CN101891240A - Preparation method of CdO porous nanometer material - Google Patents
Preparation method of CdO porous nanometer material Download PDFInfo
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- CN101891240A CN101891240A CN201010225276.1A CN201010225276A CN101891240A CN 101891240 A CN101891240 A CN 101891240A CN 201010225276 A CN201010225276 A CN 201010225276A CN 101891240 A CN101891240 A CN 101891240A
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- 239000000463 material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 230000035484 reaction time Effects 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000002086 nanomaterial Substances 0.000 claims description 19
- 239000000047 product Substances 0.000 claims description 13
- 238000005516 engineering process Methods 0.000 claims description 9
- 239000013543 active substance Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000002127 nanobelt Substances 0.000 claims description 7
- 239000002070 nanowire Substances 0.000 claims description 7
- 239000012265 solid product Substances 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 5
- 238000009954 braiding Methods 0.000 claims description 4
- 230000001105 regulatory 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
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 2
- 238000007669 thermal treatment Methods 0.000 claims 1
- 239000002243 precursor Substances 0.000 abstract description 11
- 238000000034 method Methods 0.000 abstract description 9
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- QOYRNHQSZSCVOW-UHFFFAOYSA-N cadmium nitrate tetrahydrate Chemical compound O.O.O.O.[Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QOYRNHQSZSCVOW-UHFFFAOYSA-N 0.000 abstract 3
- 238000009415 formwork Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229960004756 ethanol Drugs 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000000103 photoluminescence spectrum Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000001241 arc-discharge method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of a CdO porous nanometer material, which comprises following steps of: dissolving Cd(NO3)2.4H2O in solvent formed by ethanol and water according to a certain ratio in a closed container, and adjusting the ratio of the ethanol to the water, the concentration of the Cd(NO3)2.4H2O, the reaction temperature and the reaction time without using any template and adding any surfactant to obtain Cd5(OH)8(NO3)2(H2O)2 precursors with different nanometer structures; slowly heating the precursors with the nanometer structures in the air to obtain the CdO porous nanometer material with a high specific area; and slowing heating the CdO porous nanometer material to 350-500 DEG C at a rate of 0.2-2 DEG C per minute. In the preparation process of the precursors, the volume ratio of the ethanol to the water is 100:0-60:40, the concentration of the Cd(NO3)2.4H2O is 0.01-0.1 mol/L, the reaction time lasts for 3-50 hours, and the reaction temperature is controlled at 120-200 DEG C. The invention has simple preparation process, low cost, easily controlled process, environment friendliness and no pollution.
Description
One, technical field
The present invention relates to a kind of important photoelectric functional material--the preparation method of CdO porous nanometer material.
Two, background technology
CdO is important n-N-type semiconductorN material, its direct band gap 2.5eV, indirect band gap 1.98eV.The CdO nano material is important photoelectric functional material, has broad application prospects in many fields such as solar cell, optotransistor, optical diode, catalysis and gas sensors.Synthetic technology such as vapor transportation methods, chemical Vapor deposition process, arc discharge method, laser melting that adopt of the CdO nano material of present bibliographical information more, required equipment requires height, the facility investment scale is big, synthesis technique is complicated, preparation process is loaded down with trivial details, is not suitable for scale operation.Also there is bibliographical information to adopt chemical process to synthesize CdCO earlier
3Or Cd
4Cl
3(OH)
5As precursor, pyroprocessing obtains the CdO of nanostructure in oxygen then etc. nano material.But the synthesizing of Cd nanostructure precursor that contain that up to the present document is reported all adopted inorganic or organic formwork, or interpolation organic surface active agent, synthetic cost height, the difficult control of technology, and organic formwork and tensio-active agent all are decomposed into gaseous product in building-up process, not only waste but also in the face of many problem of environmental pollutions.
