WO2022127314A1 - 一种用于锂过渡金属氧化物烧结的匣钵及其制备方法 - Google Patents

一种用于锂过渡金属氧化物烧结的匣钵及其制备方法 Download PDF

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Publication number
WO2022127314A1
WO2022127314A1 PCT/CN2021/123395 CN2021123395W WO2022127314A1 WO 2022127314 A1 WO2022127314 A1 WO 2022127314A1 CN 2021123395 W CN2021123395 W CN 2021123395W WO 2022127314 A1 WO2022127314 A1 WO 2022127314A1
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Prior art keywords
saggar
parts
raw materials
oxide
magnesia
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PCT/CN2021/123395
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English (en)
French (fr)
Inventor
李斌
阮丁山
唐盛贺
李玲
吴星宇
李长东
Original Assignee
广东邦普循环科技有限公司
湖南邦普循环科技有限公司
湖南邦普汽车循环有限公司
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Application filed by 广东邦普循环科技有限公司, 湖南邦普循环科技有限公司, 湖南邦普汽车循环有限公司 filed Critical 广东邦普循环科技有限公司
Priority to EP21905243.8A priority Critical patent/EP4265585A4/en
Priority to HU2200285A priority patent/HUP2200285A1/hu
Priority to GB2310083.7A priority patent/GB2616802A/en
Publication of WO2022127314A1 publication Critical patent/WO2022127314A1/zh
Priority to US18/210,097 priority patent/US20230322636A1/en

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Definitions

  • the present disclosure relates to the technical field of lithium transition metal oxide materials, in particular to a saggar for sintering lithium transition metal oxides and a preparation method thereof.
  • Lithium transition metal oxide materials include lithium cobalt oxide, lithium nickel oxide, lithium manganate, lithium iron phosphate, lithium nickel cobalt manganate, etc. and their corresponding modified materials. Lithium transition metal oxide materials are used as cathode materials for lithium batteries.
  • high-temperature solid-phase synthesis is generally used in industry, and the high-temperature saggars used in the synthesis process are generally cordierite, mullite, quartz, and magnesium-aluminum tips.
  • High temperature resistant saggars composed of spar, corundum, zircon, etc., of which cordierite, mullite, and magnesia-aluminum spinel are used more.
  • the alkaline lithium oxide will chemically react with the acidic substances and amphoteric oxides in the saggar, so it will erode the saggar and form
  • the precipitation of a compound compound leads to the phenomenon of pulverization, cracking, peeling, and slag removal of the saggar, which greatly reduces the service life of the saggar, and at the same time causes pollution to the material and affects the quality of the product.
  • the application of high temperature and high lithium ratio is more and more common, and higher requirements are also put forward for the performance of saggars for sintering.
  • the semi-molded bowl is immersed in the liquid as a whole, taken out after standing, or the liquid is evenly sprayed on the surface of the semi-molded bowl, then taken out and air-dried, and the air-dried semi-molded bowl is sent to the calciner.
  • the kiln was fired at a temperature of 1400 °C, thereby improving the corrosion resistance of the saggar; then the obtained saggar only improved the corrosion resistance, but the thermal shock stability, strength, thermal expansion coefficient, etc. of the saggar did not improve;
  • Some related technologies use silicon solution, acrylic emulsion, vinyl acetate, calcined a-Al 2 O 3 powder, lightly burned magnesia powder, fused silica powder and zircon powder to coat the surface of the saggar evenly, which can improve the quality of the saggar. Cracking, peeling, slag and other phenomena, but the corrosion resistance, thermal shock stability, strength, thermal expansion coefficient of the saggar have not improved, and the formula of organic compounds is complicated, and it is difficult to control the process stability;
  • the embodiments of the present disclosure provide a saggar for sintering lithium transition metal oxide and the same.
  • the preparation method, the saggar prepared by the method has good corrosion resistance, a small thermal expansion coefficient, and the positive electrode material is not easy to crack, peel, slag and other corrosion phenomena when it is in contact with the saggar, thereby improving the service life of the saggar.
  • the inner surface of the saggar is coated with another material, the operation process is relatively simple, and the use cost is reduced.
  • an embodiment of the present disclosure provides a saggar for lithium transition metal oxide sintering, comprising a base layer, a shallow layer on the surface of the base layer, and a coating layer; wherein,
  • the base layer includes the following raw materials: silicon carbide, magnesia-aluminum spinel, alumina-magnesia-yttrium oxide composite fiber, zircon powder and a binder;
  • the shallow layer includes the following raw materials: silicon carbide, magnesia-aluminum spinel, alumina-titanium oxide composite fiber, yttria-zirconia composite fiber and binder;
  • the coating layer includes the following raw materials: silicon carbide, magnesia-aluminum spinel, magnesia, fibrous zirconia, lithium transition metal oxide powder, and a binder.
  • the silicon carbide is a high-purity silicon carbide powder with a purity of ⁇ 99%.
