CN106747440B - 一种可见光透明储能陶瓷及其制备方法 - Google Patents

一种可见光透明储能陶瓷及其制备方法 Download PDF

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CN106747440B
CN106747440B CN201611201094.4A CN201611201094A CN106747440B CN 106747440 B CN106747440 B CN 106747440B CN 201611201094 A CN201611201094 A CN 201611201094A CN 106747440 B CN106747440 B CN 106747440B
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刘国保
王�华
许积文
周昌荣
杨玲
袁昌来
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Abstract

本发明公开了一种可见光透明储能陶瓷及其制备方法，所述陶瓷组份的化学通式用(1‑x)(K0.5Na0.5)NbO3‑xA(Me0.5Nb0.5)O3所表示，其中A为Ca、Sr、Ba中的一种或两种，Me为Al、In、Yb或两种，x表示摩尔分数，0.01≤x≤0.6。所述制备方法采用固相法制备粉体，不添加任何粘结剂，低压成型。产品同时具有高的可见光透光率和优良的电储能性能，以及介电损耗低、制备成本低、无铅环保、实用性好。

Description

一种可见光透明储能陶瓷及其制备方法
技术领域
本发明属于陶瓷材料领域，具体涉及一种铌酸钾钠基透明储能的无铅陶瓷及其制备方法。
背景技术
透明陶瓷(又称光学陶瓷)不仅具有优异的透光性，还具有陶瓷所特有的高强度、高硬度、耐腐蚀、耐高温等性能，这些性能远优于一般晶体和玻璃光学材料的性能，而且在制备成本、尺寸等方面也具有优势。因此，透明陶瓷在军民领域都具有非常重要的应用，例如激光器、坦克的观察窗、轰炸瞄准器、生活灯具等。储能陶瓷具有储能密度高，充放电速度快，适用于高温、高压等极端环境，而且性能稳定，被广泛应用于脉冲功率电源、航空航天、新能源发电等领域，铁电类陶瓷材料是一类非常重要的储能材料。
目前应用的透明铁电陶瓷中主要是铅基为主，在这类陶瓷的制备、使用以及废弃后处理过程中都可能产生对环境有害的物质，铅基材料现在已受到世界各国的法律、法规限制或禁止。另外，目前透明陶瓷一般采用共沉淀法、水热法和溶胶凝胶法等制备超细粉体，后续多采用热压烧结、热等静压烧结、等离子放电烧结、脉冲电流烧结等来排除气孔从而获得透明陶瓷，这些制备方法的设备成本及工艺成本都相对较高。
发明内容
基于上述背景，本发明提供一种铌酸钾钠基可见光透明储能陶瓷及其制备方法。所述制备方法采用固相法制备粉体，不添加任何粘结剂，低压成型。制备出的多功能陶瓷同时具有优异的可见光透光性和优良的电储能性能，以及无铅环保、介电损耗低、制备成本低、实用性好。
本发明所述陶瓷组份的化学通式可以用(1-x)(K0.5Na0.5)NbO3-xA(Me0.5Nb0.5)O3所表示，其中A为Ca、Sr、Ba中的一种或两种，Me为Al、In、Yb中的一种或两种，x表示摩尔分数，0.01≤x≤0.6。
本发明所述陶瓷的制备方法，除了现有工艺步骤外，至少还包括如下步骤：将原料按照化学通式(1-x)(K0.5Na0.5)NbO3-xA(Me0.5Nb0.5)O3进行配料。其它后续步骤如加入分散介质球磨、干燥、过筛、煅烧、合成粉体、压片等皆可以采用现有工艺。
具体实施方式
为了详细介绍本发明，在此给出一些具体的实施例，并提供了一些优选的工艺参数。
实施例1：
成分为(1-x)(K0.5Na0.5)NbO3-xSr(In0.5Nb0.5)O3，其中x表示摩尔分数，分别以x＝0.01,x＝0.25,x＝0.6进行三个组分比例的平行试验。
主要制备步骤：
(1)以分析纯粉末K2CO3、Na2CO3、SrCO3、In2O3和Nb2O5为原料，按照化学式(1-x)(K0.5Na0.5)NbO3-xSr(In0.5Nb0.5)O3进行配料，以无水乙醇为介质行星式球磨24小时，干燥后过100目筛，在坩埚中以950℃预烧保温5小时，取出粉末进行研磨，再次以950℃预烧保温5小时合成粉体。
(2)将步骤(1)获得的粉体，再次以无水乙醇为介质行星式球磨24小时，90℃烘干酒精后，过100目筛，再以200℃充分干燥粉体，在不添加任何粘结剂的情况下，直接在2MPa压力下保压1分钟压制成圆片。
(3)将成型后的圆片置于铺好氧化锆粉体的承烧板上，将少许相应成分点的粉体撒在生胚上,小坩埚倒扣生胚，再取氧化锆粉体封闭小坩埚，使小坩埚内部形成封闭式整体，最后以大坩埚倒扣小坩埚。
(4)置于马弗炉中烧结，缓慢升温(1℃/min)至1200±100℃，保温5～8小时，缓慢降温(1℃/min)至600℃后，随炉降温至室温；
(5)烧结后的样品加工成两面光滑、厚度为0.50mm的薄片进行透光率测试，之后披银电极，测试储能密度等。
实施例2：
以CaCO3替代实施例1中的SrCO3，分别以x＝0.01,x＝0.25,x＝0.6进行三个组分比例的平行试验，并采用实施例1的制备步骤，成功制备出成分为(1-x)(K0.5Na0.5)NbO3-xCa(In0.5Nb0.5)O3的透明储能陶瓷。
实施例3：
以BaCO3替代实施例1中的SrCO3，分别以x＝0.01,x＝0.25,x＝0.6进行三个组分比例的平行试验，并采用实施例1的制备步骤，成功制备出成分为(1-x)(K0.5Na0.5)NbO3-xBa(In0.5Nb0.5)O3的透明储能陶瓷。
实施例4：
以Al203替代实施例1中的In2O3，分别以x＝0.01,x＝0.25,x＝0.6进行三个组分比例的平行试验，并采用实施例1的制备步骤，成功制备出成分为(1-x)(K0.5Na0.5)NbO3-xSr(Al0.5Nb0.5)O3的透明储能陶瓷。
实施例5：
以Yb2O3替代实施例1中的In2O3，分别以x＝0.01,x＝0.25,x＝0.6进行三个组分比例的平行试验，并采用实施例1的制备步骤，成功制备出成分为(1-x)(K0.5Na0.5)NbO3-xSr(Yb0.5Nb0.5)O3的透明储能陶瓷。
实施例6：
分别以CaCO3、BaCO3或其混合物替代实施例1中的SrCO3，分别以Al203、Yb2O3或其混合物替代实施例1中的In2O3，并进行交叉组合；分别以x＝0.01,x＝0.25,x＝0.6进行三个组分比例的平行试验，采用实施例1的制备步骤，成功制备出成分为(1-x)(K0.5Na0.5)NbO3-xA(Me0.5Nb0.5)O3(其中：A为Ca、Sr、Ba中的一种或两种，Me为Al、In、Yb中的一种或两种，0.01≤x≤0.6)的透明储能陶瓷。
上述各实施例制出的透明储能陶瓷，经测试，都能达到相近的预期效果。

