CN113292349A - Sagger containing calcium hexaluminate composite layer and preparation method thereof - Google Patents
Sagger containing calcium hexaluminate composite layer and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a sagger containing a calcium hexaluminate composite layer and a preparation method thereof, wherein the sagger containing the calcium hexaluminate composite layer is a composite layer sagger and comprises a substrate layer and a calcium hexaluminate composite layer, when the sagger is prepared, a simple tool for applying composite layer powder is adopted, the powder is uniformly applied to the inner surface of the sagger, the calcium hexaluminate composite layer powder and the substrate layer powder are formed into a blank body in one step in a mould pressing mode, and the blank body is fired and formed by a high-temperature kiln, so that the sagger has the beneficial effects that: the calcium hexaluminate, the magnesia alumina spinel, the alumina and the mullite in the calcium hexaluminate composite layer provided by the invention are matched to realize that the composite layer has the advantages of high temperature resistance and corrosion resistance, and meanwhile, the calcium hexaluminate composite layer has equivalent thermal property and good matching with a substrate layer, the composite layer is not easy to separate and fall off, and the service life of the sagger is prolonged; the invention has the advantages of low production cost, simple process, energy saving and environmental protection.
Description
Technical Field
The invention relates to the technical field of composite layer saggers, in particular to a sagger containing a calcium hexaluminate composite layer and a preparation method thereof.
Background
Lithium ion batteries are currently widely used in the fields of mobile communication, energy storage, electric vehicles and the like. The main commercial anode materials at present comprise lithium cobaltate, lithium manganate, lithium iron phosphate and ternary materials, and the preparation method adopts a high-temperature solid phase method to sinter various precursors in a sagger at the temperature of 900-1300 ℃ (pushed slab kiln or roller kiln). The sagger material for firing is mainly cordierite, mullite, quartz and corundum. The sagger is rapidly cooled after being subjected to high temperature in service, the thermal shock resistance of the sagger is reduced along with the increase of the using times, the sagger is easy to crack, and the service life of the sagger is influenced. Meanwhile, in the firing process, the raw materials can be decomposed to generate a lithium compound with strong permeability and reaction activity, so that the sagger is corroded, and the problems of peeling, slag falling, raw material pollution and the like are caused.
With the increasing demand of lithium battery materials and the development trend of high voltage direction, more rigorous requirements are provided for the performance of the sagger, particularly the thermal shock stability and the erosion resistance, and the characteristics are usually difficult to be considered by a single material. The multilayer composite sagger base body is made of materials meeting the function of kiln furniture, the working surface is used as a composite layer and is made of chemical components and structures with excellent erosion resistance, and the synergistic improvement of the thermal shock resistance and the erosion resistance of the sagger can be realized while the economy is considered. However, in practical application, how to realize the combination and the thermal property matching of the composite layer and the sagger substrate is a difficult point and also an important factor for restricting the overall performance of the composite sagger.
At present, the composite layer is mostly made of one or more of zirconia, alumina, spodumene, magnesia and the like. Although several substances have strong corrosion resistance, the cost of the zirconia is high, and the mentioned substances are all thermal expansion substances, so that the composite layer is easy to crack, the adhesive force is reduced, and the protective layer falls off in the process of repeated recycling. And the composite layer is applied by adopting a dipping, spraying or secondary pressing method, so that the process is complex.
The patent technology of ' a sagger with a lithium battery high-temperature corrosion resistant coating and a preparation method thereof ' (CN201610159837.X) ' prepares a sagger body by taking mullite, cordierite and the like as raw materials, and improves the corrosion resistance by dipping glaze on the surface of the sagger body, but adds a dipping step and improves the complexity of the production process.
Disclosure of Invention
The invention aims to provide a sagger containing a calcium hexaluminate composite layer and a preparation method thereof, which aim to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a sagger containing a calcium hexaluminate composite layer comprises composite layer powder, wherein the composite layer powder comprises the following components in percentage by mass: 10-30% of calcium hexaluminate, 40-60% of magnesia-alumina spinel, 15-30% of alumina, 5-20% of mullite, 5-20% of kaolin and the balance of binder or auxiliary blank forming material.
