CN104764779A - Preparation method of flexible gas-sensitive sensor with spongy graphene/zinc oxide mixed structure - Google Patents
Preparation method of flexible gas-sensitive sensor with spongy graphene/zinc oxide mixed structure Download PDFInfo
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Abstract
The invention relates to a preparation method of a flexible gas-sensitive sensor with a spongy graphene/zinc oxide mixed structure. The preparation method comprises the following steps of: firstly placing foam metal into a heating area of a vacuum reaction furnace, vacuumizing, simultaneously heating to a preset temperature, charging hydrogen into the vacuum reaction furnace; after heating to the preset temperature, introducing a carbon source and simultaneously keeping the flow of the hydrogen constant, thus obtaining a substrate directly deposited with graphene after 10-180 minutes; then soaking the prepared graphene/foam metal in etching solution, displacing off the foam metal, fishing out flexible graphene from the etching solution, cleaning, and fishing the graphene out by using a flexible substrate; finally, with the flexible substrate coated with conductive graphene as a cathode, a platinum sheet as a counter electrode, and Ag/Cl as a reference electrode, in the filling solution, adopting by taking Zn-containing solution as electrolyte, carrying out electrolytic growth to obtain a zinc-oxide nano structure. The preparation method has the beneficial effects that the sensitivity and the response speed are improved, and the development prospect on the aspects of environmental monitoring and chemical-gas detection and the like is important.
Description
Technical field
The present invention relates to a kind of preparation method of gas nanosensor, be specifically related to a kind of gas sensor preparation method based on three-dimensional grapheme and zinc-oxide nano mixed structure, belong to sensor technical field.
Background technology
Gas sensor has important effect in current environment, chemical gas detection, the detection of food industry health etc.The research of flexible substrate low temperature gas sensor to expand sensor monitoring range, optimized fabrication technological process, reduce the aspect such as service wear and risk and have great importance.Research and development have high sensitivity, transparent/flexible gas sensitive of high selectivity, fast response and good stability has important effect to preparation high-performance gas sensor.
Independent Graphene or zinc paste gas sensor all have its defect, and not Portable belt, inflexibility, needs to find new preparation technology and is worth to improve its performance and operational, accomplish efficient convenience, large-scale production.Three-dimensional grapheme increases and gas-contact area greatly, makes its sensitivity higher.The growth of one-dimension zinc oxide nano-array is built mixing nanostructured in Flexible graphene, it is made to have the excellent air-sensitive performance of Flexible graphene and one-dimension zinc oxide nanostructured concurrently, for it opens up new footpath in the application of flexible cryogenic gas sensor, there is compared with traditional sensors more excellent detection perform.Should have better air-sensitive performance in theory, up to now, we do not retrieve relevant experimental study, and this is the important starting point of invention research.
Summary of the invention
The object of the invention is for overcoming above-mentioned the deficiencies in the prior art, the preparation method of a kind of spongy graphene/zinc paste mixed structure flexible air dependent sensor is provided.
The technical scheme that the present invention takes is:
A preparation method for spongy graphene/zinc paste mixed structure flexible air dependent sensor, comprises step as follows:
(1) chemical gaseous phase depositing process prepares spongy graphene material on foam metal
Foam metal is put into vacuum reaction stove heating region, vacuumize, heat simultaneously, hydrogen is injected vacuum reaction stove, after being heated to predetermined temperature 100-500 DEG C, then constant temperature 10-30 minute anneals, then after being heated to predetermined temperature 900-1100 DEG C, carbon source is passed into vacuum reaction stove, keep hydrogen flowing quantity constant simultaneously, grow and close gas after 5-180 minute and be down to the substrate that room temperature can obtain Direct precipitation Graphene, i.e. Graphene/foam metal;
(2) preparation of flexible spongy graphene and transfer
Be immersed in etching solution by the Graphene/foam metal of preparation, the control reaction time makes its metal be fallen to become Flexible graphene by chemical replacement, adopts seal style transfer method to be pulled out by Graphene, naturally dry, obtain flexible spongy graphene by flexible substrate;
(3) three-electrode method growth of zinc oxide nano structure on flexible substrate Graphene
Do negative electrode with the flexible substrate being coated with flexible spongy graphene, platinized platinum is cooked electrode, and Ag/Cl electrode is contrast electrode; Fill in solution at potassium chloride, with the solution containing Zn for electrolyte, electrolytic growth nano structure of zinc oxide under 20-80 DEG C of low temperature, obtains Graphene/zinc paste mixed structure;
(4) prepare electrode material at Graphene/zinc paste mixed structure two ends, just obtain corresponding gas sensor.
