CN103833076A - Nickel oxide-titanium dioxide nano composite material - Google Patents
Nickel oxide-titanium dioxide nano composite material Download PDFInfo
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- CN103833076A CN103833076A CN201210490366.2A CN201210490366A CN103833076A CN 103833076 A CN103833076 A CN 103833076A CN 201210490366 A CN201210490366 A CN 201210490366A CN 103833076 A CN103833076 A CN 103833076A
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- 239000000463 material Substances 0.000 title claims abstract description 48
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 14
- OKJMWOSMAIIUAG-UHFFFAOYSA-N oxonickel oxygen(2-) titanium(4+) Chemical compound [O-2].[O-2].[Ti+4].[Ni]=O OKJMWOSMAIIUAG-UHFFFAOYSA-N 0.000 title abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000967 suction filtration Methods 0.000 claims abstract description 14
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001868 water Inorganic materials 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004202 carbamide Substances 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 238000005554 pickling Methods 0.000 claims abstract description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 23
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 18
- 239000002127 nanobelt Substances 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000007810 chemical reaction solvent Substances 0.000 abstract description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 239000008204 material by function Substances 0.000 abstract 1
- 231100000956 nontoxicity Toxicity 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 abstract 1
- 238000007146 photocatalysis Methods 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 239000006250 one-dimensional material Substances 0.000 description 10
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 10
- 239000002086 nanomaterial Substances 0.000 description 6
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000011534 incubation Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000000593 microemulsion method Methods 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- -1 nanometer rod Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
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Abstract
The invention provides a nickel oxide-titanium dioxide nano composite material, belonging to the technical field of inorganic functional materials. The nano composite material is prepared by preparing a strip-shaped Na2Ti8O17 precursor from TiO2 serving as a basic raw material and a NaOH solution serving as a reaction solvent by using a hydrothermal method, then soaking, pickling and performing suction filtration to obtain strip-shaped H2Ti8O17, and putting the strip-shaped H2Ti8O17 into a muffle furnace for calcining for 2 hours so as to obtain a TiO2 nano strip; by taking urea, nickel nitrate, water and TiO2 as raw materials, keeping the temperature of 120 DEG C for 4-6 hours by using a homogeneous precipitation method, and then calcining for 2 hours at 400 DEG C so as to obtain a novel nickel oxide-titanium dioxide one-dimensional nano composite material which has the advantages of no toxicity, low cost, no pollution, high specific capacity, good security, good catalytic performance and the like, and has wide application prospects in fields such as lithium ion batteries, photocatalysis and the like.
Description
Technical field
The present invention relates to a kind of nickel oxide-titanic oxide nano compound material, belong to inorganic functional material field.
Background technology
Monodimension nanometer material refers in three dimensions of material have the size of two dimensions to drop on the novel nano-material between 1～100 nanometer, for example: nanotube, nano wire, nanometer rod, nano belt etc.Because one-dimensional material has physics unique compared with block materials and chemical property and obtained common people's extensive concern, in several years of the past, ZnO, SnO
2, In
2o
3, Ga
2o
3, V
2o
5, TiO
2obtain research widely Deng the monodimension nanometer material of transition metal oxide, and in the numerous areas such as semi-conductor preparation, photocatalyst material preparation, photoelectric conversion material, new energy materials, arriving widely application, the more and more important role of performer in our life.
At present, the synthetic method of monodimension nanometer material mainly contains chemical Vapor deposition process (CVD), template, hydrothermal synthesis method and microemulsion method etc.The one-dimensional material length-to-diameter ratio that chemical Vapor deposition process obtains is all larger, can prepare the one-dimensional material of different substances; But it needs high-temperature evaporation material, need cost higher, application is restricted.Template is one of method of at present the most frequently used nano materials, has the advantages such as aperture is adjustable, shape is controlled and can effectively prevent nano material reunion; But its monodimension nanometer material uniformity coefficient of preparing is not high, affect structure and the performance of material.Microemulsion method is also a kind of effective ways of preparing monodimension nanometer material, and synthetic one-dimensional material structure is better, but step is comparatively loaded down with trivial details compared with hydrothermal method.Hydrothermal synthesis method preparation method is easy, and raw material sources are abundant, and due to its environment that High Temperature High Pressure is provided, promoted material even growth in one direction, thereby can prepare all comparatively good one-dimensional materials of structure properties.
