CN102897843A - Method for synthesis of tetracalcium aluminoferrite by sol-gel technology - Google Patents
Method for synthesis of tetracalcium aluminoferrite by sol-gel technology Download PDFInfo
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Abstract
本发明属建筑材料技术领域，具体涉及一种用溶胶-凝胶法合成铁铝酸四钙的方法。本合成方法中用到的原料有四水硝酸钙、九水硝酸铝、九水硝酸铁、一水合柠檬酸、乙二醇和水。具体合成步骤为，将一定化学计量比的三种无机盐溶解在去离子水中并混合均匀，加入柠檬酸制得淡黄色的金属-柠檬酸螯合物溶液，然后加入乙二醇发生酯化反应，将所得溶胶在80度充分搅拌下陈化得到粘性湿凝胶，继续在150℃温度下干燥24小时得到干凝胶，将所得干凝胶粉磨、煅烧得到铁铝酸四钙单矿物。采用溶胶-凝胶法制得的铁铝酸四钙粉体具有高纯度、超细性、易烧结等特点。
The invention belongs to the technical field of building materials, and in particular relates to a method for synthesizing tetracalcium aluminoferrite by a sol-gel method. The raw materials used in the synthesis method include calcium nitrate tetrahydrate, aluminum nitrate nonahydrate, iron nitrate nonahydrate, citric acid monohydrate, ethylene glycol and water. The specific synthesis steps are as follows: dissolve three kinds of inorganic salts with a certain stoichiometric ratio in deionized water and mix evenly, add citric acid to obtain a light yellow metal-citric acid chelate solution, and then add ethylene glycol to undergo esterification reaction , Aging the obtained sol at 80 degrees under full stirring to obtain a viscous wet gel, continuing to dry at 150°C for 24 hours to obtain a xerogel, grinding and calcining the obtained xerogel to obtain tetracalcium aluminoferrite single mineral. The tetracalcium aluminoferrite powder prepared by the sol-gel method has the characteristics of high purity, ultrafineness, and easy sintering.
Description
技术领域 technical field
本发明属建筑材料技术领域，具体涉及一种用溶胶-凝胶法合成铁铝酸四钙的方法。 The invention belongs to the technical field of building materials, and in particular relates to a method for synthesizing tetracalcium aluminoferrite by a sol-gel method.
背景技术 Background technique
水泥熟料主要是由硅酸三钙、硅酸二钙、铝酸三钙和铁铝酸四钙等矿物组成的固溶体。虽然铁铝酸四钙在这四种矿物中所占比例较小，但是在煅烧熟料的过程中，它能降低熟料的熔融温度和熔化成液体（在煅烧熟料过程中所出现的液体，统称为液相）的粘度，有利于硅酸三钙的生成。 Cement clinker is mainly a solid solution composed of minerals such as tricalcium silicate, dicalcium silicate, tricalcium aluminate and tetracalcium aluminoferrite. Although tetracalcium aluminoferrite accounts for a small proportion of these four minerals, it can reduce the melting temperature of the clinker and melt into liquid (the liquid that appears in the process of calcining clinker) during the calcination of clinker , collectively referred to as the liquid phase) viscosity is conducive to the formation of tricalcium silicate.
铁铝酸四钙作为硅酸盐水泥熟料的重要组成部分，其含量一般为10%~18%（质量分数），其水化速度在早期介于铝酸三钙与硅酸三钙之间，虽早期强度类似于铝酸三钙，但后期还能不断增长，类似于硅酸三钙。铁铝酸四钙的水化热较铝酸三钙低，且抗冲击性能和抗硫酸盐性能较好，因此在制造抗硫酸盐水泥或大体积工程用水泥时，适当提高铁铝酸四钙含量是有利的。铁铝酸四钙矿物的水化、凝结和硬化等行为，以及其在不同条件下所形成的水化产物微结构的差异，将对水泥基材料的使用性能产生重要影响。因此，在实验室条件下合成高纯度的铁铝酸四钙并研究其水化以及水化产物凝胶微结构的形成过程，对于利用现代分析方法从纳米尺度揭示水泥基材料的本构关系是必要的。 Tetracalcium aluminoferrite is an important part of Portland cement clinker, its content is generally 10%~18% (mass fraction), and its hydration rate is between tricalcium aluminate and tricalcium silicate in the early stage. , although the early strength is similar to tricalcium aluminate, but it can continue to grow in the later stage, similar to tricalcium silicate. The heat of hydration of tetracalcium aluminoferrite is lower than that of tricalcium aluminate, and its impact resistance and sulfate resistance are better. Therefore, when manufacturing sulfate-resistant cement or cement for large-volume engineering, the tetracalcium aluminoferrite should be appropriately increased. content is favorable. The behaviors of hydration, coagulation and hardening of tetracalcium aluminoferrite minerals, as well as the differences in the microstructure of hydration products formed under different conditions, will have an important impact on the performance of cement-based materials. Therefore, the synthesis of high-purity tetracalcium aluminoferrite under laboratory conditions and the study of its hydration and the formation process of the gel microstructure of the hydration product are important for revealing the constitutive relationship of cement-based materials from the nanoscale using modern analytical methods. necessary.