  • the raw materials of the base layer are in parts by weight: 40-85 parts of silicon carbide, 2-10 parts of magnesia-aluminum spinel, 5-15 parts of alumina-magnesia-yttrium oxide composite fibers, zirconium 5-10 parts of British powder and 2-10 parts of binder; raw materials of the shallow layer are calculated in parts by weight: 30-50 parts of silicon carbide, 10-30 parts of magnesium-aluminum spinel, and 5 parts of alumina-titanium oxide composite fibers ⁇ 20 parts, 5-20 parts of yttrium oxide-zirconia composite fibers and 5-10 parts of binder; raw materials of the coating layer by weight: 5-20 parts of silicon carbide, 5-20 parts of magnesium aluminum spinel parts, 6-10 parts of magnesium oxide, 3-10 parts of fibrous zirconia, 5-25 parts of lithium cobalt oxide powder and 10-20 parts of binder.
  • the magnesia is fibrous magnesia and micro/nano magnesia
  • the mass ratio of the fibrous magnesia to micro/nano magnesia is (3 ⁇ 10):(3 ⁇ 10), wherein,
  • the particle size of the micro-nano magnesium oxide is 10-500 nm.
  • the binding agent is at least one of dextrin, polyvinyl alcohol, polyether-modified polydimethylsilane, or silica-alumina sol.
  • the dextrin can be yellow dextrin
  • the polyvinyl alcohol is selected from PVA-M with a concentration of less than 5 wt%.
  • the lithium transition metal oxide powder is one or more of lithium cobaltate, lithium manganate, lithium nickelate and lithium nickel cobalt manganate.
  • the lithium cobalt oxide is modified by doping and/or coating, and the doping element is at least one of Mg, Al, Ti, Zr, Ni, Mn, La, Y, Si and W , the coating element is at least one of Mg, Al, Ti, Zr, Ni, Mn, La, Y, Si and W, and the particle size of the lithium transition metal oxide powder is micron-scale, in some embodiments, The particle size of the lithium transition metal oxide powder is 0.5-5 ⁇ m.
  • the alumina-magnesia-yttrium oxide composite fiber is formed by stirring and compounding fibrous alumina, fibrous magnesia and fibrous yttria at 50-100°C; the alumina-titanium oxide composite fiber The fiber is made of fiber alumina and fiber titania by stirring and compounding at 50-200 °C; the yttria-zirconia composite fiber is made by stirring and compounding fiber yttria and fiber zirconia at 100-200 °C.
  • An embodiment of the present disclosure provides a preparation method for a lithium transition metal oxide sintering sagger, comprising the following steps:
  • the spraying method is as follows: uniformly spraying the coating agent on the inner surface of the intermediate saggar with a spray gun, and spraying multiple times to make the coating agent as uniform as possible without dripping, convex marks, etc. Cracks appeared in the coating during use.
  • water is used as a medium when the raw materials of the base layer, the shallow layer and the coating layer are mixed and pulped. 4-10% of the total mass of the raw materials, and water in the coating layer accounts for 50-80% of the total mass of the raw materials of the coating layer.
  • the binder in the shallow layer accounts for 4-6% of the total mass of the raw material of the shallow layer
  • the binder in the coating layer accounts for 12-20% of the total mass of the raw material of the coating layer.
  • the stale time is 10-24 hours.
  • the obtained slurry in step (2), can be uniformly distributed on the surface of the primary green body by a cloth machine or manually.
  • step (3) the drying process is to dry the green body in the shade for 15-30 hours under normal temperature and ventilation conditions, and then dry the green body.
  • the sintering temperature is 1320-2000° C.
  • the sintering time is 2-5 h
  • the sintering atmosphere is vacuum or inert.
  • step (4) after the micro-fire treatment, the process of performing spraying and micro-fire treatment is repeated, and the number of spraying and micro-fire treatment is ⁇ 2 times.
  • the temperature of the low-fire treatment is 50-200° C., and the treatment time is 5-180 min.
  • silicon carbide Based on the matrix layer composed of silicon carbide and various fiber composite oxides, in order to overcome the shortcomings of poor strength of the saggar and improve the overall strength of the saggar, at the same time, silicon carbide has the characteristics of strong thermal radiation ability, which reduces to a certain extent. The energy consumption makes the saggar more evenly heated and easier to relieve stress.
  • Fiber products such as alumina-magnesia-yttrium oxide composite fibers, alumina-titanium oxide composite fibers, and yttria-zirconia composite fibers in the matrix and shallow layers have excellent corrosion resistance, which can improve the corrosion resistance to a certain extent. , Due to the easy diffusion of magnesium oxide, etc., the structural stability of the substrate, shallow layer and coating layer is improved.
  • the similarity between the corresponding composition and the lithium transition metal oxide gradually increases, which greatly reduces the reaction between the saggar and the transition metal oxide, and inhibits surface cracking, peeling, slag, etc. Corrosion phenomenon, improve the corrosion resistance of the saggar.
  • the fibrous material is phase-transformed and toughened, and the fiber is toughened.
  • the fibrous material forms a large number of three-dimensional network structure composite oxides in the saggar, which can better connect the matrix, the shallow layer and the coating layer.
  • the fibrous material also inhibits the peeling of the surface layer to a certain extent, thereby greatly improving the service life of the saggar.