Thereby monocrystalline one-dimensional material has good performance owing to having the peculiar property of one-dimensional material, but monocrystal material still has the defect of himself sometimes, thereby impel present researcher further research on the basis of synthesizing one-dimensional nano material to its adulterate, be coated, modification, thereby on the basis of preparing one-dimensional material, can prepare the matrix material of different-shape, these matrix materials had both had the characteristic of one-dimensional material, there is again dopant, thereby expand the application prospect of one-dimensional material, strengthened the performance of one-dimensional nano-composite material.So having unique morphology, high-performance, high efficiency new one-dimensional nano composite material synthetic becomes researchers' study hotspot.
Summary of the invention
The object of the present invention is to provide a kind of nickel oxide-titanic oxide nano compound material.
Technical scheme of the present invention is: a kind of preparation method of nickel oxide-titanic oxide nano compound material, is characterized in that, with TiO
2(P-25) being body material, take 10M(mol/L) NaOH solution is reaction solvent, adopts hydrothermal method to prepare Na
2ti
8o
17nano material, then soaks, pickling, suction filtration, obtains banded H
2ti
8o
17, be placed in retort furnace, under 400-700 ℃ of condition, calcine 2h, obtain TiO
2nano belt; Adopt sluggish precipitation, with urea, nickelous nitrate, water and TiO
2for raw material, at 120 ℃ of insulation 4-6h, then under 400 ℃ of conditions, calcine 2h, can obtain leaf mosaic shape nickel oxide-titanium dioxide one-dimensional nano-composite material.
The invention has the beneficial effects as follows: compared with existing matrix material, the NiO-TiO that the present invention is prepared
2for one-dimensional nano-composite material, there is nontoxic, low cost, the advantage such as pollution-free, specific storage is high, security is good, catalytic performance, in the wide application prospect in the field such as lithium ion battery, photochemical catalysis.The characteristic of its monodimension nanometer material structure makes it have more advantage compared with current material, to preparing the power cell of high-energy-density, dye sensitization solar battery, the high efficiency photocatalyst material etc. of high conversion provides favourable support, energy-saving material-saving effect is remarkable.
Accompanying drawing explanation
Fig. 1 is H prepared by embodiment 1
2ti
8o
17xRD figure spectrum;
Fig. 2 is TiO prepared by embodiment 1
2xRD figure spectrum;
Fig. 3 is NiO-TiO prepared by embodiment 1
2sEM image;
Fig. 4 is NiO-TiO prepared by embodiment 1
2xRD figure spectrum.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described.Must be pointed out, embodiments of the invention are not limited in this.
64g NaOH is placed in to the beaker that fills 160ml distilled water, magnetic agitation is to room temperature, then by 2g TiO
2(P-25) pour in beaker, ultrasonic cleaning 5min, mixes solution.Mixing solutions is evenly divided into 4 parts, gets a copy of it and be placed in the stainless steel cauldron that 40ml liner is tetrafluoroethylene, seal, tighten reactor, this reactor is placed in to the Constant Temp. Oven of 180 ℃, incubation water heating reaction 72h.After completion of the reaction, naturally cool to room temperature, product taken out and puts into beaker with glass stick, add distilled water, repeatedly with cleaning, suction filtration to solution is neutral, carrying out after pickling, suction filtration, puts it in the loft drier of 100 ℃ and is dried 4h, obtains H
2ti
8o
17.
By the H obtaining
2ti
8o
17be placed in retort furnace, be warming up to 400 ℃ with the heat-up rate of 5 ℃/min, calcining 2h, furnace cooling, to room temperature, obtains TiO
2nano belt.Get 0.5g TiO
2nano belt, 0.4g urea, 0.522g nickelous nitrate and 40ml water are placed in beaker, in 120 ℃ of baking ovens, place 6h, within every 30 minutes, stir once, calcine 2h again through suction filtration, the dry material obtaining under 400 ℃ of conditions, make NiO-TiO
2nano composite material.
Be illustrated in figure 1 H prepared by the present embodiment
2ti
8o
17xRD figure, there are three comparatively significantly diffraction peaks, respectively corresponding H in the position that prepared material is 25.251 °, 44.599 °, 48.567 ° at 2 θ
2ti
8o
17(203),
(020) three crystal face.
Be illustrated in figure 2 the TiO that the present embodiment makes
2the XRD figure of nano belt, there are five comparatively significantly diffraction peaks, respectively corresponding TiO in the position that prepared material is 24.979 °, 28.596 °, 43.486 °, 48.634 °, 58.474 ° at 2 θ
2(110), (002), (003), (020),
five crystal faces.
Be illustrated in figure 3 the NiO-TiO that the present embodiment makes
2the SEM figure of nano composite material, TiO in figure
2present band shape, NiO presents sheet, the NiO nanometer sheet direction of growth and TiO
2substantially in vertical direction, and NiO nanometer sheet is at TiO for nano belt
2in nano belt, distribute not only more even, and sheet presents a kind of pattern that is similar to leaf mosaic in biology.
