CN102807841B - Method for preparing aluminum nitride/graphene nanometer compound material - Google Patents
Method for preparing aluminum nitride/graphene nanometer compound material Download PDFInfo
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- CN102807841B CN102807841B CN201210298812.XA CN201210298812A CN102807841B CN 102807841 B CN102807841 B CN 102807841B CN 201210298812 A CN201210298812 A CN 201210298812A CN 102807841 B CN102807841 B CN 102807841B
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Abstract
The invention discloses a method for preparing an aluminum nitride/graphene nanometer compound material. The method comprises the steps as follows: dissolving urea in absolute ethanol to prepare into a urea-ethanol solution; ultrasonically processing a graphene dispersion solution for 30-120 min, adding into the urea-ethanol solution, and stirring for 20-60 min at the temperature of 60-80 DEG C; dissolving an aluminum chloride salt in the absolute ethanol to prepare into an aluminum salt-ethanol solution, dropwise adding the aluminum salt-ethanol solution into a graphene-urea mixed solution while stirring at the temperature of 70-80 DEG C, and stirring for 15-60 min; carrying out suction filtration and drying on the product; placing the dried product into an atmosphere protection tube type furnace, filling nitrogen, heating to be 850-1000 DEG C at a speed of 1-5 DEG C/min, insulating for 3-10 min, and cooling to be room temperature under the protection of the nitrogen so as to obtain the aluminum nitride/graphene nanometer compound material, wherein the grain size of the aluminum nitride is 10-50 nm. The method has the advantages of simple process, short preparation cycle, low requirement on production equipment, low energy consumption and the like.
Description
Technical field
The invention belongs to inorganic nano composite material field, be specifically related to a kind of method of preparing nitride aluminum/graphite alkene nano composite material.
Background technology
Graphene is the carbon material by the former molecular bi-dimensional cellular shape crystalline network of monolayer carbon, and it has very large specific surface area, higher Young's modulus and unique electric heating property, and wherein thermal conductivity can reach 5000W/ (mK).The performance that these are excellent and special two-dirnentional structure make Graphene become study hotspot in recent years, obtain broad research at electron device, matrix material, stored energy and biomedical sector.
Wherein graphene composite material receives much attention, and at present common is that graphene composite material mostly is the compound acquisitions such as Graphene and metal oxide, metallics, high molecular polymer.About the preparation method of the matrix material of nitride and Graphene, the Graphene and the titanium nitride composite material that have Wen to be reported at Advanced Materials 2011 (23) 5445-5450 of open report at present, preparation method is at graphene oxide surface coverage C3N4 polymeric coating, the solution of C3N4/ graphene composite material being put into source metal carries out particle absorption, then product is carried out to anneal obtains nitride and graphene composite material.CN102332567A graphene/chromium nitride nano-composite material and preparation method thereof of openly knowing clearly: add chromium nitrate urea title complex in graphene suspension; obtain chromic oxide/graphene composite material, chromic oxide/Graphene is carried out to nitrogen protective sintering and obtain graphene/chromium nitride nano-composite material.This kind of method will be through chromium peroxide/Graphene intermediate product, if chromic oxide transforms not exclusively to chromium nitride, the graphene/chromium nitride nano-composite material purity obtaining is not high, still can contain chromic oxide.
Summary of the invention
For above-mentioned prior art, the invention provides a kind of method of preparing nitride aluminum/graphite alkene nano composite material, the feature have directly, succinct, nitride aluminum/graphite alkene nano composite material is prepared in low consumption.
