CN112624765A - 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
CN112624765A
CN112624765A CN202011476844.5A CN202011476844A CN112624765A CN 112624765 A CN112624765 A CN 112624765A CN 202011476844 A CN202011476844 A CN 202011476844A CN 112624765 A CN112624765 A CN 112624765A
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China
Prior art keywords
sagger
parts
raw materials
fiber
alumina
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CN202011476844.5A
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CN112624765B (zh
Inventor
李斌
阮丁山
唐盛贺
李玲
吴星宇
李长东
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Hunan Brunp Recycling Technology Co Ltd
Guangdong Brunp Recycling Technology Co Ltd
Hunan Bangpu Automobile Circulation Co Ltd
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Hunan Brunp Recycling Technology Co Ltd
Guangdong Brunp Recycling Technology Co Ltd
Hunan Bangpu Automobile Circulation Co Ltd
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Application filed by Hunan Brunp Recycling Technology Co Ltd, Guangdong Brunp Recycling Technology Co Ltd, Hunan Bangpu Automobile Circulation Co Ltd filed Critical Hunan Brunp Recycling Technology Co Ltd
Priority to CN202011476844.5A priority Critical patent/CN112624765B/zh
Publication of CN112624765A publication Critical patent/CN112624765A/zh
Priority to PCT/CN2021/123395 priority patent/WO2022127314A1/zh
Priority to EP21905243.8A priority patent/EP4265585A4/en
Priority to GB2310083.7A priority patent/GB2616802A/en
Priority to HU2200285A priority patent/HU231545B1/hu
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Publication of CN112624765B publication Critical patent/CN112624765B/zh
Priority to US18/210,097 priority patent/US20230322636A1/en
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Abstract

本发明属于锂过渡金属氧化物材料技术领域，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，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。本发明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
本发明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；
现有技术有的采用硅溶溶液、丙烯酸乳液、乙酸乙烯、煅烧a-Al2O3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；
现有技术还有的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，本发明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，本发明采用以下技术方案：
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；
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。
其中，碳化硅为纯度≥99％的高纯度碳化硅粉体。
优选地，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。
优选地，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。
优选地，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。其中，糊精可以是黄糊精，聚乙烯醇选用浓度小于5wt％的PVA-M。
优选地，所述锂过渡金属氧化物粉末为钴酸锂、锰酸锂，镍酸锂或镍钴锰酸锂中的一种或几种，更具体地，钴酸锂经过掺杂或/和包覆的改性，掺杂的元素是Mg、Al、Ti、Zr、Ni、Mn，La、Y、Si、W中的至少一种，包覆的元素是Mg、Al、Ti、Zr、Ni、Mn，La、Y、Si、W中的至少一种，锂过渡金属氧化物粉末的粒径为微米级，更优选为0.5-5μm。
优选地，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。
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。
具体的喷涂方法为：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。
优选地，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％。
优选地，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％。
优选地，步骤(1)中，所述陈腐的时间为10～24h。
优选地，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。
优选地，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。
优选地，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。
优选地，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。
优选地，步骤(4)中，所述微火处理的温度为50～200℃，处理的时间为5～180min。
本发明的优点：
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，使的匣钵受热更均匀，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，同时极大的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，更好的连接基体、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、本发明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，本发明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
为了对本发明进行深入的理解，下面结合实例对本发明优选实验方案进行描述，以进一步的说明本发明的特点和优点，任何不偏离本发明主旨的变化或者改变能够为本领域的技术人员理解，本发明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，最终得到成品匣钵。
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，最终得到成品匣钵。
实施例3
实施例3的步骤与实施例1一致，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1一致，区别在实施例5中步骤(5)的微米级改性钴酸锂粉末改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：
表1
Figure BDA0002837489950000071
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 BDA0002837489950000081
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 BDA0002837489950000082
Figure BDA0002837489950000091
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。
以上对本发明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发明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发明的方法及其核心思想，包括最佳方式，并且也使得本领域的任何技术人员都能够实践本发明，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，在不脱离本发明原理的前提下，还可以对本发明进行若干改进和修饰，这些改进和修饰也落入本发明权利要求的保护范围内。本发明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，其特征在于，包括基体层和在所述基体层表面上的浅层以及涂覆层；
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，其特征在于，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，其特征在于，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，其特征在于，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。
5.根据权利要求1所述的匣钵，其特征在于，所述锂过渡金属氧化物粉末为钴酸锂、锰酸锂，镍酸锂或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，其特征在于，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任一项所述匣钵的制备方法，其特征在于，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，其特征在于，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，其特征在于，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，其特征在于，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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