The invention also provides a preparation method of the sagger with the calcium hexaluminate composite layer, which comprises the following steps:
step one, weighing 10-30% of calcium hexaluminate, 40-60% of magnesia alumina spinel, 15-30% of alumina, 5-20% of mullite, 5-20% of kaolin and a binder by mass, placing the materials in a stirrer, stirring the materials uniformly, and ageing the materials to obtain calcium hexaluminate composite layer powder;
step two, when the sagger is pressed to be damaged, cleaning the lower die surface of the die by using a brush;
wherein the mold requires: when the mold is opened, the opening direction of the sagger faces downwards, and the lower mold surface of the mold is arranged on a lower mold plate of a press;
the design requirement of the tool is as follows: the composite layer powder applying tool is internally provided with an opening and sleeved on the lower die surface of the die, and the material baffle is bent to enable the tool to contain corresponding materials without falling;
composite layer application method: the non-opening part between the bottom of the composite layer powder applying tool and the bent baffle plate is filled with composite layer powder, after the composite layer powder applying tool is sleeved on the lower die surface of the die, a scraper is used for scraping the material, the material at the opening of the composite layer powder applying tool falls on the lower die surface of the die, and then the composite layer powder applying tool is removed, so that the composite layer powder is uniformly distributed on the top of the lower die surface of the die;
adding a base material of the sagger, wherein the base material is mullite, cordierite, quartz or corundum base material, scraping the base material, closing the die by a press to complete green body pressing, and uniformly distributing composite layer powder on the inner bottom surface of the sagger product;
step four, naturally airing the sagger product covered with the calcium hexaluminate composite layer, and transferring the sagger product to a drying room for drying;
and fifthly, putting the dried sagger product covered with the calcium hexaluminate composite layer into a high-temperature kiln for sintering to obtain the sagger covered with the calcium hexaluminate composite layer.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
1. the invention has the beneficial effects that: the calcium hexaluminate, the magnesia alumina spinel, the alumina and the mullite in the calcium hexaluminate composite layer provided by the invention are matched to realize that the composite layer has the advantages of high temperature resistance and corrosion resistance, and meanwhile, the calcium hexaluminate composite layer has equivalent thermal property and good matching with a substrate layer, the composite layer is not easy to separate and fall off, and the service life of the sagger is prolonged;
2. according to the sagger, the calcium hexaluminate composite layer and the sagger substrate are optimally matched in characteristics, a spraying, infiltrating or secondary pressing method is not needed, the calcium hexaluminate composite layer powder can be applied to the inner bottom surface of the sagger through primary pressing, and the sagger substrate is effectively compounded through high-temperature sintering;
the invention has the advantages of low production cost, simple process, energy saving and environmental protection, and the manufactured sagger for sintering the lithium ion battery anode material has excellent erosion resistance and long service life.
Drawings
FIG. 1 is a schematic view showing a corresponding relationship between a sagger and a lower mold surface of a mold according to the present invention;
FIG. 2 is a schematic view of a simple tool for applying powder to a composite layer according to the present invention.
In the figure: 1. a sagger product; 2. a lower die surface of the die; 3. applying a simple tool for composite layer powder; 4. the striker plate is bent.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to avoid repetition, the materials and related technical parameters to be related in this embodiment are described in a unified manner as follows, which will not be described in the embodiments:
the MgO content of the magnesium aluminate spinel is more than or equal to 25 wt%; the particle size of the magnesium aluminate spinel is less than or equal to 1.0 mm.
The Al2O3 content of the alumina powder is more than or equal to 98 wt%; the grain diameter of the alumina powder is less than or equal to 0.10mm
The Al2O3 content of the mullite is more than or equal to 65 wt%; the grain diameter of the mullite is less than or equal to 1.0 mm.
The Al2O3 content of the kaolin is more than or equal to 33 wt%. The grain diameter of the kaolin is less than or equal to 0.10 mm.
