CN103601169A - Preparation method of carbon-hybrid nano belt - Google Patents
Preparation method of carbon-hybrid nano belt Download PDFInfo
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- CN103601169A CN103601169A CN201310233277.4A CN201310233277A CN103601169A CN 103601169 A CN103601169 A CN 103601169A CN 201310233277 A CN201310233277 A CN 201310233277A CN 103601169 A CN103601169 A CN 103601169A
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Abstract
A preparation method of a carbon-hybrid nano belt comprises the following steps: evenly mixing nitrate and triethanolamine according to a mass ratio of 1:6 to 1:12, placing the mixture in a baking oven, heating for 4 to 8 hours at the temperature of 150 DEG C until the water is totally evaporated, taking out the mixture; raising the temperature in the baking oven to 170 to 180 DEG C, putting the sample in the baking oven, controlling the temperature to slowly reach the kindling point of triethanolamine; putting the sample in a ceramic boat, placing the ceramic boat into the center of a tube furnace; filling up another ceramic boat with sublimed sulphur, selenium powder or a mixture of sublimed sulphur and selenium powder, placing the ceramic boat on the gas inlet side of the tube furnace, exhausting the air in the tube furnace, inducing into mixed gas of nitrogen gas with a content of 92 to 97% and hydrogen gas with a content of 3 to 8%, and annealing for 3 hours at the temperature of 600 DEG C. The preparation method has a simple process, and can obtain a sulfide (selenide)/carbon hybrid nano belt with a high purity, small particle size, excellent shape, high activity.
Description
Technical field
The invention belongs to material technology field.
Technical background
In recent years, the nano composite material of carbon nanometer and semiconductor material is studied widely due to its unique physico-chemical property with in the potential using value aspect electronics, optics, biological medicine.And sulphur (selenium) compound/carbon hybrid nanostructure is also wherein to study Yi Ge branch very widely.The main method of preparing before this sulphur (selenium) compound matrix material has: thermal evaporation, position reduction precipitation method, solvent thermal are synthetic, electrochemical deposition, photochemical method, sonochemical method etc.
Summary of the invention
The invention provides a kind of preparation method of carbon hybridized nanometer band, the sulphur that processability is good, pattern is good (selenium) compound/carbon hybridized nanometer band.
The present invention is achieved by the following technical solutions.
The concrete preparation process of the present invention is as follows.
(1) nitrate is dissolved in a small amount of pure water, until completely dissolved, by nitrate: the mass ratio that trolamine is 1:6～1:12, add trolamine, stir concussion, to mixing completely, then the solution mixing is placed in to baking oven, at 150 ℃ of heating 4 h ~ 8 h.Therebetween, every one hour, take out, stir and put into again baking oven continuation heating, until the complete evaporate to dryness of moisture takes out standby.
(2) baking oven is opened, when temperature rises to 170 ~ 180 ℃, the sample of processing through step (1) is placed in one, control oven temperature and slowly reach trolamine point of ignition, make trolamine ignition and discharge a large amount of gas, obtaining fluffy nano belt initial sample.
(3) the nano belt initial sample of getting step (2) packs ceramic boat into, is placed in tube furnace central authorities.By another ceramic boat, fill with again the mixture of sublimed sulphur, selenium powder or sublimed sulphur and selenium powder, be placed in tube furnace inlet mouth one side, after emptying air, pass into the mixed gas that the hydrogen of 92 ~ 97% nitrogen and 3 ~ 8% forms, 600 ℃ of annealing three hours.
What the present invention adopted is low-temperature combustion synthesis, then compound sulphur (selenium) compound/carbon hybridized nanometer band that obtains in tube furnace.Process is simple, and sulphur (selenium) compound/carbon hybridized nanometer band high-purity, that granularity is little, pattern is good, activity is high that is easy to get.The method is not only time saving and energy saving, has also improved the activity of sulphur (selenium) compound/carbon hybridized nanometer band.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is described in further detail.
