CN109219588A - 敞口容器及其用途 - Google Patents

敞口容器及其用途 Download PDF

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Publication number
CN109219588A
CN109219588A CN201780034243.9A CN201780034243A CN109219588A CN 109219588 A CN109219588 A CN 109219588A CN 201780034243 A CN201780034243 A CN 201780034243A CN 109219588 A CN109219588 A CN 109219588A
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component
oxide
green compact
container
container according
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B·卡洛
W·达洛兹
M·L·潘丘拉
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BASF SE
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BASF SE
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    • C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
    • C04B37/021—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles in a direct manner, e.g. direct copper bonding [DCB]
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00—Crucible or pot furnaces
    • F27B14/08—Details peculiar to crucible or pot furnaces
    • F27B14/10—Crucibles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/18—Layered products comprising a layer of metal comprising iron or steel
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    • B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
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    • C01G45/1242—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [Mn2O4]-, e.g. LiMn2O4, Li[MxMn2-x]O4
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Abstract

选自坩埚、平底锅、敞口杯和烧箱的容器，其基本上包含两种组分，其中：(A)一种组分为陶瓷基体复合材料，且(B)第二组分选自金属或合金，且其中组分(A)为内部组分。

Description

敞口容器及其用途
本发明涉及选自坩埚、平底锅、敞口杯和烧箱的容器，其基本上包含两种组分，其中：
(A)一种组分为陶瓷基体复合材料，和
(B)第二组分选自金属或合金，
且其中组分(A)为内部组分。