  • the preparation method of the embodiment of the present disclosure has the advantages of simple process operation, low cost and high production efficiency; and the spraying amount of the coating layer is controllable and the thickness is controllable.
  • the existence of the middle fiber layer in the saggar of the example is conducive to the separation of the coating layer, the base layer and the shallow layer as a whole, so the base layer can be recycled, which reduces the discharge of solid waste and is beneficial to the improvement of the production efficiency of the enterprise.
  • a preparation method for lithium transition metal oxide sintering sagger comprising the following steps:
  • step (1) The base layer raw material in step (1) is mixed and pulped with deionized water as a medium, and the amount of deionized water is 6% of the total mass of the base layer raw material. After the mixed slurry is evenly stirred, it is aged for 15 hours, and then Press the slurry through the molding equipment to obtain the primary green body;
  • step (3) mixing and pulping the shallow-layer raw materials in step (3) with deionized water as a medium, and the amount of deionized water is 5% of the total mass of the shallow-layer raw materials.
  • the mixed slurry is evenly stirred, the mixed slurry is mixed It is evenly distributed on the surface of the base layer to form the required thickness, and is pressed and molded by the molding equipment again to obtain a green body; it is dried at room temperature, then dried, and then sintered at 1350 ° C for 3 hours to obtain an intermediate saggar;
  • a preparation method for lithium transition metal oxide sintering sagger comprising the following steps:
  • step (3) mixing and pulping the shallow-layer raw materials of step (3) with deionized water as a medium, and the amount of deionized water is 10% of the total mass of the shallow-layer raw materials.
  • the mixed slurry is evenly stirred, the mixed slurry is mixed. It is evenly distributed on the surface of the base layer to form the required thickness, and is pressed and molded by the molding equipment again to obtain a green body; it is dried at room temperature, then dried, and then sintered at 1350 ° C for 4 hours to obtain an intermediate saggar;
  • the coating layer raw material of step (5) is mixed and pulped with deionized water as a medium, and the consumption of deionized water is 70% of the total mass of the coating layer raw material; the coating agent is obtained after the raw materials are mixed evenly, The coating agent was evenly sprayed on the inner surface of the intermediate saggar, and the second spraying was continued after 10 min of micro-fire treatment at 80° C., and the finished saggar was obtained by 50° C. micro-fire treatment for 20 min.
  • Example 3 The steps of Example 3 are basically the same as those of Example 1, except that the binding agent used in Example 3 is polyether-modified polydimethylsilane.
  • Example 4 The steps of Example 4 are basically the same as those of Example 1, except that the binding agent used in Example 4 is PVA-M.
  • Example 5 The steps of Example 5 are basically the same as those of Example 1, except that the micron-scale modified lithium cobalt oxide powder in step (5) in Example 5 is replaced with micron-scale nickel-cobalt lithium manganate oxide.
  • Comparative Example 1 The steps in Comparative Example 1 are basically the same as those in Example 1, except that in Comparative Example 1, only steps (1) and (2) are performed, and the obtained primary green body is directly sintered into a saggar.
  • Comparative Example 2 The steps of Comparative Example 2 are basically the same as those of Example 1, except that in Comparative Example 2, only steps (1) to (4) are carried out, and then the obtained green body is directly sintered into a saggar.
  • Comparative Example 3 The steps of Comparative Example 3 are basically the same as those of Example 1, the difference is that in Step (5) of Comparative Example 3, no micron-sized modified lithium cobalt oxide powder is added to the coating layer.
  • Comparative Example 4 The steps of Comparative Example 4 are basically the same as those of Example 1, except that no fiber oxide is added to the coating layer in Step (5) of Comparative Example 4.
  • Comparative Example 5 are basically the same as those of Example 1, except that no fiber oxide is added to the shallow layer of Step (3) in Comparative Example 5.
  • Comparative Example 6 The steps of Comparative Example 6 are basically the same as those of Example 1, the difference is that only Step 1, Step 2, Step 5 and Step 6 are performed in Comparative Example 6.
  • Comparative Example 7 The steps of Comparative Example 7 are basically the same as those of Example 1, except that no binding agent is used in Comparative Example 7.
  • Table 1 is the saggars obtained from the treatment of Examples 1-2 and Comparative Examples 1-6, and 8 saggars were randomly selected for each example, and the service life of the saggars was tested, as shown in Table 1 below:
  • Example 1 when the 8 saggars obtained in Example 1 and Example 2 were used 15 times, none of the saggars were scrapped, indicating that high-purity silicon carbide powder, magnesium-aluminum spinel, oxidized Aluminum-magnesium oxide-yttrium oxide composite fiber, zircon powder, silica-alumina sol and water, high-purity silicon carbide powder, magnesium-aluminum spinel, alumina-titanium oxide composite fiber, yttria-zirconia composite fiber for the shallow layer Fiber and silica-alumina sol and water, high-purity silicon carbide powder, magnesium-aluminum spinel, fiber-magnesium oxide, fiber-zirconia, micro-nano magnesium oxide, micron-grade modified lithium cobalt oxide powder and silicon-alumina are used for the coating layer
  • the saggar obtained by the combined action of sol and water has good thermal shock stability, strong corrosion resistance, and high saggar strength, which is reflected in the
  • Example 3 only one saggar that was stuck to the bottom and was scrapped appeared.