In order to solve the problems of the technologies described above, the method that the present invention prepares nitride aluminum/graphite alkene nano composite material comprises the following steps:
Step 1, urea is dissolved in dehydrated alcohol, is mixed with 0.8 ~ 2.4mol/L urea ethanolic soln;
Step 2, by after ultrasonic graphene dispersing solution 30 ~ 120 minutes, join the urea ethanol being obtained by step 1 molten in, at 60 ~ 80 DEG C of temperature, stir 20 ~ 60 minutes;
Step 3, aluminum chloride salt is dissolved in dehydrated alcohol, be mixed with 0.4 ~ 0.8mol/L aluminium salt ethanolic soln, at 70 ~ 80 DEG C of temperature, while stirring aluminium salt ethanolic soln is added drop-wise in the Graphene urea mixing solutions that step 2 obtains, in aluminium salt ethanolic soln dropping process, can produce throw out, be added dropwise to complete rear stirring 15 ~ 60 minutes;
Step 4, throw out is carried out to suction filtration, be placed in 60 ~ 150 DEG C of vacuum drying ovens dry 5 ~ 15 hours;
Step 5, dried product is put into atmosphere protection tube furnace, pass into nitrogen, be warming up to 850～1000 DEG C with 1 ~ 5 DEG C/min; be incubated 3 ~ 10 hours, under nitrogen protection, be cooled to room temperature, obtain nitride aluminum/graphite alkene nano composite material; wherein, the grain-size of aluminium nitride is 10 ~ 50nm.
The present invention prepares nitride aluminum/graphite alkene nano composite material, and by weight percentage, aluminium nitride content is 99.5 ~ 99.9wt%, and Graphene content is 0.1 ~ 0.5wt%.
Wherein, the thickness of Graphene is 0.8 ~ 5nm, and diameter is 0.5 ~ 2 μ m.Aluminum chloride salt is Aluminum Chloride Hexahydrate salt.
Compared with prior art, the invention has the beneficial effects as follows: preparation method of the present invention has that technique is simple, preparation cycle is short,, low power consumption and other advantages low to production unit requirement.
Brief description of the drawings:
Fig. 1 is nitride aluminum/graphite alkene nano composite material scanning electron microscope (SEM) picture in embodiment 1, aluminum nitride grain is of a size of 10-50nm as can be seen from the picture, can see that Graphene is connected between aluminum nitride grain, what circle marked is Graphene;
Fig. 2 is nitride aluminum/graphite alkene nano composite material transmission electron microscope (TEM) picture in embodiment 1, and aluminum nitride grain is distributed on Graphene as we can see from the figure;
Fig. 3 is nitride aluminum/graphite alkene nano composite material X-ray diffraction (XRD) picture in embodiment 1, can see the diffraction peak of obvious aluminium nitride and Graphene from picture.
Embodiment
The present invention prepares the method for nitride aluminum/graphite alkene nano composite material, comprises the following steps:
Step 1, urea is dissolved in dehydrated alcohol, is mixed with 0.8 ~ 2.4mol/L urea ethanolic soln;
Step 2, by after ultrasonic graphene dispersing solution 30～120 minutes, join the urea ethanol being obtained by step 1 molten in, at 60 ~ 80 DEG C of temperature, stir 20 ~ 60 minutes;
Step 3, aluminum chloride salt is dissolved in dehydrated alcohol, be mixed with 0.4 ~ 0.8mol/L aluminium salt ethanolic soln, at 70 ~ 80 DEG C of temperature, while stirring aluminium salt ethanolic soln is added drop-wise in the Graphene urea mixing solutions that step 2 obtains, in aluminium salt ethanolic soln dropping process, can produce throw out, be added dropwise to complete rear stirring 15 ~ 60 minutes;
Step 4, throw out is carried out to suction filtration, be placed in 60～150 DEG C of vacuum drying ovens dry 5 ~ 15 hours;
Step 5, dried product is put into atmosphere protection tube furnace, pass into nitrogen, be warming up to 850～1000 DEG C with 1 ~ 5 DEG C/min; be incubated 3 ~ 10 hours, under nitrogen protection, be cooled to room temperature, obtain nitride aluminum/graphite alkene nano composite material; wherein, the grain-size of aluminium nitride is 10 ~ 50nm.
The nitride aluminum/graphite alkene nano composite material of utilizing above-mentioned preparation method to obtain, by weight percentage, aluminium nitride content is 99.5 ~ 99.9wt%, Graphene content is 0.1 ~ 0.5wt%.The thickness of Graphene is 0.8 ~ 5nm, and diameter is 0.5 ~ 2 μ m.Aluminum chloride salt is Aluminum Chloride Hexahydrate salt.