此外，本发明涉及本发明容器的用途，以及制造本发明容器的方法。
锂化过渡金属氧化物目前用作锂离子电池的阴极活性材料。在过去数年中，已进行了广泛的研究和开发工作，以改善诸如电荷密度、能量的性能，以及诸如可能对锂离子电池的寿命或适用性产生不利影响的缩短的循环寿命和容量损失的其他性能。已进行了额外的工作来改进制备方法。
在制备用于锂离子电池的阴极材料的常规方法中，首先通过以碳酸盐、氧化物的形式或者优选以氢氧化物(可为碱性的或可为非碱性的)的形式共沉淀过渡金属来形成所谓的前体。然后，将前体与锂盐(例如但不限于LiOH、Li2O、LiNO3或者尤其是Li2CO3)混合，并在高温下煅烧(焙烧)。锂盐可以以水合物或以脱水形式使用。煅烧(或焙烧，通常也称为前体的热处理)通常在600-1000℃的温度下进行。在热处理期间，发生固态反应，并形成阴极活性材料。热处理在烘箱或窑的加热区中进行。
实现将前体输送至加热区中以及从加热区中移除阴极活性材料的两种一般类型是最广泛使用的。一种类型是使粉末料流移动通过加热区，例如在回转窑中。然而，回转窑面临的挑战是强腐蚀性前体可能会损坏窑材料。
此外，当可能关注交叉污染时，回转窑对多产品设施而言是非常不利的。
另一种方法包括将前体置于容器(例如坩埚或烧箱)中，并将该容器移动通过烘箱或窑的加热区的步骤。该方法允许非常舒适地更换多产品设施的产品。尽管腐蚀效应的程度得以降低，然而由于需要长时间来加热容器，因此该方法具有共同的缺点。通常，该容器由陶瓷材料制成。该陶瓷材料往往表现为绝热材料。靠近容器壁或处于块芯中的前体需要比上表面更长的加热时间，因此可能需要长得多的反应时间。此外，为了避免损坏陶瓷容器(例如由于热冲击)，它们只能缓慢地加热。典型的加热速率为1-3℃/分钟。同样的挑战对热处理后的冷却也成立。生产设施需要很大的空间来实现无裂纹地加热和冷却。
一些材料(例如特定的陶瓷基体复合材料)不具有同样的加热和冷却速率限制。可使用完全由陶瓷基体复合材料制成的烧箱，然而陶瓷基体复合材料的成本通常非常高。也不需要缓慢加热和冷却的由金属制成的烧箱通常不具有足够的耐腐蚀性。
因此，目的是提供一种制备氧化物材料的方法，其可用于与腐蚀性材料接触并且允许在给定的加热过程中实现更高的转化率。另一目的是提供该方法所需的设备。
因此，已发现了开头所定义的方法(下文也称为本发明的方法或根据发明的方法)。此外，已发现了开头所定义的敞口容器(下文也称为本发明的容器或根据本发明的容器)。下文将更详细地定义本发明的容器。
本发明的容器选自坩埚、平底锅、敞口杯和烧箱。本发明的容器优选为敞口的，这意味着在本发明的上下文中，它们没有盖子。在一些实施方案中，本发明的容器具有一个或多个手柄，然而优选它们不具有手柄。
在本发明的上下文中，平底锅和敞口杯各自具有圆形底座，并且它们通过尺寸更好地区分。在平底锅中，壁占底座直径的至多25％，例如5-25％，而在敞口杯中，壁占底座直径的26-300％。
本发明的容器包含两种组分，
(A)一种组分为陶瓷基体复合材料，下文也称为组分(A)或基体复合材料(A)，和
(B)第二组分选自金属或合金，下文也称为组分(B)，
且其中组分(A)为内部组分。
下文将更详细地解释所述两种组分(A)和(B)。
在本发明的上下文中，“基本上包含”意指至少90重量％的该本发明的容器为组分(A)或组分(B)。在本发明的优选实施方案中，除组分(A)或组分(B)以外的组分占本发明容器的0-5重量％。除组分(A)和组分(B)以外的(任选)组分的实例称为组分(C)。组分(C)的实例为用作组分(A)和(B)之间的粘合材料的中间层。任选组分(C)的另一实例为涂层或增强热传递的层。任选组分(C)的另一实例为密封层，其允许处理部分或完全熔融的材料。在本发明的甚至更优选的实施方案中，本发明的容器由组分(A)和组分(B)组成。
在本发明容器包含除组分(A)和组分(B)以外的组分的实施方案中，除组分(A)和组分(B)以外的该类组分表现出高的热稳定性。例如，它们的熔融温度和软化温度(如果适用)高于1,100℃，例如为1,200-3,000℃。
