CN108931560A - A kind of preparation method based on monodimension nanometer material sensor - Google Patents
A kind of preparation method based on monodimension nanometer material sensor Download PDFInfo
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Abstract
The invention discloses a kind of preparation method based on monodimension nanometer material sensor, this method is stood in the suspended drop substrate of monodimension nanometer material after at the uniform velocity being combed using Tool brush, and monodimension nanometer material is engaged by Van der Waals force with substrate closer after drying；To substrate surface solution evaporation after removing photoresist, it is evenly distributed that large area is formed on the substrate in monodimension nanometer material；Interdigital electrode figure is obtained using photoetching process；The characteristics of removing obtains monodimension nanometer material sensor after substrate surface is gold-plated, which has electric property excellent, high sensitivity.The method of the present invention is suitable for zinc oxide, a variety of monodimension nanometer materials such as silicon, and is suitable for different base such as silica, glass etc..The distribution density of monodimension nanometer material and the uniformity of arrangement can be realized by changing the size of assembling tool, if being expected to realize the production of large area using large scale delicate mechanical assembling tool.This method has wide application prospects in nano-device manufacture integration field.
Description
Technical field
The invention belongs to the preparation technical fields of the assembling of nano material and sensor, and in particular to one kind is based on one-dimensional
The preparation method of nano material sensor.
Background technique
Sensor technology is one of the new and high technology that the fast development that the world today attracts people's attention is got up, and contemporary section
One important symbol of technology development.Sensor research based on monodimension nanometer material is the forward position focus of various countries' research, is
The most important component of application value in sensor technical field.Monodimension nanometer material is as a kind of widely used group
Unit is filled, suffers from noticeable application in multiple fields such as electronics, optics, bioscience, energy storage etc..With tradition
Planar semiconductor material is compared, characteristic of the monodimension nanometer material due to being limited dimension conducting with biggish specific surface area and two dimension,
Possess the properties such as unique electricity, optics.Sensor is prepared with monodimension nanometer material, how a problem to be solved is
Large scale highdensity assembles monodimension nanometer material.The bottleneck that in order to solve the problems, such as, Smith et al. [Smith,
P.A.； Nordquist,C.D.；Jackson,T.N.；Mayer,T.S.；Martin,B.R.；Mbindyo,J.；Mallouk,
T.E. Electric-field assisted assembly and alignment of metallic
Nanowires.Appl.Phys. Lett.2000,77,1399-1401.] it will be in two electrodes using electric field-assisted assemble method
Between dielectric in the nano wire positioning that suspends on silicon oxide substrates, but this method is only applicable to metallic character
Nano material.Fan et al. [Smith, P.A.；Nordquist,C.D.；Jackson,T.N.；Mayer,T.S.；Martin,
B.R.； Mbindyo,J.；Mallouk,T.E.Electric-field assisted assembly and alignment
Of metallic nanowires.Appl.Phys.Lett.2000,77,1399-1401.] it will using the method for contact printing
Semiconductor nano material ordered arrangement may destroy surface due to the poor contact between nano material and matrix.Whang
Et al. [Whang, D.；Jin,S.；Wu,Y.；Lieber,C.M.Large-scale hierarchical organization
Of nanowire arrays for integratednanosystems.Nano Lett.2003,3,253-256.] it uses
Langmuir-Blodgett method controls the tissue and level of One-dimensional Silicon Nanomaterials, however the technology needs complicated table
Face is modified, and the arrangement of monodimension nanometer material depends on the control of surface pressing.Zhang et al. [Zhang Q, Gupta S,
Todd Emrick A,et al.Surface-Functionalized CdSe Nanorods for Assembly in
Diblock Copolymer Templates[J].Journal of the American Chemical Society,2006,
128(12):3898-3899.] use geometrical pattern template-mediated successfully to assemble CdSe nanometer rods, but technique is more multiple
It is miscellaneous.Above method requires greatly expensive instrument and equipment, higher cost.
Summary of the invention
For above-mentioned defect existing in the prior art and deficiency, the purpose of the present invention is to provide one kind based on one-dimensional
The preparation method of nano material sensor, the sensor based on this method preparation have electric property excellent, the spy of high sensitivity
Point.