传统的铁铝酸四钙单矿物的合成是用固相合成法，即将一定化学计量比的各种氧化物粉磨并混合均匀，并在高温下煅烧而成。根据相关资料，用固相合成发合成铁铝酸四钙需要经过至少3次（每次6h）1320℃的高温煅烧。用固相法，由于原料均为固态粉末状混合，可能导致反应物混合不均匀，在煅烧过程中例子扩散困难，烧成温度高、时间长、能耗大，并且产物纯度不高。 The traditional tetracalcium aluminoferrite single mineral is synthesized by solid-phase synthesis, that is, various oxides of a certain stoichiometric ratio are ground and mixed uniformly, and calcined at high temperature. According to relevant information, the synthesis of tetracalcium aluminoferrite by solid phase synthesis requires at least 3 times (6 hours each time) high-temperature calcination at 1320°C. With the solid-phase method, since the raw materials are mixed in solid powder form, it may lead to uneven mixing of the reactants, difficulty in the diffusion of samples during the calcination process, high calcination temperature, long time, high energy consumption, and low purity of the product.
近年来，随着各种化学合成制备方法的发展，带来了水泥熟料合成方法的革命。溶胶-凝胶方法是材料制备的重要方法，其在制备纳米材料、薄膜、涂层材料、功能材料和纤维材料等领域有广泛的应用。该方法利用液体化学试剂（或粉末溶于溶剂）为原料（高化学活性的含材料成分的化学物前驱体），在液相下将这些原料均匀混合，并进行一系列的水解、缩合的化学反应，在溶液中形成稳定的透明溶胶液体系；溶胶经过陈化，胶粒间缓慢聚合，形成以前驱体为骨架的三维聚合物或者是颗粒空间网络，网络中充满失去流动性的溶剂，这就是凝胶；凝胶在经过干燥，脱去其间溶剂而形成一种多孔结构的干凝胶或气凝胶；最后，经过烧结固化制备所需材料。溶胶-凝胶方法反应过程易于控制，化学计量准确，产物的纯度很高。该方法的应用不但节省资源，而且对能源消耗少，同时在治理环境污染方面也将发挥重要的作用。 In recent years, with the development of various chemical synthesis preparation methods, it has brought about a revolution in the synthesis method of cement clinker. The sol-gel method is an important method for material preparation, and it has a wide range of applications in the preparation of nanomaterials, thin films, coating materials, functional materials and fiber materials. This method uses liquid chemical reagents (or powder dissolved in a solvent) as raw materials (highly chemically active chemical precursors containing material components), uniformly mixes these raw materials in the liquid phase, and performs a series of hydrolysis and condensation chemical reactions. reaction, forming a stable transparent sol system in the solution; after the sol is aged, the colloidal particles are slowly aggregated to form a three-dimensional polymer with the precursor as the skeleton or a particle space network, and the network is full of solvents that have lost fluidity. It is a gel; the gel is dried and the solvent is removed to form a porous structure of xerogel or aerogel; finally, the required material is prepared by sintering and curing. The reaction process of the sol-gel method is easy to control, the stoichiometry is accurate, and the purity of the product is very high. The application of this method not only saves resources, but also consumes less energy, and will also play an important role in controlling environmental pollution.
发明内容 Contents of the invention
本发明的目的在于克服传统合成铁铝酸四钙单矿物中存在的问题，提供一种用溶胶-凝胶法合成铁铝酸四钙的方法。 The object of the present invention is to overcome the problems existing in the traditional synthesis of tetracalcium aluminoferrite single mineral, and provide a method for synthesizing tetracalcium aluminoferrite by sol-gel method.