Fig. 1 is the environmental scanning electronic microscope map analysis of cadmium selenide // carbon hybridized nanometer band, and as can be seen from the figure its structure is banded, and cadmium selenide is relatively evenly distributed on carbon nanobelts.
Fig. 2 is the XRD test analysis figure of lead sulfide/carbon hybridized nanometer band.
Fig. 3 is the transmission electron microscope map analysis of lead sulfide/carbon hybridized nanometer band, can find out that its dispersity of lead sulfide/carbon nanobelts structure is all better on picture.
Fig. 4 is the analysis of sulphur lead selenide/carbon hybridized nanometer band environment scanning electron microscope (SEM) photograph.
Fig. 5 is the XRD test analysis figure of sulphur lead selenide/carbon hybridized nanometer band.
Embodiment
The present invention will be described further by following examples.
The chemical reagent purity that this experiment adopts is analytical pure.Present method adopts trolamine as incendiary material, complexing agent and promoting agent, and nitrate, by low-temperature burning, is obtained to preliminary sample.Then with selenium powder (or sublimed sulphur or both) 600 ℃ of annealing three hours in hydrogen (nitrogen protection) atmosphere, obtain sulphur (selenium) compound/carbon hybridized nanometer band.
Embodiment 1.
Preparation process is as follows, and (1) is dissolved in the cadmium nitrate of 0.03 mol in a small amount of pure water, until completely dissolved, the trolamine that adds 55 ml left and right, stirs concussion, to mixing completely, then the solution mixing is placed in to baking oven, 150 ℃ are heated 5 hours.Therebetween, every one hour, take out, stir and put into again baking oven continuation heating, until the complete evaporate to dryness of moisture takes out standby.(2) while, oven temperature being heated to 170 ℃, the sample of processing through step (1) is placed in to baking oven, control oven temperature and slowly reach trolamine point of ignition, make trolamine ignition and discharge a large amount of gas, obtain fluffy nano belt initial sample.(3), with a ceramic boat dress, get the initial sample of step (2), another ceramic boat fills with the protective gas that selenium powder is placed in 600 ℃, tube furnace anneals three hours, the mixed gas that the nitrogen that wherein protective gas is 92% and 8% hydrogen form.Make as the cadmium selenide/carbon hybridized nanometer band in Fig. 1.
Embodiment 2.
Preparation process is as follows, and (1) is dissolved in the cadmium nitrate of 0.03 mol in a small amount of pure water, until completely dissolved, the trolamine that adds 55 ml left and right, stirs concussion, to mixing completely, then the baking oven solution mixing being placed in heats, and 150 ℃ are heated 5 hours.Therebetween, every one hour, take out, stir and put into again baking oven continuation heating, until the complete evaporate to dryness of moisture takes out standby.(2) while oven temperature being heated to 180 ℃, the sample of handling well through step (1) is placed in to baking oven, control oven temperature and slowly reach trolamine point of ignition, make trolamine ignition and discharge a large amount of gas, obtain fluffy nano belt initial sample.(3) with a ceramic boat dress, get the initial sample of step (2), another ceramic boat fills with the protective gas that sulphur powder is placed in 600 ℃, tube furnace anneals three hours, the mixed gas that the nitrogen that wherein protective gas is 97% and 3% hydrogen form.Make Cadmium Sulfide/carbon hybridized nanometer band.
Embodiment 3.
Preparation process is as follows, and (1) is dissolved in the lead nitrate of 0.03 mol in a small amount of pure water, until completely dissolved, the trolamine that adds 50 ml left and right, stirs concussion, to mixing completely, then the solution mixing is placed in to baking oven, 150 ℃ are heated 5 hours.Therebetween, every one hour, take out, stir and put into again baking oven continuation heating, until form solid state.(2) another baking oven is opened, when oven temperature is heated to 175 ℃, the sample of processing through step (1) is placed in to baking oven, controls oven temperature and slowly reach trolamine point of ignition, make trolamine ignition and discharge a large amount of gas, obtaining fluffy nano belt initial sample.(3) with a ceramic boat dress, get the initial sample of step (2), another ceramic boat fills with the protective gas that selenium powder is placed in 600 ℃, tube furnace anneals three hours, the mixed gas that the nitrogen that wherein protective gas is 95% and 5% hydrogen form.Make lead sulfide/carbon nanobelts, if Fig. 2 is its XRD figure spectrum, Fig. 3 is its TEM (transmission electron microscope) analysis figure.