In above-mentioned preparation method,
Foam metal described in step () is one in nickel foam, palladium, ruthenium, iridium, copper or foamed alloy.Described foam metal is of a size of 1cm × 1cm-30cm × 30cm.Described carbon source is one or several in methane, acetylene, ethene.The flow control of described carbon source is at 1-300sccm, and purity is higher than 99.99%; The flow control of described hydrogen is at 1-100sccm, and purity is higher than 99.99%.Described vacuum reaction stove evacuation degree is 3 × 10
-3-3 × 10
-6torr, to remove the active gases in furnace chamber, keeps clean growing environment.Described annealing refers to process substrate surface being dispelled to the magazines such as oxide.After obtaining the substrate of Direct precipitation Graphene, close carbon-source gas valve, keep the constant cooling of hydrogen flowing quantity, take out the Graphene of deposition afterwards.
The method of taking out backing material is closed hydrogen gas valve, vacuum pump, with air, reacting furnace cavity is filled to an atmospheric pressure state, is then taken out by backing material after being to wait vacuum reaction furnace temperature to drop to room temperature.In the Graphene/foam metal of preparation, the number of plies of Graphene is 1-10 layer.
Described in step (two), etching solution is iron chloride or iron nitrate solution, and described solution concentration is 0.5-5mol/L; Described flexible substrate is the substrates such as PMMA, PDFS; The described reaction time is between 15-1000 minute, and described temperature of reaction is 10-50 DEG C; Described seal style transfer method is specially: cover in spongy graphene by flexible substrate, gently presses 10-30 second, then slowly lifts gently from a side of substrate, utilize the little contact force between Graphene and substrate, pulled out by graphene substrate.
Filling solution described in step (three) is KCl solution, and concentration is 1.5-5mol/L; Described electrolyte is zinc nitrate aqueous solution, and concentration is 1.5-5mol/L.
Prepare electrode material in step (four) and comprise two kinds of methods, one, directly can to stretch the disconnected two ends sticking at Graphene/zinc paste mixed structure of conductive material with adhesive tape or glue; Described electrode material comprises the conductive carbon fibre that can stretch, conductive carbon nanotube fiber, conductive graphene fiber etc. can drawing of fiber electrode.Its two be utilize depositing device directly the two ends of the Graphene that can stretch/zinc paste mixed structure deposition on disconnected electrode material, specifically comprise following preparation process:
(1) Graphene/zinc paste mixed structure is put into low temperature depositing system;
(2) prepare the shutter that there is the empty bar of rectangle at two ends, be placed in the top of Graphene/zinc paste mixed structure, attention can not contact mixed structure, in order to avoid damage the gas sensitive of preparation;
(3) depositing device is utilized to deposit the metal electrode of not UNICOM at Graphene/zinc paste mixed structure two ends;
Described depositing device comprises the low temperature depositing systems such as magnetron sputtering deposition system, evaporator, impulse laser deposition system; Described electrode material comprises the metal materials such as copper, iron, silver, platinum.
Graphene prepared by the present invention/zinc paste mixed structure has extraordinary electric conductivity, does not need middle grid electrode, unlike Semiconductor gas sensors material.
The present invention utilizes chemical vapour deposition technique to prepare the Graphene of large area different shape, is transferred to flexible substrate by wet method, through optimization Graphene and zinc paste two kinds of gas sensitives, prepares gas sensor.Flexible substrate expands sensing range, environmental protection and with low cost, light flexible, and abandoning tradition rigid material is heavy, not Portable belt and inflexible shortcoming; Three-dimensional structure adds and gas-contact area, takes full advantage of the adsorptive power of Graphene; Zinc paste has excellent gas-sensitive property, and the two mixing makes this invention have the excellent properties of two kinds of gas sensitives concurrently, thus improves sensitivity and response speed, in environmental monitoring, chemical gas detection etc., have important development prospect.
The invention has the beneficial effects as follows,
1) spongy graphene growth temperature accurately controls;
2) the Graphene defect peak grown is low, has high crystal mass;
3) Graphene grown has fabulous conductivity;
4) the Graphene size grown only by the restriction of CVD cavity, can realize the large area deposition of Graphene;
5) do not need in wet method transfer process to use PMMA glue, time saving and energy saving;
6) transfer process adopts seal style transfer, and Graphene can not arbitrarily drift in the solution, and avoid the damage of Graphene in transfer process, process is simple.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that the embodiment of the present invention prepares Graphene/zinc paste mixed structure.
Fig. 2 is the SEM figure that the embodiment of the present invention prepares Graphene/zinc paste mixed structure.
Flexible spongy graphene/zinc paste mixed structure the formation state (left side) of Fig. 3 and case of bending (right side) image.
Fig. 4 is the air-sensitive character test pattern under the case of bending of Graphene/zinc paste mixed structure prepared by the embodiment of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only limitted to interpretation the present invention, be not intended to limit the present invention.Described material all can obtain from open commercial sources if no special instructions.