本发明提出的一种用溶胶-凝胶法合成铁铝酸四钙的方法，具体步骤如下： A kind of method that the present invention proposes synthesizes tetracalcium aluminoferrite with sol-gel method, concrete steps are as follows:
(1)按质量比精确称取Ca(NO3)2·4H2O、Al(NO3)3·9H2O、Fe(NO3)3·9H2O、一水合柠檬酸、乙二醇和水； (1) Accurately weigh Ca(NO 3 ) 2 4H 2 O, Al(NO 3 ) 3 9H 2 O, Fe(NO 3 ) 3 9H 2 O, citric acid monohydrate, ethylene glycol and water;
(2)反应物溶解：在磁力搅拌机上，以50~60℃加热，将Ca(NO3)2·4H2O、Al(NO3)3·9H2O、Fe(NO3)3·9H2O分别加入水中，加热搅拌20~30min至完全溶解，将三种溶液混合后备用； (2) Dissolution of reactants: on a magnetic stirrer, heat at 50~60°C to dissolve Ca(NO 3 ) 2 ·4H 2 O, Al(NO 3 ) 3 ·9H 2 O, Fe(NO 3 ) 3 ·9H Add 2 O into water respectively, heat and stir for 20~30min until completely dissolved, and mix the three solutions for later use;
(3)金属阳离子的螯合：将一水合柠檬酸颗粒加入到步骤(2)制得的三种溶液的混合体中，加热搅拌40~50min得到清澈的淡黄色溶液； (3) Chelation of metal cations: adding citric acid monohydrate particles into the mixture of the three solutions prepared in step (2), heated and stirred for 40 to 50 min to obtain a clear light yellow solution;
(4)酯化反应：将乙二醇加入到淡黄色硝酸盐-柠檬酸螯合物溶液中，发生酯化反应， 在50~60℃温度下反应30~40min； (4) Esterification reaction: add ethylene glycol into the light yellow nitrate-citric acid chelate solution, esterification reaction occurs, and react at a temperature of 50~60°C for 30~40min;
(5)陈化：将磁力搅拌机温度调节至80~85℃，陈化4~6h，得到粘性湿凝胶； (5) Aging: adjust the temperature of the magnetic stirrer to 80-85°C, and age for 4-6 hours to obtain a viscous wet gel;
(6)干燥：把湿凝胶放在温度为150℃的烘箱中干燥24h，得到干凝胶，粉磨后得到干凝胶粉末并储存在干燥器中； (6) Drying: dry the wet gel in an oven at 150°C for 24 hours to obtain a dry gel, which is powdered to obtain a dry gel powder and stored in a desiccator;
(7)煅烧：将所得到的干凝胶粉末，直接放在1000℃高温炉中煅烧3~5h制得铁铝酸四钙。 (7) Calcination: The obtained xerogel powder is directly calcined in a high-temperature furnace at 1000°C for 3-5 hours to obtain tetracalcium aluminoferrite.
其中：各组分的重量比为： Wherein: the weight ratio of each component is:
Ca(NO3)2·4H2O 100 Ca(NO 3 ) 2 4H 2 O 100
Al(NO3)3·9H2O 79.4 Al(NO 3 ) 3 9H 2 O 79.4
Fe(NO3)3·9H2O 85.6 Fe(NO 3 ) 3 9H 2 O 85.6
一水合柠檬酸 178.0 Citric acid monohydrate 178.0
乙二醇 105.1~210.2 Ethylene glycol 105.1~210.2
水 600~1000。 Water 600~1000.
本发明中，所用Ca(NO3)2·4H2O、Al(NO3)3·9H2O、Fe(NO3)3·9H2O和乙二醇均为市售的化学分析纯试剂。 In the present invention, Ca(NO 3 ) 2 .4H 2 O, Al(NO 3 ) 3 .9H 2 O, Fe(NO 3 ) 3 .9H 2 O and ethylene glycol are commercially available pure reagents for chemical analysis .
本发明中，所用一水合柠檬酸为市售的优级纯试剂，其为白色固体颗粒。 In the present invention, the citric acid monohydrate used is a commercially available superior-grade pure reagent, which is a white solid particle.
