CN104528686B - A kind of preparation method of Fluorin doped spiral carbon nanotubes - Google Patents
A kind of preparation method of Fluorin doped spiral carbon nanotubes Download PDFInfo
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- CN104528686B CN104528686B CN201410825814.9A CN201410825814A CN104528686B CN 104528686 B CN104528686 B CN 104528686B CN 201410825814 A CN201410825814 A CN 201410825814A CN 104528686 B CN104528686 B CN 104528686B
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Abstract
The invention discloses the preparation method of a kind of Fluorin doped spiral carbon nanotubes.First preparing the oxide nano particles of nickel with sol-gal process, be then reduced to nano nickel particles and as catalyst Pintsch process acetylene using hydrogen, product and xenon difluoride react the spiral carbon nanotubes obtaining fluorination.The raw material of sol-gal process selects Nickelous nitrate hexahydrate, monohydrate potassium, and dehydrated alcohol selected by solvent.The luminescence generated by light of the Fluorin doped spiral carbon nanotubes of the present invention is promoted to 263nm and 291nm deep ultraviolet region, greatly fill up the existing semi-conducting material deficiency in this region, photoetching technique, optical information storage and pharmaceutical analysis field can be applied to as ultra-violet light-emitting, the basic material of ultraviolet detector.
Description
Technical field
The invention belongs to carbon nanotube preparation technology field, preparation method particularly to a kind of Fluorin doped spiral carbon nanotubes with DUV Photoluminescence Properties, this CNT can be used in ultra-violet light-emitting material and stores and the application of pharmaceutical analysis at photoetching technique, optical information, additionally can also be used to the basic material of ultra-violet light-emitting, ultraviolet detector.
Background technology
Spiral carbon nanotubes (HCNTs), since within 1994, being found, with the physics of its excellence and chemical property and wide application prospect, has just caused researchers and has paid close attention to greatly.It is periodically insert in the hexatomic ring network of the CNT of straight-bar five-membered ring and heptatomic ring to and the Helix-shaped Carbon Nanotubes of a kind of spring-like shape that constitutes.The helical structure of its uniqueness determines it and all has the character of uniqueness at aspects such as optics, electricity, magnetics, microwave absorption, mechanics and chemistry, has the biggest theoretical research and potential using value.Especially, spiral carbon nanotubes has stronger luminescence generated by light (PL) effect at the ultraviolet region of 368nm, and the N doping of pyrimidine Type and graphite mould can effectively strengthen its ultraviolet photoluminescence performance.But it is intended to that there is deeper ultra-violet (UV) band photoluminescence property (emission wavelength is less than 300 nm), and then has the spiral carbon nanotubes material of the deep-UV light-emitting characteristic less than 300nm have not been reported.
On the other hand, it was noticed that be the extremely effective method of one widening material with carbon element energy band band gap by fluorination.Such as, Graphene be a kind of can band band gap be the material with carbon element of zero, perfluorinated after, its band gap is up to 3.8eV, thus is expected to have good photoluminescence property at DUV region (3.8eV, corresponding to ultraviolet photoluminescence wavelength ~ 327nm).Thus, we are by being fluorinated spiral carbon nanotubes, it is thus achieved that have the fluorination spiral carbon nanotubes (F-HCNT) of good photoluminescence performance in 263nm and 291nm deep ultraviolet region.It will have the ultraviolet laser of minimum wavelength to manufacture, and the pharmaceutical analysis with deep-UV light-emitting characteristic has a good application prospect.
Summary of the invention
The preparation method that a kind of Fluorin doped spiral carbon nanotubes with DUV Photoluminescence Properties is provided of the purpose of the present invention.
Concretely comprise the following steps:
(1) 0.01mol Nickelous nitrate hexahydrate and 0.03mol monohydrate potassium are added in the conical flask filling 100ml dehydrated alcohol, heating in water bath is to 60 DEG C and stirs, proceed in beaker after keeping 8 hours, after it is dried by 85 DEG C substantially, then at 175 DEG C, it is dried completely, finally put it in Muffle furnace 375 DEG C to calcine 4 hours, prepare nickel oxide nanoparticle.