Embodiment 1
At nickel foam Grown Graphene also final growing graphene/zinc paste mixed structure, as shown in Figure 1, comprise following preparation process
1. get and be of a size of 6cm × 8cm nickel foam and be placed in tubular furnace;
2. open vacuum pump and the air pressure of tubular furnace is evacuated to end vacuum state 3 × 10
-6holder (Torr);
3. keep vacuum state 3 × 10
-6torr is (the vacuum effect of 15 minutes is the impurity, air etc. of dispelling quartz ampoule inside, guarantees that reaction chamber is clean) after 15 minutes, and the air pressure of quartz ampoule 3 is raised to 3 × 10
-3torr;
4. hydrogen flowmeter is set as 100sccm, and hydrogen is injected vacuum chamber;
5. tubular furnace temperature is to after 300 DEG C, and constant temperature is annealed for 20 minutes;
6. tubular furnace temperature is to after 10000 DEG C, and methane is injected vacuum chamber, gas meter is set as 200sccm, stops and grows for 30 minutes;
7. close methane gas flowmeter and tubular furnace temperature is down to room temperature fast with the speed of 30-60 DEG C/min;
8. close hydrogen flowmeter and vacuum pump;
9. open valve, with air, quartz ampoule air pressure is filled to an atmospheric pressure state;
10. open quartz ampoule vacuum interface, take out the nickel foam of deposited graphite alkene;
Graphene/the nickel foam of 11. preparations is immersed in FeCl
3(1mol/L) in solution 180 minutes;
Spongy graphene acetone, ethanol and deionized water are cleaned 3 minutes by 12. respectively;
13. cover graphenic surface by flexible substrate, and light pressure 15 seconds, then slowly lifts from a side of substrate gently;
14. dry in the air 3 hours in an atmosphere;
The Flexible graphene substrate of preparation is put into the KCl solution of 1.5mol/L by 15., do negative electrode with the flexible substrate covering conductive graphene, platinized platinum is cooked electrode, and Ag/Cl electrode is contrast electrode, take zinc nitrate solution as electrolyte, at low temperatures growth of zinc oxide nano structure;
The gas-sensitive property of Graphene/zinc paste mixed structure is prepared in test: the SEM that accompanying drawing 2 prepares Graphene/zinc paste mixed structure for the embodiment of the present invention schemes.Accompanying drawing 4 prepares the air-sensitive character figure of mixed structure for the present invention, has good air-sensitive performance.
16. prepare electrode material at Graphene/zinc paste mixed structure two ends, just obtain corresponding gas sensor.
Embodiment 2
At foam copper Grown Graphene also final growing graphene/zinc paste mixed structure, as shown in Figure 1, comprise following preparation process
1. get and be of a size of 6cm × 8cm foam copper and be placed in tubular furnace;
2. open vacuum pump and the air pressure of tubular furnace is evacuated to end vacuum state 3 × 10
-6holder (Torr);
3. keep vacuum state 3 × 10
-6torr is (the vacuum effect of 15 minutes is the impurity, air etc. of dispelling quartz ampoule inside, guarantees that reaction chamber is clean) after 15 minutes, and the air pressure of quartz ampoule 3 is raised to 3 × 10
-3torr;
4. hydrogen flowmeter is set as 100sccm, and hydrogen is injected vacuum chamber;
5. tubular furnace temperature is to after 300 DEG C, and constant temperature is annealed for 20 minutes;
6. tubular furnace temperature is to after 10000 DEG C, and methane is injected vacuum chamber, gas meter is set as 200sccm, stops and grows for 30 minutes;
7. close methane gas flowmeter and tubular furnace temperature is down to room temperature fast with the speed of 30-60 DEG C/min;
8. close hydrogen flowmeter and vacuum pump;
9. open valve, with air, quartz ampoule air pressure is filled to an atmospheric pressure state;
10. open quartz ampoule vacuum interface, take out the foam copper of deposited graphite alkene;
Graphene/the foam copper of 11. preparations is immersed in FeCl
3(1mol/L) in solution 180 minutes;
Spongy graphene acetone, ethanol and deionized water are cleaned 3 minutes by 12. respectively;
13. can cover graphenic surface by stretch tape with the 3M of prestretched, and light pressure 15 seconds, then slowly lifts from a side of substrate gently;
14. dry in the air 3 hours in an atmosphere, allow the substrate of prestretched reply the original length;
The stretched graphene substrate of preparation is put into the KCl solution of 1.5mol/L by 15., do negative electrode with the flexible substrate covering conductive graphene, platinized platinum is cooked electrode, and Ag/Cl electrode is contrast electrode, take zinc nitrate solution as electrolyte, at low temperatures growth of zinc oxide nano structure;
16. prepare electrode material at Graphene/zinc paste mixed structure two ends, just obtain corresponding gas sensor.
