CN108862247A - A kind of gas molecule detection composite membrane - Google Patents
A kind of gas molecule detection composite membrane Download PDFInfo
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- CN108862247A CN108862247A CN201810753283.5A CN201810753283A CN108862247A CN 108862247 A CN108862247 A CN 108862247A CN 201810753283 A CN201810753283 A CN 201810753283A CN 108862247 A CN108862247 A CN 108862247A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
Abstract
The invention discloses a kind of gas molecule detection membranes, are prepared by the following：The functional layer of one layer of nanometer grade thickness is deposited in the graphene oxide film surface being deposited in AAO substrate, then removes graphene-based composite nanometer film using water stripping means.Present invention obviates reduction removing, etching two kinds of removing means of removing, the graphene film that guarantee removing obtains keeps its original form, structure and performance on AAO basilar memebrane not by any destruction.It is reusable meanwhile to AAO basilar memebrane also without generating any destruction.Since this graphene film thickness is small, it might even be possible to reach several nanometers, this detection membrane has high sensitivity.
Description
Technical field
The present invention relates to sensor fields more particularly to a kind of gas molecule to detect composite membrane.
Background technique
Since 2010, graphene and its derivative have obtained the pass of every field due to its brilliant physical and chemical performance
Note.Graphene oxide is the most important presoma for preparing graphene, while it also has itself unique physical property, has
A large amount of defect, oxygen-containing functional group etc., therefore there is very high optical clarity, high-hydrophilic, high band gap etc..Based on this,
It is got the attention in terms of humidity detection.
Mainly with the methods of drop coating, spin coating, spraying in terms of humidity detection, the method has following graphene oxide at present
Drawback：First, surface texture is uncontrollable；Second, uniformity is uncontrollable；Third, thickness are uncontrollable；4th, film internal structure is not
Controllably.In summary factor, the graphite oxide alkenyl humidity detection membrane done do not have good linear response, and when response
Between it is very long.
For this purpose, we devise nanometer thickness fold graphene film.The structure of fold ensure that the response of gas molecule detection
Area.Its nanoscale thickness and the numerous empty structure of chemical oxidation graphene surface make gas whole with quick penetration
A film, ensure that film height responsiveness and the very short response time.
In addition, graphene is not omnipotent material, under special cases, polymer or metal can make up graphene
Deficiency so that film reaches application demand.Based on this, we devise the separation side of nanometer thickness graphene composite film
Graphene is filtered form a film first by method, then by modes such as suction filtration, spin coating, magnetron sputterings by metal or inorganic nano-particle
Son etc. uniformly invests graphene surface, is prepared into graphene/inorganic nano-particle (or metal) composite membrane.Then graphite is utilized
Alkene and the method for sole separation prepare the graphene composite film bubbled through the water column.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of gas molecule detection composite membrane.
The purpose of the present invention is what is be achieved through the following technical solutions：A kind of gas molecule detection composite membrane, by following
Method is prepared：
(1) it is filtered on AAO basilar memebrane and obtains graphene oxide membrane；
(2) in graphene oxide basement membrane surface metal composite oxide layer or metal layer, ultrathin membrane is formed；
(3) AAO for being loaded with membrane structure is placed on the water surface with face-up where ultrathin membrane；AAO is pressed, so that under AAO
It is heavy, obtain the graphene-based ultrathin membrane for floating on the water surface.
(4) the graphene-based ultrathin membrane for floating on the water surface is picked up from the bottom up with silicon wafer substrate, so that graphene film is flat
It is laid on substrate surface；
(5) moisture in graphene-based ultrathin membrane is evaporated at room temperature, so that water content is greater than 50wt%；After evaporation process
Graphene-based ultrathin membrane be freeze-dried, graphene oxide membrane from silicon chip surface be detached from.
(6) graphene-based ultrathin membrane is restored, so that its conductivity is greater than 50S/cm.
Further, the thickness of the ultrathin membrane is less than 100nm.
Further, the thickness of the graphene-based counterdie is less than 100nm.