The present invention adopts the following technical scheme that realize：
A kind of preparation method based on monodimension nanometer material sensor, includes the following steps：
(1) it prepares monodimension nanometer material suspension and prepares substrate；
Monodimension nanometer material is soaked in deionized water, the solution of monodimension nanometer material is formed, in ultrasonic cleaning pond
In ultrasonic vibration is carried out to solution, until obtain finely dispersed monodimension nanometer material suspension；
Prepare substrate；
Substrate is cleaned up, is then dried；The spin coating photoresist in substrate uses the mask with narrow slot after front baking
Version carries out alignment exposure, and development obtains the substrate with narrow slot structure after drying, corrode and removing photoresist afterwards；
(2) monodimension nanometer material is assembled；
By the suspended drop of monodimension nanometer material in step (1) ready substrate, the arrangement at random in substrate is obtained
Monodimension nanometer material；Then it is stood after at the uniform velocity being combed from left to right in substrate using Tool brush；Substrate is dried on hot plate
It is dry so that monodimension nanometer material engaged by Van der Waals force with substrate it is closer；
(3) preparation step of sensor；
Sol solution is removed into the substrate for being attached with monodimension nanometer material immersion, until photomask surface glue is removed, is removed simultaneously
The not strong nano wire of part adhesive force；Substrate is taken out, after the volatilization of its surface solution, monodimension nanometer material is formed on the substrate
Large area is evenly distributed；Ultraviolet photolithographic technique is carried out using litho machine, obtains interdigital electrode figure；Existed using electron beam evaporation plating
Substrate surface plates the gold of one layer of 50-200nm thickness；Monodimension nanometer material sensor is obtained after being removed by stripper.
A further improvement of the present invention lies in that monodimension nanometer material is nano wire, nanometer rods and nanotube in step (1)
One of monodimension nanometer material.
A further improvement of the present invention lies in that the substrate of preparation is silicon base in step (1), it is coated with the silicon substrate of golden film
One of bottom and substrate of glass.
A further improvement of the present invention lies in that the Tool brush for assembling monodimension nanometer material is paintbrush brush in step (1), change
Adornment brush or writing brush type brush.
A further improvement of the present invention lies in that the monodimension nanometer material sensor of preparation can be used in detecting multiple gases,
Including：Carbon monoxide, nitrogen dioxide, ammonia and hydrogen.
The present invention has following beneficial technical effect：
1, the present invention provides a kind of effective ways in any any monodimension nanometer material of substrate over-assemble, due to group
Holding tool is compliant tool, will not lesioned sample, be greatly broadened assembling object range；
2, it is good to arrange consistency in substrate for the monodimension nanometer material after present invention assembling, good with the associativity of substrate,
Stable contact is formed between monodimension nanometer material and substrate.Nanostructure is formed such that sensor has big specific surface area,
Be conducive to the adsorption and diffusion of gas, while more reaction sites and adsorption gas molecule effect being provided, to be conducive to accelerate
Response and raising response sensitivity；
3, the assembling procedure of monodimension nanometer material is simple and assembling tool is simply easily obtained, and improve this method can
Row.Expensive experimental facilities is not needed, experimental cost has been saved；
4, repeatability and high reliablity, the distribution density of monodimension nanometer material and the neat degree of arrangement can be by changing
Become the size of assembling tool to realize, if being expected to realize the production of large area using large scale delicate mechanical assembling tool.
Detailed description of the invention
Fig. 1 is main-process stream schematic diagram in the present invention；
Fig. 2 is to prepare chemical vapor deposition (CVD) tube furnace that monodimension nanometer material uses in the specific embodiment of the invention
Schematic diagram.
Fig. 3 is the scanning electron microscope photograph of the Tool brush that monodimension nanometer material is assembled in the present invention and individual bristle
Piece；
Fig. 4 is monodimension nanometer material assembling flow path schematic diagram in the present invention；
Fig. 5 is the electron scanning micrograph of assembling zinc oxide nano wire on a silicon substrate in present example, Fig. 5
(a) it is assembled in the slot of photoresist formation for the arrangement of four column zinc oxide nanowires, Fig. 5 (b) is the amplification of first row in Fig. 5 (a)
Figure, it is seen that the orientation of nano wire is almost the same, and Fig. 5 (c) is the angular distribution figure of zinc oxide nanowire in Fig. 5 (b), surpasses
The nano wire for crossing 80% is the proper alignment in 20 ° of angle, and consistent with combing direction.
Fig. 6 is the electron scanning micrograph of the sensor prepared in present example, and Fig. 6 (a) is on a silicon substrate
After assembling zinc oxide nano wire, the zinc oxide nanowire sensor (dotted line expression interdigital electrode) with interdigital electrode of preparation,
Fig. 6 (b) is the enlarged drawing of Fig. 6 (a).It can be seen that zinc oxide nanowire still proper alignment is on a silicon substrate after vapor deposition gold electrode.
