CN102998344A - Novel nanosheet film for sensor and preparation method thereof - Google Patents

Novel nanosheet film for sensor and preparation method thereof Download PDF

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CN102998344A
CN102998344A CN2012105349823A CN201210534982A CN102998344A CN 102998344 A CN102998344 A CN 102998344A CN 2012105349823 A CN2012105349823 A CN 2012105349823A CN 201210534982 A CN201210534982 A CN 201210534982A CN 102998344 A CN102998344 A CN 102998344A
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film
alloy
electrolytic solution
nanometers
nanometer sheet
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CN102998344B (en
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凌云汉
高武斌
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Tsinghua University
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Abstract

The invention belongs to the cross field of semiconductor materials and chemical engineering, relates to a preparation method of a sensor film, and particularly relates to a novel nanosheet film for a sensor and a preparation method thereof. The nanosheet film comprises of 35-100 wt% of one or more selected from nanosheet WO3 and MoO3, and 0-65 wt% of one or more selected from W and Mo. According to the invention, one or more selected from Na2WO4 and Na2MoO4, FeSO4, and (NH4)2C4H4O6 are used to prepare an electrolyte; an alloy coating is prepared by electrodeposition coating; the alloy coating grows on substrate metal sheet in situ; Fe component in the alloy is removed; and the nanosheet deposition film is oxidized to obtain the product. The method provided by the invention does not require sophisticated equipment or dangerous medicine and solvent, and has the advantages of simple process, low production cost, and uniform thickness of the nanosheet WO3 film.

