CN116062790A - 一种稳定化类球形多面体氧化锆微晶的制备方法 - Google Patents
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Abstract
本发明公开一种稳定化类球形多面体氧化锆微晶的制备方法，称取一定量ZrCl4加入到无水乙醇中，搅拌至澄清后加入沉淀剂无水乙酸；溶液经水浴回流24 h形成沉淀，干燥后得到含锆前驱体；将前驱体与熔盐和添加剂按一定比例混合研磨，在指定温度下热处理后反复洗涤干燥，即得稳定化类球形多面体氧化锆微晶。本发明对设备要求低、操作简单，有望通过调节参数控制产物晶面暴露比例和催化活性，在光催化降解和生物传感器等领域具有广泛的应用前景。
Description
技术领域
本发明属于无机材料制备技术领域，具体涉及到一种稳定化类球形多面体氧化锆微晶的制备方法。
背景技术
近年来，制备具有特定形貌和几何结构的单分散微晶已成为材料化学领域的热点问题。这是因为晶体材料的性能不仅取决于材料本身的物化特性，其微观尺寸和形貌也对材料的应用起着重要的影响作用。作为一种重要的无机氧化物材料，氧化锆微晶以其优异的光学、电学、热学、催化和机械性能，在燃料电池、氧传感器、透明光学器件、催化及催化载体、电化学电容电极、热障涂层和生物陶瓷等领域有着广泛的应用。G. Poungchan等人采用一步水热法制备了碳掺杂的部分稳定花状氧化锆，显著提高了对可见光的吸收和对罗丹明B的降解性能[One-step synthesis of flower-like carbon-doped ZrO2 for visible-light-
responsive photocatalyst [J]. Materials & design, 2016,89:137-145]。Dong等人采用离子液体法制备了直径50 nm，长度达20 μm的单斜氧化锆纳米线，其对钒元素显示出了优异的探测灵敏度[Synthesis of ZrO2 nanowires by ionic-liquid route[J]. Journal of colloid and interface science, 2009, 333(2): 734-740.]。
目前氧化锆微晶的制备以湿化学法为主，包括沉淀法、离子液体法、水热法、溶胶-凝胶法和喷雾热解法等。但这些方法一般以水作为溶剂，由于水的表面张力较大，因此沉淀物在干燥时会产生较大的毛细管力，从而导致颗粒容易团聚。此外，由于氧化锆存在单斜、四方和立方三种晶相，单斜氧化锆在高温下会发生相变，并伴随着显著的体积变化，从而严重影响材料性能，因此其稳定化具有重要意义。在稳定化的基础上，进一步实现氧化锆的微观形貌调控更加具有挑战性。通过调控氧化锆晶体不同晶面的裸露和比例，有望推动稳定化氧化锆在催化和生物传感器领域的应用。据了解，目前尚无有关稳定化类球形多面体氧化锆微晶的研究和报道。
发明内容
本发明要解决的技术问题是提供一种性能稳定、操作方便、成本低廉的稳定化类球形多面体氧化锆微晶的制备方法。
为解决以上技术问题，本发明的技术方案是：一种稳定化类球形多面体氧化锆微晶的制备方法，其特征在于包括如下步骤：
步骤一：配制一定质量浓度的ZrCl4-乙醇溶液，搅拌至澄清后加入沉淀剂；
步骤二：将步骤一制得的混合溶液经水浴回流24 h形成沉淀，然后在110℃烘箱中干燥得到前驱体；
步骤三：将步骤二制得的前驱体与熔盐KCl和添加剂YF3按一定质量比混合研磨，在一定温度下热处理；
步骤四：将步骤三制得的热处理产物用去离子水清洗三次，再用乙醇清洗一次后，即得到稳定化类球形多面体氧化锆微晶。
所述步骤一中的沉淀剂为无水乙酸，其浓度为6～10 mol/L。
所述步骤一中ZrCl4-乙醇溶液的浓度为0.5～4 mol/L。
所述步骤二中的水浴温度为70～90℃。
所述步骤二中前驱体与熔盐KCl与添加剂YF3的质量比为10:5～20:0.5～2。
所述步骤三中热处理温度为800～950℃，保温时间3～7 h。
