CN106757347B - 一种非水解溶胶-凝胶法结合熔盐工艺制备氧化锆晶须的方法 - Google Patents
一种非水解溶胶-凝胶法结合熔盐工艺制备氧化锆晶须的方法 Download PDFInfo
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- 150000003839 salts Chemical class 0.000 title claims abstract description 44
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- -1 calcirm-fluoride Chemical compound 0.000 claims description 2
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 claims description 2
- 235000003270 potassium fluoride Nutrition 0.000 claims description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- OMQSJNWFFJOIMO-UHFFFAOYSA-J zirconium tetrafluoride Chemical compound F[Zr](F)(F)F OMQSJNWFFJOIMO-UHFFFAOYSA-J 0.000 claims description 2
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- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 2
- IVORCBKUUYGUOL-UHFFFAOYSA-N 1-ethynyl-2,4-dimethoxybenzene Chemical compound COC1=CC=C(C#C)C(OC)=C1 IVORCBKUUYGUOL-UHFFFAOYSA-N 0.000 description 1
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
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- C—CHEMISTRY; METALLURGY
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B9/00—Single-crystal growth from melt solutions using molten solvents
- C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
- C30B9/08—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
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Abstract
本发明公开一种非水解溶胶‑凝胶法结合熔盐工艺制备氧化锆晶须的方法,其特征在于包括如下步骤:在通风橱中称取一定量的无水锆源放入锥形瓶中,加入适量的无水有机溶剂搅拌至锆源全部溶解形成透明溶液;透明溶液经油浴加热回流24h后得到均匀的氧化锆溶胶,然后置于烘箱干燥,经预锻烧后形成氧化锆干凝胶粉;将干凝胶粉与熔盐、熔盐添加剂混合,经热处理、洗涤、干燥得到氧化锆晶须。该方法原料成本低,工艺简单,易于控制,可大规模生产,因此具有广阔的市场空间。
Description
技术领域
本发明属于新材料技术领域,具体涉及一种非水解溶胶-凝胶法结合熔盐工艺制备氧化锆晶须的方法。
背景技术
氧化锆具有熔点高(2715℃)、韧性好、强度大、抗磨损、耐腐蚀以及抗氧化等一系列优异性能,可用于制备航空发动机组件、燃料电池和氧传感器、人造骨骼、催化剂载体、过滤钢水所用的泡沫陶瓷、抗氧化及耐腐蚀涂层、切削刀具、磨具以及特种耐火材料。氧化锆陶瓷拥有众多优异的物理和化学性能,而晶须通常是指具有一定长径比,且直径较小的一种单晶纤维状材料,其强度接近完整晶体的理论值。因此若将氧化锆制备成氧化锆晶须,便能充分发挥氧化锆与晶须材料两者的优势,可大幅提升陶瓷、金属基复合材料的机械性能,如用于增韧补强氧化锆陶瓷材料;利用其膨胀系数与金属材料接近的特点,用作高温金属合金材料增强体等,应用前景十分广阔。目前,国内外制备氧化锆一维材料的研究集中在氧化锆纳米管、纳米棒以及纳米线等一维纳米材料,它们主要应用于功能材料领域;而对能够应用于结构材料领域增韧补强的氧化锆晶须的研究则少之又少,经检索只查阅到采用化学气相沉积(CVD)法或水热法制备氧化锆晶须的6 篇文献。CVD法[江頭誠, 勝木宏昭, 高月誠治, 岩永浩. 単斜晶ZrO2ウイスカーの気相成長. 窯業協會誌, 1987, 95(1), 138-143.]存在温度高,能耗大,设备要求高,工艺复杂,产率低等缺点;而水热法[Murase Y,Kato E. Preparation of Zirconia Whiskers from Zirconium Hydroxide in SulfuricAcid Solutions under Hydrothermal Conditions at 200° C [J]. J Am. Ceram Soc,2001, 84(1), 2705-2706] 需要使用高压釜形成一定的蒸汽压,对设备要求较高,控制难度大,并且周期长,产率低,难以大规模工业化生产。