The main chemical components of the calcium hexaluminate are as follows: more than or equal to 88 weight percent of Al2O3, and more than or equal to 7.6 weight percent of CaO; the volume density of the calcium hexaluminate is more than or equal to 2.8g/cm3, and the particle size of the calcium hexaluminate is less than or equal to 0.10 mm.
The technical scheme provided by the invention is that the sagger containing the calcium hexaluminate composite layer comprises composite layer powder, and is characterized in that the composite layer powder comprises the following components in percentage by mass: 10-30% of calcium hexaluminate, 40-60% of magnesia-alumina spinel, 15-30% of alumina, 5-20% of mullite, 5-20% of kaolin and the balance of binder or auxiliary blank forming material, wherein the sagger takes the calcium hexaluminate as a main anti-erosion component, and other materials are taken as a composite layer of the sagger, the composite layer powder applying simple tool is adopted, one-step blank forming is carried out during die pressing, the bottom size of the composite layer powder applying tool is matched with the top size of a lower die surface of a die, and a bent baffle plate is further arranged at the bottom of the inner wall of the composite layer powder applying tool.
The invention also provides a preparation method of the sagger with the calcium hexaluminate composite layer, which comprises the following steps:
step one, weighing 10-30% of calcium hexaluminate, 40-60% of magnesia alumina spinel, 15-30% of alumina, 5-20% of mullite, 5-20% of kaolin and a binder by mass, placing the materials in a stirrer, stirring the materials uniformly, and ageing the materials to obtain calcium hexaluminate composite layer powder;
step two, when the sagger is pressed to be damaged, cleaning the lower die surface of the die by using a brush;
wherein the mold requires: when the mold is opened, the opening of the sagger product faces downwards, and the lower mold surface 2 of the mold is arranged on the lower mold plate of the press;
the design requirement of the tool is as follows: the composite layer powder applying tool 3 is internally opened and sleeved on the lower die surface 2 of the die, and the baffle plate 4 is bent to enable the tool to contain corresponding materials without falling;
composite layer application method: the non-opening part between the bottom of the composite layer powder applying tool 3 and the bent baffle plate 4 is filled with composite layer powder, after the composite layer powder applying tool is sleeved on the lower die surface of the die, a scraper is used for scraping the material, the material at the opening of the composite layer powder applying tool 3 falls on the lower die surface 2 of the die, and then the composite layer powder applying tool 3 is removed, so that the composite layer powder is uniformly distributed on the top of the lower die surface 2 of the die;
adding a base material of the sagger, wherein the base material is mullite, cordierite, quartz or corundum base material, scraping the base material, closing the die by a press to complete green body pressing, and uniformly distributing composite layer powder on the inner bottom surface of the sagger product 1;
step four, naturally airing the sagger product 1 covered with the calcium hexaluminate composite layer, and transferring the sagger product to a drying room for drying;
step five, putting the dried sagger product 1 covered with the calcium hexaluminate composite layer into a high-temperature kiln for sintering to obtain the sagger covered with the calcium hexaluminate composite layer
The first embodiment is as follows:
a sagger containing a calcium hexaluminate composite layer comprises composite layer powder, wherein the composite layer powder comprises the following components in percentage by mass: 5-18 wt% of calcium hexaluminate, 25-50 wt% of magnesia-alumina spinel, 10-20 wt% of alumina, 10-35 wt% of mullite, 5-10 wt% of kaolin, 5-8 wt% of polyvinyl alcohol solution (the concentration is 3-5 wt%),
step one, mixing 15 wt% of calcium hexaluminate, 40 wt% of magnesia-alumina spinel, 15 wt% of alumina, 20 wt% of mullite, 5 wt% of kaolin and 5 wt% of polyvinyl alcohol solution (the concentration is 3-5 wt%), placing the mixture in a stirrer, stirring until the mixture is uniformly mixed, and ageing for 24 hours to obtain calcium hexaluminate composite layer powder;
secondly, cleaning the lower die surface of the die by using a brush when a sagger blank is pressed, then using a composite powder applying tool 3 to contain the powder calcium hexaluminate composite layer powder prepared in the first step, then sleeving the powder on the lower die surface 2 of the die, using a scraper to strickle off and removing the tool, so that the calcium hexaluminate composite layer powder is uniformly distributed on the inner bottom surface of the sagger blank and has the thickness of 2-3 mm;
adding a base material of the sagger product 1, wherein the base material is conventional mullite, cordierite, quartz or corundum base material, and pressing the base material by a press after the base material is strickled off to complete green body pressing;
step four, naturally airing the sagger product 1 covered with the calcium hexaluminate composite layer, and then transferring the sagger product to a drying room for drying for 48 hours, wherein the drying temperature is controlled to be 90-100 ℃;
and step five, putting the sagger product 1 which is dried in the step four and covered with the calcium hexaluminate composite layer into a high-temperature kiln for sintering, wherein the sintering temperature is 1330-1420 ℃, and the sintering time is 8-12 h, so that the sagger containing the calcium hexaluminate composite layer is prepared.