Fig. 7 is the electrology characteristic phenogram of the sensor prepared in present example, and Fig. 7 (a) is that six experiments measure
I-v curve, the curve that six experimental results measure essentially coincide, and repeatability and flatness demonstrate zinc oxide nanowire
Steady contact between electrode.Non-linear and symmetrical curve shows Schottky characteristic.Fig. 7 (b) is for bias voltage
Ultraviolet lighting characteristic curve when 0.5V.
Fig. 8 is the relational graph of carbonomonoxide concentration and sensitivity under different temperatures.
Fig. 9 is the scanning electron microscope being assembled in zinc oxide nanowire in embodiment 2 on the silicon substrate for being coated with golden film
Image；
Figure 10 is the angular distribution figure of silicon nanowires in embodiment 2.
Specific embodiment
Illustrate the embodiment of the present invention or technical solution in the prior art in order to clearer, below will to embodiment or
Attached drawing needed to be used in the description of the prior art is briefly described.
Embodiment 1
The present embodiment prepares gas sensor based on the assemble method of zinc oxide nanowire and is used to detect carbon monoxide,
Include the steps that preparing zinc oxide nanowire, the assembling steps of zinc oxide nanowire and gas sensor preparation step, such as Fig. 1
For main-process stream schematic diagram in invention；
The step of preparing zinc oxide nanowire：
Silicon wafer as shown in Fig. 2, is cut into the sheet of 2cm*2cm, and using ethyl alcohol, go by preparation facilities before preparation
Ionized water, acetone are respectively washed silicon wafer 5min, are placed on removing residual liquid on hot plate later.By zinc powder, (purity is
99.99%) it is put into aluminium oxide boat, the center of aluminium oxide boat merging quartz ampoule, substrate is then placed on the right side of zinc source 3-4 lis
At rice.When with mechanical pump air exhaust duct vacuum degree 10Pa, in-furnace temperature is increased to 600-750 DEG C, heating rate is about 30 DEG C/
min.It is passed through the mixed gas of argon gas and oxygen simultaneously, wherein argon flow control is 140sccm, and oxygen flux control is
After 10sccm, about 15-20min, stop heating, by furnace temperature cooled to room temperature.The white product covered on substrate is oxygen
Change zinc nano wire.
The assembling steps of zinc oxide nanowire：
(1) zinc oxide nanowire suspension is prepared：
The zinc oxide nanowire of preparation is soaked in deionized water, zinc oxide nanowire solution is formed, it is clear in ultrasonic wave
Ultrasonic vibration 10min is carried out to solution in wash pool, obtains finely dispersed zinc oxide nanowire suspension；
(2) prepare substrate：
Silicon base is cleaned first, is then dried.One layer of positive photoresist of spin coating, low speed rotation 200rpm rotate 6s,
High speed rotation is 2500rpm, rotates 30s；It is placed on hot plate and carries out front baking, temperature sets 90 DEG C, time 5min；It will have
The mask plate of narrow slot pattern is directed at base part, carries out 7s exposure using ABM double-sided alignment exposure machine, configures 0.5% NaOH
Substrate sample is immersed and carries out 20s development, can be seen that the narrow slot pattern on mask plate is transferred to silicon base at this time by solution
On.
(3) assembling zinc oxide nano wire
With the suspension 1-2 drop of zinc oxide nanowire prepared by dropper aspiration step (1), drip ready in step (2)
It is carved in the silicon base of photoetching glue groove, obtains the zinc oxide nanowire of the arrangement at random in substrate；Then using small size tool
Brush, the electron scanning micrograph of the single hairbrush of Tool brush is as shown in figure 3, use work according to assembling steps as shown in Figure 4
Tool brush at the uniform velocity combs from left to right in substrate, stands for 24 hours；Silicon base is dried into 10min under conditions of 500 DEG C, so that oxygen
Change zinc nano wire is engaged by Van der Waals force with silicon base closer；
(4) preparation of gas sensor
The silicon base for being attached with zinc oxide nanowire is immersed into acetone soln, until photomask surface glue is removed；Take out silicon
Substrate, after the volatilization of its surface solution, it is evenly distributed that zinc oxide nanowire forms large area on a silicon substrate；It will have interdigital
The electrode section of the mask plate alignment sample of electrode pattern, carries out 7s exposure, configuration 0.5% using ABM double-sided alignment exposure machine
NaOH solution, by sample be immersed carry out 20s development, can be seen that the interdigital electrode pattern on mask plate is transferred at this time
Sample surfaces；The gold of one layer of 100nm thickness is plated in substrate surface using electron beam evaporation plating；After being removed by stripper
Obtain zinc oxide gas sensor.As shown in figure 5, the scanning electron microscope for the sensor prepared in present example is shone
Piece,
Zinc oxide nanowire assembles result characterization：
Fig. 5 show the electron scanning micrograph of silicon base over-assemble zinc oxide nanowire, and Fig. 5 (a) is four column oxygen
Change zinc nanowire alignment to be assembled in the narrow slot of photoresist formation, it is seen that the assemble method of combing is highly desirable by zinc oxide
Nano wire comb is into the slot with photolithography method preparation；Fig. 5 (b) is the enlarged drawing of first row in Fig. 5 (a), it is seen that zinc oxide nano
The orientation of rice noodles is almost the same；Fig. 5 (c) is the angular distribution figure of zinc oxide nanowire in Fig. 5 (b), soft with AutoCAD
Part measures the nano wire being distributed in figure, and depicts curve graph, knows that the nano wire more than 80% is at 20 ° by figure
Proper alignment in angle, and it is consistent with combing direction.