此外，本发明的容器包含陶瓷基体复合材料(A)。所述陶瓷基体复合材料(A)包含陶瓷纤维，并且额外包含陶瓷基体材料，也称为陶瓷基体。陶瓷纤维和陶瓷基体可具有相同或不同的组成。在本发明的上下文中，陶瓷基体复合材料(A)包含包埋在陶瓷氧化物或非氧化物基体中的纤维。纤维和基体之间的粘合力相对较低。氧化物基体材料如氧化铝优选呈颗粒形式。
陶瓷纤维和陶瓷基体材料可各自选自氧化物和非氧化物陶瓷。非氧化物陶瓷的实例为碳化物、硼化物、氮化物和氧氮化物。非氧化物陶瓷的特定实例为碳化硅、硼化硅、氮化硅、氧氮化硅、硅-硼氮化物(下文也称为SiBN)，硅碳氮化物(下文也称为SiCN)，特别是SiC和Si3N4的组合。优选为氧化物陶瓷(下文也称为氧化物基陶瓷)。氧化物陶瓷为至少一种选自Be、Mg、Ca、Sr、Ba、稀土金属，Ti、Zr、Hf、V、Nb、Ta、Cr、Mo、W、Mn、Fe、Co、Ni、Zn、B、Al、Ga、Si、Ge、Sn、Re、Ru、Os、lr、In、Y的元素的氧化物，以及前述至少两种的混合物。氧化物基陶瓷可选自掺杂陶瓷，其中一种主要组分掺杂有至多1摩尔％的除主要组分以外的组分；以及选自增强陶瓷，其中一种组分为主要组分(例如至少50摩尔％)，且一种或多种其他组分(增强组分)以1.1-25摩尔％的量存在。其他实例为钛酸盐和硅酸盐。
钛酸盐的优选实例为钛酸铝。硅酸盐的优选实例为硅酸镁。
增强陶瓷的实例为增强氧化铝和增强氧化锆。它们可含有两种或更多种不同的增强氧化物，因此可称为二元或三元混合物。以下二元和三元混合物是优选的：用1.1-25重量％的以下物质之一增强的氧化铝：氧化铈CeO2、氧化镱Yb2O3、氧化镁MgO、氧化钙CaO、氧化钪Sc2O3、氧化锆ZrO2、氧化钇Y2O3、氧化硼B2O3，SiC和Al2O3的组合，或钛酸铝。更优选的增强组分为B2O3、ZrO2和Y2O3。
优选的氧化锆增强的氧化铝为具有10-20摩尔％ZrO2的Al2O3。增强氧化锆的优选实例选自用10-20摩尔％，特别是16摩尔％CaO，10-20摩尔％，优选16摩尔％MgO，或5-10摩尔％，优选8摩尔％Y2O3，或1-5摩尔％，优选4摩尔％Y2O3增强的ZrO2。优选的三元混合物的实例为80摩尔％Al2O3、18.4摩尔％ZrO2和1.6摩尔％Y2O3。
优选的纤维材料为氧化物陶瓷材料、碳化物陶瓷材料、氮化物陶瓷材料、碳纤维、SiBCN纤维、玄武岩、氮化硼、碳化钨、氮化铝、二氧化钛、钛酸钡、锆钛酸铅和碳化硼。甚至更优选的纤维材料为Al2O3、富铝红柱石、SiC、ZrO2和碳纤维。
在本发明的一个实施方案中，组分(A)包含选自碳化硅、氮化硅、氧氮化硅、碳纤维或其组合的纤维和选自SiC、氮化硅、氧氮化硅、氧化铝、二氧化硅、富铝红柱石、堇青石、尖晶石和前述至少两种的组合的陶瓷。
在本发明的一个实施方案中，纤维由氧化铝制成，并且陶瓷基体复合材料包含选自如下组的陶瓷基体材料：氧化铝、硅酸盐、富铝红柱石、尖晶石、堇青石和至少两种前述物质的组合。优选为氧化铝。
优选的是抗蠕变纤维。在本发明的上下文中，抗蠕变纤维是在高达1,400℃的温度下表现出最小—或者没有—永久伸长或其他永久变形的纤维。
在本发明的一个实施方案中，陶瓷纤维可具有7-12μm的直径。其长度可为1mm至1km或者甚至更长，即所谓的无端纤维。在一个实施方案中，若干纤维彼此组合成纱线、织物带、软管等。在优选实施方案中，本发明所用的陶瓷纤维的拉伸强度为至少50MPa，优选至少70MPa，更优选至少100MPa，甚至更优选至少120MPa。本发明所用的陶瓷纤维的拉伸强度的最大值为3,100MPa或者甚至为10,000MPa。拉伸强度可用拉伸试验机测定。典型的测量条件为1.2-1.3cm/分钟，例如1.27cm/分钟的十字头速度，和7.61cm的规格。
在本发明的一个实施方案中，基体由氧化物陶瓷或碳化物制成。用于基体的优选氧化物陶瓷材料为Al2O3、富铝红柱石、SiC、ZrO2和尖晶石，MgAl2O4。
特别优选的组分为SiC/SiC、C/SiC、ZrO2/ZrO2、ZrO2/Al2O3、Al2O3/ZrO2，Al2O3/Al2O3和富铝红柱石/富铝红柱石。在前述每种情况下，纤维材料为第一种材料，而基体为第二种材料。