  • Comparative Example 7 a series of corrosion, falling off, and corrosion occurred in the saggar that did not use the binding agent. Slag, cracking, sticking to the bottom phenomenon.
  • Table 3 shows the material quality changes of the sintering reaction raw materials in the saggers of Example 1 and Comparative Examples 1 and 2 before and after being sintered in the furnace.
  • the material quality before and after sintering of the raw materials for the sintering reaction in the saggar of Example 1 has a small change, and the average value is 0.0037kg, which indicates that the material has less corrosion to the saggar, and at the same time, the material in the saggar enters the material. less, less pollution to the material, thus improving the service life of the saggar; the average increase of 0.024kg in Comparative Example 1, indicating that part of the material in the saggar of Comparative Example 1 fell off, and the slag fell off and was corroded, so that the material in the saggar entered the material.

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Abstract

一种用于锂过渡金属氧化物烧结的匣钵及其制备方法，该匣钵包括基体层和在基体层表面上的浅层以及涂覆层，基体层包括以下原料：碳化硅、镁铝尖晶石、氧化铝-氧化镁-氧化钇复合纤维、锆英粉和结合剂，浅层包括以下原料：碳化硅、镁铝尖晶石、氧化铝-氧化钛复合纤维、氧化钇-氧化锆复合纤维和结合剂，涂覆层包括以下原料：碳化硅、镁铝尖晶石、氧化镁、纤维氧化锆、锂过渡金属氧化物粉末和结合剂。本公开实施例匣钵具有良好的耐腐蚀性能，较小的热膨胀系数，正极材料与该匣钵接触时不易开裂、起皮、掉渣等腐蚀现象，从而提高匣钵使用寿命。

Description

一种用于锂过渡金属氧化物烧结的匣钵及其制备方法 技术领域
本公开涉及锂过渡金属氧化物材料技术领域，特别是涉及一种用于锂过渡金属氧化物烧结的匣钵及其制备方法。
背景技术
锂过渡金属氧化物材料包括钴酸锂、镍酸锂、锰酸锂、磷酸铁锂、镍钴锰酸锂等以及其对应的改性材料。锂过渡金属氧化物材料作为锂电池正极材料，目前工业上一般都采用高温固相合成法，而合成过程中所用到的耐高温匣钵一般为堇青石、莫来石、石英质、镁铝尖晶石、刚玉质、锆英石等组成的耐高温匣钵，其中堇青石、莫来石、镁铝尖晶石用得较多。然而在合成正极材料过程中会分解产生渗透和反应活性强的氧化锂，在高温下碱性氧化锂与匣钵中的酸性物质和两性氧化物发生化学反应，因此会对匣钵产生侵蚀，形成一种复合化合物并析出导致匣钵粉化、开裂、起皮、掉渣等现象，使得匣钵的使用寿命大大降低，同时对材料造成污染，影响了产品质量。随着锂过渡金属氧化物材料向着高电压方向发展，高温高锂比应用越发普遍，进而对烧结用匣钵的性能也提出了更高的要求。
目前，国内匣钵的使用寿命较短，国外进口匣钵成本又较高，因此，如何提高烧结用匣钵的使用寿命，具有重要意义。
现有技术有的采用半成型钵体整体浸入料液中，静置后取出或者将料液均匀的喷涂在半成型钵体的表面，然后取出风干，将风干后的半成型钵体送入烧成窑，以1400℃的温度进行烧制，从而提高了匣钵抗腐蚀能力；然后所得匣钵只是抗腐蚀能力提高，匣钵的热震稳定性、强度、热膨胀系数等并未改善；