The performance characterization of gas sensor：
In order to verify this monodimension nanometer material assemble method feasibility, inventor is prepared for gas sensor, surveys
Current-voltage characteristic curve and ultraviolet lighting characteristic curve have been tried, and has been passed through CO gas and tests the sensitive of the device
Degree.
(1) electrology characteristic
As shown in Fig. 7 (a), six tests are carried out, the curve of obtained Current Voltage essentially coincides, repeatability peace
Slip demonstrates the steady contact between zinc oxide nanowire and gold electrode.Experiment curv is non-linear and symmetrical, shows Xiao Te
Base characteristic.
(2) ultraviolet lighting characteristic
The ultraviolet lighting characteristic curve that Fig. 7 (b) is bias voltage when being 0.5V.Initial current is 3.3A, is shone in ultraviolet light
Penetrating down increases to 72.2A, almost the 22 of initial current times.On-off ratio is much higher than Oliver et al. [Harnack, O.；
Pacholski,C.；Weller,H.；Yasuda,A.；Wessels,J.M.Rectifying Behavior of
Electrically Aligned ZnO Nanorods.Nano Lett.2003,3,1097-1101.] result that measures.It rings
Between seasonable and die-away time is respectively 22.98s and 34.14s.
(3) gas-sensitive property
The rate that is passed through of carbon monoxide is 20mL/min, and Fig. 8 is the pass of carbonomonoxide concentration and sensitivity under different temperatures
System's figure.As can be seen that the sensor is more sensitive to the variation of small concentration, there is very high response speed.In different operation temperature
Under degree, carbon monoxide gas concentration increases, sensitivity decrease.When carbon monoxide gas concentration is greater than 500ppm, when concentration drops
When low, the carrier concn in zinc oxide nanowire tends to be saturated, and sensitivity is not significantly different.It is sensed when temperature is 300 DEG C
Mechanism may include two kinds of reactions, may be O in the main oxygen type of zinc oxide surface absorption-And O2-.In addition, with work
Make the increase of temperature, the increase of reaction of carbon monoxide rate can be construed to thermal energy high enough to overcoming the activation energy barrier of reaction
Hinder.When temperature is increased to 400 DEG C, the sensitivity decrease of carbon monoxide transducer, this may be because these absorption oxygen start
It is removed at this temperature from zinc oxide surface.In addition, being prepared in the present invention when the concentration of carbon monoxide is 500ppm
The sensitivity of sensor is 0.0093ppm, this is than Hsueh et al. [Hsueh, T.J.；Chen,Y.W.； Chang,S.J.；
Wang,S.F.；Hsu,C.L.；Lin,Y.R.；Lin,T.S.；Chen,I.C.ZnO nanowire-basedCO sensors
Prepared at various temperatures.J.Electrochem.Soc. 2007,154, J393-J396.] in phase
The result to work like at a temperature of wants high.This is because the large surface area of the zinc oxide nanowire after assembling will lead to adsorbed gas
Interaction between body and sensor surface is stronger, to keep gas sensing sensitivity higher.
Embodiment 2
The present embodiment assembles silicon nanowires, has changed simultaneously the class of substrate to verify universality of the invention
Type uses the silicon substrate for having plated golden film.
The step of preparing silicon nanowires：
(1) firstly, the monocrystalline silicon piece in p-type (100) direction is cut into 1*1cm2Small pieces, silicon wafer is then immersed into second
In alcoholic solution, ultrasonic cleaning 10min is carried out in ultrasonic cleaning pond, removes surface organic matter；
(2) silicon wafer is put into the H of configuration2SO4:H2O2It is cleaned by ultrasonic 10min in solution, further removes surface organic matter,
Oxide layer is formed, then silicon wafer is cleaned with 5% HF, removes surface oxide layer；
(3) HF-AgNO of various concentration is configured3Corrosive liquid is placed in the reaction kettle tetrafluoroethene liner of 100ml, fills out
Degree of filling 85%；
(4) silicon wafer after cleaning is immersed in corrosive liquid, seals postposition 85 DEG C of reaction 6h in a vacuum drying oven；
(5) it after reaction was completed, with tweezers clipping silicon chip, immerses deionized water and is cleaned, finally by the silicon wafer after corrosion
It immerses in concentrated nitric acid solution and handles 30min, remove the metal ion on surface.Obtain silicon nanowires.