Be illustrated in figure 4 the NiO-TiO that the present embodiment makes
2the XRD figure of nano composite material, in figure except the corresponding peak of TiO2, still there are five comparatively significantly diffraction peaks, respectively (111), (200), (220), (311), (222) five crystal faces of corresponding NiO in the position that is 37.245 °, 43.275 °, 62.861 °, 75.392 °, 79.385 ° at diffraction angle 2 θ.From Fig. 3 and the comprehensive analysis of Fig. 4, NiO nanometer sheet is grown in TiO
2in nano belt, the two has formed a kind of nano material with unique novel appearance structure.
64g NaOH is placed in to the beaker that fills 160ml distilled water, magnetic agitation is to room temperature, then by 2g TiO
2(P-25) pour in beaker, ultrasonic cleaning 5min, mixes solution.Mixing solutions is evenly divided into 4 parts, gets a copy of it and be placed in the stainless steel cauldron that 40ml liner is tetrafluoroethylene, seal, tighten reactor, this reactor is placed in to the Constant Temp. Oven of 200 ℃, incubation water heating reaction 48h.After completion of the reaction, naturally cool to room temperature, product taken out and puts into beaker with glass stick, add distilled water, repeatedly with cleaning, suction filtration to solution is neutral, carrying out after pickling, suction filtration, puts it in the loft drier of 100 ℃ and is dried 4h, obtains H
2ti
8o
17.
By the H obtaining
2ti
8o
17be placed in retort furnace, be warming up to 700 ℃ with the heat-up rate of 5 ℃/min, calcining 2h, furnace cooling, to room temperature, obtains TiO
2nano belt.Get 0.5g TiO
2nano belt, 0.4g urea, 0.522g nickelous nitrate and 40ml water are placed in beaker, in 120 ℃ of baking ovens, place 4h, within every 30 minutes, stir once, calcine 2h again through suction filtration, the dry material obtaining under 400 ℃ of conditions, make NiO-TiO
2nano composite material.
Embodiment 3
64g NaOH is placed in to the beaker that fills 160ml distilled water, magnetic agitation is to room temperature, then by 2g TiO
2(P-25) pour in beaker, ultrasonic cleaning 5min, mixes solution.Mixing solutions is evenly divided into 4 parts, gets a copy of it and be placed in the stainless steel cauldron that 40ml liner is tetrafluoroethylene, seal, tighten reactor, this reactor is placed in to the Constant Temp. Oven of 160 ℃, incubation water heating reaction 60h.After completion of the reaction, naturally cool to room temperature, product taken out and puts into beaker with glass stick, add distilled water, repeatedly with cleaning, suction filtration to solution is neutral, carrying out after pickling, suction filtration, puts it in the loft drier of 100 ℃ and is dried 4h, obtains H
2ti
8o
17.
By the H obtaining
2ti
8o
17be placed in retort furnace, be warming up to 600 ℃ with the heat-up rate of 5 ℃/min, calcining 2h, furnace cooling, to room temperature, obtains TiO
2nano belt.Get 0.5g TiO
2nano belt, 0.4g urea, 0.522g nickelous nitrate and 40ml water are placed in beaker, in 120 ℃ of baking ovens, place 5h, within every 30 minutes, stir once, calcine 2h again through suction filtration, the dry material obtaining under 400 ℃ of conditions, make NiO-TiO
2nano composite material.
Claims (5)
1. a preparation method for nickel oxide-titanic oxide nano compound material, is characterized in that, 64g NaOH is placed in to the beaker that fills 160ml distilled water, and magnetic agitation is to room temperature, then by 2g TiO
2pour in beaker, ultrasonic cleaning 5min, solution is mixed, mixing solutions is evenly divided into 4 parts, getting a copy of it is placed in the stainless steel cauldron that 40ml liner is tetrafluoroethylene, seal, tighten reactor, this reactor is placed in to Constant Temp. Oven and carries out hydro-thermal reaction, after completion of the reaction, naturally cool to room temperature, product is taken out and puts into beaker with glass stick, adding distilled water, is neutral with cleaning, suction filtration to solution repeatedly, is carrying out after pickling, suction filtration, put it into dry 4h in the loft drier of 100 ℃, obtain H
2ti
8o
17; By the H obtaining
2ti
8o
17be placed in retort furnace, be warming up to respectively 400-700 ℃ with the heat-up rate of 5 ℃/min, calcining 2h, furnace cooling, to room temperature, obtains TiO
2nano belt; Get 0.5g TiO
2nano belt, 0.4g urea, 0.522g nickelous nitrate and 40ml water are placed in beaker, in 120 ℃ of baking ovens, place 4-6h, within every 30 minutes, stir once, calcine 2h again through suction filtration, the dry material obtaining under 400 ℃ of conditions, make NiO-TiO
2nano composite material.
