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CN109081687A - A kind of highly heatproof and shockproof ceramic crucible and preparation method thereof suitable for calcining anode material of lithium battery - Google Patents

A kind of highly heatproof and shockproof ceramic crucible and preparation method thereof suitable for calcining anode material of lithium battery Download PDF

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CN109081687A
CN109081687A CN201811121863.9A CN201811121863A CN109081687A CN 109081687 A CN109081687 A CN 109081687A CN 201811121863 A CN201811121863 A CN 201811121863A CN 109081687 A CN109081687 A CN 109081687A
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crucible
thermal shock
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lithium battery
ceramic crucible
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CN109081687B (en
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包启富
周健儿
黄武清
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Jingdezhen Ceramic Institute
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Abstract

本发明公开了一种适用于煅烧锂电池正极材料的高抗热震陶瓷坩埚及其制备方法,陶瓷坩埚材料其化学组成为：SiO2 45～60wt%、Al2O3 25～35wt%、Li2O 3～5wt%、ZrO2 3～8wt%、MgO1～3wt%、TiO2 1～5 wt%。经配料、球磨、过筛、压滤脱水、真空练泥、冲压成型、干燥而得到坩埚坯体，最后在还原气氛下进行烧成。本发明坩埚生产成本低、成型性能好，有效提高了产品的抗热震性能、耐碱性能强，能够很好地满足煅烧锂电池正极材料的耐碱使用要求，从而有利于促进坩埚产业的技术进步和应用发展，因此具有广阔的市场前景。The invention discloses a high thermal shock-resistant ceramic crucible suitable for calcining lithium battery cathode materials and a preparation method thereof. The chemical composition of the ceramic crucible material is: SiO 2 45-60 wt%, Al 2 O 3 25-35 wt%, Li 2 O 3~5wt%, ZrO 2 3~8wt%, MgO 1~3wt%, TiO 2 1~5wt%. The crucible body is obtained by batching, ball milling, sieving, dehydration by pressing, vacuum refining, stamping and drying, and finally fired in a reducing atmosphere. The crucible of the present invention has low production cost and good molding performance, effectively improves the thermal shock resistance of the product, has strong alkali resistance, and can well meet the alkali resistance requirements of calcined lithium battery positive electrode materials, thereby helping to promote the technology of the crucible industry Progress and application development, so it has broad market prospects.