Further, in the step 3, pressing position is the edge of AAO.
Further, the graphene-based counterdie with a thickness of 4nm.
Further, the porosity on the surface of the AAO basilar memebrane is not less than 40%.
Further, the metal layer is Pt, and complex method is magnetron sputtering.
Further, the metal oxide layer is SnO2、ZnO、WO3、Cu2O、Co3O4、NiO、In2O3、MoO2.Composite square
Method is magnetron sputtering, spin coating.
Further, in the step 5, restoring method includes electronation, thermal reduction；What the electronation used goes back
Former agent is selected from hydrazine hydrate, hydroiodic acid；Thermal reduction is specially：200 DEG C of aqueous vapour reducings.
The beneficial effects of the present invention are：The method that the present invention filters prepares film, ensure that the uniform of laminated film
The stability of property and device；It is improved using the method that water shifts by the thickness control of graphene composite film in Nano grade
The responsiveness of film, while in transfer process, microcosmic fold is introduced, the response speed of film is increased.Whole process letter
List, easily operates green.
Detailed description of the invention
Fig. 1 is the flow diagram of AAO substrate film stripping graphene film.
Fig. 2 is the experimentation figure of embodiment 1AAO substrate film stripping graphene film.
Fig. 3 is the atomic force microscopy diagram of graphene film made from embodiment 1.
Fig. 4 is the scanning figure for the graphene-based Pt nanometer film that embodiment 2 is prepared.
Fig. 5 is the atomic force microscopy diagram of graphene-based Pt nanometer film made from embodiment 2.
Fig. 6 is the graphene-based SnO that embodiment 3 is prepared2The atomic force microscopy diagram of nanometer film.
Fig. 7 is the atomic force microscopy diagram for the graphene film that embodiment 4 is prepared.
Fig. 8 is the graphene-based MoO that embodiment 5 is prepared2The atomic force microscopy diagram of nanometer film.
Fig. 9 is the experimentation figure of comparative example 1MCE substrate film stripping graphene film.
Specific embodiment
Embodiment 1
By controlling the concentration of graphene solution, filter to obtain ultra-thin oxygen reduction in AAO basilar memebrane by suction filtration method
Graphite alkene film；Surface is fitted with to the AAO basilar memebrane (porosity 40%) of redox graphene film, with graphene film institute
It is face-up, be placed on the water surface, such as Fig. 1 a and 2a；AAO basilar memebrane is pressed, such as Fig. 2 b, AAO basilar memebrane starts to sink, and such as schemes
2c, finally, AAO basilar memebrane is sunken to bottom of a cup, graphene film (in virtual coil) floats on the water surface, such as Fig. 1 b and 2d.
The graphene film for floating on the water surface is picked up from the bottom up with silicon wafer substrate, so that graphene film is laid in substrate table
It is tested with a thickness of 4nm, as shown in Figure 3 by atomic force microscope after natural drying in face.
Embodiment 2
(1) it according to the suction filtration method of such as embodiment 1, filters to obtain the reduction-oxidation graphite with a thickness of 4nm in AAO basilar memebrane
Alkenyl counterdie.
(2) by magnetically controlled sputter method, Pt nanometer layer is sputtered in the graphene membrane surface of step 1；
(3) it with face-up where ultrathin membrane, is placed on the water surface；The edge AAO is pressed, AAO basilar memebrane starts to sink, most
Afterwards, AAO basilar memebrane is sunken to bottom of a cup, and graphite film floats on the water surface, and graphene-based Pt nanometer film is successfully removed.
The graphene-based Pt nanometer film for floating on the water surface is picked up from the bottom up with silicon wafer substrate, so that graphene-based Pt receives
Rice film is laid in substrate surface, at room temperature the moisture 30min in thin evaporated film, and measuring water content is 67wt%；By evaporation process
Graphene-based Pt nanometer film afterwards is freeze-dried, and is detached from from silicon chip surface, and surface has a large amount of folds, as shown in Figure 4；It is logical
It crosses atomic force microscope and tests it with a thickness of 18nm, as shown in Figure 5.