发明内容
本发明要解决的技术问题是提供一种原料成本低,工艺简单,易于控制,可大规模生产的氧化锆晶须的制备方法。
为解决以上技术问题,本发明的技术方案是:一种非水解溶胶-凝胶法结合熔盐工艺制备氧化锆晶须的方法,其特征在于包括如下步骤:
步骤一:在通风橱中称取一定量的无水锆源放入锥形瓶中,加入适量的无水有机溶剂搅拌至锆源全部溶解形成透明溶液;
步骤二:透明溶液经油浴加热回流24h后得到均匀的氧化锆溶胶,然后置于烘箱干燥,经预锻烧后形成氧化锆干凝胶粉;
步骤三:将干凝胶粉与熔盐、熔盐添加剂混合,经热处理、洗涤、干燥得到氧化锆晶须。
所述无水锆源为无水氯化锆、氟化锆、无水硫酸锆、无水醋酸锆中的一种。
所述无水溶剂为乙醇、异丙醇、正丙醇、丁醇中的一种。
所述熔盐添加剂为氟化钠、氟化钾、氟化锂、氟化铵、氟化钙、氟化镁中的一种。
所述步骤二制得氧化锆溶胶中无水锆源的浓度为0.2~1.0 mol/L。
所述步骤二中回流的温度为100~140℃之间。
所述步骤三中熔盐为偏钒酸钠或磷酸钠。
所述步骤三中干凝胶粉,熔盐,熔盐添加剂的摩尔比为:5~10:5~10:0.5~1。
所述步骤三中热处理温度为800~1000℃,保温时间为0.5~5h。
本专利采用非水解溶胶-凝胶法制备氧化锆干凝胶粉,然后将其与特定的熔盐混合,充分利用熔盐中的氟离子易于吸附在氧化锆高表面能晶面上的特点,与现有的CVD法和水热法相比,具有设备要求不高,工艺简单,控制要求低,晶须产率高且质量好,易于工业化推广等优点,因此市场应用前景十分广阔。
附图说明
图1为本发明氧化锆晶须的FE-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
以无水ZrCl4(工业纯)为锆源,无水乙醇(化学纯)为溶剂,NaVO3(化学纯)为熔盐,NaF(化学纯)为熔盐添加剂,首先称取7.00g无水ZrCl4溶于30 ml无水乙醇中配成1.0 mol/L 的溶液,搅拌1 h得到澄清溶液后,置于120℃油浴锅中冷凝回流24h,得到均匀透明的氧化锆溶胶,将溶胶置于130 ℃烘箱内干燥,然后在300℃锻烧得到干凝胶粉,将干凝胶粉、熔盐与熔盐添加剂按照摩尔比6:6:1混合后置于刚玉坩埚内,加热至850 ℃,并保温3 h,经洗涤、干燥后得到氧化锆晶须。
实施例2
以无水ZrCl4为锆源,无水乙醇为溶剂,NaVO3为熔盐, NaF为熔盐添加剂,制备氧化锆晶须的工艺与实例1相同,只是热处理温度为900℃保温5 h。
实施例3
以无水Zr(SO4)2为锆源,无水乙醇为溶剂,NaVO3为熔盐, LiF为熔盐添加剂,制备氧化锆晶须的工艺与实例1相同,只是干凝胶粉、熔盐与氟化物摩尔比变为10:10:1。
实施例4
以无水醋酸锆为锆源,无水丁醇为溶剂,NaVO3为熔盐, NH4F为熔盐添加剂,制备氧化锆晶须的工艺与实例1相同,只是回流温度为140℃,热处理温度为950℃保温3 h。
实施例5
以无水ZrCl4为锆源,无水正丙醇为溶剂,Na3PO4为熔盐, KF为熔盐添加剂,制备氧化锆晶须的工艺与实例1相同,只是干凝胶粉、熔盐与氟化物摩尔比变为6:10:1,热处理900℃,保温3 h。
实施例6
以无水ZrF4为锆源,无水异丙醇为溶剂,NaVO3为熔盐, NH4F为熔盐添加剂,制备氧化锆晶须的工艺与实例1相同,只是溶胶的回流温度为110 ℃,ZrCl4前驱体浓度为0.2mol/L。
实施例7
以无水ZrCl4为锆源,无水乙醇为溶剂,Na3PO4为熔盐, NaF为熔盐添加剂,制备氧化锆晶须的工艺与实例1相同,只是ZrCl4前驱体浓度为0.5 mol/L。
实施例8
以无水ZrCl4为锆源,无水乙醇为溶剂,Na3PO4为熔盐,CaF2为熔盐添加剂,制备氧化锆晶须的工艺与实例1相同,只是ZrCl4前驱体浓度为0.3 mol/L。
实施例9
以无水ZrCl4为锆源,无水乙醇为溶剂,NaVO3为熔盐,MgF2为熔盐添加剂,制备氧化锆晶须的工艺与实例1相同,只是前驱体浓度为0.75 mol/L保温时间为0.5 h。
Claims (6)
1.一种非水解溶胶-凝胶法结合熔盐工艺制备氧化锆晶须的方法,其特征在于包括如下步骤:
步骤一:在通风橱中称取一定量的无水锆源放入锥形瓶中,加入适量的无水有机溶剂搅拌至锆源全部溶解形成透明溶液;
步骤二:透明溶液经油浴加热回流24h后得到均匀的氧化锆溶胶,然后置于烘箱干燥,经预锻烧后形成氧化锆干凝胶粉;
步骤三:将干凝胶粉与熔盐、熔盐添加剂混合,经热处理、洗涤、干燥得到氧化锆晶须;
所述步骤三中熔盐为偏钒酸钠或磷酸钠;
所述熔盐添加剂为氟化钠、氟化钾、氟化锂、氟化铵、氟化钙、氟化镁中的一种;
所述步骤三中热处理温度为800~1000℃,保温时间为0.5~5h。
2.根据权利要求1所述制备氧化锆晶须的方法,其特征在于:所述无水锆源为无水氯化锆、氟化锆、无水硫酸锆、无水醋酸锆中的一种。
3.根据权利要求1所述制备氧化锆晶须的方法,其特征在于:所述无水溶剂为乙醇、异丙醇、正丙醇、丁醇中的一种。
4.根据权利要求1所述制备氧化锆晶须的方法,其特征在于:所述步骤二制得氧化锆溶胶中无水锆源的浓度为0.2~1.0 mol/L。
5.根据权利要求1所述制备氧化锆晶须的方法,其特征在于:所述步骤二中回流的温度为100~140℃之间。
6.根据权利要求1所述制备氧化锆晶须的方法,其特征在于:所述步骤三中干凝胶粉,熔盐,熔盐添加剂的摩尔比为:5~10:5~10:0.5~1。
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