Description

A kind of highly heatproof and shockproof ceramic crucible and its system suitable for calcining anode material of lithium battery Preparation Method
Technical field
The invention belongs to technical field of refractory materials, and in particular to a kind of highly resistance suitable for calcining anode material of lithium battery Thermal shock ceramic crucible and preparation method thereof.
Background technique
Ceramic crucible is the important component of refractory material, it is the appearance of fusing and calcining and solid-liquid heating, reaction Device is the basis for guaranteeing chemical reaction and going on smoothly, and prepares the necessary articles of high pure oxide.
The synthesis of anode material of lithium battery needs crucible, currently, it is used to calcine the crucible material of anode material of lithium battery, it is main There is mullite-cordierite material crucible, it is cheap, it easily obtains, so being widely used.But this crucible has fatal lack It falls into, structure is porous, not alkali corrosion resistance, and service life is short, unstable；Meanwhile particle is thick, is easy when in use It falls off, pollutes anode material of lithium battery.So that crucible access times are low, and produce many solid wastes, cause environment dirty Dye, it is difficult to handle.Under current environmental protection pressure and lithium battery price competition pressure, enterprise has to find new crucible material Material, develops alkali corrosion resistance, and fine and close, high thermal shock stability, crucible with long service life are extremely urgent.
Summary of the invention
That the technical problem to be solved in the present invention is to provide a kind of thermal shock resistances is good, alkali resistance is strong, High anti bending strength, cost Low, long service life and the highly heatproof and shockproof ceramic crucible and its system for being suitable for calcining anode material of lithium battery free from environmental pollution Preparation Method.
In order to solve the above technical problems, the technical scheme is that it is a kind of suitable for calcining anode material of lithium battery Highly heatproof and shockproof ceramic crucible, it is characterised in that: use natural mineral raw and industrial chemicals, chemical composition percentage Are as follows: SiO2 45~60wt%, Al2O3 20~35wt%, Li23~5wt% of O, ZrO2 3~8wt%, MgO1~3wt%, TiO2 1~5 wt%。
The ZrO2The raw material used uses for 8%mol yttria-stabilized zirconia powder as resistance to alkaline agent；It is described TiO2The raw material used is 100nm titanium oxide powder below for average grain diameter, is used as sintering aid.
The crucible flexural strength is 70~80MPa, coefficient of expansion α(800~20 DEG C)≤1.0×10-6/ DEG C, fastness to alkali >= 98.5%, 1000~20 DEG C of thermal shock resistance it is air-cooled >=do not split for 25 times.
The preparation method of above-mentioned highly heatproof and shockproof ceramic crucible, it is characterised in that include the following steps:
Step 1: ball-grinding machine is used to be crushed to granularity as D90=45 micron or less the raw material for crucible；
Step 2: according to mixed after the chemical composition percentage ingredient of formula, ball milling, sieving, filter-press dehydration, vacuum practice Mud, punch forming are dried to obtain crucible green body；
Step 3: it is burnt into using reducing atmosphere.
Ball-grinding machine is airflow milling or Raymond mill in the step 1.
The time of ball milling is 3~5h in the step 2.
The system being burnt into the step 3 is to be burnt slowly from room temperature through 9~10h to 1290~1330 DEG C, after keeping the temperature 1~2h, Cooled to room temperature.
The invention has the following advantages:
(1) high-performance low bulk crucible of the present invention has product, and production cost is low and processability is good, and thermal shock resistance is high, production Qualification rate is high；
(2) resistance to alkaline agent is introduced in blank of the present invention, alkaline resistance properties significantly improves；
(3) its flexural strength of high-performance low bulk crucible of the present invention is 70~80MPa, coefficient of expansion α(800~20 DEG C)≤1 ×10-6/ DEG C, fastness to alkali >=98.5%, 1000~20 DEG C of thermal shock resistance it is air-cooled >=do not split, therefore have a vast market for 25 times Prospect.
Specific embodiment
The present invention will be further described in detail with reference to the specific embodiments.
The embodiment of the present invention is suitable for calcining the chemical composition and system of the highly heatproof and shockproof ceramic crucible of anode material of lithium battery Standby technological parameter is as shown in the table.
。
The embodiment of the present invention be suitable for calcine anode material of lithium battery highly heatproof and shockproof ceramic crucible the preparation method is as follows:
Above-mentioned raw material for crucible provided by the invention first has to that hard material and soft feed powder are broken to grain by airflow milling or Raymond mill Degree, hereinafter, after then mixing according to formula ingredient, carries out ball milling, sieving, filter-press dehydration, vacuum pugging, punching for D90=45 micron Molded, drying obtains crucible green body, is finally burnt into.The firing is burnt into using the slow firing technique of reducing flame, i.e., It is burnt slowly from room temperature at porcelain temperature using reducing atmosphere, warm rear cooled to room temperature obtains and is suitable for calcining lithium battery The highly heatproof and shockproof ceramic crucible product of positive electrode.
The performance indicator that the embodiment of the present invention calcines the highly heatproof and shockproof ceramic crucible of anode material of lithium battery is as shown in the table.
。
The test method of above-mentioned performance indicator are as follows:
1, fastness to alkali test method is that the crucible product of firing is taken one piece, is put into 10% sodium hydroxide solution at 105 DEG C Slightly boiled 1h, percentage of the remaining sample mass compared with sample initial mass, the as fastness to alkali of crucible material after corrosion；
2, the coefficient of expansion is measured with thermal expansion coefficient instrument, model DIL402PC；
3, flexural strength is measured with digital display type engineering ceramics bending strength tester, and model is GWQ-20000；
4, thermal shock resistance is burnt sample to 1000 DEG C with electrical kiln, and heat preservation 1h temperature is uniformly taken out afterwards, and electricity consumption fan is air-cooled, and seeing is It is no to burst.

Claims (7)

