, compressive resistance is high, thermal shock resistance is excellent and erosion-resisting characteristics is good.
Specific embodiment
The invention will be further described With reference to embodiment, not to the limitation of its protection scope.
It is first that material Unify legislation involved in present embodiment is as follows to avoid repeating, it is no longer superfluous in embodiment
It states:
The chemical component of the mullite particle is: Al2O3>=67.3wt%, SiO2>=30.4wt%, Fe2O3≥
0.92wt%;The density of the mullite particle is 2.82~2.97g/cm3, granularity≤3mm of mullite particle.
The mullite fine powder includes mullite fine powder described in mullite fine powder and step 2 described in step 1.It is described not come
The chemical component of stone fine powder is: Al2O3>=67.3wt%, SiO2>=30.4wt%, Fe2O3>=0.92wt%;The mullite is thin
The density of powder is 2.82~2.97g/cm3, granularity≤0.088mm of mullite fine powder.
The chemical component of the cordierite particle is: Al2O3>=34.1wt%, SiO2>=42.2wt%, MgO >=
14.3wt%;The density of the cordierite particle is 2.67~2.79g/cm3, granularity≤3mm of cordierite particle.
Granularity≤0.088mm of the dextrin.
The chemical component of the Guangxi white clay is: Al2O3>=35.2wt%, SiO2Containing >=48.1wt%, K2O≥
2.1wt%;Granularity≤0.088mm of the Guangxi white clay.
The chemical component of the magnesium aluminate spinel fine powder: content of MgO >=46.3wt%, Al2O3Content >=46.2wt%;Institute
State granularity≤0.088mm of magnesium aluminate spinel fine powder.
The chemical component of the andalusite fine powder is: Al2O3>=61.8wt%, SiO2≥29.7;The andalusite fine powder
Granularity≤0.088mm.
Implement 1
A kind of mullite-cordierite matter anode material of lithium battery sintering saggar and preparation method thereof.Described in the present embodiment
Preparation method is:
Step 1: by the mullite particle of 30~32wt%, the mullite fine powder of 20~22wt%, 33~35wt% violet
The Guangxi white clay of bluestone particle, the dextrin of 4~7wt% and 5~7wt% is placed in batch mixer, is stirred 1~1.2h, is obtained mixture
A。
Step 2: by the mullite fine powder of 30~32wt%, the magnesium aluminate spinel fine powder of 33~35wt% and 35~
The andalusite fine powder of 36wt% is placed in batch mixer, stirs 1~1.2h, and 1~2h is dried under the conditions of 100~110 DEG C, is ground to
Granularity≤0.048mm obtains mixture B.
Step 3: first the mixture A is placed in mold, one layer of mixture B is uniformly spilt then at pressure head surface, with pot mouth
Mode directed downwardly mechanical pressing under conditions of 120~130MPa, then dry 20 under the conditions of 100~110 DEG C~for 24 hours, in
5~6 hours are kept the temperature under the conditions of 1300~1325 DEG C, mullite-cordierite matter anode material of lithium battery sintering saggar is made.
Implement 2
A kind of mullite-cordierite matter anode material of lithium battery sintering saggar and preparation method thereof.Described in the present embodiment
Preparation method is:
Step 1: by the mullite particle of 31~33wt%, the mullite fine powder of 21~23wt%, 32~34t% violet
The Guangxi white clay of bluestone particle, the dextrin of 4~7wt% and 5~7wt% is placed in batch mixer, is stirred 1~1.2h, is obtained mixture
A。
Step 2: by the mullite fine powder of 31~33wt%, the magnesium aluminate spinel fine powder of 32~34wt% and 35~
The andalusite fine powder of 36wt% is placed in batch mixer, stirs 1~1.2h, and 1~2h is dried under the conditions of 100~110 DEG C, is ground to
Granularity≤0.048mm obtains mixture B.
Step 3: first the mixture A is placed in mold, one layer of mixture B is uniformly spilt then at pressure head surface, with pot mouth
Mode directed downwardly mechanical pressing under conditions of 130~140MPa, then dry 20 under the conditions of 100~110 DEG C~for 24 hours, in
5~6 hours are kept the temperature under the conditions of 1325~1350 DEG C, mullite-cordierite matter anode material of lithium battery sintering saggar is made.
Implement 3
A kind of mullite-cordierite matter anode material of lithium battery sintering saggar and preparation method thereof.Described in the present embodiment
Preparation method is:
Step 1: by the mullite particle of 32~34wt%, the mullite fine powder of 22~24wt%, 31~33wt% violet
The Guangxi white clay of bluestone particle, the dextrin of 4~7wt% and 5~7wt% is placed in batch mixer, is stirred 1~1.2h, is obtained mixture
A。
Step 2: by the mullite fine powder of 32~34wt%, the magnesium aluminate spinel fine powder of 31~33wt% and 35~
The andalusite fine powder of 36wt% is placed in batch mixer, stirs 1~1.2h, and 1~2h is dried under the conditions of 100~110 DEG C, is ground to
Granularity≤0.048mm obtains mixture B.
