CN106298398A - There is preparation and the application of the situ Al doping SiC nanowire of net shape skin - Google Patents
There is preparation and the application of the situ Al doping SiC nanowire of net shape skin Download PDFInfo
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- CN106298398A CN106298398A CN201610861725.9A CN201610861725A CN106298398A CN 106298398 A CN106298398 A CN 106298398A CN 201610861725 A CN201610861725 A CN 201610861725A CN 106298398 A CN106298398 A CN 106298398A
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- 239000002070 nanowire Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 16
- 239000010439 graphite Substances 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 12
- 229920003257 polycarbosilane Polymers 0.000 claims abstract description 11
- 239000000758 substrate Substances 0.000 claims abstract description 11
- 239000010406 cathode material Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 235000013312 flour Nutrition 0.000 claims abstract description 8
- 239000002086 nanomaterial Substances 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 4
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000002077 nanosphere Substances 0.000 claims abstract description 4
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 4
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 4
- 238000010792 warming Methods 0.000 claims abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- VWWHFOBVDHPEKJ-UHFFFAOYSA-N aluminum ethanol trinitrate Chemical compound C(C)O.[N+](=O)([O-])[O-].[Al+3].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] VWWHFOBVDHPEKJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 239000011812 mixed powder Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- 238000004320 controlled atmosphere Methods 0.000 claims 1
- 238000003823 mortar mixing Methods 0.000 claims 1
- 230000005684 electric field Effects 0.000 abstract description 7
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 abstract description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- 230000000877 morphologic effect Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- SICLLPHPVFCNTJ-UHFFFAOYSA-N 1,1,1',1'-tetramethyl-3,3'-spirobi[2h-indene]-5,5'-diol Chemical compound C12=CC(O)=CC=C2C(C)(C)CC11C2=CC(O)=CC=C2C(C)(C)C1 SICLLPHPVFCNTJ-UHFFFAOYSA-N 0.000 description 1
- IZMPACFDPANMBU-UHFFFAOYSA-N C(C)O.[AlH3] Chemical compound C(C)O.[AlH3] IZMPACFDPANMBU-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J1/00—Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
- H01J1/02—Main electrodes
- H01J1/30—Cold cathodes, e.g. field-emissive cathode
- H01J1/304—Field-emissive cathodes
Abstract
A kind of situ Al doping SiC nanowire with net shape skin, it is characterised in that the surface of Al doping SiC nanowire be one layer by SiO2Nanosphere couples the network nano structure that Al doping SiC nanowire is constituted, and its preparation method specifically includes that with Polycarbosilane, silica flour and aluminum nitrate as reaction raw materials, and nickel nitrate is catalyst；Graphite substrate by the reaction raw materials after mixed grinding with catalyst is placed in graphite reative cell, puts into vacuum atmosphere oven；Logical Ar gas, is evacuated to 50～80Pa, is warming up to 1350～1450 DEG C with the heating rate of 15 DEG C/min, is incubated 60～90min.The situ Al doping SiC nanowire with net shape skin obtained, as filed emission cathode material, shows the lowest threshold electric field (0.5V/ μm) and threshold field (2.8V/ μm), and has high field emission stability.
Description
Technical field
The invention belongs to field of nano material preparation, relate to a kind of situ Al doping SiC nanowire with net shape skin
Preparation method and as the application of filed emission cathode material.
Background technology
SiC is a kind of important third generation semi-conducting material, and its low-dimensional nano structure is owing to having high energy gap, high
The saturated mobility of electronics and thermal conductivity, little dielectric constant and the preferable excellent specific property such as mechanical performance, at micro-nano photoelectricity
The fields such as device have a wide range of applications.In recent years, owing to SiC low-dimensional nano structure is at flat faced display and Flied emission electricity
Potential application in the fields such as sub-rifle, gradually causes the extensive concern of domestic and international research worker.In order to promote SiC low-dimensional nanometer
Structure is done a lot of work in terms of its Morphological control as the actual application of filed emission cathode material, research worker, existing many
The novel SiC nanostructured of kind and the report of field emission performance thereof, such as: Renbing Wu et al. has prepared taper SiC nanowire,
Possess good field emission characteristic, its threshold electric field be 1.2V/ μm (Wu RB, Zhou K, Wei J, Huang YZ, Su F,
Chen JJ,et al.Growth of tapered SiC nanowires on flexible carbon fabric:
toward field emission applications.J Phys Chem C 2012；116:12940–5.)；Chen Shanliang etc.
