CN102115161B - Alkaline-earth metal titanate nano powder and preparation method thereof - Google Patents
Alkaline-earth metal titanate nano powder and preparation method thereof Download PDFInfo
- Publication number
- CN102115161B CN102115161B CN201110076579A CN201110076579A CN102115161B CN 102115161 B CN102115161 B CN 102115161B CN 201110076579 A CN201110076579 A CN 201110076579A CN 201110076579 A CN201110076579 A CN 201110076579A CN 102115161 B CN102115161 B CN 102115161B
- Authority
- CN
- China
- Prior art keywords
- earth metal
- alkaline earth
- amorphous glass
- preparation
- metal titanate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 229910052784 alkaline earth metal Inorganic materials 0.000 title claims abstract description 34
- 239000011858 nanopowder Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- -1 Alkaline-earth metal titanate Chemical class 0.000 title abstract description 30
- 239000002245 particle Substances 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 26
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011521 glass Substances 0.000 claims abstract description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910021538 borax Inorganic materials 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 6
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 6
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 5
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims 1
- 238000009826 distribution Methods 0.000 abstract description 11
- 230000015572 biosynthetic process Effects 0.000 abstract description 10
- 238000010438 heat treatment Methods 0.000 abstract description 10
- 239000000203 mixture Substances 0.000 abstract description 10
- 238000003786 synthesis reaction Methods 0.000 abstract description 10
- 239000004408 titanium dioxide Substances 0.000 abstract description 5
- 238000010791 quenching Methods 0.000 abstract description 4
- 239000000843 powder Substances 0.000 description 26
- 239000002994 raw material Substances 0.000 description 10
- 239000000047 product Substances 0.000 description 8
- 238000005406 washing Methods 0.000 description 7
- 239000002351 wastewater Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 238000003746 solid phase reaction Methods 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 150000004703 alkoxides Chemical class 0.000 description 2
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 2
- 229910001863 barium hydroxide Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005285 chemical preparation method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明涉及一种碱土金属钛酸盐纳米粉体及其制备方法。其技术方案是：先将7～30wt％的二氧化钛、50～70wt％的硼砂和10～30wt％的碱土金属氢氧化物混合均匀，以5～15℃/分的升温速率加热至1000～1200℃，保温1～3小时，得到均匀熔体；再将均匀熔体采用对辊冷却法冷却，获得非晶态玻璃鳞片，或再将均匀熔体进行水淬，获得非晶态玻璃颗粒；然后将非晶态玻璃鳞片或非晶态玻璃颗粒在630～680℃条件下保温1～5小时，先后用10％的稀醋酸和去离子水进行洗涤，干燥，即得碱土金属钛酸盐纳米粉体。本发明具有成本低、合成工艺简单、合成过程易于控制的特点，所制备的碱土金属钛酸盐纳米粉体纯度高，粒度分布均匀。The invention relates to an alkaline earth metal titanate nanopowder and a preparation method thereof. The technical solution is: first mix 7-30wt% of titanium dioxide, 50-70wt% of borax and 10-30wt% of alkaline earth metal hydroxide, and heat it to 1000-1200°C at a heating rate of 5-15°C/min. , keep warm for 1 to 3 hours to obtain a uniform melt; then cool the uniform melt by roller cooling method to obtain amorphous glass flakes, or water quench the uniform melt to obtain amorphous glass particles; then Amorphous glass flakes or amorphous glass particles are kept at 630-680°C for 1-5 hours, washed with 10% dilute acetic acid and deionized water, and dried to obtain alkaline earth metal titanate nanopowder . The invention has the characteristics of low cost, simple synthesis process and easy control of the synthesis process, and the prepared alkaline earth metal titanate nanopowder has high purity and uniform particle size distribution.
Description
技术领域 technical field
本发明属于碱土金属钛酸盐粉体技术领域。具体涉及一种碱土金属钛酸盐纳米粉体及其制备方法。The invention belongs to the technical field of alkaline earth metal titanate powder. It specifically relates to an alkaline earth metal titanate nanopowder and a preparation method thereof.