Description

A kind of novel nano sheet film that can be used for sensor and preparation method thereof
Technical field
The invention belongs to the crossing domain of semiconductor material and chemical technology, relate to the preparation method of colorimetric sensor films, be specifically related to a kind of novel nano sheet film that can be used for sensor and preparation method thereof.
Background technology
The semi-conductor type gas sensor is to utilize gas to be measured to carry out adsorption reaction on the inductive material surface, the inductive material surface can absorb or emit unnecessary electronics, and the electron density on inductive material surface is changed, therefore cause the variation of inductive material resistance value, decide thus the concentration of gas to be measured according to the variable quantity of its resistance.
Tungstic acid is a kind of n-type metal oxide semiconductor of energy gap, is widely used in such as fields such as gas sensor and efficient wide catalyzer as a kind of important functional material.While is owing to its distinguished galvanochemistry and contact performance, WO 3It is a kind of engineering material that haves a great attraction.WO 3And WO 3Based sensor is widely used in surveying NO 2, NO and H 2S gas.
The inductive material of existing tungstic acid sensor mostly is greatly fine and close or many empty particle type WO 3 films, the method of preparation has sol-gal process [Sivakumar R, MosesEzhilRaj A, Subramanian B, et al. Preparation and characterization of spray deposited n-type WO3 thin films for electrochromic devices. Mater ResBull 2004,39 (10): 1479 – 1489.], chemical vapor deposition [N. Shankar, M.F. Yu, S.P. Vanka, N.G. Glumac, Synthesis of tungsten oxide (WO 3) nanorods using carbon nanotubes as templates by hot filament chemical vapor deposition, Mater. Lett. 2006,60:771 – 774.], magnetron sputtering [Stankova M, Vilanova X, Llobet E, et al. Influence of the annealing and operating temperatureson the gas-sensing properties of rf sputtered WO 3Thin-film sensors. Sensors Actuators B 2005,105 (2): 271 – 277] etc.
Publication number is that the Chinese patent of CN101318702 discloses " a kind of tungstic trioxide nano-slice and preparation method thereof ", it is precursor that the method adopts wolframic acid base organic or inorganic stratiform to mix micro-/ nano band (pipe), removes to obtain the after-baking of wolframic acid nanometer sheet behind the organism between precursor layer and obtain the tungstic oxide nano-sheets dusty material.Publication number is that the Chinese patent of CN1935671 discloses " a kind of tungsten oxide material with nano band array structure and preparation method thereof ", the method adopt tungsten basal body self-heating under the low vacuum and outwards the method for the banded tungsten oxide of growing nano on tungsten basal body, directly prepare membraneous material.Publication number is that the Chinese patent of CN1974890 discloses " a kind of nanometer porous tungsten trioxide material and its preparation method and application ", the method adopts constant current anode oxidation tungsten matrix, makes its self assembly form the tungsten trioxide nano material of nanoporous shape.But be also not reporting of growth in situ nano-sheet, relevant air-sensitive performance research also has no its report.
Summary of the invention
Not enough for prior art, the invention provides a kind of novel nano sheet film that can be used for sensor and preparation method thereof.
Basic conception of the present invention is according to the metallic iron of live dialling preferential corrosion and gradually dissolving and tungsten and molybdenum of the ripple of deviating to stay more not live from alloy in acid solution, then under higher temperature, tungsten and molybdenum and airborne oxygen generation oxidation reaction, by to the control of taking off alloy extent, the control of high-temperature oxydation temperature and time, and obtain that specific surface area is large, tungsten oxide and the Electrochromic Molybdenum Oxide Coatings material of nano-sheet.
A kind of novel nano sheet film that can be used for sensor, its nanometer sheet film is by the nano-sheet WO that accounts for its quality 35% ~ 100% 3And MoO 3In one or more, and account for the W of its quality 0% ~ 65% or one or more compositions among the Mo.
Nanometer sheet length is 100 nanometers ~ 600 nanometers in the described nanometer sheet film, and width is 50 nanometers ~ 300 nanometers, and thickness is 20 nanometers ~ 100 nanometers.
The integral thickness of described nanometer sheet film is 1 micron ~ 50 microns.
A kind of novel nano sheet thin film technology method that can be used for sensor is with Na 2WO 4And Na 2MoO 4In one or more, FeSO 4, (NH4) 2C 4H 4O 6Configuration electrolytic solution prepares alloy layer by electro-deposition, and described alloy layer growth in situ is on the parent metal sheet; Obtain product by the deposit film of deviating from the Fe composition rear oxidation nano-sheet in the alloy, concrete steps are as follows:
(1) configuration electrolytic solution, wherein electrolytic solution is composed as follows:
Na in the electrolytic solution 2WO 4And Na 2MoO 4Total concentration be 0.15 ~ 0.25mol/L, FeSO 4Concentration be 0.02 ~ 0.03 mol/L, (NH 4) 2C 4H 4O 6Concentration be 0.2 ~ 0.3 mol/L;
(2) electrodeposition technology:
Matrix is cut into required form, after sand papering, use successively respectively ultrasonic cleaning 10 min of acetone, alcohol and deionized water; Then the pH value of regulating electrolytic solution is 3 ~ 5; Then electrolytic solution is put into heating arrangement, heating and temperature control is at 40 ℃ ~ 60 ℃; Take matrix as negative electrode, graphite is anode, passes into 0.05 A/cm 2~ 0.4 A/cm 2Direct current carry out electro-deposition, electrodeposition time is controlled at 2 min ~ 15 min; The complete coating of electro-deposition dries after washing, i.e. the alloy layer of system;
(3) take off alloying technology:
Compound concentration is the aqueous hydrochloric acid solution of 1 mol/L, at room temperature will deposit good alloy layer and place hydrochloric acid solution, and the Fe composition in the alloy layer and HCl reaction are and dissolved, and control is taken off the time of alloy at 3 hours ~ 24 hours; It is complete through washed with de-ionized water to take off alloy, obtains deposit film after naturally drying;
(4) deposit film oxidation technology:
The deposit film that will take off after the alloy treatment places tubular furnace, and in 450 ℃ ~ 700 ℃ lower sintering, sintering time is controlled at 30 min ~ 240 min, namely makes the nanometer sheet film in the air atmosphere.
Described matrix is pure tungsten, stainless steel or fine copper metal.
Beneficial effect of the present invention is:
The inventive method need not used complicated equipment, also need not use dangerous medicine and solvent, has that technique is simple, production cost is low, nanometer sheet WO 3The advantages such as film thickness is even.
Description of drawings
Fig. 1 is that embodiment 1 is through taking off the nano-sheet W scanning electron microscope (SEM) photograph (SEM) of alloy treatment;
Fig. 2 is the tungsten oxide film scanning electron microscope (SEM) photograph (SEM) of embodiment 1 nanometer sheet;
Fig. 3 is the X-ray diffractogram (XRD) of embodiment 1 nano-sheet tungsten oxide;
Fig. 4 be embodiment 1 nanometer sheet tungsten oxide under 100 ℃ to NO 2Response curve.
Embodiment
The invention provides a kind of novel nano sheet film that can be used for sensor and preparation method thereof, the present invention will be further described below in conjunction with the drawings and specific embodiments.
Embodiment 1
Tungstic oxide nano-sheets thin film technology step take the tungsten sheet as reactive matrix is as follows:
The first step cuts into the pure tungsten sheet and is of a size of 15 mm * 15 mm, carefully polishes through 500#, 1000#, 2000# sand paper, successively with acetone and each 10 min of deionized water difference ultrasonic cleaning.
The analytically pure Na of second step 2WO 42H 2O, FeSO 47H 2O and (NH 4) 2C 4H 4O 6The electrolytic solution of preparation tungstenic, ferric ion, wherein Na 2WO 42H 2O, FeSO 47H 2O and (NH 4) 2C 4H 4O 6Concentration be followed successively by 0.25 mol/L, 0.02 mol/L and 0.25 mol/L regulate electrolyte PH value to 4 with sulfuric acid, electrolytic solution liquid adopts the deionized water preparation.
The 3rd step packed the electrolytic solution for preparing in the beaker into, placed water-bath, and negative electrode connects through the pretreated matrix of step 1, and anode connects graphite flake.Start temperature control device for water bath, the control temperature passes into direct current 0.2 A/cm behind 60 ℃ of lower insulation 30 min 2Carry out electro-deposition, electrode is taken out in the source that cuts off the power supply immediately behind electro-deposition 5 min.
The 4th step at room temperature will deposit the hydrochloric acid solution that good W-Fe alloy layer places 1 mol/L, and the Fe composition in the alloy and HCl react and deviate from, and the time that alloy is taken off in control is 24 hours; Take off that alloy is complete to be dried after deionization washing.
The matrix that the 5th step will take off after the alloy treatment places tubular furnace, and in 500 ℃ of lower sintering, sintering time is controlled to be 120 min, namely makes nanometer sheet WO 3Film.
Measure the tungsten oxide material of the nano-sheet that obtains, its film thickness is 7 μ m.
The scanning electron microscope (SEM) photograph (as shown in Figure 1) of the tungsten nano-chip arrays film of embodiment 1 is to adopt Hitachi S-4800 scanning electron microscope, and accelerating potential is 20 kV, takes above matrix.As seen from Figure 1, the tungsten after HCl takes off alloy treatment presents unordered nano-sheet array structure.
The scanning electron microscope (SEM) photograph (as shown in Figure 2) of the tungstic oxide nano-sheets array film of embodiment 1 is to adopt Hitachi S-4800 scanning electron microscope, and accelerating potential is 20 kV, takes above matrix.As seen from Figure 2, the tungstic oxide nano-sheets film presents unordered array structure.
The X-ray diffractogram (as shown in Figure 3) of the tungstic oxide nano-sheets film of embodiment 1 is to adopt the D-8Advanced diffractometer, at 40 kV, scans under the 20 mA conditions, and sweep speed is 0.02 °/S.
Fig. 4 is the nanometer sheet tungsten oxide film of embodiment 1 NO to 1 ppm, 2 ppm, 4 ppm and 8 ppm concentration under 100 ℃ working temperature 2The response curve of gas.
Embodiment 2
Molybdena nanometer sheet thin film technology step take the metal copper sheet as reactive matrix is as follows:
The first step cuts into 15 mm * 15 mm with copper sheet, plays acetone, deionized water ultrasonic cleaning through 500#, 1000#, 2000# sand paper before the deposition.
Second step is to analyze pure Na 2MoO 42H 2O, FeSO 47H 2O and (NH4) 2C 4H 4O 6Preparation contains the electrolytic solution of molybdenum, ferric ion, wherein Na 2MoO 42H 2O, FeSO 47H 2O and (NH4) 2C 4H 4O 6Concentration be respectively 0.15 mol/L, 0.03 mol/L and 0.3 mol/L regulate electrolyte PH value to 5.5, electrolytic solution adopts the deionized water preparation.
The 3rd step packed the electrolytic solution for preparing in the beaker into, placed water-bath, and negative electrode connects through the pretreated matrix of step 1, and anode connects graphite flake.Start temperature control device for water bath, the control temperature passes into direct current 0.05 A/cm behind 50 ℃ of lower insulation 30 min 2Carry out electro-deposition, electrode is taken out in the source that cuts off the power supply immediately behind electro-deposition 3 min.
The 4th step at room temperature will deposit the hydrochloric acid solution that good Mo-Fe alloy layer places 1 mol/L, and the Fe composition in the alloy and HCl react and deviate from, and the time that alloy is taken off in control is 12 hours; Take off that alloy is complete to be dried after deionization washing.
The matrix that the 5th step will take off after the alloy treatment places tubular furnace, and in 600 ℃ of lower sintering, sintering time is controlled to be 90 min, namely makes thickness and be 2 microns nanometer sheet MoO 3Film.