一些相关技术采用硅溶溶液、丙烯酸乳液、乙酸乙烯、煅烧a-Al 2O 3粉末、轻烧氧化镁粉末、熔融石英粉与锆英粉等混匀涂覆在匣钵表面，可以改善匣钵开裂、起皮、掉渣等现象，但匣钵的抗腐蚀能力、热震稳定性、强度、热膨胀系数等并未改善，同时用到有机物配方复杂，工艺稳定性把控较难；
还有一些相关技术通过回收的铝酸钠制备氧化铝，将氧化铝与SiC等其它原料制备匣钵修复材料，修复所得匣钵能够减少掉渣，提高使用次数，但是SiC涂料的使用次数往往受到限制，随着使用次数的不断增加，几乎都会出现圈裂现象，造成较多落渣缺陷的情况，同时匣钵的 热震稳定性，强度，热膨胀系数并未改善。
发明内容
为了至少在一定程度上解决匣钵强度差、抗热震差、匣钵易受侵蚀现象及表面易脱落等问题，本公开实施例提供一种用于锂过渡金属氧化物烧结的匣钵及其制备方法，通过该方法制得的匣钵具有良好的耐腐蚀性能，较小的热膨胀系数，正极材料与该匣钵接触时不易开裂、起皮、掉渣等腐蚀现象，从而提高匣钵使用寿命，同时采用在匣钵内表层涂覆另外一种材料，操作工艺较简单，降低使用成本。
为实现上述目的，本公开实施例提供了一种用于锂过渡金属氧化物烧结的匣钵，包括基体层和在所述基体层表面上的浅层以及涂覆层；其中，
所述基体层包括以下原料：碳化硅、镁铝尖晶石、氧化铝-氧化镁-氧化钇复合纤维、锆英粉和结合剂；
所述浅层包括以下原料：碳化硅、镁铝尖晶石、氧化铝-氧化钛复合纤维、氧化钇-氧化锆复合纤维和结合剂；
所述涂覆层包括以下原料：碳化硅、镁铝尖晶石、氧化镁、纤维氧化锆、锂过渡金属氧化物粉末和结合剂。
在一些实施例中，碳化硅为纯度≥99％的高纯度碳化硅粉体。
在一些实施例中，所述基体层的原料按重量份计：碳化硅40～85份、镁铝尖晶石2～10份、氧化铝-氧化镁-氧化钇复合纤维5～15份、锆英粉5～10份和结合剂2～10份；所述浅层的原料按重量份计：碳化硅30～50份、镁铝尖晶石10～30份、氧化铝-氧化钛复合纤维5～20份、氧化钇-氧化锆复合纤维5～20份和结合剂5～10份；所述涂覆层的原料按重量份计：碳化硅5～20份、镁铝尖晶石5～20份、氧化镁6～10份、纤维氧化锆3～10份、钴酸锂粉末5～25份和结合剂10～20份。
在一些实施例中，所述氧化镁为纤维氧化镁和微纳级氧化镁，所述纤维氧化镁和微纳级氧化镁的质量比为(3～10):(3～10)，其中，微纳级氧化镁的粒径为10～500nm。
在一些实施例中，所述结合剂为糊精、聚乙烯醇、聚醚改性聚二甲基硅烷或硅铝溶胶中的至少一种。在一些实施例中，糊精可以是黄糊精，聚乙烯醇选用浓度小于5wt％的PVA-M。
在一些实施例中，所述锂过渡金属氧化物粉末为钴酸锂、锰酸锂、镍酸锂和镍钴锰酸锂中的一种或几种。在一些实施例中，钴酸锂经过掺杂和/或包覆的改性，掺杂的元素是Mg、Al、Ti、Zr、Ni、Mn、La、Y、Si和W中的至少一种，包覆的元素是Mg、Al、Ti、Zr、Ni、Mn、La、Y、Si和W中的至少一种，锂过渡金属氧化物粉末的粒径为微米级，在一些实施 例中，锂过渡金属氧化物粉末的粒径为0.5-5μm。
在一些实施例中，所述氧化铝-氧化镁-氧化钇复合纤维是由纤维氧化铝、纤维氧化镁和纤维氧化钇在50～100℃下搅拌复合而成；所述氧化铝-氧化钛复合纤维是由纤维氧化铝和纤维氧化钛在50～200℃下搅拌复合而成；所述氧化钇-氧化锆复合纤维是由纤维氧化钇和纤维氧化锆在100～200℃下搅拌复合而成。
本公开实施例提供了一种用于锂过渡金属氧化物烧结匣钵的制备方法，包括如下步骤：
(1)将所述基体层的原料混合制浆，经陈腐处理后将所得浆料压制成型，得到初级生坯；
(2)将所述浅层的原料混合制浆，然后将所得浆料均匀涂布在所述初级生坯的表面，再次压制成型，得到生坯；
(3)将所述生坯进行干燥、烧结，得到中间品匣钵；
(4)将所述涂覆层的原料混合制浆得到涂覆剂，将涂覆剂喷涂在所述中间品匣钵的内表面，再进行微火处理，制得成品匣钵。
在一些实施例中，喷涂方法为：将涂覆剂用喷枪均匀喷涂于中间品匣钵的内表面，多次喷涂，使涂覆剂尽量均匀，不能出现滴落、凸痕等，以防止在使用过程中涂覆层出现龟裂。
在一些实施例中，基体层、浅层和涂覆层的原料进行混合制浆时采用水作为介质，基体层中水占基体层原料总质量的4～10％，浅层中水占浅层原料总质量的4～10％，涂覆层中水占涂覆层原料总质量的50～80％。
在一些实施例中，所述浅层中的结合剂占浅层原料总质量的4～6％，所述涂覆层中的结合剂占涂覆层原料总质量的12～20％。
