CN109354496A - 一种钒酸钇透明陶瓷的制备方法 - Google Patents

一种钒酸钇透明陶瓷的制备方法 Download PDF

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CN109354496A
CN109354496A CN201811214466.6A CN201811214466A CN109354496A CN 109354496 A CN109354496 A CN 109354496A CN 201811214466 A CN201811214466 A CN 201811214466A CN 109354496 A CN109354496 A CN 109354496A
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郭艳艳
王殿元
王庆凯
段兴凯
吴杏华
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Abstract

一种钒酸钇透明陶瓷的制备方法，该方法包括以下步骤：先将六水硝酸钇溶于去离子水，磁力搅拌得到硝酸钇水溶液，然后加入适量柠檬酸和偏钒酸铵，磁力搅拌得到混合溶液；再将混合溶液置于烘箱内蒸发掉水分，得到褐色固体产物，产物粉碎后于马弗炉内退火，用稀硝酸和去离子水洗涤、干燥，得到钒酸钇纳米粉末；最后将所得钒酸钇纳米粉末干压成型，空气气氛下无压烧结得到钒酸钇透明陶瓷。通过本发明制备的钒酸钇陶瓷致密度高、透光性好，并且本发明方法具有烧结温度低、制备工艺简单、生产周期短、成本低等优点，适于钒酸钇透明陶瓷材料的工业化生产。