本发明中，所用水为去离子水。 In the present invention, the water used is deionized water. the
本发明中，用溶胶-凝胶法来合成水泥单矿物铁铝酸四钙，其制备过程简单且易于控制，反应物前驱物在溶液中以原子水平混合均匀，克服了传统固相合成法煅烧温度高、煅烧次数多以及产物纯度不高等缺点。 In the present invention, a sol-gel method is used to synthesize cement monomineral tetracalcium aluminoferrite. The preparation process is simple and easy to control. The precursors of the reactants are uniformly mixed at the atomic level in the solution, which overcomes the traditional solid-phase synthesis method of calcining. Disadvantages such as high temperature, many times of calcination and low product purity.
采用本发明方法所合成的铁铝酸四钙矿物，经X射线衍射分析，发现铁铝酸四钙的特征峰非常明显，峰值强度高。 The tetracalcium aluminoferrite mineral synthesized by the method of the invention is analyzed by X-ray diffraction, and it is found that the characteristic peak of the tetracalcium aluminoferrite is very obvious and the peak intensity is high.
附图说明 Description of drawings
图1 为铁铝酸四钙X射线衍射图谱。 Figure 1 is the X-ray diffraction pattern of tetracalcium aluminoferrite.
具体实施方式 Detailed ways
下面结合具体实施案例对本发明进行详细说明。 The present invention will be described in detail below in conjunction with specific implementation cases.
实施例1，一种用溶胶-凝胶法合成铁铝酸四钙的方法，其原料的重量比为：Ca(NO3)2·4H2O 100、Al(NO3)3·9H2O 79.4、Fe(NO3)3·9H2O 85.6、一水合柠檬酸178.0、乙二醇105.1和水600。采用如下合成方法：在磁力搅拌机上，以50℃加热，将Ca(NO3)2·4H2O、Al(NO3)3·9H2O、Fe(NO3)3·9H2O分别加入水中，加热搅拌30min至完全溶解；将白色一水合柠檬酸颗粒加入到三种硝酸盐溶液的混合体中，加热搅拌50min得到清澈的淡黄色溶液；将乙二醇加入到淡黄色硝酸盐-柠檬酸螯合物溶液中，发生酯化反应，在50℃温度下反应40min；将磁力搅拌机温度调节至80℃，陈化6h，得到粘性湿凝胶；把湿凝胶放在温度为150℃的烘箱中干燥24h，得到干凝胶，粉磨后得到干凝胶粉末并储存在干燥器中；将所得到的干凝胶粉末，直接放在1000℃高温炉中煅烧3h制得铁铝酸四钙。所得产物的X射线衍射谱图的衍射峰与铁铝酸四钙标准卡片匹配良好，证明产物纯度较高。 Example 1, a method for synthesizing tetracalcium aluminoferrite by sol-gel method, the weight ratio of raw materials is: Ca(NO 3 ) 2 ·4H 2 O 100, Al(NO 3 ) 3 ·9H 2 O 79.4, Fe(NO 3 ) 3 ·9H 2 O 85.6, citric acid monohydrate 178.0, ethylene glycol 105.1 and water 600. The following synthesis method is adopted: on a magnetic stirrer, heating at 50°C, adding Ca(NO 3 ) 2 ·4H 2 O, Al(NO 3 ) 3 ·9H 2 O, Fe(NO 3 ) 3 ·9H 2 O respectively In water, heat and stir for 30 minutes until completely dissolved; add white citric acid monohydrate particles to the mixture of three nitrate solutions, heat and stir for 50 minutes to obtain a clear light yellow solution; add ethylene glycol to light yellow nitrate-lemon In the acid chelate solution, an esterification reaction occurs, and react at a temperature of 50°C for 40 minutes; adjust the temperature of the magnetic stirrer to 80°C, and age for 6 hours to obtain a viscous wet gel; put the wet gel at a temperature of 150°C Dry in an oven for 24 hours to obtain xerogel. After grinding, the xerogel powder is obtained and stored in a desiccator; the obtained xerogel powder is directly calcined in a high-temperature furnace at 1000°C for 3 hours to obtain tetraaluminoferrite calcium. The diffraction peaks of the X-ray diffraction spectrum of the obtained product match well with the tetracalcium aluminoferrite standard card, which proves that the product has a high purity.