在一些实施例中，步骤(1)中，所述陈腐的时间为10～24h。
在一些实施例中，步骤(2)中，可通过布料机或者人工将所得浆料均匀分布在初级生坯表面。
在一些实施例中，步骤(3)中，所述干燥的过程是将生坯在常温通风条件下阴干15～30h，而后进行烘干。
在一些实施例中，步骤(3)中，所述烧结的温度为1320～2000℃，烧结的时间为2～5h，烧结的气氛为真空或惰性。
在一些实施例中，步骤(4)中，所述微火处理后还包括再重复进行喷涂和微火处理的工序，所述进行喷涂和微火处理的次数≥2次。
在一些实施例中，步骤(4)中，所述微火处理的温度为50～200℃，处理的时间为5～180min。
本公开实施例的优点：
1、基于碳化硅及多种纤维复合氧化物构成的基体层，以此克服匣钵强度差等缺点，提高匣钵的整体强度，同时碳化硅具有热辐射能力强的特点，在一定程度上降低能耗，使得匣钵受热更均匀，更易消除应力。
2、基体及浅层的氧化铝-氧化镁-氧化钇复合纤维、氧化铝-氧化钛复合纤维、氧化钇-氧化锆复合纤维等纤维制品具有优异耐腐蚀性能，在一定程度上提高抗腐蚀性能，由于氧化镁等容易扩散，提高基体、浅层及涂覆层的结构稳定性。
3、涂覆层中易扩散纤维氧化物及微米级锂过渡金属氧化物粉末的加入，使得涂覆层和锂过渡金属氧化物部分成分相似，提高匣钵表层的抗侵蚀能力，抑制表层脱落，提高了匣钵使用寿命，同时极大地提高了锂过度金属氧化物的纯度，提高合格率。
4、从浅层部分到涂覆层部分，其对应成分与锂过渡金属氧化物成份相似度逐渐升高，极大降低匣钵与过渡金属氧化物反应，抑制表层开裂、起皮、掉渣等腐蚀现象，提高匣钵耐腐蚀性。
5、整个结构中纤维物质相变增韧、纤维增韧，纤维状物质在匣钵中形成了大量的三维网状结构复合氧化物，更好地连接基体、浅层及涂覆层，引入的纤维状物质也在一定程度上抑制表层脱落，从而大大提高了匣钵的使用寿命。
6、本公开实施例的制备方法工艺操作简单、成本低廉且生产效率高；并且涂覆层喷涂量可控，厚度可控，区别于传统对于在烧结所得产品进行表面处理的工艺，本公开实施例的匣钵由于中间纤维层的存在，有利于涂覆层、基体层及浅层整体的分离，因此基体层可回收利用，减少了固体垃圾的排放，有利于企业生产效益的提高。
具体实施方式
为了对本公开进行深入的理解，下面结合实施例对本公开一些实验方案进行描述，以更好地说明本公开的特点和优点，任何不偏离本公开主旨的变化或者改变能够为本领域的技术人员理解，本公开的保护范围由所属权利要求范围确定。
实施例1
一种用于锂过渡金属氧化物烧结匣钵的制备方法，包括以下步骤：
(1)基体层原料总和100份，准备70份高纯度碳化硅粉体、5份镁铝尖晶石、10份氧化铝-氧化镁-氧化钇复合纤维和5份锆英粉，然后加入基体层原料总质量10％的硅铝溶胶作为结合剂；
(2)将步骤(1)的基体层原料以去离子水作为介质进行混合制浆，去离子水的用量为基体层原料总质量的6％，待混合浆料搅拌均匀后，陈腐15h，然后将浆料通过成型设备压制 型，得到初级生坯；
(3)浅层原料总和100份，准备50份高纯度碳化硅粉体、镁铝尖晶石20份、氧化铝-氧化钛复合纤维15份、氧化钇-氧化锆复合纤维10份，然后加入浅层原料总质量5％的硅铝溶胶作为结合剂；
(4)将步骤(3)的浅层原料以去离子水作为介质进行混合制浆，去离子水的用量为浅层原料总质量的5％，待混合浆料搅拌均匀后，将混合浆料均匀分布在基体层表面形成所需厚度，再次通过成型设备压制成型，得到生坯；在常温下干燥处理，然后进行烘干，继而在1350℃条件下烧结3h，得到中间品匣钵；
(5)涂覆层原料总和100份，准备20份高纯度碳化硅粉体，镁铝尖晶石10份，纤维氧化镁10份，纤维氧化锆10份，微纳级氧化镁10份，微米级改性钴酸锂粉末20份，然后加入涂覆层原料总质量20％的硅铝溶胶作为结合剂；
(6)将步骤(5)的涂覆层原料以去离子水作为介质进行混合制浆，去离子水的用量为涂覆层原料总质量的60％；待原料混合均匀后得到涂覆剂，将涂覆剂均匀喷涂到中间品匣钵的内表面，80℃微火处理10min后继续第二次喷涂，50℃微火处理20min，得到成品匣钵。
实施例2
一种用于锂过渡金属氧化物烧结匣钵的制备方法，包括以下步骤：
(1)基体层原料总和100份，准备65份高纯度碳化硅粉体、10份镁铝尖晶石、15份氧化铝-氧化镁-氧化钇复合纤维和5份锆英粉，然后加入基体层原料总质量5％的硅铝溶胶作为结合剂；