在本发明的一个实施方案中，组分(A)包含20-60体积％的陶瓷纤维。
组分(A)是多孔的。在许多情况下，其总共包含50-80％的陶瓷基体复合材料，其余为气体，例如空气(孔隙率)。
在本发明的一个实施方案中，组分(A)的孔隙率为20-50％；因此，在DIN 623-2的意义上，组分(A)不是气密的。
在本发明的一个实施方案中，陶瓷基体复合材料(A)包含氧化铝纤维和选自氧化铝、石英、富铝红柱石、堇青石和前述至少两种的组合的陶瓷，例如氧化铝和富铝红柱石或氧化铝和堇青石。甚至更优选地，陶瓷基体复合材料(A)包含氧化铝纤维和氧化铝陶瓷。
在本发明的一个实施方案中，组分(A)的内表面对肉眼是光滑的。在其他实施方案中，组分(A)的内表面显示出一定的粗糙度。在该上下文中，粗糙度指的是指峰谷高度差高达3mm。
组分(B)选自金属或合金。可用的金属为钨、钼、铁、镍和钛。可用的合金为钢和钴耐火合金。在优选实施方案中，组分(B)由钢制成，例如300系列不锈钢，304、309和316。合适的钢的实例为1.46xx、1.47xx和1.48xx，钴基合金如Haynes 25，和2.48xx级镍基合金，特别是1.48xxx级，2.4856级和2.4851级。可用合金的另一实例为钼钛锆，简称TZM。
在本发明的一个实施方案中，组分(B)由在1000℃下具有15-35W/mK导热率的合金制成。
在本发明的一个实施方案中，本发明容器的组分(A)的平均壁厚为0.5-5mm，优选为0.75-4mm，更优选为1-3mm。组分(A)具有平底座的实施方案中的组分(A)的底座可具有相同的厚度或更厚或更薄，例如至多10mm，优选2-5mm。
在本发明的一个实施方案中，在组分(A)中，各壁与底座之间的角度为90°。在优选实施方案中，组分(A)具有弯曲的壁，并且各壁与底座之间的角度为91-100°。
在本发明的优选实施方案中，本发明的容器可含有100ml至25L，优选2-20L，甚至更优选3-15L的颗粒材料。本发明的较小容器是可能的，但它们在经济上是不利的。在现有技术的容器中，如下传热方式可能是不利的：在加热和/或冷却区中的停留时间不利地长或者观察到待热处理的粉末中的不利于均质产物的显著温度分布。如果在本发明的容器中进行热处理，则会促进和加速热传递。这导致热处理材料的均匀性提高。
本发明的容器有利于在固态反应中由前体在固态反应中制备氧化物材料的任何固态反应。通过使用本发明的容器，可容易地克服开头所讨论的已知方法的缺点。产品的更换是容易的，并且热处理前后的加热和冷却可比已知容器快得多的速率进行。
组分(A)和(B)的形状可相同或不同。在本发明的一个实施方案中，组分(A)和(B)的形状相同，且组分(A)以形状匹配的方式位于组分(B)中。
组分(B)可具有圆形或椭圆形或多边形，例如矩形或四边形的底座。本发明的容器优选具有矩形，特别是四边形底座，例如为具有矩形底座，特别是具有正方形底座的容器。本发明的具有四边形底座的容器的具体实施方案为具有圆角的那些，尤其是具有带圆角的正方形底座的本发明容器。
组分(A)可具有圆形或椭圆形或多边形，例如矩形或四边形的底座。在组分(A)具有底座的那些实施方案中，优选本发明容器具有矩形，特别是四边形底座，例如具有矩形底座，特别是具有正方形底座的容器。组分(A)可根本没有底座，例如在组分(A)具有半球形状的实施方案中。
在优选实施方案中，组分(A)和(B)的形状是不同的。
在不同形状的组分(A)和(B)的一个实例中，组分(A)和(B)各自具有杯子或坩埚或烧箱或敞口平底锅的形状，然而一个具有球形底座，而另一个具有例如正方形底座。
在本发明的另一实施方案中，组分(A)本身具有杯子或坩埚或烧箱或敞口平底锅的形状，但组分(B)为具有开口侧或部分开口侧的物体，例如网、笼或带，或者垂直环或盘，并且可任选具有水平杆或支柱。
在本发明的一个实施方案中，将组分(A)置于组分(B)中而没有任何紧固装置。在其他实施方案中，组分(A)通过一个或多个紧固装置与组分(B)连接，例如一个或多个螺钉或螺栓。