Claims (1)

1.一种可见光透明储能陶瓷，其特征在于：所述可见光透明储能陶瓷的组成用化学通式(1-x)(K0.5Na0.5)NbO3-xA(Me0.5Nb0.5)O3所表示；其中：A为Ca、Sr、Ba中的一种或两种，Me为Al、Yb中的一种或两种，x表示摩尔分数，0.01≤x≤0.6；
所述可见光透明储能陶瓷的制备方法包括如下步骤：将粉体原料按照上述化学通式进行配料，加入分散介质后球磨、干燥、过筛、煅烧合成粉体；
所述煅烧合成粉体步骤如下：配料粉以无水乙醇为介质行星式球磨24小时，干燥后过100目筛，在坩埚中以950°C预烧保温5小时，取出粉末进行研磨，再次以950°C预烧保温5小时合成粉体；
所述可见光透明储能陶瓷的制备方法还包括如下步骤：再次以无水乙醇为介质行星式球磨24小时，90℃烘干酒精后，过100目筛，再以200℃充分干燥粉体，在不添加任何粘结剂的情况下，直接在2MPa压力下保压1分钟压制成圆片；将成型后的圆片置于铺好氧化锆粉体的承烧板上，将少许相应成分点的粉体撒在生胚上,小坩埚倒扣生胚，再取氧化锆粉体封闭小坩埚，使小坩埚内部形成封闭式整体，最后以大坩埚倒扣小坩埚，然后烧结；烧结时以1℃/min速率缓慢升温至1100-1300℃，保温5-8小时，以1℃/min速率缓慢降温至600℃后，随炉降温至室温。
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CN104098333A (zh) * 2014-06-05 2014-10-15 中国人民解放军空军工程大学 一种(K0.5Na0.5)NbO3-Sr(Sc0.5Nb0.5)O3无铅透明铁电陶瓷材料及其制备方法

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