背景技术 Background technique
碱土金属钛酸盐产品凭借优异的物理、光学和化学等性能，在电子陶瓷领域占据重要位置。电子陶瓷材料的优良性能要通过其特殊的化学组成和微观结构来实现，粉体制备是第一步，其品质直接影响陶瓷材料的组成、结构与性能。随着微电子技术的发展，电子元器件的小型、轻量和薄型化成为趋势，对钛酸盐纳米粉体提出了越来越高的要求。如颗粒细、纯度高、尺寸分布均匀、无团聚等。因此，高纯、超细、化学均匀和成分可控及烧结活性大的碱土金属钛酸盐纳米粉体制备技术一直是国内外学者研究的重点和热点。Alkaline earth metal titanate products occupy an important position in the field of electronic ceramics due to their excellent physical, optical and chemical properties. The excellent performance of electronic ceramic materials is realized through its special chemical composition and microstructure. Powder preparation is the first step, and its quality directly affects the composition, structure and performance of ceramic materials. With the development of microelectronics technology, the miniaturization, light weight and thinning of electronic components has become a trend, and higher and higher requirements are put forward for titanate nanopowders. Such as fine particles, high purity, uniform size distribution, no agglomeration, etc. Therefore, the preparation technology of alkaline earth metal titanate nanopowders with high purity, ultrafine, chemical uniformity, controllable composition and high sintering activity has been the focus and hotspot of domestic and foreign scholars.
迄今为止，人们提出了许多制备碱土金属钛酸盐纳米粉体的方法，但这些方法都不同程度地存在着一些不足。传统的制备方法是固相反应法，即将原料混合、研磨后进行高温煅烧，使其发生固相反应，然后再磨细得到一定颗粒尺度的粉体。固相反应法所用设备简单、操作方便、易于实现工业化生产，但在研磨过程中易引入杂质、造成材料纯度下降，而且得到的粉体颗粒尺寸分布范围宽、难以控制产品的均匀性，另外，粉体的结晶性和烧结性等方面也存在一定的不足。So far, many methods for preparing alkaline earth metal titanate nanopowders have been proposed, but these methods have some shortcomings to varying degrees. The traditional preparation method is the solid phase reaction method, that is, the raw materials are mixed and ground, then calcined at a high temperature to cause a solid phase reaction, and then ground to obtain a powder with a certain particle size. The equipment used in the solid phase reaction method is simple, easy to operate, and easy to realize industrial production, but it is easy to introduce impurities during the grinding process, resulting in a decrease in material purity, and the obtained powder particle size distribution range is wide, and it is difficult to control the uniformity of the product. In addition, There are also certain deficiencies in the crystallinity and sinterability of the powder.
针对固相法存在的缺点，人们发展了一系列湿化学制备方法。如沉淀法、溶胶-凝胶法、水热法等，所制备的碱土金属钛酸盐纳米粉体具有纯度高、活性大等特点，采用这些粉体作为原料有可能使陶瓷材料具有优异的性能。但是，这些合成方法也存在一些问题。沉淀法是利用适当的沉淀剂使混合的金属盐溶液反应生成组成均匀的沉淀，热分解得到高纯粉体材料。该法反应条件温和、前驱体煅烧温度低，但在制备过程中操作条件的微小变化和体系局部pH值得改变，往往对产物的理化性能产生较大影响，并易引入杂质，因此，其反应过程要求非常严格。溶胶-凝胶法一般采用碱土金属醇盐作为原料，按反应化学计量比溶解在醇中，或用碱土金属无机盐与含钛醇盐为原料，在一定条件下形成溶胶，陈化、烘干的凝胶前驱体经过热处理就得到了碱土金属钛酸盐粉体。该法制得的粉体具有纯度高、分散性好、粒度小等优点。但醇盐成本很高，容易吸潮水解，并且存在热处理易导致粉体团聚、工艺条件不易控制等缺点。水热法则需借助高压釜，在一定温度和压力下合成粉体。该法的最大优点是，能够在较低的温度下，直接从溶液中获得晶粒发育完整的粉末，粉体的纯度高、化学成分均匀、粒径小、粒子尺寸分布好。但是，水热法有时需要采用与溶胶-凝胶法相同的价格较高的前驱体，在制备过程中需要较高的压力，设备要求严格，并且需要非常精确地控制反应体系的pH值，否则容易出现其他杂相。最近发展起来的微波加热法、超声分散法、溶剂热法、喷热分解法等，仍处于实验室探索阶段。Aiming at the shortcomings of the solid phase method, a series of wet chemical preparation methods have been developed. Such as precipitation method, sol-gel method, hydrothermal method, etc., the prepared alkaline earth metal titanate nanopowder has the characteristics of high purity and high activity. Using these powders as raw materials may make ceramic materials have excellent properties. . However, these synthetic methods also have some problems. The precipitation method is to use an appropriate precipitant to react the mixed metal salt solution to form a uniform precipitate, and thermally decompose it to obtain a high-purity powder material. The reaction conditions