在本发明的一个实施方案中，本发明的容器包含选自石墨、钼箔和涂层的其他组分(C)。箔的厚度可为1μm至0.5mm，涂层的厚度可为100nm至1mm。选自石墨和钼箔的其他组分(C)优选位于组分(A)和组分(B)之间。组分(A)外表面上的涂层可用于增强传热(通过辐射)，组分(A)内表面上的涂层可用于避免扩散到组分(A)中或确保流体密封性。涂层可选自陶瓷、玻璃或碳基涂层。组分(A)内表面上的优选涂层为二氧化硅、氧化铝、氧化锆或氧化钇陶瓷，或硅酸钠或石英玻璃。选自涂层的其他组分(C)优选位于组分(A)的内表面或组分(B)的外表面上。
本发明的另一方面涉及一种制备本发明容器的方法(下文也称为本发明的制备方法或根据本发明的制备方法)。本发明的方法包括若干步骤(下文也称为步骤(α)、步骤(β)等)，这将在下文更详细地说明。
本发明制备方法的步骤为：
(α)提供组分(A)的相应生坯，
(β)提供组分(B)，
(γ)任选地，通过真空处理、压制或干燥而预处理组分(A)的生坯，
(δ)焙烧组分(A)的生坯，或者如果合适的话，焙烧根据步骤(γ)预处理的生坯，
(ε)使组分(B)与步骤(γ)之前的组分(A)的生坯或根据步骤(γ)预处理的生坯或焙烧后的组分(A)接触。
在步骤(α)中，提供组分(A)的生坯。生坯基本上包括未焙烧的基体复合材料。未焙烧的基体复合材料包含纤维和陶瓷材料，并且该生坯的制备基本上包括将陶瓷纤维(或碳纤维)与陶瓷材料的前体组合的一个或多个步骤。
在步骤(α)的一个实施方案中，组分(A)的生坯通过将织物布置在成型体周围而制备，其中所述织物由陶瓷纤维制成，并且用陶瓷材料或其前体的浆料浸泡。在该实施方案中，成型体优选具有组分(A)的形状。
在步骤(α)的一个实施方案中，组分(A)的生坯的形状没有最终确定，而是在其与组分(B)接触时形成最终形状。
织物可为陶瓷纤维的织造或非织造结构。甚至更优选地为单向取向的纤维或单向取向的粗纱。所述织物用含有陶瓷材料或陶瓷前体的浆料浸泡。所述浸泡可通过使织物移动通过含有所述浆料的浴来实施。在其他实施方案中，所述浸泡可静态实施。所述浸泡可实施一次或重复数次，例如多达10次。
浆料含有所谓的陶瓷前体，例如呈溶胶或凝胶状态的氢氧化铝、水和任选的填料，例如有机酸或无机酸。所述浆料的固含量可为10-80％，优选为20-60％，更优选为25-45％。
在本发明的一个实施方案中，织物在所述浆料中的平均停留时间为1秒钟至24小时，优选5秒钟至10小时，优选1分钟至5小时。
在用所述浆料浸泡织物后，获得预浸料。在一些实施方案中，然后使预浸料与上述成型体接触。所述接触通过将织物以使得外表面部分或完全被至少一层浸泡织物覆盖的方式布置在上述成型体外表面上来进行。在重复实施浸泡的情况下，可能只有在所述重复浸泡之后才实现完全覆盖。所述接触可在有或没有叠层的情况下进行。获得了生坯，然后将其从成型体中取出。
在步骤(α)的另一实施方案中，组分(A)的生坯通过在成型体的周围缠绕粗纱、丝束、纤丝或纱线而制备，其中所述粗纱、丝束、纤丝或纱线用陶瓷材料或其前体的浆料浸渍。在该实施方案中，成型体优选具有组分(A)的形状。
为此，使所述粗纱、纱线、丝束或纤丝移动通过浆料，例如牵引。所述浆料含有所谓的陶瓷前体，例如呈溶胶或凝胶状态的氢氧化铝、水和任选的填料，参见上文。所述浆料的固含量可为10-80％，优选为20-60％，更优选为25-45％。
该粗纱、纱线、丝束或纤丝的直径可为0.1-5mm，优选为0.2-3mm，更优选为0.3-2mm。
所述缠绕可包括一层或多层，例如2-10层粗纱、丝束或纤丝。由步骤(α)获得了生坯，然后将其从成型体中取出。
在步骤(β)中，提供组分(B)。组分(B)的一些实施方案是可商购获得的，例如钢制杯子和烧箱。其他实施方案可通过铸造、焊接、冲切或模塑制备。
在焙烧之前，可根据一个或多个任选步骤(γ)处理根据步骤(α)获得的生坯，例如真空处理或压制或干燥，尤其是真空处理或高压釜处理。可实施所述任选步骤以在焙烧之前移除一定百分比的水。任选的干燥步骤可在10-300℃，优选80-200℃的温度下进行。在环境气氛中且随后在烘箱中组合干燥是优选的。
