CN106809800A - A kind of preparation method of silicon nanowires/silver four cyano 1,4-benzoquinone nano-wire composite construction - Google Patents
A kind of preparation method of silicon nanowires/silver four cyano 1,4-benzoquinone nano-wire composite construction Download PDFInfo
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- CN106809800A CN106809800A CN201610776643.4A CN201610776643A CN106809800A CN 106809800 A CN106809800 A CN 106809800A CN 201610776643 A CN201610776643 A CN 201610776643A CN 106809800 A CN106809800 A CN 106809800A
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Abstract
The invention discloses a kind of preparation method of silicon nanowires/silver four cyano 1,4-benzoquinone nano-wire composite construction, it is characterised in that comprise the following steps：S1. silicon chip is placed in the mixed solution of hydrofluoric acid and silver nitrate and is reacted, deionized water rinsing silicon chip is used after reaction；S2. reacted silicon chip in S1 and four cyano 1,4-benzoquinone bismethane powder are fitted into glass tube, and be positioned on warm table, glass tube is heated, silicon nanowires/silver four cyano 1,4-benzoquinone nano-wire composite construction is obtained by being cleaned with acetone after cooling on silicon chip.The preparation method low cost of silicon nanowires of the present invention/silver four cyano 1,4-benzoquinone nano-wire composite construction, reaction are gentle, obtain silicon nanowires/silver four cyano 1,4-benzoquinone nano-wire composite construction and possess excellent field emission performance.
Description
Technical field
The present invention relates to composite construction preparation method field, more particularly to a kind of silicon nanowires/silver-four cyano 1,4-benzoquinone two
The preparation method of methane nanowire composite structures.
Background technology
Metal-four cyano 1,4-benzoquinone bismethane (metal-TCNQ) is a kind of charge transfer type metal organic complex, is had
Very special electronic structure.Optical storage characteristic, optoelectronic switch characteristic, gas-sensitive property and Flied emission about metal-TCNQ
The research of energy is constantly seen in report（Muller, R.; Genoe, J.; Heremans, P.Appl. Phys. Lett.
2006, 88, 242105；Potember, R. S.; Poehler, T. O.Appl. Phys. Lett. 1979, 34,
405；Liu, H. B.; Zhao, Q.; Li, Y. L. J.et.al.J. Am. Chem. Soc. 2005, 127,
1120）, and cause the great interest of people.The commercial test stage is had been enter into as optical recording media by the use of metal-TCNQ, is shown
Huge application prospect is shown.
Although there is many methods for preparing metal-TCNQ at present, preparation process is comparatively laborious, and majority is used
Reacted on metal substrate, the metal-TCNQ nano wire draw ratios for obtaining are restricted, affected the field hair of metal-TCNQ
Penetrate performance.Liu Huibiao etc. is on January 9th, 2008 in publication date, discloses one kind in Publication No. CN101100737A and prepares gold
The method for belonging to-TCNQ nano wires, the method is directly placed in metal substrate and TCNQ in tube furnace, and constant temperature adds under protective atmosphere
Thermal response, obtains metal-TCNQ nano wires on metal substrate.The method needs to need in metal substrate, and course of reaction lazy
Property gas shield, while the metal-TCNQ nano wire draw ratios for obtaining are restricted, is unfavorable for metal-TCNQ as optical recording
Medium is promoted the use of.
The content of the invention
In order to solve the problems of the prior art, it is an object of the invention to provide one kind prepare at ambient pressure silicon nanowires/
The method of silver-four cyano 1,4-benzoquinone nano-wire composite construction.The preparation method is simple, low cost, reaction are gentle, passes through
Changing reaction condition can obtain various sizes of silicon nanowires/silver-four cyano 1,4-benzoquinone nano-wire composite construction, real
The controllable effect of existing size.