Step 3: first the mixture A is placed in mold, one layer of mixture B is uniformly spilt then at pressure head surface, with pot mouth
Mode directed downwardly mechanical pressing under conditions of 140~150MPa, then dry 20 under the conditions of 100~110 DEG C~for 24 hours, in
5~6 hours are kept the temperature under the conditions of 1350~1375 DEG C, mullite-cordierite matter anode material of lithium battery sintering saggar is made.
Implement 4
A kind of mullite-cordierite matter anode material of lithium battery sintering saggar and preparation method thereof.Described in the present embodiment
Preparation method is:
Step 1: by the mullite particle of 33~35wt%, the mullite fine powder of 23~25wt%, 30~32wt% violet
The Guangxi white clay of bluestone particle, the dextrin of 4~7wt% and 5~7wt% is placed in batch mixer, is stirred 1~1.2h, is obtained mixture
A。
Step 2: by the mullite fine powder of 33~35wt%, the magnesium aluminate spinel fine powder of 30~32wt% and 35~
The andalusite fine powder of 36wt% is placed in batch mixer, stirs 1~1.2h, and 1~2h is dried under the conditions of 100~110 DEG C, is ground to
Granularity≤0.048mm obtains mixture B.
Step 3: first the mixture A is placed in mold, one layer of mixture B is uniformly spilt then at pressure head surface, with pot mouth
Mode directed downwardly mechanical pressing under conditions of 150~160MPa, then dry 20 under the conditions of 100~110 DEG C~for 24 hours, in
5~6 hours are kept the temperature under the conditions of 1375~1400 DEG C, mullite-cordierite matter anode material of lithium battery sintering saggar is made.
Present embodiment has the advantage that compared with prior art
1, prepared mixture A is placed in mold by present embodiment, spills one layer of preparation in pressure head surface
Mullite-cordierite matter anode material of lithium battery is made through dry and firing in mixture B, pot mouth mode mechanical pressing directed downwardly
Sintering saggar (hereinafter referred to as " saggar "), therefore simple process;Inner surface in sintering process in saggar forms fine and close protection
Layer, increases the erosion-resisting characteristics of saggar, improves the service life of saggar.
2, present embodiment is using cordierite particle as aggregate, since the crystal structure of cordierite particle makes its anti-thermal shock
Property it is good, therefore, prepared saggar have excellent thermal shock resistance.
The raw material sources of 3 present embodiments are abundant and low in cost, without special installation during preparing saggar
It is required that preparation is short with firing time, thus it is at low cost and easy to industrialized production.
Mullite-cordierite matter anode material of lithium battery sintering saggar is through detecting prepared by present embodiment:
Yield rate is 99.6~99.9%;Apparent porosity is 8.4~10.4gcm3;Bulk density is 2.86~3.26gcm3;Anti- folding
Intensity is 10.2~13.2MPa;Compressive resistance is 42.42~48.47MPa;900 DEG C of Static crucible method anti-slags test erosion index
It is 2.2~3.7%.
Therefore, present embodiment has the characteristics that low in cost, simple process and high yield rate;Prepared does not come
Cordierite anode material of lithium battery sintering saggar bulk density is big, compressive resistance is high, thermal shock resistance is excellent and anti-erosion for stone-
Performance is good.
Claims (9)
1. a kind of preparation method of mullite-cordierite matter anode material of lithium battery sintering saggar, it is characterised in that the system
Preparation Method comprises the concrete steps that:
Step 1: by the mullite particle of 30~35wt%, the mullite fine powder of 20~25wt%, 30~35wt% cordierite
The Guangxi white clay of particle, the dextrin of 4~7wt% and 5~7wt% is placed in batch mixer, is stirred 1~1.2h, is obtained mixture A;
Step 2: by the mullite fine powder of 30~35wt%, the magnesium aluminate spinel fine powder of 30~35wt% and 35~36wt%
Andalusite fine powder is placed in batch mixer, stir 1~1.2h, under the conditions of 100~110 DEG C dry 1~2h, be ground to granularity≤
0.048mm obtains mixture B;
Step 3: first the mixture A is placed in mold, one layer of mixture B is uniformly spilt then at pressure head surface, downward with pot mouth
Mode under conditions of 120~160MPa mechanical pressing, then dry 20 under the conditions of 100~110 DEG C~for 24 hours, in 1300
5~6 hours are kept the temperature under the conditions of~1400 DEG C, mullite-cordierite matter anode material of lithium battery sintering saggar is made.
2. the preparation method of mullite-cordierite matter anode material of lithium battery sintering saggar according to claim 1,
Being characterized in that the chemical component of the mullite particle is: Al2O3>=67.3wt%, SiO2>=30.4wt%, Fe2O3≥
0.92wt%;The density of the mullite particle is 2.82~2.97g/cm3, granularity≤3mm of mullite particle.