of this method are mild and the calcination temperature of the precursor is low, but the small changes in the operating conditions and the local pH value of the system during the preparation process often have a greater impact on the physical and chemical properties of the product and are easy to introduce impurities. Therefore, the reaction process The requirements are very strict. The sol-gel method generally uses alkaline earth metal alkoxides as raw materials, which are dissolved in alcohol according to the reaction stoichiometric ratio, or alkaline earth metal inorganic salts and titanium-containing alkoxides are used as raw materials to form sols under certain conditions, aged and dried Alkaline earth metal titanate powder is obtained by heat treatment of the gel precursor. The powder prepared by this method has the advantages of high purity, good dispersibility and small particle size. However, the cost of alkoxide is high, it is easy to absorb moisture and hydrolyze, and there are disadvantages such as heat treatment can easily lead to powder agglomeration, and the process conditions are not easy to control. The hydrothermal method needs the help of an autoclave to synthesize powder under a certain temperature and pressure. The biggest advantage of this method is that it can directly obtain powder with fully developed crystal grains from the solution at a lower temperature. The powder has high purity, uniform chemical composition, small particle size, and good particle size distribution. However, the hydrothermal method sometimes needs to use the same higher-priced precursor as the sol-gel method, requires higher pressure in the preparation process, requires strict equipment, and needs to control the pH value of the reaction system very accurately, otherwise Other miscellaneous phases are prone to appear. The recently developed microwave heating method, ultrasonic dispersion method, solvothermal method, spray thermal decomposition method, etc. are still in the stage of laboratory exploration.
综上所述，目前针对碱土金属钛酸盐纳米粉体所采用的制备方法，存在前驱体价格昂贵、合成工艺复杂、合成过程不易控制、易引入杂相等缺陷。In summary, the current preparation methods for alkaline earth metal titanate nanopowders have defects such as expensive precursors, complex synthesis processes, difficult control of the synthesis process, and easy introduction of impurities.
发明内容 Contents of the invention
本发明旨在克服现有技术存在的不足，目的是提供一种成本低、合成工艺简单、合成过程易于控制的碱土金属钛酸盐纳米粉体的制备方法。The invention aims to overcome the shortcomings of the prior art, and aims to provide a preparation method of alkaline earth metal titanate nanopowder with low cost, simple synthesis process and easy control of the synthesis process.
为实现上述目的，本发明的技术方案是：先将7～30wt％的二氧化钛、50～70wt％的硼砂(Na2B4O7·10H2O)和10～30wt％的碱土金属氢氧化物混合均匀，以5～15℃/分的升温速率加热至1000～1200℃，保温1～3小时，得到均匀熔体；再将均匀熔体采用对辊冷却法冷却，获得非晶态玻璃鳞片，或再将均匀熔体进行水淬，获得非晶态玻璃颗粒；然后将非晶态玻璃鳞片或非晶态玻璃颗粒在630～680℃条件下保温1～5小时，先后用10％的稀醋酸和去离子水进行洗涤，干燥，即得碱土金属钛酸盐纳米粉体。In order to achieve the above object, the technical scheme of the present invention is: first mix 7～30wt% titanium dioxide, 50～70wt% borax (Na 2 B 4 O 7 10H 2 O) and 10～30wt% alkaline earth metal hydroxide Mix evenly, heat to 1000-1200°C at a heating rate of 5-15°C/min, and keep warm for 1-3 hours to obtain a uniform melt; then cool the uniform melt by roller cooling to obtain amorphous glass flakes, Or quench the homogeneous melt with water to obtain amorphous glass particles; then keep the amorphous glass flakes or amorphous glass particles at 630-680°C for 1-5 hours, and then wash them with 10% dilute acetic acid washing with deionized water and drying to obtain alkaline earth metal titanate nanopowder.