It is transferred in 200 DEG C of vapor and is restored, restore 1h, measure its conductivity 54S/cm after dry.In graphene
The both ends spraying gold electrode of film is exported for electric signal.
Graphene composite film (size 2mm) after above-mentioned reduction is placed in H2To be supervised in the vacuum glove box of 1ppm in real time
Its resistance variations is surveyed, as shown in table 1.
Embodiment 3
(1) it according to the suction filtration method of such as embodiment 1, filters to obtain the reduction-oxidation graphite with a thickness of 4nm in AAO basilar memebrane
Alkenyl counterdie.
(2) by magnetically controlled sputter method, SnO is filtered in the graphene membrane surface of step 12Nanometer layer；
(3) it with face-up where ultrathin membrane, is placed on the water surface；The edge AAO is pressed, AAO basilar memebrane starts to sink, most
Afterwards, AAO basilar memebrane is sunken to bottom of a cup, and graphite film floats on the water surface, and graphene-based SnO2 nanometer film is successfully removed.
The graphene-based SnO of the water surface will be floated on silicon wafer substrate2Nanometer film picks up from the bottom up, so that graphene-based
SnO2Nanometer film is laid in substrate surface, at room temperature the moisture 30min in thin evaporated film, and measuring water content is 54wt%；It will steam
Hair treated graphene-based SnO2Nanometer film is freeze-dried, and is detached from from silicon chip surface, and surface has a large amount of folds；Pass through
Atomic force microscope tests it with a thickness of 38nm, as shown in Figure 6.
It is transferred in hydroiodic acid steam and is restored, restore 0.5h, measure its conductivity 86S/cm after dry.In graphene
The both ends spraying gold electrode of film is exported for electric signal.
Graphene composite film (size 2mm) after above-mentioned reduction is placed in the vacuum glove box that NO is 10ppm, is supervised in real time
Its resistance variations is surveyed, as shown in table 1.
Embodiment 4
By controlling the concentration of graphene solution, filter to obtain ultra-thin oxidation stone in AAO basilar memebrane by suction filtration method
Black alkene film；Surface is fitted with to the AAO basilar memebrane (porosity 60%) of graphene oxide membrane, with facing where graphene film
On, it is placed on the water surface, presses AAO substrate film edge, AAO basilar memebrane starts to sink, finally, AAO basilar memebrane is sunken to bottom of a cup, graphite
Alkene film floats on the water surface, and graphene film is successfully removed.
The graphene film for floating on the water surface is picked up from the bottom up with silicon wafer substrate, so that graphene film is laid in substrate table
It is tested with a thickness of 14nm, as shown in Figure 7 by atomic force microscope after natural drying in face.
Embodiment 5
(1) it according to the suction filtration method of such as embodiment 4, filters to obtain the graphene oxide with a thickness of 14nm in AAO basilar memebrane
Basilar memebrane.
(2) by suction filtration method, MoO is filtered in the graphene membrane surface of step 12Nanometer layer；
(3) it with face-up where ultrathin membrane, is placed on the water surface；The edge AAO is pressed, AAO basilar memebrane starts to sink, most
Afterwards, AAO basilar memebrane is sunken to bottom of a cup, and graphite film floats on the water surface, graphene-based MoO2Nanometer film is successfully removed.
The graphene-based MoO2 nanometer film for floating on the water surface is picked up from the bottom up with silicon wafer substrate, so that graphene-based poly-
Vinyl alcohol nanometer film is laid in substrate surface, at room temperature the moisture 30min in thin evaporated film, and measuring water content is 89wt%；It will
Graphene-based MoO after evaporation process2Nanometer film is freeze-dried, and is detached from from silicon chip surface, and surface has a large amount of folds；It is logical
It crosses atomic force microscope and tests it with a thickness of 66nm, as shown in Figure 8.
It is transferred in hydroiodic acid steam and is restored, restore 0.5h, measure its conductivity 84S/cm after dry.In graphene
The both ends spraying gold electrode of film is exported for electric signal.
