CN101880067A - Preparation method of bar-shaped NiTiO3 nano-crystalline - Google Patents
Preparation method of bar-shaped NiTiO3 nano-crystalline Download PDFInfo
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- CN101880067A CN101880067A CN 201010227795 CN201010227795A CN101880067A CN 101880067 A CN101880067 A CN 101880067A CN 201010227795 CN201010227795 CN 201010227795 CN 201010227795 A CN201010227795 A CN 201010227795A CN 101880067 A CN101880067 A CN 101880067A
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Abstract
The invention relates to a preparation method of bar-shaped NiTiO3 nano-crystalline, which comprises the following steps that: nickel nitrate hexahydrate is added into ethanol to obtain solution A; tetrabutyl titanate, oxalic acid and water are added into solution A to obtain solution B; after the solution B is arranged into a ultraviolet microwave instrument to be radiated for a given period of time, sediment is produced in the solution. The filtered sediment is arranged inside a drying box to be dried after being washed by acetone to obtain the final product - bar-shaped NiTiO3 nano-crystalline without any foreign matters. The prepared NiTiO3 nano-crystalline particles have small size, good dispersion, uniform distribution of particles, less agglomeration phenomenon and is free from containing any foreign matters; the prepared NiTiO3 nano-crystalline has short reaction period, good repeatability, simple preparation, convenient operation, easy obtaining of raw material and low preparation cost.
Description
Technical field
The present invention relates to a kind of NiTiO
3Preparation of nano crystal is specifically related to a kind of bar-shaped NiTiO
3The preparation method that nanocrystalline UV-light-microwave combines.
Background technology
NiTiO
3The trigonal system that belongs to ilmenite structure.At semiconductor rectifier, dehydrogenation of hydrocarbons adds in the industry such as sulfur catalysis and has a wide range of applications.In addition, NiTiO
3Can also be at the coating material that does not have to reduce as high temperature under the condition of liquid lubricant friction and loss.Because it is little that nano material has size, specific surface is big, and characteristics such as surface effects and quantum size effect, expection nanometer NiTiO
3Performance can be better than conventional NiTiO significantly
3Material, thereby cause that people study interest greatly.
Prepare NiTiO at present
3The report of nano-powder is less, main preparation method has solid sintering technology (F.Tietz, F.J.Dias, B.Dubiel, et al.Materials Science and Engineering.1999,68:35-41), chemical precipitation method (A.Vadivel Murugan, Violet Samuel, S.C.Navale, et al.Materials Letters, 2006,60:1791-1792) (Peng Zifei, Wang Guozhong, Zhang Lide. synthetic chemistry, 1996, (2): 99-101) (Zhou Lan, Liu Xiaojun, Zhang Shuyi, etc. Nanjing University's journal, 1997,33 (1): 32-36) etc., wherein solid sintering technology need just can make crystallization NiTiO completely usually under at least 1000 ℃ high temperature
3Powder, and the powder that adopts additive method low temperature to prepare down generally all contains impurity, prepares purified NiTiO under relatively low temperature
3The report of powder is less.Therefore, how to adopt rational operational path, prepare the product of high-purity nano level granularity, become the important topic in the research field.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, provide that a kind of not only preparation cost is low, simple to operate, reaction time is short, and can prepare bar-shaped NiTiO free from foreign meter at a lower temperature
3Preparation of nano crystal.
For achieving the above object, the present invention adopts technical scheme to be:
Step 1: analytically pure Nickelous nitrate hexahydrate is added in the dehydrated alcohol, and constantly stir, be mixed with Ni
2+Concentration is that the clear solution of 0.5mol/L～1mol/L is designated as A;
Step 2: in A solution, add analytically pure tetrabutyl titanate, make Ni
2+With Ti
4+Mol ratio be 1: 1, and constantly stir mixing solutions, and then in mixing solutions, add oxalic acid, make oxalic acid and all cationic mol ratios be (0.5～2): 1, the last water that adds dehydrated alcohol volume 4～8 again leaves standstill formation solution and is designated as B after stirring;
Step 3: with above-mentioned solution B be placed on shine 12h～72h in UV-light-microwave instrument after, solution has precipitation to produce, filtering-depositing and clean with acetone after put into loft drier, at 80 ℃～120 ℃ dry 8h～12h down, promptly obtain final product-bar-shaped NiTiO free from foreign meter
3Nanocrystalline.