在上述技术方案中：洗涤过程所产生的废水经蒸馏后，所得粉末按化学计量作为原料再次使用；碱土金属氢氧化物为氢氧化钙、或为氢氧化镁、或为氢氧化钡；In the above technical scheme: after the waste water produced in the washing process is distilled, the obtained powder is reused as a raw material according to stoichiometry; the alkaline earth metal hydroxide is calcium hydroxide, or magnesium hydroxide, or barium hydroxide;
由于采用上述技术方案，本发明所提供的碱土金属钛酸盐纳米粉体及其制备方法，具有以下突出特点：Due to the adoption of the above technical scheme, the alkaline earth metal titanate nanopowder and its preparation method provided by the present invention have the following prominent features:
1、制备工艺简单，不需要昂贵的设备；1. The preparation process is simple and does not require expensive equipment;
2、原料易得；2. Raw materials are easy to get;
3、制备过程易于控制，晶型、晶粒形貌和粒径等参数可以通过改变热处理制度进行调节；3. The preparation process is easy to control, and parameters such as crystal form, grain morphology and particle size can be adjusted by changing the heat treatment system;
4、粉体产物纯度高，粒度分布均匀，制得的碱土金属钛酸盐纳米粉体的颗粒直径为40～80nm；4. The powder product has high purity and uniform particle size distribution. The particle diameter of the prepared alkaline earth metal titanate nanopowder is 40-80nm;
5、有利于环境保护，粉体洗涤过程中产生的废水可循环用于粉体制备。5. It is conducive to environmental protection, and the waste water generated during the powder washing process can be recycled for powder preparation.
因此。本发明具有成本低、合成工艺简单、合成过程易于控制的特点，所制备的碱土金属钛酸盐纳米粉体纯度高，粒度分布均匀。therefore. The invention has the characteristics of low cost, simple synthesis process and easy control of the synthesis process, and the prepared alkaline earth metal titanate nanopowder has high purity and uniform particle size distribution.
具体实施方式 Detailed ways
下面结合具体实施方式对本发明做进一步的描述，并非对其保护范围的限制。The present invention will be further described below in combination with specific embodiments, which are not intended to limit the protection scope thereof.
实施例1Example 1
一种碱土金属钛酸盐纳米粉体及其制备方法。先将7～12wt％的二氧化钛、60～70wt％的硼砂(Na2B4O7·10H2O)和20～30wt％的氢氧化钡混合均匀，以5～10℃/分的升温速率加热至1000～1100℃，保温1～2小时，得到均匀熔体；再将均匀熔体采用对辊冷却法冷却，获得非晶态玻璃鳞片；然后将非晶态玻璃鳞片在650～680℃条件下保温1～2.5小时，先后用10％的稀醋酸和去离子水进行洗涤，干燥，即得碱土金属钛酸盐纳米粉体。An alkaline earth metal titanate nanopowder and a preparation method thereof. First mix 7-12wt% titanium dioxide, 60-70wt% borax (Na 2 B 4 O 7 10H 2 O) and 20-30wt% barium hydroxide, and heat at a heating rate of 5-10°C/min. to 1000-1100°C, keep it warm for 1-2 hours to obtain a uniform melt; then cool the uniform melt by the roller cooling method to obtain amorphous glass flakes; then place the amorphous glass flakes under the condition of 650-680°C heat preservation for 1-2.5 hours, wash with 10% dilute acetic acid and deionized water successively, and dry to obtain alkaline earth metal titanate nanopowder.
本实施例的洗涤过程所产生的废水经蒸馏后，所得粉末按化学计量作为原料再次使用。After the waste water produced in the washing process of this embodiment is distilled, the obtained powder is stoichiometrically used as a raw material again.
本实施例所制得的碱土金属钛酸盐纳米粉体的颗粒直径为40～60nm，该粉体产物纯度高和粒度分布均匀。The particle diameter of the alkaline earth metal titanate nanopowder prepared in this example is 40-60 nm, and the powder product has high purity and uniform particle size distribution.
实施例2Example 2
一种碱土金属钛酸盐纳米粉体及其制备方法。先将20～30wt％的二氧化钛、50～60wt％的硼砂(Na2B4O7·10H2O)和10～20wt％的氢氧化钙混合均匀，以8～15℃/分的升温速率加热至1100～1200℃，保温2～3小时，得到均匀熔体；再将均匀熔体进行水淬，获得非晶态玻璃颗粒；然后将非晶态玻璃颗粒在630～660℃条件下保温3～5小时，先后用10％的稀醋酸和去离子水进行洗涤，干燥，即得碱土金属钛酸盐纳米粉体。An alkaline earth metal titanate nanopowder and a preparation method thereof. First mix 20-30wt% titanium dioxide, 50-60wt% borax (Na 2 B 4 O 7 10H 2 O) and 10-20wt% calcium hydroxide, and heat at a heating rate of 8-15°C/min. Heat at 1100-1200°C for 2-3 hours to obtain a uniform melt; then quench the uniform melt with water to obtain amorphous glass particles; then keep the amorphous glass particles at 630-660°C for 3-3 After 5 hours, wash with 10% dilute acetic acid and deionized water successively, and dry to obtain alkaline earth metal titanate nanopowder.