The sagger containing the calcium hexaluminate composite layer prepared in the example 1 is detected: the breaking strength is 9-12 MPa; when the sagger is used for producing ternary lithium serving as a lithium battery cathode material, the use frequency can reach 52 times, the corrosion resistance is excellent, and the service life is long.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (2)
1. The sagger containing the calcium hexaluminate composite layer comprises composite layer powder, and is characterized in that the composite layer powder comprises the following components in percentage by mass: 10-30% of calcium hexaluminate, 40-60% of magnesia-alumina spinel, 15-30% of alumina, 5-20% of mullite, 5-20% of kaolin and the balance of binder or auxiliary blank forming material.
2. The method for preparing a sagger with a calcium hexaluminate composite layer as claimed in claim 1, comprising the steps of:
step one, weighing 10-30% of calcium hexaluminate, 40-60% of magnesia alumina spinel, 15-30% of alumina, 5-20% of mullite, 5-20% of kaolin and a binder by mass, placing the materials in a stirrer, stirring the materials uniformly, and ageing the materials to obtain calcium hexaluminate composite layer powder;
step two, when the sagger is pressed to be damaged, cleaning the lower die surface of the die by using a brush;
wherein the mold requires: when the mold is opened, the opening direction of the sagger is downward, and the lower mold surface (2) of the mold is arranged on the lower mold plate of the press;
the design requirement of the tool is as follows: the composite layer powder applying tool (3) is internally opened and sleeved on the lower die surface (2) of the die, and the striker plate (4) is bent to enable the tool to contain corresponding materials without falling;
composite layer application method: the non-opening part between the bottom of the composite layer powder applying tool (3) and the bent baffle plate (4) is filled with composite layer powder, after the composite layer powder applying tool is sleeved on the lower die surface of a die, a scraper is used for scraping the material, the material at the opening of the composite layer powder applying tool (3) falls on the lower die surface (2) of the die, and then the composite layer powder applying tool (3) is removed, so that the composite layer powder is uniformly distributed on the top of the lower die surface (2) of the die;
adding a base material of the sagger, wherein the base material is mullite, cordierite, quartz or corundum base material, scraping the base material, closing the die by a press to complete green body pressing, and uniformly distributing composite layer powder on the inner bottom surface of the sagger product (1);
step four, naturally airing the sagger product (1) covered with the calcium hexaluminate composite layer, and transferring the sagger product to a drying room for drying;
and fifthly, putting the dried sagger product (1) covered with the calcium hexaluminate composite layer into a high-temperature kiln for sintering to obtain the sagger covered with the calcium hexaluminate composite layer.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110694463.2A CN113292349B (en) | 2021-06-22 | 2021-06-22 | Sagger containing calcium hexaluminate composite layer and preparation method thereof |
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| 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 |
| CN115353372A (en) * | 2022-08-19 | 2022-11-18 | 武汉科技大学 | Sagger for sintering lithium battery positive electrode material and preparation method thereof |
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