Three, summary of the invention
The present invention seeks to, propose a kind of preparation method of synthetic CdO porous nanometer material newly.Especially without any need for template, do not need to add under the situation of any tensio-active agent and prepare,
Technical scheme of the present invention is: the preparation method of CdO porous nanometer material, and in stainless steel (inner liner polytetrafluoroethylene) encloses container, with Cd (NO
3)
24H
2O is dissolved in the solvent of being made up of a certain proportion of second alcohol and water, without any need for template, do not need to add under the situation of any tensio-active agent, by regulating ratio, the Cd (NO of second alcohol and water
3)
24H
2The concentration of O, temperature of reaction, reaction times obtain having the Cd of different nanostructures
5(OH)
8(NO
3)
2(H
2O)
2Presoma (nanometer " felt " that can synthesize nano line cluster, nano belt selectively, become by nano wire " braiding ", the flower-shaped thing of forming by nanometer rod of radial pattern etc.).At Cd
5(OH)
8(NO
3)
2(H
2O)
2Among the preparation technology of presoma, the volume ratio of second alcohol and water is 100: 0-60: 40, and Cd (NO
3)
24H
2The concentration of O is the 0.01-0.1 mol, and the reaction times is 3-50 hour, and temperature of reaction is 120-200 ℃.With the Cd that obtains
5(OH)
8(NO
3)
2(H
2O)
2The slow heating in air or oxygen of nanostructure presoma can obtain having the CdO porous nanometer material of high-specific surface area.Slowly be heated to temperature 350-500 ℃, temperature rise rate 0.2-2 ℃/minute, soaking time is 1-20 hour.
The CdO porous nanometer material for preparing with method of the present invention has kept Cd basically
5(OH)
8(NO
3)
2(H
2O)
2The pattern of presoma has a large amount of nanometer cavity structures, and the specific surface area height can be applicable to many fields such as solar cell, optotransistor, optical diode, catalysis and gas sensor.Compare with the method for preparing the CdO nano material of bibliographical information, maximum difference of the present invention is not use any template, does not need to add any tensio-active agent, and economic environmental protection helps scale production.
Product with the present invention preparation carries out structure and performance characterization by following means: the D/Max-RA type rotating anode X-ray diffractometer (XRD) that the thing of product adopts Japanese Rigaku company to make is mutually analyzed (CuK α); Sirion field emission scanning electron microscope (FE-SEM) and JEOL-2010 type high resolution transmission electron microscopy (HRTEM) that the pattern of product adopts JSM-5610LV type scanning electronic microscope (SEM), FEI Co. to produce characterize, and adopt He-Cd laser apparatus (excitation wavelength: 325nm) tested the photoluminescence spectrum (PL) of sample.
The invention has the beneficial effects as follows: the preparation method of the synthetic CdO porous nanometer material of the present invention.Especially without any need for template, do not need to add under the situation of any tensio-active agent and prepare, in encloses container, with Cd (NO
3)
24H
2O is a raw material, and the second alcohol and water is a solvent, by regulating ratio, the Cd (NO of second alcohol and water
3)
24H
2The concentration of O, temperature of reaction, reaction times optionally synthesize the Cd of multiple pattern
5(OH)
8(NO
3)
2(H
2O)
2Presoma is then with Cd
5(OH)
8(NO
3)
2(H
2O)
2Presoma slowly heats the CdO porous nanometer material that obtains having high-specific surface area in air.Owing in entire synthesis process, do not need to add any organic formwork and tensio-active agent, saved material cost, and environmental friendliness, pollution-free.This preparation technology's equipment is simple, cost is low, process is controlled easily, is easy to mass-producing; By changing ambient conditions, ratio, temperature of reaction, reaction times or heat-treat condition etc. as the second alcohol and water, can control shape, size and the aperture of CdO porous nanometer material, thereby realization is to effective control of CdO porous nanometer material bulk property.Especially obtain the CdO porous nanometer material of the nano line cluster of long number micron.