在步骤(β)和步骤(γ)(如果合适的话)之后，将如此获得的生坯焙烧(步骤(δ))。步骤(δ)可通过在800-1,500℃，优选900-1,450℃，优选1,000-1,400℃的温度下热处理生坯来进行。
步骤(δ)可实施10分钟至48小时，优选30分钟至24小时，优选1-10小时的时间。在有或没有中间冷却的情况下，在不同温度下停留可能是优选的。
在焙烧后，获得组分(A)。在焙烧后，将组分(A)冷却。
步骤(ε)包括使组分(B)与步骤(γ)之前的组分(A)的生坯或(如果合适的话)根据步骤(γ)预处理的生坯或焙烧后的组分(A)接触。优选将组分(B)与呈其最终形式的组分(A)接触。通过该接触，获得了本发明的容器。取决于紧固装置(如果有的话)，优选在本发明制备方法中尽可能晚地使组分(A)和(B)接触，尤其是在步骤(δ)之后的冷却之后。作为步骤(ε)的要素，使用紧固装置如螺钉螺栓。
本发明的另一方面涉及一种制备氧化物材料的方法(下文也称为本发明的方法或根据本发明的方法)，所述方法包括以下步骤：
(a)提供至少两种固体颗粒材料的混合物，其中至少一种为氧化物或氢氧化物或碳酸盐，
(b)使所述混合物在本发明的容器中移动通过设备，在该设备中对所述混合物进行热处理，由此使颗粒材料彼此反应，
(c)冷却由步骤(b)得到的材料。
在本发明的一个实施方案中，氧化物材料选自阴极活性材料，尤其是用于锂离子电池的阴极活性材料。用于锂离子电池的阴极活性材料的实例为LiCoO2；LiNiO2；LiMnO2；具有通式Li(1+z)[NiaCobMnc](1-z)O2+e的具有层状结构的混合过渡金属氧化物(也称为锂化层状氧化物)，其中z为0-0.3，a、b和c可相同或不同并且选自0.0-0.8，其中a+b+c＝1，且-0.1≤e≤0.1；锂化尖晶石(“NMO”)，例如含锰尖晶石如LiMn2O4和通式Li1+tM2-tO4-d的尖晶石，其中d为0-0.4，t为0-0.4且M为Mn与至少一种选自Co和Ni的其他金属的组合；和锂化的镍钴铝氧化物(“NCA”)，后者为通式Li(1+g)[NihCoiAlj](1-g)O2的材料。g、h、i和j的典型值为：g为0.0-0.1，h为0.80-0.85，i＝0.15-0.20，j＝0.02-0.03。在优选实施方案中，阴极活性材料选自锂化层状氧化物、锂化尖晶石和锂化镍钴铝氧化物。
在本发明的一个特定实施方案中，氧化物材料选自LiCoO2涂覆的掺杂或非掺杂的层状镍-钴-镁氧化物，例如LiCoO2涂覆的LiNi0.9Co0.09Mg0.01O2。可用于制备LiCoO2涂覆的层状镍-钴-镁氧化物的各热处理步骤可在本发明的容器中进行。
本发明的方法从至少两种颗粒材料的混合物开始，其中至少一种为步骤(a)的氧化物或氢氧化物或碳酸盐。例如，一种颗粒材料为锂盐，优选为氧化锂或氢氧化锂，或者优选为碳酸锂Li2CO3，并且一种颗粒材料为所谓的前体，例如选自Ni、Mn和Co的过渡金属的氢氧化物或氧化物或羟基氧化物或碳酸盐，或者至少两种选自Ni、Mn和Co中的至少两种过渡金属的混合氢氧化物或氧化物或羟基氧化物或碳酸盐。在优选实施方案中，一种颗粒材料为碳酸锂，另一种为Ni、Co和Mn的混合羟基氧化物或Ni、Co和Al的混合羟基氧化物。
在其他实施方案中，本发明的方法从所谓的预煅烧物开始，所述预煅烧物为锂化合物与预处理的氢氧化物的混合物。
在该颗粒材料中，锂盐和前体的颗粒可各自具有2-20μm，优选5-15μm的平均粒径(D50)。在本发明方法的步骤(a)中使用的锂盐优选具有4-7μm的平均粒径(D50)。可观察到在步骤(a)的许多实施方案中，形成了含有多种选自干燥或脱水前体和锂盐的颗粒的附聚物。
锂与除锂之外的金属的摩尔比可在一定范围内选择，在锂化尖晶石的情况下，其为锂:过渡金属1:2。在NCA的情况下，其为1:1-1.02:1，在锂化层状氧化物的情况下，其为1:1-1.86:1。
将锂盐和前体充分混合，并提供所得的混合物(步骤(a))。
