CN114014646A - 一种柠檬酸螯合法制备纳米铝酸钆粉体材料的方法 - Google Patents
一种柠檬酸螯合法制备纳米铝酸钆粉体材料的方法 Download PDFInfo
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000000843 powder Substances 0.000 title claims abstract description 35
- -1 gadolinium aluminate Chemical class 0.000 title claims abstract description 34
- 229910052688 Gadolinium Inorganic materials 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 title claims abstract description 25
- 230000009920 chelation Effects 0.000 title claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 19
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002738 chelating agent Substances 0.000 claims abstract description 9
- 239000002270 dispersing agent Substances 0.000 claims abstract description 9
- 239000011858 nanopowder Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims abstract description 3
- 229910002614 GdAlO3 Inorganic materials 0.000 claims description 8
- 150000001768 cations Chemical class 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- RJOJUSXNYCILHH-UHFFFAOYSA-N gadolinium(3+) Chemical compound [Gd+3] RJOJUSXNYCILHH-UHFFFAOYSA-N 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 6
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 22
- 239000011259 mixed solution Substances 0.000 description 6
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 239000011240 wet gel Substances 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
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- 239000002994 raw material Substances 0.000 description 2
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- 238000002441 X-ray diffraction Methods 0.000 description 1
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- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
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- 238000001027 hydrothermal synthesis Methods 0.000 description 1
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Abstract