3. the preparation method of mullite-cordierite matter anode material of lithium battery sintering saggar according to claim 1,
Being characterized in that the chemical component of the mullite fine powder is: Al2O3>=67.3wt%, SiO2>=30.4wt%, Fe2O3≥
0.92wt%;The density of the mullite fine powder is 2.82~2.97g/cm3, granularity≤0.088mm of mullite fine powder.
4. the preparation method of mullite-cordierite matter anode material of lithium battery sintering saggar according to claim 1,
Being characterized in that the chemical component of the cordierite particle is: Al2O3>=34.1wt%, SiO2>=42.2wt%, MgO >=
14.3wt%;The density of the cordierite particle is 2.67~2.79g/cm3, granularity≤3mm of cordierite particle.
5. the preparation method of mullite-cordierite matter anode material of lithium battery sintering saggar according to claim 1,
It is characterized in that granularity≤0.088mm of the dextrin.
6. the preparation method of mullite-cordierite matter anode material of lithium battery sintering saggar according to claim 1,
Being characterized in that the chemical component of the Guangxi white clay is: Al2O3>=35.2wt%, SiO2Containing >=48.1wt%, K2O≥
2.1wt%;Granularity≤0.088mm of the Guangxi white clay.
7. the preparation method of mullite-cordierite matter anode material of lithium battery sintering saggar according to claim 1,
It is characterized in that the chemical component of the magnesium aluminate spinel fine powder: content of MgO >=46.3wt%, Al2O3Content >=46.2wt%;Institute
State granularity≤0.088mm of magnesium aluminate spinel fine powder.
8. the preparation method of mullite-cordierite matter anode material of lithium battery sintering saggar according to claim 1,
Being characterized in that the chemical component of the andalusite fine powder is: Al2O3>=61.8wt%, SiO2≥29.7;The andalusite fine powder
Granularity≤0.088mm.
9. a kind of mullite-cordierite matter anode material of lithium battery sintering saggar, it is characterised in that the mullite-cordierite
Matter anode material of lithium battery sintering saggar be any one of according to claim 1~8 described in mullite-cordierite matter lithium
Mullite-cordierite matter anode material of lithium battery sintering casket prepared by the preparation method of cell positive material sintering saggar
Alms bowl.
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CN112010661A (en) * | 2020-09-03 | 2020-12-01 | 深圳市飞粤新材料科技有限公司 | Sagger for lithium battery positive electrode material and preparation method thereof |
CN112279662A (en) * | 2020-11-06 | 2021-01-29 | 湘潭海泡石科技有限公司 | Sagger for magnesium aluminate spinel-cordierite calcined lithium battery positive electrode material and preparation method thereof |
CN112358304A (en) * | 2020-11-06 | 2021-02-12 | 湘潭海泡石科技有限公司 | Sagger for cordierite-magnesium aluminate spinel calcined lithium battery positive electrode material and preparation method thereof |
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CN112279662A (en) * | 2020-11-06 | 2021-01-29 | 湘潭海泡石科技有限公司 | Sagger for magnesium aluminate spinel-cordierite calcined lithium battery positive electrode material and preparation method thereof |
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CN112759377A (en) * | 2021-02-07 | 2021-05-07 | 山东万乔集团有限公司 | Sagger for roasting lithium battery positive electrode material and preparation method thereof |
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CN113200752B (en) * | 2021-04-02 | 2023-07-28 | 武汉科技大学 | Shaft kiln lining for roasting lithium battery anode material and preparation method thereof |
CN113416068A (en) * | 2021-07-09 | 2021-09-21 | 阳泉银宇新材料有限责任公司 | Double-layer composite structure sagger for lithium battery positive electrode material and preparation method thereof |
CN113480300A (en) * | 2021-07-13 | 2021-10-08 | 武汉科技大学 | Mullite composite sagger and preparation method thereof |
CN113480300B (en) * | 2021-07-13 | 2023-07-21 | 武汉科技大学 | Mullite composite sagger and preparation method thereof |
CN113387712A (en) * | 2021-08-02 | 2021-09-14 | 湖南荣晟昌新材料科技有限公司 | Sagger formula for producing ternary cathode material and production method |
CN113773067A (en) * | 2021-11-11 | 2021-12-10 | 长沙中瓷新材料科技有限公司 | Sagger based on cordierite and production process thereof |
CN113773067B (en) * | 2021-11-11 | 2022-01-18 | 长沙中瓷新材料科技有限公司 | Sagger based on cordierite and production process thereof |
CN114644525A (en) * | 2022-03-04 | 2022-06-21 | 北方民族大学 | Composite sagger added with waste materials and preparation method thereof |
CN115536406A (en) * | 2022-09-02 | 2022-12-30 | 洛阳欧斯特新材料有限公司 | Sagger for calcining negative electrode material |
CN115466128A (en) * | 2022-09-27 | 2022-12-13 | 中钢集团洛阳耐火材料研究院有限公司 | Sagger with titanium-containing composite layer |
CN116621591A (en) * | 2023-05-17 | 2023-08-22 | 厦门中科金源新能源科技有限公司 | Sagger for lithium battery anode material and preparation method thereof |
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