People discloses the preparation method of a kind of SiC nanoneedle, and as filed emission cathode material, its threshold electric field is 0.5～2.8V/ μm
(Chinese invention patent, application number 201510511409.4, a kind of N doping SiC nanoneedle and application thereof).It addition, by SiC
Low-dimensional nano structure carries out the atom doped research to improve its field emission performance and also achieves certain progress: this seminar uses
Chemical vapour deposition technique and gas phase doping method, be prepared for the SiC nanowire of La or N doping respectively, and its threshold electric field is respectively
1.2V/ μm and 0.9V/ μm (the .Acta Phys.-Chim.Sin.2015 such as Li Zhenjiang, Ma Fenglin, Zhang Meng, 31 (6), 1191-
1198)；Yang Weiyou et al. have studied P doping SiC nanowire and the application in filed emission cathode material (Chinese invention is special
Profit, application number 201510510679.3P adulterates SiC nanowire application in filed emission cathode material).Yang Yang et al.
It is prepared for B and N codope SiC by pyrolysis organic precursor, and obtains threshold electric field (Yang, the Y. of 1.35V/ μm；Yang,
H.；Wei,G.D.；Wang,L.；Shang,M.H.；Yang,Z.B.；Tang,B.；Yang,W.Y.J.Mater.Chem.C
2014,2,4515.)。
Research to SiC low-dimensional nano structure field emission performance at present is concentrated mainly on to be regulated and controled by single shape or element
Morphological control and element doping two ways, to improve its field emission performance, are combined by doping, are improving SiC low-dimensional nano junction
While structure field emission performance, strengthening its launch stability, this is really applied to Flied emission for realizing SiC low-dimensional nano structure
Field, significant.Therefore, the present invention has considered Morphological control and Al element doping to improving SiC low-dimensional nanometer
The synergism of structure field emission performance, synthesizes a kind of situ Al doping SiC nanowire with net shape skin, opens in reduction
While opening electric field and threshold field, also improve the stability of its Flied emission, make prepared Al doping SiC low-dimensional nano junction
Structure has more excellent field emission performance, and it can be made to send out in EED, vacuum electron device, backlight module and field
Penetrate the fields such as lighting source to have broad application prospects.
Summary of the invention
It is an object of the invention to obtain a kind of situ Al doping SiC nanowire with net shape skin, due to the net on top layer
The common effect of shape structure and Al doping makes it have the field emission performance of excellence.
The purpose of the present invention can be achieved through the following technical solutions:
1) selecting solid-state Polycarbosilane is Si source and C source, and silica flour is auxiliary Si source, by Polycarbosilane 230 DEG C of insulations
40min, carries out pre-oxidation treatment, and selecting aluminum nitrate is Al source, prepares the aluminum nitrate ethanol solution of 0.2mol/L in advance；
2) be (2～3) according to mass ratio: 1 weigh pre-oxidation treatment after Polycarbosilane and Si powder be placed in agate mortar
Mixed grinding 30～40min, then adds the aluminum nitrate ethanol solution 0.5～1.5mL prepared in advance in mixed powder, is placed in
In drying baker, 75 DEG C were dried after 2 hours, then mixing raw material is ground 40min；
3) graphite substrate after cleaning, drying, is immersed the Ni (NO of 0.01mol/L in ultrasonic washing unit3)3Ethanol solution
In, ultrasonic vibration 5 minutes, takes out nature and dries, obtain the substrate with catalyst；
4) being placed on by reaction raw material on double-deck carbon cloth, the graphite substrate with catalyst is placed in the upper of mixing raw material
Side, its spacing is 3～5mm, puts into graphite reative cell the most together, is put in vacuum atmosphere oven by graphite reative cell；
5) vacuum atmosphere oven is evacuated to 50～80Pa, with the heating rate of 15 DEG C/min furnace temperature risen to 1350～
1450 DEG C, it is incubated 60～90min, it is achieved there is the preparation of the situ Al doping SiC nanowire of net shape skin.