实施例2，一种用溶胶-凝胶法合成铁铝酸四钙的方法，其原料的重量比为：Ca(NO3)2·4H2O 100、Al(NO3)3·9H2O 79.4、Fe(NO3)3·9H2O 85.6、一水合柠檬酸178.0、乙二醇160和水800。采用如下合成方法：在磁力搅拌机上，以55℃加热，将Ca(NO3)2·4H2O、Al(NO3)3·9H2O、Fe(NO3)3·9H2O分别加入水中，加热搅拌25min至完全溶解；将白色一水合柠檬酸颗粒加入到三种硝酸盐溶液的混合体中，加热搅拌45min得到清澈的淡黄色溶液；将乙二醇加入到淡黄色硝酸盐-柠檬酸螯合物溶液中，发生酯化反应， 在55℃温度下反应35min；将磁力搅拌机温度调节至83℃，陈化5h，得到粘性湿凝胶；把湿凝胶放在温度为150℃的烘箱中干燥24h，得到干凝胶，粉磨后得到干凝胶粉末并储存在干燥器中；将所得到的干凝胶粉末，直接放在1000℃高温炉中煅烧4h制得铁铝酸四钙。所得产物的X射线衍射谱图的衍射峰与铁铝酸四钙标准卡片匹配良好，证明产物纯度较高。 Example 2, a method for synthesizing tetracalcium aluminoferrite by sol-gel method, the weight ratio of raw materials is: Ca(NO 3 ) 2 ·4H 2 O 100, Al(NO 3 ) 3 ·9H 2 O 79.4, Fe(NO 3 ) 3 .9H 2 O 85.6, citric acid monohydrate 178.0, ethylene glycol 160 and water 800. The following synthesis method is adopted: on a magnetic stirrer, heating at 55°C, adding Ca(NO 3 ) 2 ·4H 2 O, Al(NO 3 ) 3 ·9H 2 O, Fe(NO 3 ) 3 ·9H 2 O respectively In water, heat and stir for 25 minutes until completely dissolved; add white monohydrate citric acid particles to the mixture of three nitrate solutions, heat and stir for 45 minutes to obtain a clear light yellow solution; add ethylene glycol to light yellow nitrate-lemon In the acid chelate solution, an esterification reaction occurs, react at a temperature of 55°C for 35min; adjust the temperature of the magnetic stirrer to 83°C, and age for 5h to obtain a viscous wet gel; place the wet gel at a temperature of 150°C Dry in an oven for 24 hours to obtain xerogel. After grinding, the xerogel powder is obtained and stored in a desiccator; the obtained xerogel powder is directly calcined in a high-temperature furnace at 1000°C for 4 hours to obtain tetraaluminoferrite calcium. The diffraction peaks of the X-ray diffraction spectrum of the obtained product match well with the tetracalcium aluminoferrite standard card, which proves that the product has a high purity.
实施例3，一种用溶胶-凝胶法合成铁铝酸四钙的方法，其原料的重量比为：Ca(NO3)2·4H2O 100、Al(NO3)3·9H2O 79.4、Fe(NO3)3·9H2O 85.6、一水合柠檬酸178.0、乙二醇210.2和水 1000。采用如下合成方法：在磁力搅拌机上，以60℃加热，将Ca(NO3)2·4H2O、Al(NO3)3·9H2O、Fe(NO3)3·9H2O分别加入水中，加热搅拌20min至完全溶解；将白色一水合柠檬酸颗粒加入到三种硝酸盐溶液的混合体中，加热搅拌40min得到清澈的淡黄色溶液；将乙二醇加入到淡黄色硝酸盐-柠檬酸螯合物溶液中，发生酯化反应， 在60℃温度下反应30min；将磁力搅拌机温度调节至85℃，陈化4h，得到粘性湿凝胶；把湿凝胶放在温度为150℃的烘箱中干燥24h，得到干凝胶，粉磨后得到干凝胶粉末并储存在干燥器中；将所得到的干凝胶粉末，直接放在1000℃高温炉中煅烧5h制得铁铝酸四钙。所得产物的X射线衍射谱图的衍射峰与铁铝酸四钙标准卡片匹配良好，证明产物纯度较高。 Example 3, a method for synthesizing tetracalcium aluminoferrite by sol-gel method, the weight ratio of the raw materials is: Ca(NO 3 ) 2 ·4H 2 O 100, Al(NO 3 ) 3 ·9H 2 O 79.4, Fe(NO 3 ) 3 ·9H 2 O 85.6, citric acid monohydrate 178.0, ethylene glycol 210.2 and water 1000. The following synthesis method is adopted: on a magnetic stirrer, heating at 60°C, adding Ca(NO 3 ) 2 ·4H 2 O, Al(NO 3 ) 3 ·9H 2 O, Fe(NO 3 ) 3 ·9H 2 O respectively In water, heat and stir for 20 minutes until completely dissolved; add white citric acid monohydrate particles to the mixture of three nitrate solutions, heat and stir for 40 minutes to obtain a clear light yellow solution; add ethylene glycol to light yellow nitrate-lemon In the acid chelate solution, an esterification reaction occurs, react at 60°C for 30 minutes; adjust the temperature of the magnetic stirrer to 85°C, and age for 4 hours to obtain a viscous wet gel; put the wet gel at a temperature of 150°C Dry in an oven for 24 hours to obtain xerogel. After grinding, the xerogel powder is obtained and stored in a desiccator; the obtained xerogel powder is directly calcined in a high-temperature furnace at 1000°C for 5 hours to obtain tetraaluminoferrite calcium. The diffraction peaks of the X-ray diffraction spectrum of the obtained product match well with the tetracalcium aluminoferrite standard card, which proves that the product has a high purity.