CN101891240B - Preparation method of CdO porous nanometer material - Google Patents
Preparation method of CdO porous nanometer material Download PDFInfo
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- CN101891240B CN101891240B CN2010102252761A CN201010225276A CN101891240B CN 101891240 B CN101891240 B CN 101891240B CN 2010102252761 A CN2010102252761 A CN 2010102252761A CN 201010225276 A CN201010225276 A CN 201010225276A CN 101891240 B CN101891240 B CN 101891240B
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- presoma
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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-type, semiconductor 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, the preparation process is loaded down with trivial details, not suitable for mass production.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; The synthetic cost is high, difficult technique control; 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, need not 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, need not add under the situation of any tensio-active agent, through 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 specific surface area is high, 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, need add any tensio-active agent, and economic environmental protection helps scale prodn.
Product with the present invention's preparation carries out structure and performance characterization through following means: the thing of product adopts the D/Max-RA type rotating anode X-ray diffractometer (XRD) of Japanese Rigaku manufactured to analyze (CuK α) mutually; 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 sem (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, need not 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, through 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, need not 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; Through changing ambient conditions; Ratio, temperature of reaction, reaction times or heat-treat condition etc. like the second alcohol and water; Can control shape, size and the aperture of CdO porous nanometer material, thereby realize effective control 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 precursor that b) obtains for embodiment 1, pattern are nano line cluster; (c, the precursor that d) 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 precursor that d) 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, the porous C dO nanostructure that b) obtains for embodiment 1; Fig. 3 (c, d, e, f, the porous C dO nanostructure that g) obtains for embodiment 2; Fig. 3 (h, the porous C dO nanostructure that i) obtains for embodiment 4.
Five, embodiment
Below be embodiments of the invention (agents useful for same is a CP 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 drum, obtain solid product.With the solid product spinning, water and ethanol cleaning many times obtain Cd
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 absolute ethyl 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 absolute ethyl 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 drum, obtain solid product.With the solid product spinning, water and ethanol cleaning many times obtain Cd
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 (3)
1.CdO the preparation method of porous nanometer material is characterized in that: 0.62 gram Cd (NO
3)
24H
2O is dissolved in 40 mL ethanol and water volume ratio is in the solution of 63:37 composition; Solution is transferred in the container of tetrafluoroethylene lining, is placed into the stainless steel encloses container then and in baking oven, is incubated 24 ± 4 hours under 150 ± 2 ℃ of temperature, behind the cool to room temperature; Open reactor drum; Obtain the presoma solid product, with the spinning of presoma solid product, water and ethanol cleaning many times obtain Cd
5(OH)
8(NO
3)
2(H
2O)
2Presoma obtains 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.
2.CdO the preparation method of porous nanometer material is characterized in that: 0.62 gram Cd (NO
3)
24H
2O is dissolved in the solution that volume ratio=75:25 formed of 40 mL second alcohol and waters; Fully obtaining stirring formation concentration is the clear solution of 0.05 mol/L; Solution is transferred in the container of tetrafluoroethylene lining, is placed into the stainless steel encloses container then and in baking oven, is incubated 24 ± 4 hours under 150 ± 2 ℃ of temperature, naturally cool to room temperature after; Open reactor drum; Obtain the presoma solid product, with the spinning of presoma solid product, water and ethanol cleaning many times obtain Cd
5(OH)
8(NO
3)
2(H
2O)
2Presoma, pattern are wide 150 nanometers, thick 25 nanometers, and 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.
3.CdO the preparation method of porous nanometer material is characterized in that: 0.62 gram Cd (NO
3)
24H
2O is dissolved in the pure alcohol solvent of 40mL, and fully obtaining stirring formation concentration is the clear solution of 0.05 mol/L, 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; After naturally cooling to room temperature, open reactor drum, obtain the presoma solid product; With the spinning of presoma solid product, water and ethanol cleaning many times obtain Cd
5(OH)
8(NO
3)
2(H
2O)
2Presoma, pattern is by nano wire weave in " felt " shape product; 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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|---|---|---|---|
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|---|---|---|---|
| CN2010102252761A CN101891240B (en) | 2010-07-14 | 2010-07-14 | Preparation method of CdO porous nanometer material |
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| 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 |
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 |
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| 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 |
|---|
| Zai-xing Yang et al..Controllable Synthesis of Single-Crystalline CdO and Cd(OH)2 Nanowires by a Simple Hydrothermal Approach.《Nanoscale Res Lett》.2010,第5卷961-965. * |
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