The bar-shaped NiTiO that the present invention makes
3Nanocrystalline grain-size is less, good dispersion, and particle distribution is even, and agglomeration is less, and does not contain any impurity; Preparation NiTiO
3Nanocrystalline reaction time is short, and temperature is low, good reproducibility, and preparation is simple, and easy to operate, raw material is easy to get, and preparation cost is lower.
Description of drawings
Fig. 1 is the NiTiO of the present invention's preparation
3Nanocrystalline X-ray diffraction (XRD) collection of illustrative plates;
Fig. 2 is the bar-shaped NiTiO of the present invention's preparation
3Nanocrystalline scanning electron microscope (SEM) photo.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail.
Embodiment 1: analytically pure Nickelous nitrate hexahydrate is added in the dehydrated alcohol, and constantly stir, be mixed with Ni
2+Concentration is that the clear solution of 0.5mol/L is designated as A; In A solution, add analytically pure tetrabutyl titanate, make Ni
2+With Ti
4+Mol ratio be 1: 1, and constantly stir mixing solutions, and then in mixing solutions, add oxalic acid, making oxalic acid and all cationic mol ratios is 0.5: 1, adds the water of 4 times of dehydrated alcohol volumes at last again, leaves standstill after stirring to form solution and be designated as B; After above-mentioned solution B was placed in UV-light-microwave instrument irradiation 25h, solution had precipitation to produce, filtering-depositing and clean with acetone after put into loft drier, at 80 ℃ of dry 12h down, promptly obtain final product-bar-shaped NiTiO free from foreign meter
3Nanocrystalline.
NiTiO with gained
3The Japanese D/max2000PC x-ray diffractometer analytic sample of science of nanocrystalline usefulness finds that product is the NiTiO that JCPDS is numbered 33-0960
3(Fig. 1).This sample is observed with the JSM-6390A type scanning electronic microscope (Fig. 2) that Japanese JEOL company produces, from the prepared as can be seen NiTiO of photo
3Nanocrystalline is rod-shpaed particle.
Embodiment 2: analytically pure Nickelous nitrate hexahydrate is added in the dehydrated alcohol, and constantly stir, be mixed with Ni
2+Concentration is that the clear solution of 0.6mol/L is designated as A; In A solution, add analytically pure tetrabutyl titanate, make Ni
2+With Ti
4+Mol ratio be 1: 1, and constantly stir mixing solutions, and then in mixing solutions, add oxalic acid, making oxalic acid and all cationic mol ratios is 1: 1, adds the water of 4 times of dehydrated alcohol volumes at last again, leaves standstill after stirring to form solution and be designated as B; After above-mentioned solution B was placed in UV-light-microwave instrument irradiation 12h, solution had precipitation to produce, filtering-depositing and clean with acetone after put into loft drier, at 100 ℃ of dry 10h down, promptly obtain final product-bar-shaped NiTiO free from foreign meter
3Nanocrystalline.
Embodiment 3: analytically pure Nickelous nitrate hexahydrate is added in the dehydrated alcohol, and constantly stir, be mixed with Ni
2+Concentration is that the clear solution of 0.8mol/L is designated as A; In A solution, add analytically pure tetrabutyl titanate, make Ni
2+With Ti
4+Mol ratio be 1: 1, and constantly stir mixing solutions, and then in mixing solutions, add oxalic acid, making oxalic acid and all cationic mol ratios is 1.5: 1, adds the water of 6 times of dehydrated alcohol volumes at last again, leaves standstill after stirring to form solution and be designated as B; After above-mentioned solution B was placed in UV-light-microwave instrument irradiation 36h, solution had precipitation to produce, filtering-depositing and clean with acetone after put into loft drier, at 90 ℃ of dry 11h down, promptly obtain final product-bar-shaped NiTiO free from foreign meter
3Nanocrystalline.
Embodiment 4: analytically pure Nickelous nitrate hexahydrate is added in the dehydrated alcohol, and constantly stir, be mixed with Ni
2+Concentration is that the clear solution of 1mol/L is designated as A; In A solution, add analytically pure tetrabutyl titanate, make Ni
2+With Ti
4+Mol ratio be 1: 1, and constantly stir mixing solutions, and then in mixing solutions, add oxalic acid, making oxalic acid and all cationic mol ratios is 0.9: 1, adds the water of 5 times of dehydrated alcohol volumes at last again, leaves standstill after stirring to form solution and be designated as B; After above-mentioned solution B was placed in UV-light-microwave instrument irradiation 72h, solution had precipitation to produce, filtering-depositing and clean with acetone after put into loft drier, at 120 ℃ of dry 8h down, promptly obtain final product-bar-shaped NiTiO free from foreign meter
3Nanocrystalline.