Claims (5)

1. novel nano sheet film that can be used for sensor, it is characterized in that: described nanometer sheet film is by the nano-sheet WO that accounts for its quality 35% ~ 100% 3And MoO 3In one or more, and account for the W of its quality 0% ~ 65% or one or more compositions among the Mo.
2. nanometer sheet film according to claim 1, it is characterized in that: nanometer sheet length is 100 nanometers ~ 600 nanometers in the described nanometer sheet film, and width is 50 nanometers ~ 300 nanometers, and thickness is 20 nanometers ~ 100 nanometers.
3. nanometer sheet film according to claim 1, it is characterized in that: the integral thickness of described nanometer sheet film is 1 micron ~ 50 microns.
4. a novel nano sheet thin film technology method that can be used for sensor is characterized in that, with Na 2WO 4And Na 2MoO 4In one or more, FeSO 4, (NH4) 2C 4H 4O 6Configuration electrolytic solution prepares alloy layer by electro-deposition, and described alloy layer growth in situ is on the parent metal sheet; Obtain product by the deposit film of deviating from the Fe composition rear oxidation nano-sheet in the alloy, concrete steps are as follows:
(1) configuration electrolytic solution, wherein electrolytic solution is composed as follows:
Na in the electrolytic solution 2WO 4And Na 2MoO 4Total concentration be 0.15 ~ 0.25mol/L, FeSO 4Concentration be 0.02 ~ 0.03 mol/L, (NH 4) 2C 4H 4O 6Concentration be 0.2 ~ 0.3 mol/L;
(2) electrodeposition technology:
Matrix is cut into required form, after sand papering, use successively respectively ultrasonic cleaning 10 min of acetone, alcohol and deionized water; Then the pH value of regulating electrolytic solution is 3 ~ 5; Then electrolytic solution is put into heating arrangement, heating and temperature control is at 40 ℃ ~ 60 ℃; Take matrix as negative electrode, graphite is anode, passes into 0.05 A/cm 2~ 0.4 A/cm 2Direct current carry out electro-deposition, electrodeposition time is controlled at 2 min ~ 15 min; The complete coating of electro-deposition dries after washing, i.e. the alloy layer of system;
(3) take off alloying technology:
Compound concentration is the aqueous hydrochloric acid solution of 1 mol/L, at room temperature will deposit good alloy layer and place hydrochloric acid solution, and the Fe composition in the alloy layer and HCl reaction are and dissolved, and control is taken off the time of alloy at 3 hours ~ 24 hours; It is complete through washed with de-ionized water to take off alloy, obtains deposit film after naturally drying;
(4) deposit film oxidation technology:
The deposit film that will take off after the alloy treatment places tubular furnace, and in 450 ℃ ~ 700 ℃ lower sintering, sintering time is controlled at 30 min ~ 240 min, namely makes the nanometer sheet film in the air atmosphere.
5. method according to claim 4, it is characterized in that: described matrix is pure tungsten, stainless steel or fine copper metal.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105510398A (en) * 2015-09-08 2016-04-20 浙江大学 Film-type alcohol gas-sensitive sensor and preparation method thereof
CN106746724A (en) * 2017-02-21 2017-05-31 上海第二工业大学 A kind of molybdenum oxide electrochromism nano thin-film and preparation method thereof
CN107522229A (en) * 2017-07-24 2017-12-29 桂林理工大学 One kind (Y1‑xLnx)2(MoO4)3The direct preparation method of film
CN108107098A (en) * 2018-01-30 2018-06-01 集美大学 Based on WO3The method of alcoholic strength in/FTO photoelectric materials detection white wine

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105510398A (en) * 2015-09-08 2016-04-20 浙江大学 Film-type alcohol gas-sensitive sensor and preparation method thereof
CN106746724A (en) * 2017-02-21 2017-05-31 上海第二工业大学 A kind of molybdenum oxide electrochromism nano thin-film and preparation method thereof
CN106746724B (en) * 2017-02-21 2019-11-12 上海第二工业大学 A kind of molybdenum oxide electrochromism nano thin-film and preparation method thereof
CN107522229A (en) * 2017-07-24 2017-12-29 桂林理工大学 One kind (Y1‑xLnx)2(MoO4)3The direct preparation method of film
CN107522229B (en) * 2017-07-24 2019-10-11 桂林理工大学 One kind (Y1-xLnx)2(MoO4)3The direct preparation method of film
CN108107098A (en) * 2018-01-30 2018-06-01 集美大学 Based on WO3The method of alcoholic strength in/FTO photoelectric materials detection white wine

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