To achieve these goals, the technical solution adopted by the present invention：A kind of silicon nanowires/silver-four cyano 1,4-benzoquinone two
The preparation method of methane nanowire composite structures, it is characterised in that comprise the following steps：S1. silicon chip is placed in hydrofluoric acid and nitre
In the mixed solution of sour silver, deionized water rinsing silicon chip is used after reaction, obtain silicon nanowires；S2. by reacted silicon chip in S1
It is respectively charged into glass tube with four cyano 1,4-benzoquinone bismethane powder, and is positioned on warm table, glass tube is heated, it is cold
But acetone rinsing silicon chip is used afterwards, you can silicon nanowires/silver-four cyano 1,4-benzoquinone nano-wire composite junction is obtained on silicon chip
Structure.
Wherein, the silicon chip in the S1 using preceding respectively with the watery hydrochloric acid, deionization that acetone, concentration are 0.1 mol/L
Water and EtOH Sonicate are cleaned.
Wherein, the die size in the S1 is 1cm × 1cm.
Wherein, the mixed solution in the S1 be 4.6 mol/L hydrofluoric acid solution and 0.04 mol/L silver nitrate it is molten
Liquid is mixed.
Wherein, the reaction temperature in the S1 is 50-55 DEG C.
Wherein, the reaction time in the S1 is 5~40 minutes.
Wherein, when the reaction time in the S1 is 5~10 minutes, the silicon nanowires length for obtaining is 10-35 microns, directly
Footpath is 60-200 nanometers.
Wherein, the consumption of the four cyano 1,4-benzoquinone bismethane powder in the S2 is 1-2 milligrams.
Wherein, the four cyano 1,4-benzoquinone bismethane powder in the S2 is positioned over glass bottom of the tube, and silicon chip is positioned over glass
Tube side face, apart from 1-3 centimetres of bottom.
Wherein, the mode of heating in the S2：Heatable glass tube is warmed up to 50~100 DEG C, maintains 1 ~ 30 minute, Ran Houji
It is continuous to be heated to 200~250 DEG C, maintain 5-30 minutes.
Compared with prior art, the beneficial effect that the present invention is realized：Silicon nanowires/silver-four cyano 1,4-benzoquinone of the invention
The preparation method of nano-wire composite construction is simple to operate, low cost, and reaction is gentle, during silicon nanowires is synthesized
Generation silver nano-grain, silver nano-grain reacts at 200 ~ 250 DEG C with the steam generation of four cyano 1,4-benzoquinone bismethane, obtains silicon
The composite construction of nano wire/silver-four cyano 1,4-benzoquinone nano-wire；Composite construction prepared by the present invention is in silicon nanowires
On the basis of synthesize silver-four cyano 1,4-benzoquinone nano-wire, relative on metal substrate prepare silver-four cyano to benzene
Quinone nano-wire, the draw ratio of composite construction is greatly increased, and improves field emission performance；Composite construction prepared by the present invention
Size it is controllable and can be widely used for field emission planar show, the aspect such as optoelectronic switch, sensor.
Brief description of the drawings
The present invention is further described below in conjunction with the drawings and specific embodiments：
Fig. 1 is the SEM figures of the silicon nanowires that the embodiment of the present invention 1 is obtained；
Fig. 2 is the SEM figures of the silicon nanowires that the embodiment of the present invention 2 is obtained；
Fig. 3 is the SEM figures of the silicon nanowires that the embodiment of the present invention 3 is obtained；
Fig. 4 is the comparison diagrams of the SEM with back scattering of the silicon nanowires that the embodiment of the present invention 3 is obtained；
Fig. 5 is the SEM of silicon nanowires/silver-four cyano 1,4-benzoquinone nano-wire composite construction that the embodiment of the present invention 4 is obtained
Figure；
Fig. 6 is the SEM of silicon nanowires/silver-four cyano 1,4-benzoquinone nano-wire composite construction that the embodiment of the present invention 5 is obtained
Figure；
Fig. 7 is the SEM of silicon nanowires/silver-four cyano 1,4-benzoquinone nano-wire composite construction that the embodiment of the present invention 6 is obtained
Figure；
Fig. 8 is silicon nanowires/silver-four cyano 1,4-benzoquinone nano-wire composite construction that the embodiment of the present invention 6 is obtained
FTIR schemes, and XRD and EDS scheme；
Fig. 9 obtains the Flied emission current density of sample and the relation curve of applied voltage for embodiment of the present invention 1-6.