Embodiment 4.
The lead nitrate of 0.03 mol is dissolved in a small amount of pure water, until completely dissolved, adds the trolamine of 50 ml left and right, stir concussion, to mixing completely, then the solution mixing is placed in to baking oven, 150 ℃ are heated 5 hours.Therebetween, every one hour, take out, stir and put into again baking oven continuation heating, until form solid state.(2) another baking oven is opened, when oven temperature is heated to 180 ℃, the sample of processing through step (1) is placed in to baking oven, controls oven temperature and slowly reach trolamine point of ignition, make trolamine ignition and discharge a large amount of gas, obtaining fluffy nano belt initial sample.(3) with a ceramic boat dress, get the sample having burnt; one ceramic boat is contained selenium powder; a ceramic boat is contained sublimed sulphur again, and the protective gas that is placed in 600 ℃, tube furnace is annealed three hours, the mixed gas that the nitrogen that wherein protective gas is 97% and 3% hydrogen form.Make as the sulphur lead selenide/carbon nanobelts in Fig. 4.Fig. 5 is its XRD test analysis figure.
Obviously, those skilled in the art can carry out various changes and distortion and not depart from the spirit and scope of the present invention sulphur of the present invention (selenium) compound/carbon hybridized nanometer band and preparation method thereof.Like this, if within these modifications of the present invention and distortion belong to the scope of the claims in the present invention and equivalent technologies thereof, the present invention is also intended to comprise these changes and distortion interior.
Claims (1)
1. a preparation method for carbon hybridized nanometer band, is characterized in that step is as follows:
(1) nitrate is dissolved in a small amount of pure water, until completely dissolved, by nitrate: the mass ratio that trolamine is 1:6～1:12, add trolamine, stir concussion, to mixing completely, then the solution mixing is placed in to baking oven, at 150 ℃ of heating 4 h ~ 8 h; Therebetween, every one hour, take out, stir and put into again baking oven continuation heating, until the complete evaporate to dryness of moisture takes out standby;
(2) baking oven is opened, when temperature rises to 170 ~ 180 ℃, the sample of processing through step (1) is placed in one, control oven temperature and slowly reach trolamine point of ignition, make trolamine ignition and discharge a large amount of gas, obtaining fluffy nano belt initial sample;
(3) the nano belt initial sample of getting step (2) packs ceramic boat into, is placed in tube furnace central authorities; By another ceramic boat, fill with again the mixture of sublimed sulphur, selenium powder or sublimed sulphur and selenium powder, be placed in tube furnace inlet mouth one side, after emptying air, pass into the mixed gas that the hydrogen of 92 ~ 97% nitrogen and 3 ~ 8% forms, 600 ℃ of annealing three hours.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1876757A (en) * | 2006-07-20 | 2006-12-13 | 长春理工大学 | Low temperature combustion synthesis method for converting luminescent material of sulfide |
| CN101880052A (en) * | 2010-06-28 | 2010-11-10 | 暨南大学 | Preparation method of nanoscale lanthanum oxide |
| CN102971254A (en) * | 2010-07-02 | 2013-03-13 | 尤米科尔公司 | Selenide powders and manufacturing process |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1876757A (en) * | 2006-07-20 | 2006-12-13 | 长春理工大学 | Low temperature combustion synthesis method for converting luminescent material of sulfide |
| CN101880052A (en) * | 2010-06-28 | 2010-11-10 | 暨南大学 | Preparation method of nanoscale lanthanum oxide |
| CN102971254A (en) * | 2010-07-02 | 2013-03-13 | 尤米科尔公司 | Selenide powders and manufacturing process |
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Application publication date: 20140226 |