(2)将步骤(1)的基体层原料以去离子水作为介质进行混合制浆，去离子水的用量为基体层原料总质量的10％，待混合浆料搅拌均匀后，陈腐15h，然后将浆料通过成型设备压制型，得到初级生坯；
(3)浅层原料总和100份，准备40份高纯度碳化硅粉体、镁铝尖晶石20份、氧化铝-氧化钛复合纤维20份、氧化钇-氧化锆复合纤维10份，然后加入浅层原料总质量10％的硅铝溶胶作为结合剂；
(4)将步骤(3)的浅层原料以去离子水作为介质进行混合制浆，去离子水的用量为浅层原料总质量的10％，待混合浆料搅拌均匀后，将混合浆料均匀分布在基体层表面形成所需厚度，再次通过成型设备压制成型，得到生坯；在常温下干燥处理，然后进行烘干，继而在1350℃条件下烧结4h，得到中间品匣钵；
(5)涂覆层原料总和100份，准备20份高纯度碳化硅粉体，镁铝尖晶石20份，纤维氧 化镁5份，纤维氧化锆10份，微纳级氧化镁5份，微米级改性钴酸锂粉末25份，然后加入涂覆层原料总质量15％的硅铝溶胶作为结合剂；
(6)将步骤(5)的涂覆层原料以去离子水作为介质进行混合制浆，去离子水的用量为涂覆层原料总质量的70％；待原料混合均匀后得到涂覆剂，将涂覆剂均匀喷涂到中间品匣钵的内表面，80℃微火处理10min后继续第二次喷涂，50℃微火处理20min，得到成品匣钵。
实施例3
实施例3的步骤与实施例1基本上一致，区别在于实施例3使用的结合剂为聚醚改性聚二甲基硅烷。
实施例4
实施例4的步骤与实施例1基本上一致，区别在于实施例4使用的结合剂为PVA-M。
实施例5
实施例5的步骤与实施例1基本上一致，区别在于实施例5中步骤(5)的微米级改性钴酸锂粉末替换为微米级镍钴锰酸锂氧化物。
对比例1
对比例1与实施例1的步骤基本上一致，区别在于对比例1只进行步骤(1)和步骤(2)，将得到的初级生坯直接烧结成匣钵。
对比例2
对比例2与实施例1的步骤基本上一致，区别在于对比例2只进行步骤(1)～步骤(4)，然后将得到的生坯直接烧结成匣钵。
对比例3
对比例3与实施例1的步骤基本上一致，区别在于对比例3中步骤(5)涂覆层未加入微米级改性钴酸锂粉末。
对比例4
对比例4与实施例1的步骤基本上一致，区别在于对比例4中步骤(5)涂覆层未加入纤维氧化物。
对比例5
对比例5与实施例1的步骤基本上一致，区别在于对比例5中步骤(3)浅层未加入纤维氧化物。
对比例6
对比例6与实施例1的步骤基本上一致，区别在于对比例6中只进行步骤1、步骤2、步骤5以及步骤6。
对比例7
对比例7与实施例1的步骤基本上一致，区别在于对比例7中未使用结合剂。
表1为实施例1-2以及对比例1-6处理所得匣钵，每个例子随机抽取8个匣钵，进行匣钵使用寿命测试，具体如下表1所示：
表1
Figure PCTCN2021123395-appb-000001
由表1可知，实施例1和实施例2所得8个匣钵，使用15次数时，所有匣钵未出现一例报废现象，说明生胚层使用高纯度碳化硅粉体、镁铝尖晶石、氧化铝-氧化镁-氧化钇复合纤维、锆英粉以及硅铝溶胶和水，浅层使用高纯度碳化硅粉体、镁铝尖晶石、氧化铝-氧化钛复合纤维、氧化钇-氧化锆复合纤维及硅铝溶胶和水，涂覆层使用高纯度碳化硅粉体，镁铝尖晶石，纤维氧化镁，纤维氧化锆，微纳级氧化镁，微米级别改性钴酸锂粉末及硅铝溶胶和水，共同作用所得到的匣钵具有的热震稳定性好，抗腐蚀性强、匣钵强度高等现象，体现在匣钵长使用次数上；对比例1直接使用初级生胚直接烧结所得匣钵，在使用过程中出现了一系列的脱皮、掉渣、开裂、粘底现象；对比例2由于缺少涂覆层，匣钵内层容易被材料腐蚀，而出现粘底现象，使得部分匣钵使用寿命降低；对比例3缺少微米级改性钴酸锂粉末，使得表层容易污染，脱皮掉渣的现象；对比例4匣钵使用15次，有4个匣钵由于开裂现象而导致报废，其原因是由于表层缺少纤维氧化物，结构稳定性降低；对比例5和6所有匣钵都未达到15次，其中原因是未添加纤维氧化物，匣钵的抗热震能力减弱，耐腐蚀能力减弱，而出现一系列脱落，掉粉，开裂现象。
表2为实施例3-5以及对比例7处理所得匣钵，每个例子随机抽取8个匣钵，进行匣钵使用寿命测试，具体如下表2：
表2
Figure PCTCN2021123395-appb-000002
由表2可知，使用不同的结合剂对匣钵的整体使用寿命影响较小，实施例3中仅出现一个粘底报废的匣钵，对比例7未使用结合剂匣钵出现一系列腐蚀、掉渣、开裂、粘底现象。
表3为实施例1与对比例1和2匣钵中的烧结反应原料在入炉烧结前后的物料质量变化。
表3
Figure PCTCN2021123395-appb-000003