本发明采用上述共沉淀辅助熔盐法制得产品的形貌为类球形多面体氧化锆微晶。通过沉淀反应得到粒度小、分散性良好的前驱体，随后在熔融盐中充分发挥钇离子的稳定作用和氟离子对氧化锆特殊晶面的吸附作用。所得微晶形状规则、产率较高，而且稳定化程度高，几乎不含单斜相。本发明技术方案既克服了马氏体相变中的体积效应问题，又展现出极为特殊的形貌和可调结的晶面比例，因而在光催化降解和生物传感器等领域的具有较高的应用潜力。
附图说明
图1为本发明实施例1制得氧化锆微晶的XRD图谱；
图2为本发明实施例1制得氧化锆微晶的SEM照片。
具体实施方式
下面结合附图和具体实施方式对本发明作进一步详细的说明。
实施例1
称取11.65 g的ZrCl4加入到50 mL无水乙醇中（浓度1 mol/L），搅拌至澄清后缓加17.10 mL无水乙酸（6 mol/L），溶液在80℃下水浴回流24 h形成沉淀，然后在110℃下干燥得到前驱体；将前驱体与熔盐KCl和添加剂YF3按质量比10：10：1混合研磨，加热至900℃并保温3 h，反复洗涤并干燥，即得稳定化类球形多面体氧化锆微晶。
实施例2
将实施例1中ZrCl4加入量改为5.83 g（浓度0.5 mol/L），前驱体与KCl、YF3的质量比改为10：5：0.5，热处理制度改为800℃保温7 h，其他条件不变， 最终得到类球形多面体氧化锆微晶。
实施例3
将实施例1中ZrCl4加入量改为46.60 g（浓度4 mol/L），无水乙酸加入量改为28mL（10 mol/L），其他条件不变，最终得到类球形多面体氧化锆微晶。
实施例4
将实施例1中水浴温度改为70℃，前驱体与KCl、YF3的质量比改为10：20：2，其他条件不变，最终得到类球形多面体氧化锆微晶。
实施例5
将实施例1中水浴温度改为90℃，热处理制度改为950℃保温3 h，其他条件不变，最终得到类球形多面体氧化锆微晶。
上述的实施例仅例示性说明本发明创造的原理及其功效，以及部分运用的实施例，而非用于限制本发明；应当指出，对于本领域的普通技术人员来说，在不脱离本发明创造构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。
Claims (6)
1.一种稳定化类球形多面体氧化锆微晶的制备方法，其特征在于包括如下步骤：
步骤一：配制一定质量浓度的ZrCl4-乙醇溶液，搅拌至澄清后加入沉淀剂；
步骤二：将步骤一制得的混合溶液经水浴回流24 h形成沉淀，然后在110℃烘箱中干燥得到前驱体；
步骤三：将步骤二制得的前驱体与熔盐KCl和添加剂YF3按一定质量比混合研磨，在一定温度下热处理；
步骤四：将步骤三制得的热处理产物用去离子水清洗三次，再用乙醇清洗一次后，即得到稳定化类球形多面体氧化锆微晶。
2.根据权利要求1所述的制备方法，其特征在于：所述步骤一中的沉淀剂为无水乙酸，其浓度为6～10 mol/L。
3.根据权利要求1所述的制备方法，其特征在于：所述步骤一中ZrCl4-乙醇溶液的浓度为0.5～4 mol/L。
4.根据权利要求1所述的制备方法，其特征在于：所述步骤二中的水浴温度为70～90℃。
5.根据权利要求1所述的制备方法，其特征在于：所述步骤二中前驱体与熔盐KCl与添加剂YF3的质量比为10:5～20:0.5～2。
6.根据权利要求1所述的制备方法，其特征在于：所述步骤三中热处理温度为800～950℃，保温时间3～7 h。
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| CN108557879A (zh) * | 2018-07-08 | 2018-09-21 | 景德镇陶瓷大学 | 一种片状部分稳定氧化锆的制备方法 |
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| CN103204542A (zh) * | 2013-05-07 | 2013-07-17 | 景德镇陶瓷学院 | 一种采用非水沉淀法制备稳定氧化锆超细粉体的方法 |
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