Graphene composite film (size 2mm) after above-mentioned reduction is placed in H2S is in the vacuum glove box of 10ppm, in real time
Its resistance variations is monitored, as shown in table 1.
Remaining composite membrane and its response performance are as shown in table 1.
Table 1
Comparative example 1
(1) according to the suction filtration parameter of such as embodiment 4, with MCE basilar memebrane (porosity 60%) suction filtration obtain with a thickness of
The graphene oxide basilar memebrane of 14nm.
(2) by suction filtration method, polyvinyl alcohol layer is filtered in the graphene membrane surface of step 1；
(3) it with face-up where ultrathin membrane, is placed on the water surface, shown in Fig. 9 a, presses MCE substrate film edge, MCE substrate
Film does not sink, and shown in Fig. 9 b, graphene-based polyvinyl alcohol nano film stripping failure cannot obtain individual graphene-based polyethylene
Alcohol nanometer film.
It should be noted that suction method is the method for most uniformly preparing graphene film generally acknowledged at present, in certain suction filtration
Under liquid measure, concentration can be regulated and controled to control the thickness of graphene film, thickness is minimum to can be one layer of graphene, with stone
The increase of black alkene concentration, under pressure, newly-increased graphene is gradually filled into the gap of first layer graphene, so that first
Layer graphene is gradually filled up completely, and then develops into the second layer, constantly repeatedly above step, can be prepared thickness and be arrived across 2 layers
The graphene nano film of up to ten thousand layers of graphene.Therefore, those skilled in the art can be adjusted by simple experiment parameter and can be obtained
The graphene film with a thickness of 4nm is obtained, equally, the method that spin coating, magnetron sputtering etc. prepare film is also technology hand mature in the industry
Section.
Claims (9)
1. a kind of gas molecule detects composite membrane, which is characterized in that be prepared by the following method to obtain：
(1) it is filtered on AAO basilar memebrane and obtains graphene oxide membrane；
(2) in graphene oxide basement membrane surface metal composite oxide layer or metal layer, ultrathin membrane is formed；
(3) AAO for being loaded with membrane structure is placed on the water surface with face-up where ultrathin membrane；AAO is pressed, so that AAO sinks,
Obtain floating on the graphene-based ultrathin membrane of the water surface；
(4) the graphene-based ultrathin membrane for floating on the water surface is picked up from the bottom up with silicon wafer substrate, so that graphene film is laid in
Substrate surface.
(5) moisture in graphene-based ultrathin membrane is evaporated at room temperature, so that water content is greater than 50wt%；By the stone after evaporation process
Mertenyl ultrathin membrane is freeze-dried, and graphene oxide membrane is detached from from silicon chip surface.
(6) graphene-based ultrathin membrane is restored, so that its conductivity is greater than 50S/cm.
2. composite membrane according to claim 1, which is characterized in that the thickness of the ultrathin membrane is less than 100nm.
3. composite membrane according to claim 1, which is characterized in that the thickness of the graphene-based counterdie is less than 100nm.
4. composite membrane according to claim 1, which is characterized in that in the step 3, pressing position is the edge of AAO.
5. composite membrane according to claim 1, which is characterized in that the graphene-based counterdie with a thickness of 4nm.
6. detection composite membrane according to claim 1, which is characterized in that the porosity one on the surface of the AAO basilar memebrane
As be not less than 40%.
7. composite membrane according to claim 1, which is characterized in that the metal layer is Pt, and complex method is magnetron sputtering.
8. composite membrane according to claim 1, which is characterized in that the metal oxide layer is SnO2、ZnO、WO3、
Cu2O、Co3O4、NiO、In2O3、MoO2It is magnetron sputtering, spin coating Deng, complex method.
9. detection composite membrane according to claim 1, which is characterized in that in the step 5, restoring method includes that chemistry is gone back
Former, thermal reduction；The reducing agent that the electronation uses is selected from hydrazine hydrate, hydroiodic acid；Thermal reduction is specially：200 DEG C of vapor
Reduction.
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