CN102897851B - A kind of method preparing nickel, cobalt and oxide nano structure thereof based on diffusional limitation cohesion (DLA) principle - Google Patents
A kind of method preparing nickel, cobalt and oxide nano structure thereof based on diffusional limitation cohesion (DLA) principle Download PDFInfo
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- CN102897851B CN102897851B CN201210176695.XA CN201210176695A CN102897851B CN 102897851 B CN102897851 B CN 102897851B CN 201210176695 A CN201210176695 A CN 201210176695A CN 102897851 B CN102897851 B CN 102897851B
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Abstract
The present invention relates to a kind of based on diffusional limitation cohesion (Diffusion-limited? Aggregation, DLA) principle, prepare the method for transiting metal nickel, cobalt and oxide nano structure thereof, belong to technical field of nano material.Its main process is: using the tinsel of nickel, cobalt as reaction source, is placed on and fills up in sodium-chlor quartz container, and heat container.When temperature reaches more than 1000 DEG C, sodium-chlor becomes molten state.Because chlorion has stronger corrodibility, metallic nickel, cobalt are corroded and produce the metal ion of nickel, cobalt, and diffuse out.When metal ion reaches certain concentration, take diffusion as primary growth power, be gathered in tinsel surface one by one according to self-assembly mode, thus form the metal Nano structure of nickel, cobalt.In reaction process, pass into appropriate oxygen, then oxidizing reaction occurs.Finally form the nanostructure of nickel, cobalt/cobalt oxide.
Description
Technical field
The present invention relates to a kind of method preparing nickel, cobalt and oxide nano structure thereof based on diffusional limitation cohesion (DLA) principle, belong to technical field of nano material.
Background technology
Transition metal Ni, Co and oxide-based nanomaterial thereof have specific physical properties, at solar cell, have important application prospect in the photoelectric devices such as detector.The existing method preparing metal oxide nano-wire array is mainly chemical gaseous phase depositing process, is realized the preparation of metal oxide nano-wire array by growth mechanisms such as VLS (solid-liquid-gas) or VS (Gu-gas).Its key step is: 1. in growth substrates gold evaporation film as catalyzer; 2. oxide compound and carbon dust are carried out mixing as reaction source by a certain percentage; 3. reaction source and substrate are together put into vacuum tube furnace, rare gas element is passed into valve tube or carries out vacuum-treat, remove plugged vents; 4. tube furnace heats up, and passes into O by a certain percentage
2/ Ar mixed gas, as oxygen source, carries out carbothermic reduction reaction, obtains oxidate nano linear array after reaction terminates.
But not there is preferential growth characteristic due to this quasi-metal oxides, its growth does not have fixed orientation, cannot form VLS or VS growth mechanism, thus cannot generate the nano-wire array of this quasi-metal oxides.Therefore chemical gaseous phase depositing process is not suitable for the preparation of Ni, Co and oxide nano thread thereof.
Summary of the invention
For Problems existing in technical background, the present invention proposes a kind of method preparing nickel, cobalt and oxide nano structure thereof based on diffusional limitation cohesion (DLA) principle, the method is simple, can be prepared for the nanostructure of transition metal and oxide compound thereof.
Concrete steps of the present invention are:
Using the tinsel of nickel, cobalt as reaction source, be placed on and fill up in sodium-chlor quartz container, and container is heated.When temperature reaches more than 1000 DEG C, sodium-chlor becomes molten state.Because chlorion has stronger corrodibility, metallic nickel, cobalt are corroded and produce the metal ion of nickel, cobalt, and diffuse out.When metal ion reaches certain concentration, take diffusion as primary growth power, be gathered in tinsel surface one by one according to self-assembly mode, thus form the metal Nano structure of nickel, cobalt.In reaction process, pass into appropriate oxygen, then oxidizing reaction occurs.Finally form the nanostructure of nickel, cobalt/cobalt oxide.
Its technique effect of the present invention is, compares the method that the tradition such as chemical vapour deposition prepare nano material, the features such as present method without particular requirement, has simple to operate to substrate, reaction source and reaction carrier gas, reproducible.
Accompanying drawing explanation
Fig. 1 is the SEM image that embodiment one obtains, the SEM image of nano-nickel oxide.Fig. 2 is the XRD diffractogram that example one obtains, the diffraction peak of the corresponding nickel oxide of asterisk mark; The diffraction peak of the corresponding nickel of round dot.Fig. 3 is the SEM image that embodiment two obtains, and it is the SEM image of transition metal oxide NiO, and passing into the per-cent that amount of oxygen accounts for mixed gas is 5%.Fig. 3 doubles as Figure of abstract.