Four, description of drawings
Fig. 1 is Cd
5(OH)
8(NO
3)
2(H
2O)
2The field emission scanning electron microscope of presoma (FE-SEM) photo.Fig. 1 (a, the b) precursor that obtains for embodiment 1, pattern are nano line cluster; (c, the d) precursor that obtains for embodiment 2, pattern are wide about 150 nanometers, thick about 25 nanometers to Fig. 1, and length is tens microns nano belt; (e f) is the precursor of embodiment 3 preparation to Fig. 1, for wide about 250 nanometers, be about 5 microns nano belt; (g, h are the precursors of embodiment 4 preparations i) to Fig. 1, can see the felt shape product that is formed by nano wire " braiding ".
Fig. 2 is Cd
5(OH)
8(NO
3)
2(H
2O)
2The field emission scanning electron microscope of presoma (FE-SEM) photo.The precursor that Fig. 2 a obtains for embodiment 5, the about 6 microns flower-shaped thing of forming by nanometer rod of emission type of diameter; (b, c, the d) precursor that obtains for embodiment 6, pattern are by the crisscross micrometer structure of forming of nanometer rod to Fig. 2.
Fig. 3 is field emission scanning electron microscope (FE-SEM) photo of porous C dO nanostructure.Fig. 3 (a, b) the porous C dO nanostructure that obtains for embodiment 1; Fig. 3 (c, d, e, f, g) the porous C dO nanostructure that obtains for embodiment 2; Fig. 3 (h, i) the porous C dO nanostructure that obtains for embodiment 4.
Five, embodiment
Below be embodiments of the invention (agents useful for same is a chemical pure among the embodiment).
Embodiment 1: with 0.62 gram Cd (NO
3)
24H
2O is dissolved in the solution of 40mL second alcohol and water (volume ratio=63: 37) composition, and fully stirring and forming concentration is the clear solution of 0.05mol/L.Solution is transferred in the polytetrafluoroethylcontainer container, is placed in the stainless steel encloses container, 150 ± 2 ℃ are incubated 24 ± 4 hours in baking oven.After naturally cooling to room temperature, open reactor, obtain solid product.With the solid product centrifugation, water and ethanol clean and obtain Cd for several times
5(OH)
8(NO
3)
2(H
2O)
2Presoma.Shown in Fig. 1 a and 1b, product be the nano wire of diameter 12-17 nanometer form be about several microns nano line cluster.Product is placed in the retort furnace, and the temperature rise rate with 1 ℃/minute in the air atmosphere slowly is warmed up to 400 ℃, is incubated naturally cooling after 3 ± 1 hours, promptly obtains having the CdO nano-material in nanometer cavity.
The nanometer " felt " that can synthesize nano line cluster, nano belt selectively, become by nano wire " braiding ", the flower-shaped thing of forming by nanometer rod of radial pattern etc.At Cd
5(OH)
8(NO
3)
2(H
2O)
2Among the preparation technology of presoma, the ratio of second alcohol and water is 100: 0-60: 40, and Cd (NO
3)
24H
2The concentration of O is the 0.01-0.1 mol, and the reaction times is 3-50 hour, and temperature of reaction is 120-200 ℃.
Embodiment 2: compare with embodiment 1, difference is that solvent is the solution of the volume ratio=formed at 75: 25 of second alcohol and water, and all the other conditions are all identical in embodiment 1.Obtain Cd
5(OH)
8(NO
3)
2(H
2O)
2The pattern of presoma is wide about 150 nanometers, thick about 25 nanometers shown in Fig. 1 c and 1d, length is tens microns nano belt.Product is placed in the retort furnace, and the temperature rise rate with 1 ℃/minute in the air atmosphere slowly is warmed up to 400 ℃, is incubated naturally cooling after 3 hours, obtains having the CdO strip material in nanometer cavity.