Specific embodiment
Following silicon nanowires, four cyano 1,4-benzoquinone bismethane, silver-four cyano 1,4-benzoquinone nano-wire, silicon nanometer
Line/silver-four cyano 1,4-benzoquinone nano-wire composite construction is briefly referred to as SiNW, TCNQ, AgTCNQ, AgTCNQ-SiNW.
Embodiment 1
A. silicon chip using it is preceding clean 15 minutes with acetone, the watery hydrochloric acid of 0.1 mol/L, deionized water and EtOH Sonicate respectively after
Dry；
B. the silicon chip after step a treatment is placed in the mixed solution of 4.6 mol/L hydrofluoric acid and 0.04 mol/L silver nitrates,
Silicon chip is taken out after standing 5 minutes at 50 DEG C, deionized water rinsing is used.
Reacted silicon chip conduction in b is adhesive on sample stage, Electronic Speculum is scanned（SEM）Test, as a result such as Fig. 1
It is shown.Fig. 1 shows the SiNW average lengths of gained for 10 microns, and average diameter is 200 nanometers, and multiple nano wires top
End flocks together to form platform-like.
Embodiment 2
A. silicon chip using it is preceding clean 15 minutes with acetone, the watery hydrochloric acid of 0.1 mol/L, deionized water and EtOH Sonicate respectively after
Dry；
B. the silicon chip after step a treatment is placed in the mixed solution of 4.6 mol/L hydrofluoric acid and 0.04 mol/L silver nitrates,
Silicon chip is taken out after standing 18 minutes at 55 DEG C, deionized water rinsing is used.
Silicon chip conduction in after b is reacted is adhesive on sample stage, is scanned Electronic Speculum test, as a result as shown in Figure 2.
Fig. 2 shows the SiNW average lengths of gained for 15 microns, and average diameter is 200 nanometers, and each nano wire is upright, dispersiveness compared with
It is good.
Embodiment 3
A. silicon chip using it is preceding clean 15 minutes with acetone, the watery hydrochloric acid of 0.1 mol/L, deionized water and EtOH Sonicate respectively after
Dry；
B. the silicon chip after step a treatment is placed in the mixed solution of 4.6 mol/L hydrofluoric acid and 0.04 mol/L silver nitrates,
Silicon chip is taken out after standing 40 minutes at 53 DEG C, deionized water rinsing is used.
Reacted silicon chip conduction in b is adhesive on sample stage, Electronic Speculum test is scanned, as a result as shown in Figure 3.
Fig. 3 shows the SiNW average lengths of gained for 35 microns, and average diameter is 100 nanometers, while each nano wire is to centroclinal,
Assemble on top.
Understood from the data of the gained of Fig. 1,2 and 3, with the extension in reaction time, SiNW length increases, and diameter diminishes, point
End becomes increasingly thinner, but when certain reaction time is reached, the SiNW of generation assembles on top.
If Fig. 4 is the SEM that same sample is measured in same time same position（4-A）With back scattering figure（4-B）.Ash in figure
Color part is SiNW, and brighter white portion occurs in the top of SiNW, is Ag particles, and Ag particles diameter in 80-
400nm。
Embodiment 4
The silicon chip obtained in embodiment 1 is positioned on glass tube side wall, is 1 centimetre apart from bottom, by 2 milligrams of four cyanos to benzene
Quinone bismethane powder（Aldrich, analysis are pure）Load glass bottom of the tube, glass tube is positioned on warm table, heatable glass tube
To 50 DEG C, maintain 2 minutes, continue to be heated to 200 DEG C, maintain 30 minutes, be cooled to room temperature, the silicon chip reacted after terminating is used third
Ketone is cleaned, and scanning electron microscope analysis are carried out after drying.From figure 5 it can be seen that at each based on the SiNW of the synthesis of embodiment 1
New nano wire is generated on direction, the length of new nano wire is 3-4 μm, a diameter of 300-500nm, and with sharp top
End；Meanwhile, the nano wire of Fig. 5 newly synthesis also further demonstrate that the SiNW tops prepared in embodiment 1 have synthesized Ag nanometers
Grain.