Description

一种钒酸钇透明陶瓷的制备方法
技术领域
本发明涉及一种钒酸钇透明陶瓷的制备方法。
背景技术
钒酸钇（YVO4）属四方晶系，具有四方相锆英石结构，空间群为D4h，晶胞参数a = b= 0.712 nm，c = 0.629 nm，密度4.22 g/cm3，熔点1825℃，热导率5.10~5.23 W/mK。钒酸钇的化学稳定性、热稳定性和机械性能都很好，可以掺杂高浓度的稀土发光离子并获得高效率的可见区荧光，因此钒酸钇是一种优良的发光基质材料。如铕离子掺杂的钒酸钇（YVO4:Eu3+）发光材料在紫外光激发下能发出比较纯正的红光，该材料在高压汞灯、阴极发射管、X射线探测器等得到广泛应用。
钒酸钇单晶是一种具有优良物理光学性能的双折射晶体材料。该晶体透光范围宽（400 ~ 5000 nm）、透过率高、双折射系数大、莫氏硬度较大、不易潮解、易于加工。因此，钒酸钇晶体也被广泛应用于光纤通信、激光、闪烁体等领域。钒酸钇单晶通常以铱坩埚作容器、中频感应加热、提拉法生长，产品的缺陷少、光学均一性高。但总的来说，生长钒酸钇晶体所需设备复杂、生产周期长、实验条件要求高、成本高、尺寸受限制，因此这些因素也严重影响了其工业化生产和应用。
近年来，随着陶瓷制备技术的发展，人们已成功制备出了Y3Al5O12（YAG）、Y2O3、CaF2等一批高光学质量的透明陶瓷，其性能已可以与单晶材料相媲美，如掺钕离子的钇铝石榴石（YAG:Nd3+）透明陶瓷已实现了瓦量级的连续激光输出，因此采用先进的透明陶瓷制备技术，制备高透光率的钒酸钇透明陶瓷必将大大提高钒酸钇的生产效率，缩短生产周期、降低生产成本。中国发明专利CN200910094955.7和CN200910094957.6中冯晶等人分别提出了一种含镧系稀土和钪的YVO4透明激光陶瓷的制备方法、一种Nd-YVO4透明激光陶瓷材料的制备方法，他们提出了以氧化钇粉、氧化钒粉为主要原料，氧化钪粉或氧化钕粉或氧化铥粉为掺杂原料，另外加入氧化镁粉、高纯TEOS为助剂，经球磨、粉体成型、真空烧结得到钒酸钇透明陶瓷，但未提供陶瓷样品的实物图片，且高温烧结温度高达1800℃，时间长达30小时。
发明内容
本发明其目的就在于提供一种钒酸钇透明陶瓷的制备方法，解决了现有技术方法存在生产成本高、操作复杂、耗时长的问题。
为实现上述目的而采取的技术方案是，一种钒酸钇透明陶瓷的制备方法，该方法包括以下步骤：
（1）将六水硝酸钇溶于去离子水，磁力搅拌得到硝酸钇水溶液；
（2）在步骤（1）得到的溶液中加入适量柠檬酸，进行磁力搅拌；
（3）在步骤（2）得到的混合溶液中加入适量偏钒酸铵，进行磁力搅拌，得到混合溶液；
（4）将步骤（3）得到的混合溶液置于电热烘箱内蒸发掉水分，得到褐色固体产物；
（5）将步骤（4）得到的产物粉碎后，于马弗炉内退火，用稀硝酸和去离子水洗涤、干燥，得到钒酸钇纳米粉末；
（6）将步骤（5）得到的钒酸钇纳米粉末干压成型，在空气气氛下无压烧结，得到钒酸钇透明陶瓷。
所述硝酸钇、柠檬酸和偏钒酸铵的摩尔比为1:0.7~0.9:1。
所述步骤（1）（2）（3）中的磁力搅拌时间为10~30 min。
所述步骤（4）中的烘箱内蒸发水分时，需先在70~80℃蒸发2~3天，再在100~120℃蒸发12~24 h。
所述步骤（5）中的退火温度为900~1000℃，时间为40~60 min。
所述步骤（6）中的成型压力为50~60 MPa，成型时间为5~10 min；所述高温烧结为两步烧结，烧结温度为1500~1600℃和1200~1300℃，保温时间分别为4~6 h和10~20 h。
有益效果
与现有技术相比本发明具有以下优点。
1.本发明中的钒酸钇纳米粉末晶粒近似球形、粒径为20~30 nm，原料粉体粒径小有利于晶界的扩散和迁移，提高烧结活性，降低陶瓷烧结温度，减弱钒酸钇陶瓷样品的双折射，透光性会更好；
2.陶瓷坯体先在1500~1600℃烧结4~6 h，使陶瓷坯体获得足够晶界扩散的热力学驱动力，致密度迅速提高而晶粒长大不明显，再在1200~1300℃烧结10~20 h，促进晶界扩散的同时抑制晶界迁移，推动致密化过程的继续进行，而晶粒不长大，故有利于钒酸钇陶瓷的致密度和透光率的显著提高；
3.本发明的制备方法具有烧结温度低、制备工艺简单、生产周期短、成本低等优点，适于钒酸钇透明陶瓷材料的工业化生产。
附图说明
以下结合附图对本发明作进一步详述。
图1为本发明实施例1所得钒酸钇透明陶瓷实物图；
图2为本发明实施例2所得钒酸钇透明陶瓷实物图；
图3为本发明实施例3所得钒酸钇透明陶瓷实物图。
具体实施方式
下面结合附图，对本发明作进一步的说明。
一种钒酸钇透明陶瓷的制备方法，该方法包括以下步骤：
（1）将六水硝酸钇溶于去离子水，磁力搅拌得到硝酸钇水溶液；
（2）在步骤（1）得到的溶液中加入适量柠檬酸，进行磁力搅拌；
（3）在步骤（2）得到的混合溶液中加入适量偏钒酸铵，进行磁力搅拌，得到混合溶液；
（4）将步骤（3）得到的混合溶液置于电热烘箱内蒸发掉水分，得到褐色固体产物；
（5）将步骤（4）得到的产物粉碎后，于马弗炉内退火，用稀硝酸和去离子水洗涤、干燥，得到钒酸钇纳米粉末；
（6）将步骤（5）得到的钒酸钇纳米粉末干压成型，在空气气氛下无压烧结，得到钒酸钇透明陶瓷。
所述硝酸钇、柠檬酸和偏钒酸铵的摩尔比为1:0.7~0.9:1。
所述步骤（1）（2）（3）中的磁力搅拌时间为10~30 min。
所述步骤（4）中的烘箱内蒸发水分时，需先在70~80℃蒸发2~3天，再在100~120℃蒸发12~24 h。
所述步骤（5）中的退火温度为900~1000℃，时间为40~60 min。
所述步骤（6）中的成型压力为50~60 MPa，成型时间为5~10 min；所述高温烧结为两步烧结，烧结温度为1500~1600℃和1200~1300℃，保温时间分别为4~6 h和10~20 h。
实施例1
（1）将3.83 g六水硝酸钇溶于40 mL去离子水中，磁力搅拌15 min，得到硝酸钇水溶液；加入1.68g一水柠檬酸，进行磁力搅拌10 min；再加入1.17 g偏钒酸铵，进行磁力搅拌30min，得到混合溶液；将混合溶液置于70℃电热烘箱内蒸发3得到溶胶，再于110℃电热烘箱内蒸发24 h得到褐色固体产物；将得到的产物于玛瑙研钵中粉碎后，于900℃马弗炉内退火60 min，用稀硝酸和去离子水洗涤多次、干燥，得到钒酸钇纳米粉末；
（2）将步骤（1）得到的钒酸钇纳米粉末置于模具中，60 MPa单向干压10 min，得钒酸钇陶瓷坯体，将坯体在空气气氛下1500℃无压烧结5 h，再在空气气氛下1200℃无压烧结15h，得到钒酸钇透明陶瓷，如图1所示。
实施例2
（1）将3.83 g六水硝酸钇溶于40 mL去离子水中，磁力搅拌15 min，得到硝酸钇水溶液；加入1.68g一水柠檬酸，进行磁力搅拌10 min；再加入1.17 g偏钒酸铵，进行磁力搅拌30min，得到混合溶液；将混合溶液置于70℃电热烘箱内蒸发3得到溶胶，再于110℃电热烘箱内蒸发24 h得到褐色固体产物；将得到的产物于玛瑙研钵中粉碎后，于900℃马弗炉内退火60 min，用稀硝酸和去离子水洗涤多次、干燥，得到钒酸钇纳米粉末；
（2）将步骤（1）得到的钒酸钇纳米粉末置于模具中，60 MPa单向干压10 min，得钒酸钇陶瓷坯体，将坯体在空气气氛下1550℃无压烧结5 h，再在空气气氛下1200℃无压烧结15h，得到钒酸钇透明陶瓷，如图2所示。
实施例3
（1）将3.83 g六水硝酸钇溶于40 mL去离子水中，磁力搅拌15 min，得到硝酸钇水溶液；加入1.68g一水柠檬酸，进行磁力搅拌10 min；再加入1.17 g偏钒酸铵，进行磁力搅拌30min，得到混合溶液；将混合溶液置于70℃电热烘箱内蒸发3得到溶胶，再于110℃电热烘箱内蒸发24 h得到褐色固体产物；将得到的产物于玛瑙研钵中粉碎后，于900℃马弗炉内退火60 min，用稀硝酸和去离子水洗涤多次、干燥，得到钒酸钇纳米粉末；
（2）将步骤（1）得到的钒酸钇纳米粉末置于模具中，60 MPa单向干压10 min，得钒酸钇陶瓷坯体，将坯体在空气气氛下1600℃无压烧结5 h，再在空气气氛下1200℃无压烧结15h，得到钒酸钇透明陶瓷，如图3所示。