2. the preparation method of nickel oxide-titanic oxide nano compound material according to claim 1, is characterized in that, hydrothermal temperature is 160-200 ℃, and the isothermal reaction time is 48-72h.
3. the preparation method of nickel oxide-titanic oxide nano compound material according to claim 2, is characterized in that, hydrothermal temperature is 180 ℃, and the isothermal reaction time is 72h.
4. the preparation method of nickel oxide-titanic oxide nano compound material according to claim 1, is characterized in that, H
2ti
8o
17presoma calcining temperature in retort furnace is 400 ℃.
5. the preparation method of nickel oxide-titanic oxide nano compound material according to claim 1, is characterized in that, described TiO
2nano belt storage period in baking oven is 6h.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105321721A (en) * | 2015-12-02 | 2016-02-10 | 常州大学 | Preparation method of dye sensitization solar cell photo-anode material |
| CN105800680A (en) * | 2016-03-14 | 2016-07-27 | 武汉理工大学 | Preparation method of titanium dioxide nanotube doped with transition metal |
| CN106582591A (en) * | 2016-11-17 | 2017-04-26 | 广东工业大学 | A kind of preparation method of square prism anatase type TiO2 |
| CN107356635A (en) * | 2017-07-13 | 2017-11-17 | 济南大学 | A kind of NiO nanometer sheets/α Fe applied to gas sensor2O3Nanocube heterojunction material |
| CN107389736A (en) * | 2017-05-22 | 2017-11-24 | 江苏时瑞电子科技有限公司 | A kind of preparation method of the humidity sensor based on sodium titanate |
| CN107570159A (en) * | 2017-09-22 | 2018-01-12 | 江苏科来材料科技有限公司 | One kind prepares high-performance black TiO2The method of photochemical catalyst |
| CN111484072A (en) * | 2020-04-23 | 2020-08-04 | 河北工业大学 | Method for preparing titanate or titanium-based composite oxide material by low-temperature crystalline phase conversion |
| CN114477789A (en) * | 2022-02-11 | 2022-05-13 | 中国海洋大学 | A kind of solvothermal preparation method of titanium-doped nickel oxide electrochromic film |
| CN114950439A (en) * | 2022-05-16 | 2022-08-30 | 扬州大学 | A kind of high-efficiency photolysis water hydrogen production MOF TiO2-NiO material and its preparation method and application |
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|---|---|---|---|---|
| CN105321721A (en) * | 2015-12-02 | 2016-02-10 | 常州大学 | Preparation method of dye sensitization solar cell photo-anode material |
| CN105321721B (en) * | 2015-12-02 | 2018-02-09 | 常州大学 | A kind of preparation method of dye-sensitized solar cell anode material |
| CN105800680A (en) * | 2016-03-14 | 2016-07-27 | 武汉理工大学 | Preparation method of titanium dioxide nanotube doped with transition metal |
| CN106582591A (en) * | 2016-11-17 | 2017-04-26 | 广东工业大学 | A kind of preparation method of square prism anatase type TiO2 |
| CN107389736A (en) * | 2017-05-22 | 2017-11-24 | 江苏时瑞电子科技有限公司 | A kind of preparation method of the humidity sensor based on sodium titanate |
| CN107356635A (en) * | 2017-07-13 | 2017-11-17 | 济南大学 | A kind of NiO nanometer sheets/α Fe applied to gas sensor2O3Nanocube heterojunction material |
| CN107570159A (en) * | 2017-09-22 | 2018-01-12 | 江苏科来材料科技有限公司 | One kind prepares high-performance black TiO2The method of photochemical catalyst |
| CN111484072A (en) * | 2020-04-23 | 2020-08-04 | 河北工业大学 | Method for preparing titanate or titanium-based composite oxide material by low-temperature crystalline phase conversion |
| CN114477789A (en) * | 2022-02-11 | 2022-05-13 | 中国海洋大学 | A kind of solvothermal preparation method of titanium-doped nickel oxide electrochromic film |
| CN114950439A (en) * | 2022-05-16 | 2022-08-30 | 扬州大学 | A kind of high-efficiency photolysis water hydrogen production MOF TiO2-NiO material and its preparation method and application |
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Application publication date: 20140604 |