(2) nickel oxide nanoparticle weighing 0.025 gram of step (1) prepared puts into tube furnace in porcelain boat; it is passed through hydrogen post-heating with the flow of 20ml/min and to 365 DEG C and keeps 1 hour prepared nano nickel particles; it is then shut off hydrogen; it is passed through acetylene with the flow of 40ml/min again and is heated to 550 ± 50 DEG C of holdings 1 hour; finally close acetylene and be passed through argon; protection at argon drops to room temperature, prepares spiral carbon nanotubes.
(3) spiral carbon nanotubes and xenon difluoride step (2) prepared is weighed by the mass ratio of 1:1 ~ 10 and mixes, put into polytetrafluoroethyltank tank, the most airtight, polytetrafluoroethyltank tank is put into stainless cylinder of steel again, with plumbing combination pliers, the lid of stainless cylinder of steel is tightened sealing, stainless cylinder of steel is put into Muffle furnace again be heated to 200 ± 20 DEG C and keep 30 ~ 72 hours, after finally naturally cooling to room temperature, i.e. prepare Fluorin doped spiral carbon nanotubes.
Described raw material Nickelous nitrate hexahydrate, monohydrate potassium and dehydrated alcohol are analytical pure；Acetylene is technical pure；Argon and xenon difluoride are chemical pure.
The standard that the lid of described stainless cylinder of steel is tightened is after jar naturally cools to room temperature, and stainless cylinder of steel does not loosen or the phenomenon of gas leakage.
The invention have the advantage that
(1) the inventive method production cost is relatively low, it is easy to processing, raw material sources are extensive.
(2) luminescence generated by light of the Fluorin doped spiral carbon nanotubes that the inventive method prepares is promoted to 263nm and 291nm deep ultraviolet region, has greatly filled up the existing semi-conducting material deficiency in this region.
Accompanying drawing explanation
Fig. 1 is the high definition stereoscan photograph of F-HCNT-1 in embodiment 1.We are it is found that Fluorin doped spiral carbon nanotubes is highly uniform, and diameter is about between 80 ~ 160nm, and length is all more than 6 μm, and is not neat linear array, but bends in various degrees and be intertwined.
Fig. 2 is embodiment 1 4(F-HCNT-1 4) electron spectrum (XPS).We are it is found that along with spiral carbon nanotubes is different from the mixed proportion of xenon difluoride, the Oil repellent of incorporation is very different.The proportion of xenon difluoride is the biggest, and it is the most that corresponding fluorine mixes.
Fig. 3 is embodiment 1 4(F-HCNT-1 4) photoluminescence spectrum.We it appeared that, although in Fluorin doped spiral carbon nanotubes, the content of fluorine changes, and it can keep stable in the photoluminescence property of 263nm and 291nm deep ultraviolet.
Detailed description of the invention
Using raw material Nickelous nitrate hexahydrate, monohydrate potassium and dehydrated alcohol in following example is analytical pure；Acetylene is technical pure；Argon and xenon difluoride are chemical pure.
Embodiment
1
:
(1) 0.01mol Nickelous nitrate hexahydrate and 0.03mol monohydrate potassium are added in the conical flask filling 100ml dehydrated alcohol, heating in water bath is to 60 DEG C and stirs, proceed in beaker after keeping 8 hours, after it is dried by 85 DEG C substantially, then at 175 DEG C, it is dried completely, finally put it in Muffle furnace 375 DEG C to calcine 4 hours, prepare nickel oxide nanoparticle.
(2) nickel oxide nanoparticle weighing 0.025 gram of step (1) prepared puts into the tube furnace that caliber is 50mm in porcelain boat; the hydrogen post-heating being passed through 20ml/min flow to 365 DEG C and keeps 1 hour; it is then shut off hydrogen to be passed through acetylene (flow is 40ml/min) and be heated to 550 DEG C and keep 1 hour; finally close acetylene and be passed through argon; protection at argon drops to room temperature, prepares spiral carbon nanotubes.
