CN109678493A - 一种Mg2+掺杂Li4Ti5O12陶瓷靶材的烧结方法 - Google Patents

一种Mg2+掺杂Li4Ti5O12陶瓷靶材的烧结方法 Download PDF

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CN109678493A
CN109678493A CN201711010521.5A CN201711010521A CN109678493A CN 109678493 A CN109678493 A CN 109678493A CN 201711010521 A CN201711010521 A CN 201711010521A CN 109678493 A CN109678493 A CN 109678493A
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董磊
尚福亮
杨海涛
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Shenzhen University
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Abstract

一种Mg2+掺杂Li4Ti5O12陶瓷靶材的制备及烧结方法。本发明公开了一种新的工艺来制备Mg2+掺杂Li4Ti5O12陶瓷靶材。本发明的优点在于用使用粉末冶金的掺杂工艺，以Mg(OH)2作为镁源，得到充分混合、均匀掺杂的Mg2+掺杂Li4Ti5O12粉体。可制备出致密度超过90％，强度超过70MPa，维氏硬度大于300HV500性能优异的Mg2+掺杂Li4Ti5O12陶瓷靶材。制备得到的掺杂Li4Ti5O12陶瓷靶材性质稳定、成分均一。由于制作工艺简单可满足工艺化大量生产，为磁控溅射制备Li4Ti5O12薄膜负极所使用的靶材提供了坚实的基础。Li4Ti5O12薄膜负极具有体积应变小、易制备、电位高、大电流充放电特性好、循环寿命长等优势。在全固态锂离子薄膜电池领域得到了极其广泛的应用，是一种被广泛研究的电池负极材料。