Embodiment
Embodiment one:
The equipment adopted is tube furnace, and the device of employing is valve tube and inlet pipe, valve tube Choice of Quartz Tube Diameters.NaCl powder is put into quartz boat, transition metal sheet cobalt sheet or nickel sheet are ridden on boat, directly over powder.This boat is put into valve tube, valve tube is put into tube furnace.Valve tube one end is connected with inlet pipe, and the other end is connected with vacuum pump.Vacuum pump adopts mechanical pump.Start vacuum pump and pass into Ar gas cleaning inlet pipe and vacuum pipe inner cavity from inlet pipe.Then by vacuum pump, valve tube is evacuated to 1 × 10
-2mbar, tube furnace intensification heating, vacuum pipe to 1000 DEG C.Now, sodium-chlor becomes steam by pressed powder, there is Na in reaction chamber
+and Cl
-because chlorion has stronger corrodibility, metallic nickel, cobalt are corroded, generate transition metal ion, when metal ion reaches certain concentration, take diffusion as primary growth power, be gathered in metal substrate surface one by one according to self-assembly mode, thus form the metal Nano structure of nickel, cobalt.If when tube furnace is warming up to 500 ~ 700 DEG C, pass into Ar gas and O
2the mixed gas of gas, O
2account for 0.5% of mixed gas volume, gas flow is 100sccm.Transition metal ion is combined with oxygen, transition metal oxide layer is generated at transition metal substrate surface, chlorion spreads downwards through the transition metal oxide layer on transition metal substrate surface, etching transition metal substrate, generate transition metal chloride, formed and be close to upright nano wire and be in array-like arrangement, then by O
2o in/Ar mixed gas
2be oxidized to transition metal oxide, see shown in accompanying drawing Fig. 1 and Fig. 2, complete the preparation of transition metal oxide nano linear array.
Embodiment two:
Using the tinsel of nickel, cobalt as reaction source, be placed on and fill up in sodium-chlor quartz container, and container is heated.When temperature reaches 1000 DEG C, sodium-chlor becomes molten state.Because chlorion has stronger corrodibility, metallic nickel, cobalt are corroded and produce the metal ion of nickel, cobalt, and diffuse out.When metal ion reaches certain concentration, take diffusion as primary growth power, be gathered in tinsel surface one by one according to self-assembly mode, thus form the metal Nano structure of nickel, cobalt.In reaction process, pass into O
2/ Ar mixed gas, O
2account for 5% of mixed gas volume, gas flow is 100sccm, then oxygen and transition metal ion generation oxidizing reaction.Finally form the nanostructure of transition metal oxide.See shown in accompanying drawing Fig. 3.
Claims (3)
1. prepare a method for nickel, cobalt and oxide nano structure thereof based on diffusional limitation cohesion (DLA) principle, concrete implementation step is:
The equipment adopted is tube furnace, the device adopted is valve tube and inlet pipe, valve tube Choice of Quartz Tube Diameters, NaCl powder is put into quartz boat, transition metal sheet cobalt sheet or nickel sheet are ridden on boat, directly over powder, this boat is put into valve tube, valve tube is put into tube furnace, valve tube one end is connected with inlet pipe, and the other end is connected with vacuum pump, and vacuum pump adopts mechanical pump, start vacuum pump and pass into Ar gas cleaning inlet pipe and vacuum pipe inner cavity from inlet pipe, then by vacuum pump, valve tube is evacuated to 1 × 10
-2mbar, tube furnace intensification heating, vacuum pipe to 1000 DEG C, now, sodium-chlor becomes steam by pressed powder, there is Na in reaction chamber
+and Cl
-because chlorion has stronger corrodibility, metallic nickel, cobalt are corroded, generate transition metal ion, when metal ion reaches certain concentration, take diffusion as primary growth power, be gathered in metal substrate surface one by one according to self-assembly mode, thus form the metal Nano structure of nickel, cobalt; If when tube furnace is warming up to 500 ~ 700 DEG C, pass into Ar gas and O
2the mixed gas of gas, O
2account for 0.5% of mixed gas volume, gas flow is 100sccm, transition metal ion is combined with oxygen, transition metal oxide layer is generated at transition metal substrate surface, chlorion spreads downwards through the transition metal oxide layer on transition metal substrate surface, and etching transition metal substrate, generates transition metal chloride, formed and be close to upright nano wire and be in array-like arrangement, then by O
2o in/Ar mixed gas
2be oxidized to transition metal oxide, complete the preparation of transition metal oxide nano linear array.
2. one according to claim 1 prepares the method for nickel, cobalt and oxide nano structure thereof based on diffusional limitation cohesion (DLA) principle, it is characterized in that, described transition metal is Ni or Co, and described transition metal oxide is NiO or CoO.
3. one according to claim 1 prepares the method for nickel, cobalt and oxide nano structure thereof based on diffusional limitation cohesion (DLA) principle, it is characterized in that, using the tinsel of sodium-chlor and transiting metal nickel, cobalt as reaction source, when not passing into oxygen, form the nanostructure of transition metal, after passing into oxygen, then form the nanostructure of transition metal oxide.
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| CN101956181A (en) * | 2010-06-30 | 2011-01-26 | 长春理工大学 | Preparation method of transition metal nickel oxide and cobalt oxide nanowire array |
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Inventor after: Gao Xian Inventor after: Fang Dan Inventor after: Wang Fei Inventor after: Chen Xinying Inventor after: Fang Xuan Inventor after: Wei Zhipeng Inventor after: Fang Fang Inventor after: Li Jinhua Inventor after: Chu Xueying Inventor after: Wang Xiaohua Inventor after: Tang Jilong Inventor before: Fang Xuan Inventor before: Chen Xinying Inventor before: Wei Zhipeng Inventor before: Fang Fang Inventor before: Li Jinhua Inventor before: Chu Xueying Inventor before: Wang Xiaohua Inventor before: Wang Fei |
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