Embodiment 5
The silicon chip obtained in embodiment 2 is positioned on glass tube side wall, is 1 centimetre apart from bottom, by 2 milligrams of four cyanos to benzene
Quinone bismethane powder（Aldrich, analysis are pure）Load glass bottom of the tube, glass tube is positioned on warm table, then heat glass
Glass pipe is warmed up to 70 DEG C, maintains 10 minutes, is then warmed up to 220 DEG C, maintains 15 minutes, room temperature is cooled to, after reaction is terminated
Silicon chip cleaned with acetone, dry after carry out scanning electron microscope analysis.From fig. 6 it can be seen that with embodiment it is 2-in-1 into SiNW be
Basis generates new nano wire in all directions, and the length of new nano wire is 4-6 μm, a diameter of 150-300nm.
Embodiment 6
The silicon chip obtained in embodiment 3 is positioned on glass tube side wall, is 1 centimetre apart from bottom, by 2 milligrams of four cyanos to benzene
Quinone bismethane powder（Aldrich, analysis are pure）Load glass bottom of the tube, glass tube is positioned on warm table, then heat glass
Glass pipe is warmed up to 100 DEG C, maintains 30 minutes, is then warmed up to 250 DEG C, maintains 5 minutes, room temperature is cooled to, after reaction is terminated
Silicon chip cleaned with acetone, dry after carry out scanning electron microscope analysis.It can be seen from figure 7 that being with the SiNW that embodiment 3 synthesizes
Basis generates new nano wire in all directions, and the length of new nano wire is 3-4 μm, a diameter of 300-500nm.
Fig. 8-A are FTIR (FTIR spectrum) figure for the AgTCNQ-SiNW that embodiment 6 is obtained, 2195cm-1 in figure
Locate the stretching vibration peak for C-N, weaker peak is the flexural vibrations peak of C-C at 1579cm-1 and 1505cm-1.
Fig. 8-B are the XRD of the AgTCNQ-SiNW that embodiment 6 is obtained（X-ray diffraction）Figure, 10.38,14.58 in figure,
Corresponding peak is matched completely with the XRD peaks of AgTCNQ in open source literature at 20.54 and 26.98, shows to be obtained in embodiment 6
AgTCNQ structures.Peak at 28.46 and 38.12 in figure is respectively the peak of Si and Ag.
Fig. 8-C are the EDS of the AgTCNQ-SiNW that embodiment 6 is obtained（Power spectrum）Figure, it can be seen that C in figure, N, Si, Al and
Ag elements, wherein C and N come from AgTCNQ, and Al comes from sample holder.
The data of complex chart 7 and Fig. 8-A, 8-B and 8-C, it was demonstrated that the sample that embodiment 6 is obtained is silicon and silver-four cyano pair
The composite construction of benzoquinones bismethane.
Embodiment 7
It is 1 × 10 in room temperature, vacuum−6The field emission performance test of SiNW and AgTCNQ-SiNW is carried out under conditions of Pa.
By the SiNW generated in embodiment 1 to 3 and generate AgTCNQ-SiNW in embodiment 4 to 6（Area is
0.25cm2）It is pasted onto in stainless steel disk as negative pole with conducting resinl respectively, an aluminium needle point disk of a diameter of 2mm is for just
Pole, two anode-cathode distances are 200 μm, carry out field emission performance test, and test process is known to the skilled person general knowledge.Survey
Test result is as shown in Fig. 9-A and 9-B.Sample I, II and III corresponds to embodiment 1,2 and 3 respectively in Fig. 9-A, in Fig. 9-B
AgTCNQ-SiNW I, II and III corresponds to embodiment 4,5 and 6 respectively.6 kinds of field emission performances of different nanostructureds are completely not
Together.SiNW cut-in voltages in embodiment 1 are 11.15 V μm−1, SiNW cut-in voltages in embodiment 2 are 8.737 V μm−1,
The SiNW cut-in voltages of embodiment 3 are 9.949 V μm−1.AgTCNQ-SiNW cut-in voltages in embodiment 6 are 6.515 V μm−1, AgTCNQ-SiNW cut-in voltages in embodiment 7 are 4.798 V μm−1, the AgTCNQ-SiNW cut-in voltages of embodiment 8 are
5.303 Vμm−1.The field emission performance of 3 kinds of different AgTCNQ-SiNW nano composite structures is substantially better than and it in example 4 to 6
Corresponding silicon nanowires, and the major diameter diameter group of AgTCNQ-SiNW affects the field emission performance of composite construction.