本发明提供一种柠檬酸螯合法制备纳米铝酸钆粉体材料的方法,涉及一种制备纳米粉体的方法,将Gd2O3溶于硝酸溶液中,与Al(NO3)3溶液混合制成稀土溶液,用柠檬酸为螯合剂,以柠檬酸铵作为分散剂,无水乙醇作为溶剂在70℃下进行剧烈混合搅拌,直至形成浓稠的淡黄色透明液体,溶液自然冷却至室温形成凝胶,经加热干燥形成黄色蓬松状前驱体,前驱体经研磨后煅烧,得到铝酸钆(GdAlO3)纳米粉体材料。本发明提供了一种柠檬酸螯合法制备纳米铝酸钆粉体材料的方法,该方法工艺简单,制备出的粉体晶体呈近球形,具有纯度高、杂质少、大小均匀、粒径尺寸小等优点,在制备发光基体材料等实际应用中有广阔的前景。
Description
技术领域
本发明属于纳米粉体材料技术领域,具体涉及一种柠檬酸螯合法制备纳米铝酸钆粉体材料的方法。
背景技术
稀土钙钛矿的晶体结构相对简单,具有独特的电、磁、光、压电、催化和磁阻特性。铝酸钆(GdAlO3)是具有钙钛矿ABO3结构的重要稀土铝酸盐,因其优异的光学性能、机械性能及稳定的物化性能,而广泛应用于新型光学基体材料、闪烁体、测温材料和复合材料增强材料,且有文献报道铝酸钆可作为新一代中子吸收材料应用,目前已材料领域的研究热点。
改善和提高粉体的特性是获得性能优异的新型陶瓷材料的关键。目前,制备铝酸钆的技术有很多,工业上一般采用固相法,利用Gd2O3和Al2O3的固态粉末在高温下煅烧制得。这种方法虽然简单易行,但工艺中原料研磨和高温煅烧过程,将会对材料的微观结构以及产物性能产生负面影响。近年共沉淀法、溶胶-凝胶法、水热合成法等湿化学法制备铝酸钆受到广泛关注。溶胶-凝胶法具有效率高、反应条件温和,制备的粉体均匀性高、粒度小等特点,但目前该方法合成的粉体尺寸和形貌远没有达到理想状态,尚无文献系统研究柠檬酸螯合法制备铝酸钆技术。
发明内容
本发明的目的在于提供一种柠檬酸螯合法制备纳米铝酸钆粉体材料的方法,该方法采用柠檬酸为螯合剂,柠檬酸铵为分散剂下合成铝酸钆纳米粉体,合成工艺简单,制备出的粉体基本呈球形、分散性良好、粒径尺寸小、大小均匀。
本发明解决其技术问题所采用的技术方案是:一种柠檬酸螯合法制备纳米铝酸钆粉体材料的方法,包括如下步骤:
(1)将钆离子溶液与铝离子溶液混合制成稀土溶液;
(2)以柠檬酸作为螯合剂,螯合剂与溶液金属阳离子的摩尔比为0~2.0;以柠檬酸铵作为分散剂,分散剂与柠檬酸的摩尔比为0~2.0;无水乙醇作为溶剂,乙醇与水的摩尔比为0~∞;用浓氨水调节稀土溶液的pH值为9~11,在70 ℃下进行剧烈混合搅拌,直至形成浓稠的淡黄色透明液体,溶液自然冷却至室温形成凝胶,经加热干燥形成黄色蓬松状前驱体;
(3)在900~1300 ℃下高温煅烧所述前驱体,煅烧保温时间为2~4 h,得到GdAlO3粉体材料。
进一步地,步骤(1)的所述稀土溶中液钆离子和铝离子的摩尔比为1:1。
进一步地,步骤(1)的所述稀土溶中总阳离子浓度在0.2~0.5 mol/L范围之内。
进一步地,所述步骤(2)中前驱体的干燥温度为90~130 ℃。
进一步地,所述步骤(3)中将前驱体升温至煅烧温度的速率为10~20 ℃/min。
进一步地,所述步骤(3)煅烧前对前驱体进行球磨,过300目筛。
与现有技术相比,本发明的优点与效果是:
1. 本发明采用柠檬酸螯合法制备纳米GdAlO3粉体材料,所用原料简单易得损失少,工艺操作简便,制备周期短,在探索制备铝酸钆纳米粉体材料制备方面具有重要的指导意义;
2. 本发明通过控制柠檬酸螯合剂加入量,调节柠檬酸铵分散剂和无水乙醇溶剂的加入量,以及在不同温度下煅烧来控制产品粉体的形貌及尺寸。前驱体经煅烧获得GdAlO3纳米粉体材料,制备出的粉体基本呈球形、分散性良好、粒径尺寸小、大小均匀。
附图说明
图1为实施例1制备的样品粉体的 XRD 图谱。
图2为实施例1制备的样品粉体的 SEM形貌。
图3为实施例2制备的样品粉体的 XRD 图谱。
图4为实施例2制备的样品粉体的 SEM形貌。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合附图及实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅用以解释本发明,并不用于限定本发明。
以下实施例中Gd2O3及Al2O3纯度均为99.99%,氨水、硝酸等为分析纯试剂,蒸馏水为二次水。以上试剂均没有经过纯化处理。
实施例1
一种柠檬酸螯合法制备纳米铝酸钆粉体材料的方法,包括如下步骤:
(1)取Gd2O3溶于稀硝酸中制成Gd (NO3)3溶液,经过充分搅拌使溶液彻底溶解后,加入无水乙醇,调节醇水摩尔比为1;
(2)将与所述Gd2O3等摩尔的Al2O3溶于稀硝酸中制成Al(NO3)3溶液;
(3)在不断搅拌下将Gd (NO3)3和Al (NO3)3溶液混合,制成总阳离子浓度为0.4mol/L的稀土溶液,其中钆离子和铝离子的摩尔比为1:1;
(4)加入螯合剂柠檬酸,控制柠檬酸的摩尔数与金属阳离子的总摩尔数之比为0.5;
(5)加入分散剂柠檬酸铵,控制柠檬酸铵与柠檬酸的摩尔数之比为0.5;
(6)用浓氨水调节混合溶液pH为9,然后置于70 ℃水浴中,持续搅拌直至形成湿凝胶;
(7)将所得湿凝胶放到真空干燥箱中,在110 ℃温度下干燥12 h,得到前驱体粉末;
(8)将干燥好的前驱体进行球磨,过300目筛,以10 ℃/min的速率升温至1000 ℃,煅烧3h后随炉冷却,得到GdAlO3纳米粉体样品。
采用日本理学(Rigaku)D/MAX-RB型X射线衍射仪和HITACHI S-3400N型扫描电镜对样品进行分析,结果表明,生成物的特征峰与标准卡片JCPDS-46-0395完全吻合,说明制备的样品为纯相GdAlO3,如附图1所示,样品粉体微观形貌基本呈球形、分散性良好、粒径尺寸小、大小均匀,直径约为100 nm,如图2所示。
实施例2
一种柠檬酸螯合法制备纳米铝酸钆粉体材料的方法,包括如下步骤:
(1)取Gd2O3溶于稀硝酸中制成Gd (NO3)3溶液,经过充分搅拌使溶液彻底溶解后,加入无水乙醇,调节醇水摩尔比为2;
(2)将与所述Gd2O3等摩尔的Al2O3溶于稀硝酸中制成Al(NO3)3溶液;
(3)在不断搅拌下将Gd (NO3)3和Al (NO3)3溶液混合,制成总阳离子浓度为0.2mol/L的稀土溶液,其中钆离子和铝离子的摩尔比为1:1;
(4)加入螯合剂柠檬酸,控制柠檬酸的摩尔数与金属阳离子的总摩尔数之比为1;
(5)加入分散剂柠檬酸铵,控制柠檬酸铵与柠檬酸的摩尔数之比为1;
(6)用浓氨水调节混合溶液pH为10,然后置于70 ℃水浴中,持续搅拌直至形成湿凝胶;
(7)将所得湿凝胶放到真空干燥箱中,在120 ℃温度下干燥12 h,得到前驱体粉末;
(8)将干燥好的前驱体进行球磨,过300目筛,以15 ℃/min的速率升温至1100 ℃,煅烧2h后随炉冷却,得到GdAlO3纳米粉体样品。
本实施例制备的GdAlO3粉体的XRD图谱如图3所示,GdAlO3粉体的微观形貌如图4所示。
以上技术方案阐述了本发明的技术思路,不能以此限定本发明的保护范围,凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上技术方案所作的任何改动及修饰,均属于本发明技术方案的保护范围。
Claims (6)
1.一种柠檬酸螯合法制备纳米铝酸钆粉体材料的方法,其特征在于,包括如下步骤:
(1)将钆离子溶液与铝离子溶液混合制成稀土溶液;
(2)以柠檬酸作为螯合剂,螯合剂与溶液金属阳离子的摩尔比为0~2.0;以柠檬酸铵作为分散剂,分散剂与柠檬酸的摩尔比为0~2.0;无水乙醇作为溶剂,乙醇与水的摩尔比为0~∞;用浓氨水调节稀土溶液的pH值为9~11,在70 ℃下进行剧烈混合搅拌,直至形成浓稠的淡黄色透明液体,溶液自然冷却至室温形成凝胶,经加热干燥形成黄色蓬松状前驱体;
(3)高温煅烧所述前驱体,球磨后得到GdAlO3纳米粉体材料,其中前驱体的煅烧温度为900~1300 ℃,煅烧保温时间为2~4 h。
2.根据权利要求1所述的一种柠檬酸螯合法制备纳米铝酸钆粉体材料的方法,其特征在于,步骤(1)的所述稀土溶中液钆离子和铝离子的摩尔比为1:1。
3.根据权利要求1所述的一种柠檬酸螯合法制备纳米铝酸钆粉体材料的方法,其特征在于,步骤(1)的所述稀土溶中总阳离子浓度在0.2~0.5 mol/L范围之内。
4.根据权利要求1所述的一种柠檬酸螯合法制备纳米铝酸钆粉体材料的方法,其特征在于,所述步骤(2)中前驱体的干燥温度为90~130 ℃。
5.根据权利要求1所述的一种柠檬酸螯合法制备纳米铝酸钆粉体材料的方法,其特征在于,所述步骤(3)中将前驱体升温至煅烧温度的速率为10~20 ℃/min。
6.根据权利要求1所述的一种柠檬酸螯合法制备纳米铝酸钆粉体材料的方法,其特征在于,所述步骤(3)煅烧前对前驱体进行球磨细化粉体,过300目筛。
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