The assembling steps of silicon nanowires：
(1) silicon nanowires suspension is prepared：
The silicon nanowires of preparation is soaked in deionized water, silicon nanowires solution is formed, it is right in ultrasonic cleaning pond
Solution carries out ultrasonic vibration 10min, obtains finely dispersed silicon nanowires suspension；
(2) prepare substrate：
Silicon base is cleaned first, is then dried.One layer is plated in silicon substrate surface using electron beam evaporation plating
The gold of 100nm thickness.
(3) silicon nanowires is assembled
With the suspension 1-2 drop of zinc oxide nanowire prepared by dropper aspiration step (1), drip ready in step (2)
It is carved in the silicon base of photoetching glue groove, obtains the zinc oxide nanowire of the arrangement at random in substrate；Then using small size tool
Brush, the electron scanning micrograph of the single hairbrush of Tool brush is as shown in Fig. 2, use work according to assembling steps as shown in Figure 3
Tool brush at the uniform velocity combs from left to right in substrate, stands for 24 hours；Silicon base is dried into 10min under conditions of 500 DEG C, so that oxygen
Change zinc nano wire is engaged by Van der Waals force with silicon base closer；
Above-mentioned steps (1) (2) do not have sequencing relationship.
Nano wire after assembling is as shown in Figure 9.Figure 10 is the angular distribution figure of silicon nanowires.Silicon nanometer as shown in Figure 10
Line orientation in the silicon base for be coated with golden film is almost the same, and the silicon nanowires more than 85% is neatly arranged in 20 ° of angle
Column.
Claims (5)
1. a kind of preparation method based on monodimension nanometer material sensor, which is characterized in that include the following steps：
(1) it prepares monodimension nanometer material suspension and prepares substrate；
Monodimension nanometer material is soaked in deionized water, the solution of monodimension nanometer material is formed, it is right in ultrasonic cleaning pond
Solution carries out ultrasonic vibration, until obtaining finely dispersed monodimension nanometer material suspension；
Prepare substrate；
Substrate is cleaned up, is then dried；The spin coating photoresist in substrate is carried out using the mask with narrow slot after front baking
Alignment exposure, development obtain the substrate with narrow slot structure after drying, corrode and removing photoresist afterwards；
(2) monodimension nanometer material is assembled；
By the suspended drop of monodimension nanometer material in step (1) ready substrate, one of the arrangement at random in substrate is obtained
Dimension nano material；Then it is stood after at the uniform velocity being combed from left to right in substrate using Tool brush；Substrate is dried on hot plate, is made
Monodimension nanometer material by Van der Waals force engaged with substrate it is closer；
(3) preparation step of sensor；
Sol solution is removed into the substrate for being attached with monodimension nanometer material immersion, until photomask surface glue is removed, while removing part
The not strong nano wire of adhesive force；Substrate is taken out, after the volatilization of its surface solution, large area is formed on the substrate in monodimension nanometer material
It is evenly distributed；Ultraviolet photolithographic technique is carried out using litho machine, obtains interdigital electrode figure；Using electron beam evaporation plating in substrate surface
Plate the gold of one layer of 50-200nm thickness；Monodimension nanometer material sensor is obtained after being removed by stripper.
2. a kind of preparation method based on monodimension nanometer material sensor according to claim 1, which is characterized in that step
(1) in, monodimension nanometer material is one of nano wire, nanometer rods and nanotube monodimension nanometer material.
3. a kind of preparation method based on monodimension nanometer material sensor according to claim 1, which is characterized in that step
(1) in, the substrate of preparation is silicon base, is coated with one of silicon base and substrate of glass of golden film.
4. a kind of preparation method based on monodimension nanometer material sensor according to claim 1, which is characterized in that step
(1) in, the Tool brush for assembling monodimension nanometer material is paintbrush brush, cosmetic brush or writing brush type brush.
5. a kind of preparation method based on monodimension nanometer material sensor according to claim 1, which is characterized in that preparation
Monodimension nanometer material sensor can be used in detect multiple gases, including：Carbon monoxide, nitrogen dioxide, ammonia and hydrogen.
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