Tell about by the following examples detailed process of the present invention, it is the convenience in order to understand that embodiment is provided, and is never restriction the present invention.
Embodiment 1
Take 7.2g urea and be dissolved in 100ml dehydrated alcohol, by after ultrasonic 0.2mg/ml graphene dispersing solution 60 minutes, join in urea ethanolic soln, add-on is 5ml, at 70 DEG C of temperature, stirs 30 minutes; Take 4.82g aluminum chloride salt and be dissolved in 50ml dehydrated alcohol, at 76 DEG C of temperature, be added drop-wise to while stirring in Graphene urea mixing solutions, be added dropwise to complete rear stirring 30 minutes; The product obtaining is carried out to suction filtration, be placed in 80 DEG C of vacuum drying ovens dry 5 hours; Dried matrix material is put into atmosphere protection tube furnace, pass into nitrogen, be warming up to 1000 DEG C with 5 DEG C/min, be incubated 5 hours, under nitrogen protection, be cooled to room temperature, obtain nitride aluminum/graphite alkene nano composite material.The nitride aluminum/graphite alkene nano composite material that embodiment 1 obtains, by weight percentage, aluminium nitride content is 99.5wt%, Graphene content is 0.5wt%.
Fig. 1 is nitride aluminum/graphite alkene nano composite material scanning electron microscope (SEM) picture in embodiment 1, aluminum nitride grain is of a size of 10-50nm as can be seen from the picture, can see that Graphene is connected between aluminum nitride grain, what circle marked is Graphene, the thickness of Graphene is 3-5nm, and diameter is 1 μ m.Fig. 2 is nitride aluminum/graphite alkene nano composite material transmission electron microscope (TEM) picture in embodiment 1, and aluminum nitride grain is distributed on Graphene as we can see from the figure; Fig. 3 is nitride aluminum/graphite alkene nano composite material X-ray diffraction (XRD) picture in embodiment 1, can see the diffraction peak of obvious aluminium nitride and Graphene from picture.
Embodiment 2
Take 7.2g urea and be dissolved in 100ml dehydrated alcohol, by after ultrasonic 0.2mg/ml graphene dispersing solution 60 minutes, join in urea ethanolic soln, add-on is 3ml, at 70 DEG C of temperature, stirs 30 minutes; Take 4.82g aluminum chloride salt and be dissolved in 50ml dehydrated alcohol, at 76 DEG C of temperature, be added drop-wise to while stirring in Graphene urea mixing solutions, be added dropwise to complete rear stirring 30 minutes; The product obtaining is carried out to suction filtration, be placed in 80 DEG C of vacuum drying ovens dry 5 hours; Dried matrix material is put into atmosphere protection tube furnace; pass into nitrogen; be warming up to 1000 DEG C with 5 DEG C/min, be incubated 5 hours, under nitrogen protection, be cooled to room temperature; obtain nitride aluminum/graphite alkene nano composite material; wherein, aluminum nitride grain is of a size of 30nm, by weight percentage; aluminium nitride content is 99.7wt%, and Graphene content is 0.3wt%.
Embodiment 3
Take 10.8g urea and be dissolved in 100ml dehydrated alcohol, by after ultrasonic 0.2mg/ml graphene dispersing solution 60 minutes, join in urea ethanolic soln, add-on is 5ml, at 70 DEG C of temperature, stirs 30 minutes; Take 4.82g aluminum chloride salt and be dissolved in 50ml dehydrated alcohol, at 76 DEG C of temperature, be added drop-wise to while stirring in Graphene urea mixing solutions, be added dropwise to complete rear stirring 30 minutes; The product obtaining is carried out to suction filtration, be placed in 80 DEG C of vacuum drying ovens dry 5 hours; Dried matrix material is put into atmosphere protection tube furnace; pass into nitrogen; be warming up to 1000 DEG C with 5 DEG C/min, be incubated 5 hours, under nitrogen protection, be cooled to room temperature; obtain nitride aluminum/graphite alkene nano composite material; wherein, aluminum nitride grain is of a size of 50nm, by weight percentage; aluminium nitride content is 99.5wt%, and Graphene content is 0.5wt%.