Embodiment 3: compare with embodiment 1, difference is that solvent is the solution of the volume ratio=formed at 88: 12 of second alcohol and water, and all the other conditions are all identical in embodiment 1.Obtain Cd
5(OH)
8(NO
3)
2(H
2O)
2The pattern of nano belt is compared with embodiment 2 shown in Fig. 1 e and 1f, and width is increased to about 250 nanometers; Contraction in length, about 5 microns.
Embodiment 4: compare with embodiment 1, difference is that solvent is pure dehydrated alcohol, and all the other conditions are all identical in embodiment 1.The Cd that obtains
5(OH)
8(NO
3)
2(H
2O)
2The pattern of presoma such as Fig. 1 (g, h, i) shown in, by nano wire weave in " felt " shape product.
Embodiment 5: with 0.124 gram Cd (NO
3)
24H
2O is dissolved in the 40mL dehydrated alcohol, and fully stirring and forming concentration is the clear solution of 0.01mol/L.Solution is transferred in the container of tetrafluoroethylene lining, is placed into then in the stainless steel encloses container, 180 ℃ are incubated 24 hours in baking oven.After naturally cooling to room temperature, open reactor, obtain solid product.With the solid product centrifugation, water and ethanol clean and obtain Cd for several times
5(OH)
8(NO
3)
2(H
2O)
2Presoma.Shown in Fig. 2 a, the flower-shaped thing of emission type that the diameter that product is made up of nanometer rod is about 6 microns.Product is placed in the retort furnace, and the temperature rise rate with 0.5 ℃/minute in the air atmosphere slowly is warmed up to 400 ℃, is incubated naturally cooling after 3 hours, promptly obtains having the CdO nano-material in nanometer cavity.
Embodiment 6: compare with embodiment 5, difference is that oven temperature is 200 ℃ of insulations 24 hours, and all the other conditions are all identical in embodiment 1.The Cd that obtains
5(OH)
8(NO
3)
2(H
2O)
2The pattern of presoma such as Fig. 2 (b, c, d) shown in, by the crisscross micrometer structure of forming of nanometer rod.Product is placed in the retort furnace, and the temperature rise rate with 1 ℃/minute in the air atmosphere slowly is warmed up to 400 ℃, is incubated naturally cooling after 3 hours, obtains having the CdO strip material in nanometer cavity.
Claims (5)
1.CdO the preparation method of porous nanometer material is characterized in that in the encloses container, with Cd (NO
3)
24H
2O is dissolved in the solvent of being made up of a certain proportion of second alcohol and water, without any need for template, do not need to add under the situation of any tensio-active agent, by regulating ratio, the Cd (NO of second alcohol and water
3)
24H
2The concentration of O, temperature of reaction, reaction times obtain having the Cd of different nanostructures
5(OH)
8(NO
3)
2(H
2O)
2Presoma; At Cd
5(OH)
8(NO
3)
2(H
2O)
2Among the preparation technology of presoma, the volume ratio of second alcohol and water is 100: 0-60: 40, and Cd (NO
3)
24H
2The concentration of O is the 0.01-0.1 mol, and the reaction times is 3-50 hour, and temperature of reaction is 120-200 ℃; The nanostructure presoma that obtains, with the nanostructure presoma that obtains in air slowly heating can obtain having the CdO porous nano material of high-specific surface area; The condition in described temperature of reaction, reaction times is: slowly be heated to temperature 350-500 ℃, temperature rise rate 0.2-2 ℃/minute, soaking time is 1-20 hour.
2. the preparation method of CdO porous nanometer material according to claim 1 is characterized in that Cd
5(OH)
8(NO
3)
2(H
2O)
2The preparation technology of nanostructure presoma is realized by following step: in encloses container, with Cd (NO
3)
24H
2O is a raw material, and the second alcohol and water is a solvent, without any need for template, do not need to add under the situation of any tensio-active agent, by regulating ratio, the Cd (NO of second alcohol and water
3)
24H
2The concentration of O, temperature of reaction, reaction times are controlled Cd
5(OH)
8(NO
3)
2(H
2O)
2The pattern of presoma, the nanometer " felt " that synthesizes nano line cluster, nano belt selectively, becomes by nano wire " braiding ", the flower-shaped thing of forming by nanometer rod of radial pattern.