Embodiment 5: analytically pure Nickelous nitrate hexahydrate is added in the dehydrated alcohol, and constantly stir, be mixed with Ni
2+Concentration is that the clear solution of 0.7mol/L is designated as A; In A solution, add analytically pure tetrabutyl titanate, make Ni
2+With Ti
4+Mol ratio be 1: 1, and constantly stir mixing solutions, and then in mixing solutions, add oxalic acid, making oxalic acid and all cationic mol ratios is 2: 1, adds the water of 8 times of dehydrated alcohol volumes at last again, leaves standstill after stirring to form solution and be designated as B; After above-mentioned solution B was placed in UV-light-microwave instrument irradiation 60h, solution had precipitation to produce, filtering-depositing and clean with acetone after put into loft drier, at 110 ℃ of dry 9h down, promptly obtain final product-bar-shaped NiTiO free from foreign meter
3Nanocrystalline.
Claims (1)
1. bar-shaped NiTiO
3Preparation of nano crystal is characterized in that:
Step 1: analytically pure Nickelous nitrate hexahydrate is added in the dehydrated alcohol, and constantly stir, be mixed with Ni
2+Concentration is that the clear solution of 0.5mol/L～1mol/L is designated as A;
Step 2: in A solution, add analytically pure tetrabutyl titanate, make Ni
2+With Ti
4+Mol ratio be 1: 1, and constantly stir mixing solutions, and then in mixing solutions, add oxalic acid, make oxalic acid and all cationic mol ratios be (0.5～2): 1, the last water that adds dehydrated alcohol volume 4～8 again leaves standstill formation solution and is designated as B after stirring;
Step 3: with above-mentioned solution B be placed on shine 12h～72h in the UV-light one microwave instrument after, solution has precipitation to produce, filtering-depositing and clean with acetone after put into loft drier, at 80 ℃～120 ℃ dry 8h～12h down, promptly obtain final product one bar-shaped NiTiO free from foreign meter
3Nanocrystalline.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2457182C1 (en) * | 2011-01-31 | 2012-07-27 | Государственное образовательное учреждение высшего профессионального образования "Челябинский государственный педагогический университет" | Method of producing nanodispersed nickel titanate |
| CN105032464A (en) * | 2015-07-16 | 2015-11-11 | 湖南大学 | Carbon nitride-nickel titanate composite material and preparation method and application thereof |
| CN105731552A (en) * | 2016-02-01 | 2016-07-06 | 浙江大学 | Talc-titanic acid nickel nanocomposite and preparing method thereof |
| CN106410117A (en) * | 2016-11-04 | 2017-02-15 | 中南大学 | Rod-like NiTiO3 negative electrode material used for sodium ion battery as well as preparation and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03275524A (en) * | 1990-02-15 | 1991-12-06 | Showa Denko Kk | Production of nitio3 |
| CN101767997A (en) * | 2009-10-30 | 2010-07-07 | 陕西科技大学 | Method for preparing NiTiO3 nano-powder by sol-gel |
-
2010
- 2010-07-15 CN CN2010102277951A patent/CN101880067B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03275524A (en) * | 1990-02-15 | 1991-12-06 | Showa Denko Kk | Production of nitio3 |
| CN101767997A (en) * | 2009-10-30 | 2010-07-07 | 陕西科技大学 | Method for preparing NiTiO3 nano-powder by sol-gel |
Non-Patent Citations (2)
| Title |
|---|
| 《Journal of Alloys and Compounds》 20080103 K.P. Lopes et al. NiTiO3 powders obtained by polymeric precursor method: Synthesis and characterization 327-332 1 第468卷, 2 * |
| 《精细化工》 20051031 冯建等 NiTiO3纳米棒的制备及表征 744-747 1 第22卷, 第10期 2 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2457182C1 (en) * | 2011-01-31 | 2012-07-27 | Государственное образовательное учреждение высшего профессионального образования "Челябинский государственный педагогический университет" | Method of producing nanodispersed nickel titanate |
| CN105032464A (en) * | 2015-07-16 | 2015-11-11 | 湖南大学 | Carbon nitride-nickel titanate composite material and preparation method and application thereof |
| CN105731552A (en) * | 2016-02-01 | 2016-07-06 | 浙江大学 | Talc-titanic acid nickel nanocomposite and preparing method thereof |
| CN106410117A (en) * | 2016-11-04 | 2017-02-15 | 中南大学 | Rod-like NiTiO3 negative electrode material used for sodium ion battery as well as preparation and application |
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| CN101880067B (en) | 2011-12-28 |
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