(3) spiral carbon nanotubes and xenon difluoride step (2) prepared is weighed by the mass ratio of 1:10 and mixes, put into polytetrafluoroethyltank tank, the most airtight, polytetrafluoroethyltank tank is put into stainless cylinder of steel again, sealing is tightened with plumbing combination pliers, stainless cylinder of steel is put into Muffle furnace again be heated to 200 DEG C and keep 30 hours, after finally naturally cooling to room temperature, i.e. prepare Fluorin doped spiral carbon nanotubes F-HCNT-1.
Embodiment
2
:
Changing the mixing quality ratio of the spiral carbon nanotubes in embodiment 1 step (3) with xenon difluoride into 1:7, other conditions are substantially identical to embodiment 1, prepare Fluorin doped spiral carbon nanotubes F-HCNT-2.
Embodiment
3
:
Changing the mixing quality ratio of the spiral carbon nanotubes in embodiment 1 step (3) with xenon difluoride into 1:5, other conditions are substantially identical to embodiment 1, prepare Fluorin doped spiral carbon nanotubes F-HCNT-3.
Embodiment
4
:
Changing the mixing quality ratio of the spiral carbon nanotubes in embodiment 1 step (3) with xenon difluoride into 1:1, other conditions are substantially identical to embodiment 1, prepare Fluorin doped spiral carbon nanotubes F-HCNT-3.
Although prior art scheme of the present invention and preferred embodiment are stated as above, so it is not limited to the present invention.Persond having ordinary knowledge in the technical field of the present invention, without departing from the spirit and scope of the present invention, when making various change, substitute and retouching.Therefore, protection scope of the present invention is when being as the criterion depending on those as defined in claim.
Claims (1)
1. the preparation method of a Fluorin doped spiral carbon nanotubes, it is characterised in that concretely comprise the following steps:
(1) 0.01mol Nickelous nitrate hexahydrate and 0.03mol monohydrate potassium are added in the conical flask filling 100ml dehydrated alcohol, heating in water bath is to 60 DEG C and stirs, proceed in beaker after keeping 8 hours, after it is dried by 85 DEG C substantially, then at 175 DEG C, it is dried completely, finally put it in Muffle furnace 375 DEG C to calcine 4 hours, prepare nickel oxide nanoparticle；
(2) nickel oxide nanoparticle weighing 0.025 gram of step (1) prepared puts into tube furnace in porcelain boat; it is passed through hydrogen post-heating with the flow of 20ml/min and to 365 DEG C and keeps 1 hour prepared nano nickel particles; it is then shut off hydrogen; it is passed through acetylene with the flow of 40ml/min again and is heated to 550 ± 50 DEG C of holdings 1 hour; finally close acetylene and be passed through argon; protection at argon drops to room temperature, prepares spiral carbon nanotubes；
(3) spiral carbon nanotubes and xenon difluoride step (2) prepared is weighed by the mass ratio of 1:1 ~ 10 and mixes, put into polytetrafluoroethyltank tank, the most airtight, polytetrafluoroethyltank tank is put into stainless cylinder of steel again, with plumbing combination pliers, the lid of stainless cylinder of steel is tightened sealing, stainless cylinder of steel is put into Muffle furnace again be heated to 200 ± 20 DEG C and keep 30 ~ 72 hours, after finally naturally cooling to room temperature, i.e. prepare Fluorin doped spiral carbon nanotubes；
Described raw material Nickelous nitrate hexahydrate, monohydrate potassium and dehydrated alcohol are analytical pure；Acetylene is technical pure；Argon and xenon difluoride are chemical pure；
The standard that the lid of described stainless cylinder of steel is tightened is after jar naturally cools to room temperature, and stainless cylinder of steel does not loosen or the phenomenon of gas leakage.
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| CN110233262B (en) * | 2019-07-03 | 2021-05-18 | 桑顿新能源科技(长沙)有限公司 | Halogen element O-site doped nickel oxide and preparation method thereof, target material, thin film material, lithium battery cathode, lithium battery and electric equipment |
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