6) in ultrahigh vacuum Flied emission test system, mix with the situ Al with netted cover layer that step (5) obtains
Miscellaneous SiC nanowire, as negative electrode, tests its field emission performance, and the copper rod of a diameter of 3mm is anode, between regulating YIN and YANG pole away from
From for 500 μm, the size of Flied emission electric current is regulated by the size adjusting load voltage, load voltage control 0～3kV it
Between, the vacuum of ultrahigh vacuum Flied emission test system is 1.0 × 10-6～2.0 × 10–6Pa。
Compared with prior art, the present invention is advantageous in that:
1) present invention uses a step chemical gas-phase reaction method, while preparation SiC nanowire, it is achieved that Al element former
Position doping, has that technique is simple, a step completes and can the advantage such as preparation in a large number, it is easier to industrial applications；
2) what the present invention was obtained has the situ Al doping SiC nanowire of net shape skin, due to the network structure on top layer
Common effect with Al doping so that it is show low threshold electric field (0.5V/ μm) and threshold value electricity as filed emission cathode material
Field (2.8V/ μm), and there is high field emission stability, it is more beneficial for it and is applied to Flied emission field.
Accompanying drawing explanation
Below in conjunction with the accompanying drawings and embodiment the invention will be further described.
Fig. 1 is the XRD diffraction pattern of the situ Al doping SiC nanowire with net shape skin obtained by embodiment 1.
Fig. 2 is the SEM photograph of the situ Al doping SiC nanowire with net shape skin obtained by embodiment 1.
Fig. 3 is the TEM photo of the situ Al doping SiC nanowire with net shape skin obtained by embodiment 1.
Fig. 4 (a) (b) is respectively the XPS of the situ Al doping SiC nanowire with net shape skin obtained by embodiment 1
Total spectrogram and the fine spectrogram of Al 2p.
Fig. 5 is that the Flied emission electric current of the situ Al doping SiC nanowire with net shape skin obtained by embodiment 1 is close
Degree-electric field curve diagram (J-E curve), illustration is corresponding F-N curve.
Fig. 6 is the field emission stability of the situ Al doping SiC nanowire with net shape skin obtained by embodiment 1
Figure.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further detailed explanation, but these embodiments are not with any side
Formula limits the scope of the present invention.
Embodiment 1
The Polycarbosilane that molecular weight is 1000～2000 selecting the National University of Defense technology to develop is Si source and C source, and purity is
The silica flour of 99.5% is auxiliary Si source, at 230 DEG C, Polycarbosilane is incubated 40min, after carrying out pre-oxidation treatment, weighs the poly-carbon of 2g
Silane and 1g silica flour are placed in mixed grinding 30～40min in agate mortar, and selecting aluminum nitrate is Al source, the nitre of preparation 0.2mol/L
Acid aluminum ethanol solution, adds 1.5mL aluminum nitrate ethanol solution, juxtaposition in Polycarbosilane after mixed grinding and silica flour mixed powder
In drying baker, 75 DEG C are dried 2 hours, are again ground 40min, obtain mixing and answer raw material；By graphite substrate in ultrasound wave
In cleaning machine after cleaning, drying, immerse the Ni (NO of 0.01mol/L3)3In ethanol solution, ultrasonic vibration 5 minutes, takes out nature and dries in the air
Dry, obtain the substrate with catalyst；Reaction raw material grinding obtained is placed on double-deck carbon cloth, with the stone of catalyst
Ink substrate is placed in the top of mixing raw material, and its spacing is 3～5mm, puts into graphite reative cell the most together, is put by graphite reative cell
In vacuum atmosphere oven, it is evacuated to 50～80Pa, with the heating rate of 15 DEG C/min, furnace temperature is risen to 1400 DEG C, insulation
90min, closes power supply, cools to room temperature with the furnace, can obtain the situ Al doping SiC nanowire with net shape skin.Produce
XRD, SEM, TEM and XPS characterization result of thing is shown in accompanying drawing 1, Fig. 2, Fig. 3 and Fig. 4 (a), (b) respectively.Result shows, the table of product
Layer is by SiO2Nanosphere couples the network structure that Al doping SiC nanowire is formed, and is SiO at the most cancellated interface2Receive
Rice ball, lower floor's product is pure Al doping SiC nanowire, and diameter is about 60～80nm.After Al doping, product is changed without other
Compound generates, and the total spectrogram and the fine spectrogram of accompanying drawing 4 (b) Al 2p by accompanying drawing 4 (a) XPS is it can be seen that Al element is successfully mixed
Enter in SiC nanowire.And the constituent content analysis of XPS shows, the atomic percentage conc of Al element is 3.74at%.