Description

一种Mg2+掺杂Li4Ti5O12陶瓷靶材的烧结方法
技术领域：
本发明属于无机非金属元素及其化合物。
背景技术：
LTO(Li4Ti5O12)薄膜是一种被广泛研究的全固态锂离子薄膜电池薄膜电池负极材料。全固态锂离子薄膜电池因为其良好的安全性和优异的性能受到广泛关注。薄膜负极是构成全固态锂离子电池的主要部分，其性能影响着全固态锂离子电池的性能。LTO负极薄膜作为一种新型脱嵌锂，具有倍率性能好、循环寿命高、快速充放电等优点，同时LTO也是一种理论上的零应变材料，可以广泛应用于全固态薄膜锂离子电池行业。
LTO薄膜的制备方法主要有：物理气相沉积、化学气相沉积、溶胶-凝胶等各种方法。由于物理气相沉积制备的薄膜与基体的结合强度高、沉积效率高、工艺成熟稳定而被广泛应用。而用物理气相沉积制备LTO薄膜需要使用高密度LTO靶材，通过能量束轰击LTO靶材将其气化，再沉积到基体表面形成透负极电膜。微量的Mg2+掺杂能提高LTO靶材的致密度，提高LTO材料的容量，对于负极薄膜性能和电池性都能有一定的提高。
发明内容：
本发明公开了一种Mg2+掺杂Li4Ti5O12陶瓷靶材的烧结方法。使用去离子水作为球磨介，将磨球、去离子水、粉料按照一定比例混合球墨。通过对成型烧结，可制备出致密度超过90％，强度超过 70MPa，维氏硬度大于300HV500性能优异的Mg2+掺杂Li4Ti5O12烧结材料，可作为溅射镀膜用的靶材。
本发明详细研究并掌握了掺杂比、烧结温度温度等对Mg2+掺杂Li4Ti5O12陶瓷靶材制备过程的影响及其烧结致密化过程的变化规律，从而可制备出高性能的烧结Mg2+掺杂Li4Ti5O12陶瓷材料。这种材料可经济、高效的制成各种复杂形状的产品，主要是溅射镀膜用的靶材(包括平面靶和旋转靶)，也可用于制造多种部件。
附图说明：
下面结合附图对本发明作进一步说明：
附图1：Mg2+掺杂Li4Ti5O12陶瓷靶材的烧结工艺流程图
下面结合附图对本发明作进一步说明：
如附图1所示，本发明的Mg2+掺杂Li4Ti5O12粉体的制备工艺流程是：先将Mg(OH)2粉末、Li4Ti5O12粉末、磨球加入到球磨机中与水溶液湿磨混合，充分混合均匀后，加入成形剂聚乙二醇(PEG)，经干燥过筛得到均匀混合的Mg2+掺杂Li4Ti5O12粉料。Mg2+掺杂Li4Ti5O12粉体，经过成型(干压、冷等静压、注射成型等)，得到生坯，经脱成型剂后，即可进行常压烧结或气压烧结，得到高强度高密度的 Mg2+掺杂Li4Ti5O12陶瓷靶材。
本发明的优点在于用使用粉末冶金的掺杂工艺，以Mg(OH)2作为镁源，得到充分混合、均匀掺杂的Mg2+掺杂Li4Ti5O12粉体。可烧结制备出性能优异的Mg2+掺杂Li4Ti5O12陶瓷靶材。
具体实施方式：
实例1：2wt.％Mg2+掺杂Li4Ti5O12陶瓷靶材的烧结制备
将市售纯度为99.9％Li4Ti5O12粉末、Mg(OH)2粉末按质量比98∶2混合，使用去离子水作为球磨介质置于球磨机中湿磨24-36h，出磨前2h加入PEG作为成型剂干燥过筛，得到各种粉料充分混合的Mg2+掺杂Li4Ti5O12粉体，在100-200MPa压力下压制成型，脱成型剂后，在高温炉内1400℃下于空气中常压烧结60-180分钟可制备出致密度超过92.47％，强度超过70MPa，维氏硬度大于302.48HV500
实例2：3wt.％Mg2+掺杂Li4Ti5O12陶瓷靶材的烧结制备
将市售纯度为99.9％Li4Ti5O12粉末、Mg(OH)2粉末按质量比97∶3混合，使用去离子水作为球磨介质置于球磨机中湿磨24-36h，出磨前2h加入PEG作为成型剂干燥过筛，得到各种粉料充分混合的Mg2+掺杂Li4Ti5O12粉体，在100-200MPa压力下压制成型，脱成型剂后，在高温炉内1400℃下于空气中常压烧结60-180分钟可制备出致密度超过94.374％，强度超过70MPa，维氏硬度大于317.39HV500
实例3：4wt％Mg2+掺杂Li4Ti5O12陶瓷靶材的烧结制备
将市售纯度为99.9％Li4Ti5O12粉末、Mg(OH)2粉末按质量比96∶4混合，使用去离子水作为球磨介质置于球磨机中湿磨24-36h，出磨前2h加入PEG作为成型剂干燥过筛，得到各种粉料充分混合的Mg2+掺杂Li4Ti5O12粉体，在100-200MPa压力下压制成型，脱成型剂后，在高温炉内1400℃下于空气中常压烧结60-180分钟可制备出致密度超过96.041％，强度超过70MPa，维氏硬度大于357.26HV500
实例4：5wt％Mg2+掺杂Li4Ti5O12陶瓷靶材的烧结制备
将市售纯度为99.9％Li4Ti5O12粉末、Mg(OH)2粉末按质量比95∶5混合，使用去离子水作为球磨介质置于球磨机中湿磨24-36h，出磨前2h加入PEG作为成型剂干燥过筛，得到各种粉料充分混合的Mg2+掺杂Li4Ti5O12粉体，在100-200MPa压力下压制成型，脱成型剂后，在高温炉内1400℃下于空气中常压烧结60-180分钟可制备出致密度超过94.564％，强度超过70MPa，维氏硬度大于325.43HV500。

Claims (3)

1.Mg2+掺杂Li4Ti5O12陶瓷靶材的制备，实验采用球磨(加成型剂)-卸料-干燥-过筛-干压成型-烧结制备工艺流程，可制备出致密度超过90％，强度超过70MPa，维氏硬度大于300HV500的高性能靶材。
2.对权利要求1所述的Mg2+掺杂Li4Ti5O12陶瓷靶材的烧结，既可采用常压烧结工艺，也适用于气压烧结工艺。
3.利用权利要求1所述的Mg2+掺杂Li4Ti5O12粉体制备的致密Mg2+掺杂Li4Ti5O12材料，可制成各种复杂形状的制品，主要是溅射镀膜用的靶材(包括平面靶和旋转靶)，也可用于制造其它多种电池部件。
CN201711010521.5A 2017-10-18 2017-10-18 一种Mg2+掺杂Li4Ti5O12陶瓷靶材的烧结方法 Pending CN109678493A (zh)

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