在步骤(b)开始时，将步骤(a)中提供的混合物转移至至少一个本发明的容器中。然后将本发明的容器与混合物一起移动通过设备，在该设备中对所述混合物进行热处理，由此使颗粒材料彼此反应。所述反应为固态反应。
在本发明的一个实施方案中，步骤(b)中的热处理在600-1,000℃的温度下进行。优选地，将温度升高，例如升至600-650℃的第一热处理温度，然后升至700-750℃的第二热处理温度，然后升至850-900℃的第三热处理温度。在一个实施方案中，将混合物在各热处理温度下保持1-10小时，优选3-8小时的时间。
在本发明的一个实施方案中，步骤(b)中的设备选自辊道窑、梭式窑、箱式炉和隧道窑。
在本发明的一个实施方案中，冷却步骤(c)或步骤(b)中的加热阶段以1-50℃/分钟，优选5-25℃/分钟的速率进行。
由于本发明容器的良好性能，本发明的方法可获得非常均匀的氧化物材料，尤其是阴极活性材料。由于提高的加热或冷却速率，加热和冷却时间较短，并且与仅由一种组分组成的容器的周转相比，可提高商业规模方法中本发明容器的周转。此外，由于良好的腐蚀稳定性，在根据本发明方法制备的阴极活性材料中没有发现可检测量的本发明容器材料。

Claims (15)

1.选自坩埚、平底锅、敞口杯和烧箱的容器，其基本上包含两种组分，其中：
(A)一种组分为陶瓷基体复合材料，和
(B)第二组分选自金属或合金，
且其中组分(A)为内部组分。
2.根据权利要求1的容器，其中所述陶瓷基体复合材料包含碳化硅、氮化硅、氧氮化硅、碳纤维或其组合的纤维和选自SiC、氮化硅、氧氮化硅、氧化铝、二氧化硅、富铝红柱石、堇青石、尖晶石和前述至少两种的组合的陶瓷。
3.根据权利要求1或2的容器，其中所述陶瓷基体复合材料包含氧化铝或富铝红柱石或其组合的纤维和选自氧化铝、二氧化硅、富铝红柱石、堇青石、尖晶石和前述至少两种的组合的陶瓷。
4.根据前述权利要求中任一项的容器，其中组分(A)的平均壁厚为0.5-5mm。
5.根据前述权利要求中任一项的容器，其中组分(A)具有正方形底座。
6.根据前述权利要求中任一项的容器，其中组分(A)和(B)的形状是不同的。
7.根据前述权利要求中任一项的容器，其中组分(B)由在1000℃下具有15-35W/mK导热率的合金制成。
8.根据前述权利要求中任一项的容器，其中组分(B)由钢制成。
9.根据前述权利要求中任一项的容器，其中所述容器包含选自石墨、钼箔和涂层的其他组分(C)。
10.制备根据前述权利要求中任一项的容器的方法，包括如下步骤：
(α)提供组分(A)的相应生坯，
(β)提供组分(B)，
(γ)任选地，通过真空处理、压制或干燥而预处理组分(A)的生坯，
(δ)焙烧组分(A)的生坯，或者如果合适的话，焙烧根据步骤(γ)预处理的生坯，
(ε)使组分(B)与步骤(γ)之前的组分(A)的生坯或根据步骤(γ)预处理的生坯或焙烧后的组分(A)接触。
11.根据权利要求10的方法，其中组分(A)的生坯通过将织物布置在成型体周围而制成的，其中所述织物由陶瓷纤维制成并用陶瓷材料或其前体的浆料浸泡。
12.根据权利要求10的方法，其中组分(A)的生坯通过在成型体周围缠绕粗纱、丝束、纤丝或纱线而制备，其中所述粗纱、丝束、纤丝或纱线浸渍有陶瓷材料或其前体的浆料。
13.制备氧化物材料的方法，所述方法包括以下步骤：
(a)提供至少两种固体颗粒材料的混合物，其中至少一种为氧化物或氢氧化物或碳酸盐，
(b)使所述混合物在根据权利要求1-9中任一项的敞口容器中移动通过设备，在该设备中对所述混合物进行热处理，由此使颗粒材料彼此反应，
(c)冷却由步骤(b)得到的材料。
14.根据权利要求13的方法，其中氧化物材料为用于锂离子电池的阴极活性材料，其选自锂化层状氧化物、锂化尖晶石(NMO)、LiCoO2涂覆的层状镍-钴-镁氧化物和锂化镍-钴铝氧化物(NCA)。
15.根据权利要求13或14的方法，其中冷却步骤(c)或步骤(b)中的加热阶段以1-50℃/分钟的速率进行。
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