1.一种适用于煅烧锂电池正极材料的高抗热震陶瓷坩埚，其特征在于：采用天然矿物原料及工业化工原料，其化学组成百分比为：SiO2 45～60wt%、Al2O3 20～35wt%、Li2O 3～5wt%、ZrO2 3～8wt%、MgO1～3wt%、TiO2 1～5 wt%。1. A high thermal shock-resistant ceramic crucible suitable for calcining lithium battery cathode materials, characterized in that: natural mineral raw materials and industrial chemical raw materials are used, and the chemical composition percentages are: SiO 2 45-60wt%, Al 2 O 3 20 ~35wt%, Li 2 O 3~5wt%, ZrO 2 3~8wt%, MgO1~3wt%, TiO 2 1~5wt%. 2.根据权利要求1所述的高抗热震陶瓷坩埚，其特征在于：所述ZrO2采用的原料为8%mol氧化钇稳定氧化锆粉体，其作为耐碱剂使用；所述TiO2采用的原料为平均粒径为100nm以下的氧化钛粉体，其作为烧结助剂使用。2. The high thermal shock-resistant ceramic crucible according to claim 1, characterized in that: said ZrO 2 The raw material adopted is 8%mol yttrium oxide stabilized zirconia powder, which is used as an alkali resistant agent; said TiO 2 The raw material used is titanium oxide powder with an average particle size below 100nm, which is used as a sintering aid. 3.根据权利要求1所述的高抗热震陶瓷坩埚，其特征在于：所述坩埚抗折强度为70～80MPa，膨胀系数为α（800～20℃）≤1.0×10-6/℃，耐碱度≥98.5%，抗热震性能1000～20℃风冷≥25次不裂。3. The high thermal shock-resistant ceramic crucible according to claim 1, characterized in that: the flexural strength of the crucible is 70-80 MPa, and the expansion coefficient is α (800-20°C) ≤ 1.0×10 -6 /°C, Alkali resistance ≥ 98.5%, thermal shock resistance 1000 ~ 20 ℃ air cooling ≥ 25 times without cracking. 4.根据权利要求1-3任一所述高抗热震陶瓷坩埚的制备方法，其特征在于包括如下步骤：4. according to the preparation method of the arbitrary described high thermal shock resistance ceramic crucible of claim 1-3, it is characterized in that comprising the steps: 步骤一：将所述坩埚原料采用球磨设备粉碎至粒度为D90=45微米以下；Step 1: The crucible raw material is pulverized by ball milling equipment to a particle size of D90=45 microns or less; 步骤二：按照配方的化学组成百分比配料后进行混合、球磨、过筛、压滤脱水、真空练泥、冲压成型、干燥得到坩埚坯体；Step 2: Mixing, ball milling, sieving, dehydration by pressure filtration, vacuum mud refining, stamping and drying to obtain a crucible body after batching according to the chemical composition percentage of the formula; 步骤三：采用还原气氛进行烧成。Step 3: firing in a reducing atmosphere. 5.根据权利要求4所述的制备方法，其特征在于：所述步骤一中球磨设备为气流磨或雷蒙磨。5. The preparation method according to claim 4, characterized in that: the ball milling equipment in the step 1 is a jet mill or a Raymond mill. 6.根据权利要求4所述的制备方法，其特征在于：所述步骤二中球磨的时间为3～5h。6. The preparation method according to claim 4, characterized in that: the time for ball milling in the second step is 3-5 hours. 7.根据权利要求4所述的制备方法，其特征在于：所述步骤三中烧成的制度为从室温经9～10h慢烧至1290～1330℃，保温1～2h后，自然冷却至室温。7. The preparation method according to claim 4, characterized in that: the firing system in step 3 is to slowly burn from room temperature to 1290-1330°C for 9-10 hours, keep warm for 1-2 hours, and then cool naturally to room temperature .
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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN113980496A (en) * 2021-09-09 2022-01-28 乳源东阳光磁性材料有限公司 Coating composition, lithium battery ternary cathode material sieving screen and preparation method thereof
CN115504653A (en) * 2022-09-15 2022-12-23 德清三明坩埚有限公司 Thermal shock cracking resistant clay crucible and preparation process thereof

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CN1253125A (en) * 1999-11-08 2000-05-17 苏君道 Non-expansion lithium ceramics and process for preparing its crucible
CN101255062A (en) * 2008-03-29 2008-09-03 山东陶瓷工业协会 Low-cost energy-saving high heat-shake resistant kiln appliance and preparation method thereof
CN101955366A (en) * 2010-10-26 2011-01-26 揭东县热金宝新材料科技有限公司 High performance and large-area fire resistance hollow slab kiln and production method thereof
CN106083017A (en) * 2016-06-22 2016-11-09 景德镇陶瓷大学 A kind of high-performance low bulk crucible and preparation method thereof
DE102017217283B3 (en) * 2017-09-28 2018-07-26 Schott Ag Process for the production of glass ceramic articles by slip casting and their use

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Publication number Priority date Publication date Assignee Title
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CN101255062A (en) * 2008-03-29 2008-09-03 山东陶瓷工业协会 Low-cost energy-saving high heat-shake resistant kiln appliance and preparation method thereof
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CN113980496A (en) * 2021-09-09 2022-01-28 乳源东阳光磁性材料有限公司 Coating composition, lithium battery ternary cathode material sieving screen and preparation method thereof
CN115504653A (en) * 2022-09-15 2022-12-23 德清三明坩埚有限公司 Thermal shock cracking resistant clay crucible and preparation process thereof
CN115504653B (en) * 2022-09-15 2024-01-12 德清三明坩埚有限公司 Preparation process of clay crucible with thermal shock cracking resistance

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