The situ Al doping SiC nanowire with net shape skin prepared is carried out field emission performance test.By attached
Fig. 5 J-E relation curve, it can be seen that current density, J all strengthens along with the enhancing of field intensity E, is opened and threshold field is respectively
0.5V/ μm and 2.8V/ μm, these indexs are far superior to other element of unadulterated SiC nanowire and existing document report and mix
Miscellaneous SiC nanowire, shows that the situ Al doping SiC nanowire with net shape skin has excellent field emission performance.Accompanying drawing 5
Illustration be F-N curve, present approximately linear, belong to field-electron emission, illustrate that Flied emission electric current mostlys come from the product of synthesis
Thing.Accompanying drawing 6 is the field emission stability curve of the prepared situ Al doping SiC nanowire with net shape skin.Power up outward
Field is fixed as 2.8V/ μm, follow-on test 120min, and its electric current density stability bandwidth is 5.8%, and show preparation has net shape skin
Situ Al doping SiC nanowire as filed emission cathode material, there is high field emission stability.
Claims (3)
1. a situ Al doping SiC nanowire with net shape skin, it is characterised in that the surface of Al doping SiC nanowire is
One layer by SiO2Nanosphere couples the network nano structure that Al doping SiC nanowire is constituted, and at the most cancellated interface is
SiO2Nanosphere, lower floor's product is pure Al doping SiC nanowire, and its preparation method comprises the following steps:
1) with solid-state Polycarbosilane for Si source and C source, silica flour is auxiliary Si source, and at 230 DEG C, solid-state Polycarbosilane is incubated 40min
After carrying out pre-oxidation treatment, weigh Polycarbosilane and silica flour according to mass ratio 2～3:1, be placed in agate mortar mixing together and grind
Mill 30～40min, the Polycarbosilane after grinding is 0.2mol/L with addition 0.5～1.5mL concentration in the mixed powder of silica flour
Aluminum nitrate ethanol solution, be placed in drying baker 75 DEG C be dried 2 hours after, regrinding 40min, obtain reaction raw material standby
With；
2) graphite substrate after cleaning, drying, is immersed the Ni (NO of 0.01mol/L in ultrasonic washing unit3)3Ethanol solution 5 points
Zhong Hou, takes out nature and dries；
3) carbon cloth, reaction raw material and graphite substrate are put into graphite reative cell together, graphite reative cell is placed in vacuum gas
In atmosphere stove, it is evacuated to 50～80Pa, is warming up to 1350～1450 DEG C with the heating rate of 15 DEG C/min, be incubated 60～90min,
Close power supply, make vacuum controlled atmosphere furnace naturally cool to room temperature, it is thus achieved that there is the situ Al doping SiC nanometer of net shape skin
Line.
A kind of situ Al doping SiC nanowire with net shape skin the most according to claim 1, it is characterised in that: band
The graphite substrate and the reaction raw material placement location in graphite reative cell that have a catalyst be: reaction raw material is placed on double
On layer carbon cloth, being placed in the top of reaction raw material with the graphite substrate of catalyst, its spacing is 3～5mm.
A kind of situ Al doping SiC nanowire with net shape skin the most according to claim 1, it is characterised in that: institute
The situ Al doping SiC nanowire with net shape skin stated can be used for filed emission cathode material.
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