本实施例的洗涤过程所产生的废水经蒸馏后，所得粉末按化学计量作为原料再次使用；After the waste water produced in the washing process of this embodiment is distilled, the obtained powder is used again as a raw material according to the stoichiometric ratio;
本实施例所制得的碱土金属钛酸盐纳米粉体的颗粒直径为50～80nm，该粉体产物纯度高和粒度分布均匀。The particle diameter of the alkaline earth metal titanate nanopowder prepared in this embodiment is 50-80nm, and the powder product has high purity and uniform particle size distribution.
实施例3Example 3
一种碱土金属钛酸盐纳米粉体及其制备方法。先将10～20wt％的二氧化钛、60～65wt％的硼砂(Na2B4O7·10H2O)和18～25wt％的氢氧化镁混合均匀，以10～15℃/分的升温速率加热至1100～1200℃，保温2～3小时，得到均匀熔体；再将均匀熔体进行水淬，获得非晶态玻璃颗粒；然后将非晶态玻璃颗粒在650～670℃条件下保温2～3小时，先后用10％的稀醋酸和去离子水进行洗涤，干燥，即得碱土金属钛酸盐纳米粉体。An alkaline earth metal titanate nanopowder and a preparation method thereof. First mix 10-20wt% titanium dioxide, 60-65wt% borax (Na 2 B 4 O 7 10H 2 O) and 18-25wt% magnesium hydroxide, and heat at a heating rate of 10-15°C/min. Heat at 1100-1200°C for 2-3 hours to obtain a uniform melt; then quench the uniform melt with water to obtain amorphous glass particles; then keep the amorphous glass particles at 650-670°C for 2-3 hours After 3 hours, wash with 10% dilute acetic acid and deionized water successively, and dry to obtain alkaline earth metal titanate nanopowder.
的洗涤过程所产生的废水经蒸馏后，所得粉末按化学计量作为原料再次使用。After the waste water produced by the washing process is distilled, the obtained powder is stoichiometrically used as a raw material again.
本实施例所制得的碱土金属钛酸盐纳米粉体的颗粒直径为40～60nm，该粉体产物纯度高和粒度分布均匀。The particle diameter of the alkaline earth metal titanate nanopowder prepared in this example is 40-60 nm, and the powder product has high purity and uniform particle size distribution.
本具体实施方式所提供的碱土金属钛酸盐纳米粉体及其制备方法，具有以下突出特点：The alkaline earth metal titanate nanopowder and its preparation method provided in this specific embodiment have the following prominent features:
1、制备工艺简单，不需要昂贵的设备；1. The preparation process is simple and does not require expensive equipment;
2、原料易得；2. Raw materials are easy to get;
3、制备过程易于控制，晶型、晶粒形貌和粒径等参数可以通过改变热处理制度进行调节；3. The preparation process is easy to control, and parameters such as crystal form, grain morphology and particle size can be adjusted by changing the heat treatment system;
4、粉体产物纯度高，粒度分布均匀，制得的碱土金属钛酸盐纳米粉体的颗粒直径为40～80nm；4. The powder product has high purity and uniform particle size distribution. The particle diameter of the prepared alkaline earth metal titanate nanopowder is 40-80nm;
5、有利于环境保护，粉体洗涤过程中产生的废水可循环用于粉体制备。5. It is conducive to environmental protection, and the waste water generated during the powder washing process can be recycled for powder preparation.