Preparation method of the invention can obtain the composite construction of different draw ratios by controlling the reaction time, and then control
The field emission performance of composite construction, realizes controllable effect.
Above-mentioned specific embodiment is exemplary, is to preferably make skilled artisans appreciate that originally
Patent, it is impossible to be not understood as including this patent the limitation of scope；As long as according to disclosed in this patent spirit made appoint
How with change or modification, the scope that this patent includes is each fallen within.
Claims (10)
1. the preparation method of a kind of silicon nanowires/silver-four cyano 1,4-benzoquinone nano-wire composite construction, it is characterised in that
Comprise the following steps：
S1. silicon chip is placed in the mixed solution of hydrofluoric acid and silver nitrate, deionized water rinsing silicon chip is used after reaction, obtained silicon and receive
Rice noodles；
S2. reacted silicon chip in S1 and four cyano 1,4-benzoquinone bismethane powder are respectively charged into glass tube, and be positioned over plus
In thermal station, glass tube is heated, acetone rinsing silicon chip is used after cooling, you can silicon nanowires/cyanogen of silver-four is obtained on silicon chip
Base 1,4-benzoquinone nano-wire composite construction.
2. the preparation side of silicon nanowires/silver as claimed in claim 1-four cyano 1,4-benzoquinone nano-wire composite construction
Method, it is characterised in that silicon chip in the S1 using preceding respectively with the watery hydrochloric acid, deionization that acetone, concentration are 0.1 mol/L
Water and EtOH Sonicate are cleaned.
3. the preparation side of silicon nanowires/silver as claimed in claim 1-four cyano 1,4-benzoquinone nano-wire composite construction
Method, it is characterised in that the die size in the S1 is 1cm × 1cm.
4. the preparation side of silicon nanowires/silver as claimed in claim 1-four cyano 1,4-benzoquinone nano-wire composite construction
Method, it is characterised in that the mixed solution in the S1 be 4.6 mol/L hydrofluoric acid solution and 0.04 mol/L silver nitrate it is molten
Liquid is mixed.
5. the preparation side of silicon nanowires/silver as claimed in claim 1-four cyano 1,4-benzoquinone nano-wire composite construction
Method, it is characterised in that the reaction temperature in the S1 is 50-55 DEG C.
6. the preparation side of silicon nanowires/silver as claimed in claim 1-four cyano 1,4-benzoquinone nano-wire composite construction
Method, it is characterised in that the reaction time in the S1 is 5~40 minutes.
7. the preparation side of silicon nanowires/silver as claimed in claim 6-four cyano 1,4-benzoquinone nano-wire composite construction
Method, it is characterised in that when the reaction time in the S1 is 5 ~ 10 minutes, the silicon nanowires length for obtaining is 10-35 microns, directly
Footpath is 60-200 nanometers.
8. the preparation side of silicon nanowires/silver as claimed in claim 1-four cyano 1,4-benzoquinone nano-wire composite construction
Method, it is characterised in that the consumption of the four cyano 1,4-benzoquinone bismethane powder in the S2 is 1-2 milligrams.
9. the preparation side of silicon nanowires/silver as claimed in claim 1-four cyano 1,4-benzoquinone nano-wire composite construction
Method, it is characterised in that the four cyano 1,4-benzoquinone bismethane powder in the S2 is positioned over glass bottom of the tube, and silicon chip is positioned over glass
Tube side face, apart from 1-3 centimetres of bottom.
10. the preparation side of silicon nanowires/silver as claimed in claim 1-four cyano 1,4-benzoquinone nano-wire composite construction
Method, it is characterised in that the mode of heating in the S2：Heatable glass tube is warmed up to 50~100 DEG C, maintains 1 ~ 30 minute, then
Continue to be heated to 200~250 DEG C, maintain 5-30 minutes.
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