Although in conjunction with figure, invention has been described above; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment is only schematic; instead of restrictive; those of ordinary skill in the art is under enlightenment of the present invention; in the situation that not departing from aim of the present invention, can also make a lot of distortion, within these all belong to protection of the present invention.
Claims (4)
1. a method of preparing nitride aluminum/graphite alkene nano composite material, is characterized in that: comprise the following steps:
Step 1, urea is dissolved in dehydrated alcohol, is mixed with 0.8～2.4mol/L urea ethanolic soln;
Step 2, by after ultrasonic graphene dispersing solution 30～120 minutes, join in the urea ethanolic soln being obtained by step 1, at 60～80 DEG C of temperature, stir 20～60 minutes;
Step 3, aluminum chloride salt is dissolved in dehydrated alcohol, be mixed with 0.4～0.8mol/L aluminium salt ethanolic soln, at 70～80 DEG C of temperature, while stirring aluminium salt ethanolic soln is added drop-wise in the Graphene urea mixing solutions that step 2 obtains, in aluminium salt ethanolic soln dropping process, can produce throw out, be added dropwise to complete rear stirring 15～60 minutes;
Step 4, throw out is carried out to suction filtration, be placed in 60～150 DEG C of vacuum drying ovens dry 5～15 hours;
Step 5, dried product is put into atmosphere protection tube furnace; pass into nitrogen; be warming up to 850～1000 DEG C with 1～5 DEG C/min; be incubated 3～10 hours; under nitrogen protection, be cooled to room temperature; obtain nitride aluminum/graphite alkene nano composite material, wherein, the grain-size of aluminium nitride is 10～50nm.
2. prepare according to claim 1 the method for nitride aluminum/graphite alkene nano composite material, it is characterized in that, obtain nitride aluminum/graphite alkene nano composite material, by weight percentage, aluminium nitride content is 99.5～99.9wt%, and Graphene content is 0.1～0.5wt%.
3. the method for preparing according to claim 1 nitride aluminum/graphite alkene nano composite material, is characterized in that, the thickness of Graphene is 0.8～5nm, and diameter is 0.5～2 μ m.
4. the method for preparing according to claim 1 nitride aluminum/graphite alkene nano composite material, is characterized in that, aluminum chloride salt is Aluminum Chloride Hexahydrate salt.
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| CN104229759B (en) * | 2014-09-09 | 2016-05-04 | 华中科技大学 | Grapheme tube coated metal nitride nano band and preparation method thereof |
| CN105413674A (en) * | 2015-11-30 | 2016-03-23 | 安徽省元琛环保科技有限公司 | Preparation method of denitration catalyst carrier with graphene |
| CN111732084B (en) * | 2020-06-23 | 2021-11-09 | 济南大学 | Method for preparing porous aluminum nitride supercapacitor material by utilizing two-dimensional carbon nitride template growth |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774575A (en) * | 2010-02-10 | 2010-07-14 | 中国科学院上海硅酸盐研究所 | Method for repairing oxidized graphene by organic matter containing amino group at low temperature |
| CN102167310A (en) * | 2011-01-30 | 2011-08-31 | 黑龙江大学 | Method for preparing nitrogen-doped graphene material with hydrothermal process |
| CN102332567A (en) * | 2011-08-15 | 2012-01-25 | 黑龙江科技学院 | Graphene/chromium nitride nano-composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101774575A (en) * | 2010-02-10 | 2010-07-14 | 中国科学院上海硅酸盐研究所 | Method for repairing oxidized graphene by organic matter containing amino group at low temperature |
| CN102167310A (en) * | 2011-01-30 | 2011-08-31 | 黑龙江大学 | Method for preparing nitrogen-doped graphene material with hydrothermal process |
| CN102332567A (en) * | 2011-08-15 | 2012-01-25 | 黑龙江科技学院 | Graphene/chromium nitride nano-composite material and preparation method thereof |
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