Claims (6)

1.一种钒酸钇透明陶瓷的制备方法，其特征在于，该方法包括以下步骤：
将六水硝酸钇溶于去离子水，磁力搅拌得到硝酸钇水溶液；
在步骤（1）得到的溶液中加入适量柠檬酸，进行磁力搅拌；
在步骤（2）得到的混合溶液中加入适量偏钒酸铵，进行磁力搅拌，得到混合溶液；
将步骤（3）得到的混合溶液置于电热烘箱内蒸发掉水分，得到褐色固体产物；
将步骤（4）得到的产物粉碎后，于马弗炉内退火，用稀硝酸和去离子水洗涤、干燥，得到钒酸钇纳米粉末；
将步骤（5）得到的钒酸钇纳米粉末干压成型，在空气气氛下无压烧结，得到钒酸钇透明陶瓷。
2.根据权利要求1所述的钒酸钇透明陶瓷的制备方法，其特征在于，所述硝酸钇、柠檬酸和偏钒酸铵的摩尔比为1:0.7~0.9:1。
3.根据权利要求1所述的一种钒酸钇透明陶瓷的制备方法，其特征在于，所述步骤（1）（2）（3）中的磁力搅拌时间为10~30 min。
4.根据权利要求1所述的一种钒酸钇透明陶瓷的制备方法，其特征在于，所述步骤（4）中的烘箱内蒸发水分时，需先在70~80℃蒸发2~3天，再在100~120℃蒸发12~24 h。
5.根据权利要求1所述的一种钒酸钇透明陶瓷的制备方法，其特征在于，所述步骤（5）中的退火温度为900~1000℃，时间为40~60 min。
6.根据权利要求1所述的一种钒酸钇透明陶瓷的制备方法，其特征在于，所述步骤（6）中的成型压力为50~60 MPa，成型时间为5~10 min；所述高温烧结为两步烧结，烧结温度为1500~1600℃和1200~1300℃，保温时间分别为4~6 h和10~20 h。
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