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271427A (en) * | 2015-11-23 | 2016-01-27 | 武汉大学 | Method for fast preparing polycrystalline tetra calcium aluminoferrite |
| CN106220005A (en) * | 2016-07-26 | 2016-12-14 | 武汉大学 | A kind of method utilizing sol-gel technique to prepare ultra-dispersed high pure state nano cement |
| CN109748326A (en) * | 2019-03-22 | 2019-05-14 | 西南石油大学 | A process for preparing tetracalcium ferric aluminate by sol-gel method |
| CN110669212A (en) * | 2019-09-18 | 2020-01-10 | 西南石油大学 | Process for preparing metal-chelate retarder by using sol-gel method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1600872A (en) * | 2004-10-26 | 2005-03-30 | 上海彭浦冶金辅料有限公司 | Dephosphorising agent for converter and preparation method |
| CN101633520A (en) * | 2009-08-25 | 2010-01-27 | 陕西科技大学 | Method for preparing barium titanate nano-powder |
| CN101730668A (en) * | 2007-02-26 | 2010-06-09 | 纳米动力学公司 | Cement and methods of preparing cement |
| CN102153144A (en) * | 2010-02-11 | 2011-08-17 | 同济大学 | Method for preparing calcium ferroaluminates |
| CN102502817A (en) * | 2011-10-27 | 2012-06-20 | 沈阳化工大学 | A kind of method for preparing Gd2Zr2O7 nanopowder by sol-gel method |
-
2012
- 2012-09-24 CN CN201210356518XA patent/CN102897843A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1600872A (en) * | 2004-10-26 | 2005-03-30 | 上海彭浦冶金辅料有限公司 | Dephosphorising agent for converter and preparation method |
| CN101730668A (en) * | 2007-02-26 | 2010-06-09 | 纳米动力学公司 | Cement and methods of preparing cement |
| CN101633520A (en) * | 2009-08-25 | 2010-01-27 | 陕西科技大学 | Method for preparing barium titanate nano-powder |
| CN102153144A (en) * | 2010-02-11 | 2011-08-17 | 同济大学 | Method for preparing calcium ferroaluminates |
| CN102502817A (en) * | 2011-10-27 | 2012-06-20 | 沈阳化工大学 | A kind of method for preparing Gd2Zr2O7 nanopowder by sol-gel method |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271427A (en) * | 2015-11-23 | 2016-01-27 | 武汉大学 | Method for fast preparing polycrystalline tetra calcium aluminoferrite |
| CN105271427B (en) * | 2015-11-23 | 2017-01-18 | 武汉大学 | Method for fast preparing polycrystalline tetra calcium aluminoferrite |
| CN106220005A (en) * | 2016-07-26 | 2016-12-14 | 武汉大学 | A kind of method utilizing sol-gel technique to prepare ultra-dispersed high pure state nano cement |
| CN106220005B (en) * | 2016-07-26 | 2017-11-10 | 武汉大学 | A kind of method that ultra-dispersed high pure state nano cement is prepared using sol-gel technique |
| CN109748326A (en) * | 2019-03-22 | 2019-05-14 | 西南石油大学 | A process for preparing tetracalcium ferric aluminate by sol-gel method |
| CN110669212A (en) * | 2019-09-18 | 2020-01-10 | 西南石油大学 | Process for preparing metal-chelate retarder by using sol-gel method |
| CN110669212B (en) * | 2019-09-18 | 2020-09-29 | 西南石油大学 | Process for preparing metal-chelate type retarder by sol-gel method |
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