Finally should be noted that, the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in previous embodiment, or to wherein partly carrying out equivalent replacement.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a preparation method for spongy graphene/zinc paste mixed structure flexible air dependent sensor, is characterized in that, comprise step as follows:
(1) chemical gaseous phase depositing process prepares spongy graphene material on foam metal
Foam metal is put into vacuum reaction stove heating region, vacuumize, heat simultaneously, hydrogen is injected vacuum reaction stove, after being heated to predetermined temperature 100-500 DEG C, then constant temperature 10-30 minute anneals, then after being heated to predetermined temperature 900-1100 DEG C, carbon source is passed into vacuum reaction stove, keep hydrogen flowing quantity constant simultaneously, grow and close gas after 5-180 minute and be down to the substrate that room temperature can obtain Direct precipitation Graphene, i.e. Graphene/foam metal;
(2) preparation of flexible spongy graphene and transfer
Be immersed in etching solution by the Graphene/foam metal of preparation, the control reaction time makes its metal be fallen to become Flexible graphene by chemical replacement, adopts seal style transfer method to be pulled out by Graphene, naturally dry, obtain flexible spongy graphene by flexible substrate;
(3) three-electrode method growth of zinc oxide nano structure on flexible substrate Graphene
Do negative electrode with the flexible substrate being coated with flexible spongy graphene, platinized platinum is cooked electrode, and Ag/Cl electrode is contrast electrode; Fill in solution at potassium chloride, with the solution containing Zn for electrolyte, electrolytic growth nano structure of zinc oxide under 20-80 DEG C of low temperature, obtains Graphene/zinc paste mixed structure;
(4) prepare electrode material at Graphene/zinc paste mixed structure two ends, just obtain corresponding gas sensor.
2. the preparation method of a kind of spongy graphene according to claim 1/zinc paste mixed structure flexible air dependent sensor, it is characterized in that, the foam metal described in step () is one in nickel foam, palladium, ruthenium, iridium, copper or foamed alloy; Described foam metal is of a size of 1cm × 1cm-30cm × 30cm.
3. the preparation method of a kind of spongy graphene according to claim 1/zinc paste mixed structure flexible air dependent sensor, is characterized in that, carbon source described in step () is one or several in methane, acetylene, ethene.
4. the preparation method of a kind of spongy graphene according to claim 1/zinc paste mixed structure flexible air dependent sensor, it is characterized in that, described in step (), the flow control of carbon source is at 1-300sccm, and purity is higher than 99.99%; The flow control of described hydrogen is at 1-100sccm, and purity is higher than 99.99%.
5. the preparation method of a kind of spongy graphene according to claim 1/zinc paste mixed structure flexible air dependent sensor, it is characterized in that, described in step (), vacuum reaction stove evacuation degree is 3 × 10
-3-3 × 10
-6torr.
6. the preparation method of a kind of spongy graphene according to claim 1/zinc paste mixed structure flexible air dependent sensor, it is characterized in that, described in step (two), etching solution is iron chloride or iron nitrate solution, and described solution concentration is 0.5-5mol/L.
7. the preparation method of a kind of spongy graphene according to claim 1/zinc paste mixed structure flexible air dependent sensor, is characterized in that, the reaction time described in step (two) is between 15-1000 minute, and described temperature of reaction is 10-50 DEG C.
8. the preparation method of a kind of spongy graphene according to claim 1/zinc paste mixed structure flexible air dependent sensor, it is characterized in that, described in step (two), seal style transfer method is specially: cover in spongy graphene by flexible substrate, light pressure 10-30 second, then slowly lift gently from a side of substrate, utilize the little contact force between Graphene and substrate, graphene substrate is pulled out.
9. the preparation method of a kind of spongy graphene according to claim 1/zinc paste mixed structure flexible air dependent sensor, it is characterized in that, the filling solution described in step (three) is KCl solution, and concentration is 1.5-5mol/L; Described electrolyte is zinc nitrate aqueous solution, and concentration is 1.5-5mol/L.
10. the preparation method of a kind of spongy graphene according to claim 1/zinc paste mixed structure flexible air dependent sensor, is characterized in that, the electrode material described in step (four) comprise metal material, can drawing of fiber electrode; Prepare electrode material and comprise two kinds of methods, one, directly can the disconnected two ends sticking at Graphene/zinc paste mixed structure of drawing of fiber electrode with adhesive tape or glue; Its two be utilize depositing device directly the two ends of the Graphene that can stretch/zinc paste mixed structure deposition on disconnected electrode material.
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