因此。本发明具有成本低、合成工艺简单、合成过程易于控制的特点，所制备的碱土金属钛酸盐纳米粉体纯度高，粒度分布均匀。therefore. The invention has the characteristics of low cost, simple synthesis process and easy control of the synthesis process, and the prepared alkaline earth metal titanate nanopowder has high purity and uniform particle size distribution.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110076579A CN102115161B (en) | 2011-03-28 | 2011-03-28 | Alkaline-earth metal titanate nano powder and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110076579A CN102115161B (en) | 2011-03-28 | 2011-03-28 | Alkaline-earth metal titanate nano powder and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102115161A CN102115161A (en) | 2011-07-06 |
| CN102115161B true CN102115161B (en) | 2012-10-03 |
Family
ID=44214104
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110076579A Expired - Fee Related CN102115161B (en) | 2011-03-28 | 2011-03-28 | Alkaline-earth metal titanate nano powder and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102115161B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857430A (en) * | 2010-06-23 | 2010-10-13 | 湖南博深实业有限公司 | Method for synthesizing titanate series electronic ceramic nano-crystalline materials |
| CN101921107A (en) * | 2010-07-21 | 2010-12-22 | 山东国瓷功能材料股份有限公司 | Process for preparing tetragonal barium titanate powder |
-
2011
- 2011-03-28 CN CN201110076579A patent/CN102115161B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857430A (en) * | 2010-06-23 | 2010-10-13 | 湖南博深实业有限公司 | Method for synthesizing titanate series electronic ceramic nano-crystalline materials |
| CN101921107A (en) * | 2010-07-21 | 2010-12-22 | 山东国瓷功能材料股份有限公司 | Process for preparing tetragonal barium titanate powder |
Non-Patent Citations (3)
| Title |
|---|
| E. CIFTCI et al..Hydrothermal precipitation and characterization of nanocrystalline BaTiO3 particles.《JOURNAL OF MATERIALS SCIENCE》.2001,第36卷第4875–4882页. * |
| 王加芳 等.纳米钛酸镁陶瓷粉体的制备研究进展.《硅酸盐通报》.2007,第26卷(第3期),第514-518、546页. * |
| 颜学敏 等.电子陶瓷钛酸钡粉体的液相合成.《化学通报》.2005,第68卷第1-7页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102115161A (en) | 2011-07-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104891542B (en) | A kind of preparation method of superfine α-Al2O3 powder | |
| CN100408480C (en) | A kind of preparation method of nano zinc oxide powder | |
| CN107151029A (en) | A kind of sol gel synthesis preparation technology of tetra phase barium titanate powder | |
| CN105000567B (en) | A kind of preparation method of high-dispersion nano silicon dioxide | |
| CN104016408B (en) | A kind of synthetic method of sodium niobate nano line | |
| CN103523824A (en) | Preparation method of nano flaky ferroelectric material for photocatalysis | |
| CN109399711A (en) | A kind of preparation method of rutile phase hypovanadic oxide nano-powder | |
| KR102590443B1 (en) | Nano barium titanate microcrystals and method for producing the same and barium titanate powder and method for producing the same | |
| CN115124072A (en) | Method for preparing high-purity nano titanium dioxide by sulfuric acid process and product | |
| CN105016382B (en) | Method for preparing pure gold redstone type titanium dioxide nanorod | |
| CN105461311A (en) | Method for preparing NaNbO3 powder by Sol-gel method and obtaining single crystal by sintering | |
| CN106801256A (en) | A kind of method that solid phase method prepares potassium hexatitanate platelet | |
| CN106044829B (en) | A kind of preparation method of white pure zirconia cerium | |
| CN101654280A (en) | Preparation method of titanium dioxide nano powder | |
| CN103882558B (en) | A kind of perovskite structure AgNbO 3fiber and preparation method thereof | |
| CN102115161B (en) | Alkaline-earth metal titanate nano powder and preparation method thereof | |
| CN101239738A (en) | A kind of preparation method of titanium dioxide nanotube | |
| CN103991897A (en) | Parallelepiped zinc oxide aggregate and preparation method thereof | |
| CN100372759C (en) | Preparation method of mesoporous metal oxide | |
| CN102887705B (en) | A kind of preparation method of tetragonal barium titanate BaTiO3 hollow nanocrystal | |
| CN102963925A (en) | Method for preparing nanometer n-zinc titanate spinel by virtue of taking zinc-titanium hydrotalcite as precursor | |
| CN101913619A (en) | A kind of preparation method of barium metaborate nanopowder | |
| CN103449512B (en) | Method for preparing monodisperse and cuboid nano-barium titanate powder by virtue of microwave hydrothermal method | |
| CN105540651B (en) | A method for preparing spherical tin oxide nanomaterials | |
| CN107792885A (en) | Orthogonal mangaic acid yttrium powder body of high infrared reflection rate based on molten-salt growth method and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20121003 Termination date: 20150328 |
|
| EXPY | Termination of patent right or utility model |