3. the preparation method of CdO porous nanometer material according to claim 2 is characterized in that Cd
5(OH)
8(NO
3)
2(H
2O)
2Among the preparation technology of presoma, the ratio of second alcohol and water is 100: 0-60: 40, and Cd (NO
3)
24H
2The concentration of O is the 0.01-0.1 mol, and the reaction times is 3-50 hour, and temperature of reaction is 120-200 ℃.
4. the preparation method of CdO porous nanometer material according to claim 1 and 2 is characterized in that Cd
5(OH)
8(NO
3)
2(H
2O)
2The thermal treatment temp 350-500 of presoma ℃, temperature rise rate 0.2-2 ℃/minute, soaking time is 1-20 hour.
5. the preparation method of CdO porous nanometer material according to claim 1 and 2, it is characterized in that 0.62 gram Cd (NO3) 24H2O is dissolved in 40mL ethanol and water volume ratio is in the solution of forming at 63: 37, solution is transferred in the container of tetrafluoroethylene lining, be placed into the stainless steel encloses container then and in baking oven, be incubated 24 ± 4 hours under 150 ± 2 ℃ of temperature, behind the cool to room temperature, open reactor, obtain the presoma solid product, with the centrifugation of presoma solid product, water and ethanol clean and obtain Cd5 (OH) 8 (NO3) 2 (H2O) 2 presomas for several times, obtain the nano line cluster of the long number micron that the nano wire of diameter 12-17 nanometer forms; This product is placed in the retort furnace, and the temperature rise rate with 1 ℃/minute in the air atmosphere slowly is warmed up to 400 ℃, be incubated 3 ± 1 hours again after naturally cooling get the CdO porous nanometer material.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102252761A CN101891240B (en) | 2010-07-14 | 2010-07-14 | Preparation method of CdO porous nanometer material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101891240A true CN101891240A (en) | 2010-11-24 |
| CN101891240B CN101891240B (en) | 2012-02-29 |
Family
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|---|---|---|---|
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|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103285803A (en) * | 2013-07-03 | 2013-09-11 | 西北师范大学 | Method of preparing porous CdO absorbent through thermal decomposition and application of porous CdO absorbent in wastewater treatment |
| CN110289172A (en) * | 2019-07-03 | 2019-09-27 | 曲靖贝塔科技有限公司 | Graphene-cadmium oxide dye-sensitized solar cell working electrode preparation method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1546382A (en) * | 2003-12-10 | 2004-11-17 | 山东师范大学 | Method for synthesizing cadmium hydroxide single-crystal nanowire |
-
2010
- 2010-07-14 CN CN2010102252761A patent/CN101891240B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1546382A (en) * | 2003-12-10 | 2004-11-17 | 山东师范大学 | Method for synthesizing cadmium hydroxide single-crystal nanowire |
Non-Patent Citations (1)
| Title |
|---|
| 《Nanoscale Res Lett》 20100411 Zai-xing Yang et al. Controllable Synthesis of Single-Crystalline CdO and Cd(OH)2 Nanowires by a Simple Hydrothermal Approach 961-965 1-5 第5卷, 2 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103285803A (en) * | 2013-07-03 | 2013-09-11 | 西北师范大学 | Method of preparing porous CdO absorbent through thermal decomposition and application of porous CdO absorbent in wastewater treatment |
| CN103285803B (en) * | 2013-07-03 | 2015-07-15 | 西北师范大学 | Method of preparing porous CdO absorbent through thermal decomposition and application of porous CdO absorbent in wastewater treatment |
| CN110289172A (en) * | 2019-07-03 | 2019-09-27 | 曲靖贝塔科技有限公司 | Graphene-cadmium oxide dye-sensitized solar cell working electrode preparation method |
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