由表3可知，在实施例1匣钵中进行烧结反应的原料烧结前后的物料质量变化较小，平均值为0.0037kg，说明材料对匣钵腐蚀较小，同时匣钵内的物质进入材料中较少，对材料污 染小，从而提高匣钵使用寿命；对比例1平均增加了0.024kg，说明对比例1匣钵中部分物质发生脱落，掉渣、被腐蚀现象使得匣钵内物质进入材料中，对材料造成污染，从而匣钵成分发生变化，也使得匣钵寿命较短；对比例2平均增加了0.0103kg，说明有匣钵少量物质进入材料，对材料造成污染，匣钵寿命次之。
以上对本公开实施例提供的用于锂过渡金属氧化物烧结的匣钵及其制备方法进行了详细的介绍，本文中应用了具体实施例对本公开的原理及实施方式进行了阐述，以上实施例的说明只是用于帮助理解本公开的方法及其核心思想，包括更好的方式，并且也使得本领域的任何技术人员都能够实践本公开的实施例，包括制造和使用任何装置或系统，和实施任何结合的方法。应当指出，对于本技术领域的普通技术人员来说，在不脱离本公开原理的前提下，还可以对本公开的实施例进行若干改进和修饰，这些改进和修饰也落入本公开权利要求的保护范围内。本公开专利保护的范围通过权利要求来限定，并可包括本领域技术人员能够想到的其他实施例。如果这些其他实施例具有不是不同于权利要求文字表述的结构要素，或者如果它们包括与权利要求的文字表述无实质差异的等同结构要素，那么这些其他实施例也应包含在权利要求的范围内。

Claims (10)

  1. 一种用于锂过渡金属氧化物烧结的匣钵，包括基体层和在所述基体层表面上的浅层以及涂覆层；其中，
    所述基体层包括以下原料：碳化硅、镁铝尖晶石、氧化铝-氧化镁-氧化钇复合纤维、锆英粉和结合剂；
    所述浅层包括以下原料：碳化硅、镁铝尖晶石、氧化铝-氧化钛复合纤维、氧化钇-氧化锆复合纤维和结合剂；
    所述涂覆层包括以下原料：碳化硅、镁铝尖晶石、氧化镁、纤维氧化锆、锂过渡金属氧化物粉末和结合剂。
  2. 根据权利要求1所述的匣钵，其中，所述基体层的原料按重量份计：碳化硅40～85份、镁铝尖晶石2～10份、氧化铝-氧化镁-氧化钇复合纤维5～15份、锆英粉5～10份和结合剂2～10份；所述浅层的原料按重量份计：碳化硅30～50份、镁铝尖晶石10～30份、氧化铝-氧化钛复合纤维5～20份、氧化钇-氧化锆复合纤维5～20份和结合剂5～10份；所述涂覆层的原料按重量份计：碳化硅5～20份、镁铝尖晶石5～20份、氧化镁6～10份、纤维氧化锆3～10份、钴酸锂粉末5～25份和结合剂10～20份。
  3. 根据权利要求1所述的匣钵，其中，所述氧化镁为纤维氧化镁和微纳级氧化镁，纤维氧化镁和微纳级氧化镁的质量比为(3～10):(3～10)。
  4. 根据权利要求1所述的匣钵，其中，所述结合剂为糊精、聚乙烯醇、聚醚改性聚二甲基硅烷和硅铝溶胶中的至少一种。
  5. 根据权利要求1所述的匣钵，其中，所述锂过渡金属氧化物粉末为钴酸锂、锰酸锂，镍酸锂和镍钴锰酸锂中的一种或几种。
  6. 根据权利要求1所述的匣钵，其中，所述氧化铝-氧化镁-氧化钇复合纤维是由纤维氧化铝、纤维氧化镁和纤维氧化钇在50～100℃下搅拌复合而成；所述氧化铝-氧化钛复合纤维是由纤维氧化铝和纤维氧化钛在50～200℃下搅拌复合而成；所述氧化钇-氧化锆复合纤维是由纤维氧化钇和纤维氧化锆在100～200℃下搅拌复合而成。
  7. 权利要求1-6中任一项所述的匣钵的制备方法，包括如下步骤：
    (1)将所述基体层的原料混合制浆，经陈腐处理后将所得浆料压制成型，得到初级生坯；
    (2)将所述浅层的原料混合制浆，然后将所得浆料涂布在所述初级生坯的表面，再次压制成型，得到生坯；
    (3)将所述生坯进行干燥、烧结，得到中间品匣钵；
    (4)将所述涂覆层的原料混合制浆得到涂覆剂，将涂覆剂喷涂在所述中间品匣钵的内表面，再进行微火处理，制得成品匣钵。
  8. 根据权利要求7所述的制备方法，其中，基体层、浅层和涂覆层的原料进行混合制浆时采用水作为介质，基体层中水占基体层原料总质量的4～10％，浅层中水占浅层原料总质量的4～10％，涂覆层中水占涂覆层原料总质量的50～80％。
  9. 根据权利要求7所述的制备方法，其中，所述浅层中的结合剂占浅层原料总质量的4～6％，所述涂覆层中的结合剂占涂覆层原料总质量的12～20％。
  10. 根据权利要求7所述的制备方法，其中，步骤(4)中，所述微火处理后还包括再重复进行喷涂和微火处理的工序，所述进行喷涂和微火处理的次数≥2次。
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