CN109904002A - A kind of preparation method and bottom-resistive electrode of bottom-resistive electrode - Google Patents
A kind of preparation method and bottom-resistive electrode of bottom-resistive electrode Download PDFInfo
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- CN109904002A CN109904002A CN201910032827.3A CN201910032827A CN109904002A CN 109904002 A CN109904002 A CN 109904002A CN 201910032827 A CN201910032827 A CN 201910032827A CN 109904002 A CN109904002 A CN 109904002A
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Abstract
The embodiment of the present invention provides the preparation method and bottom-resistive electrode of a kind of bottom-resistive electrode, and the preparation method includes: to be covered with the insulating materials of metal layer to be immersed in graphene oxide solution, forms graphene layer;The mixed solution that graphene oxide and carbon nanotube are sprayed on the graphene layer, sprays carbon nano-tube solution on the mixed solution again;Insulating materials after spraying is annealed in the lehr, so that the graphene oxide of the graphene layer becomes redox graphene, obtains low-impedance electrode.The contact berrier between current collector layer and active layer can be reduced using the embodiment of the present invention, to reduce the contact impedance of electrode.
Description
Technical field
The present embodiments relate to micro Process and electrochemical technology field more particularly to a kind of preparation sides of bottom-resistive electrode
Method and bottom-resistive electrode.
Background technique
Carbon nanotube due to the natural porosity after its one-dimentional structure, high conductivity, high mechanical strength and its networking, at
For a kind of very potential super capacitor electrode, it is commonly applied to the demand of flexible energy storage and high speed charge and discharge.Though however,
Right carbon nanotube itself has preferable electric conductivity, with usually in supercapacitor as current collector layer metal (such as Au,
Pt, Cr etc.) all there is biggish contact resistance.Carbon nanotube is divided into semi-conductor type and conductor type, wherein semi-conductor type carbon nanometer
Pipe metal between will form Schottky barrier, it is equivalent and carry out a huge contact impedance;Although conductor type theoretically with metal
Between be Ohmic contact, however on the one hand due to its surface chemistry group influence, be on the other hand between substrate due to it
Line contact leads to equally have biggish contact resistance between conductor type carbon nanotube and metal.According to current report, it is based on
The supercapacitor of carbon nanotube, especially micro super capacitor, equal series resistance are nearly all greater than 10 ohm, this pole
The earth limits the high speed charging and discharging capabilities of micro super capacitor.
Summary of the invention
For the technical problems in the prior art, the embodiment of the present invention provides a kind of preparation method of bottom-resistive electrode
And bottom-resistive electrode.
In a first aspect, the embodiment of the present invention provides a kind of preparation method of bottom-resistive electrode, comprising:
The insulating materials for being covered with metal layer is immersed in graphene oxide solution, forms graphene layer;
The mixed solution that graphene oxide and carbon nanotube are sprayed on the graphene layer, sprays again on the mixed solution
Apply carbon nano-tube solution;
Insulating materials after spraying is annealed in the lehr, so that the graphene oxide of the graphene layer becomes oxygen reduction
Graphite alkene obtains low-impedance electrode.
Second aspect, the embodiment of the present invention provide a kind of bottom-resistive electrode, comprising: including the use of Low ESR electricity described above
Electrode made from the preparation method of pole.
The preparation method and bottom-resistive electrode of bottom-resistive electrode provided in an embodiment of the present invention, using in current collector layer and activity
One layer of graphene layer is increased between layer, the bottom-resistive electrode is consequently formed, reduces connecing between current collector layer and active layer
Potential barrier is touched, contact impedance is reduced.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is this hair
Bright some embodiments for those of ordinary skill in the art without creative efforts, can be with root
Other attached drawings are obtained according to these attached drawings.
Fig. 1 is the flow diagram of the preparation method of bottom-resistive electrode provided in an embodiment of the present invention;
Fig. 2 is the original provided in an embodiment of the present invention using graphene interlayers to reduce carbon nanotube electrode contact resistance
Manage schematic diagram;
Fig. 3 is electrode preparation method provided in an embodiment of the present invention and schematic illustration;
Fig. 4 a is the photo for the low-impedance device that one embodiment of the invention provides;
Fig. 4 b is the interdigital electrode front SEM figure that one embodiment of the invention provides;
Fig. 4 c is the carbon nanotube layer front SEM figure that further embodiment of this invention provides;
Fig. 4 d-4e is the single-layer graphene SEM figure in self assembly provided in an embodiment of the present invention;
Fig. 4 f is that the section SEM of entire electrode provided in an embodiment of the present invention schemes;
Fig. 5 is the impedance spectrum test comparison curve graph for the bottom-resistive electrode that one embodiment of the invention provides;
Fig. 6 is the cyclic voltammetry comparison diagram for the bottom-resistive electrode that one embodiment of the invention provides.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art
Every other embodiment obtained without creative efforts, shall fall within the protection scope of the present invention.
Fig. 1 is the flow diagram of the preparation method of bottom-resistive electrode provided in an embodiment of the present invention, as shown in Figure 1, institute
The method of stating includes:
S101, the insulating materials for being covered with metal layer are immersed in graphene oxide solution, form graphene layer;
The mixed solution that graphene oxide and carbon nanotube are sprayed on S102, the graphene layer, in the mixed solution
On spray carbon nano-tube solution again;
Insulating materials after S103, spraying is annealed in the lehr, so that the graphene oxide of the graphene layer becomes
Redox graphene obtains low-impedance electrode.
The embodiment of the present invention provides a kind of preparation method of bottom-resistive electrode, and the embodiment of the present invention is primarily directed to carbon nanometer
Impedance between pipe and metal substrate, the embodiment of the present invention is using there are biggish between the carbon nanotube and metal substrate of script
Contact berrier, after introducing graphene interlayers, former big potential barrier has been converted into is almost equal to zero between carbon nanotube and graphene
Potential barrier, in addition with contact berrier lesser between graphene and metal.
Specifically: since metal substrate immerses in ready PDDA (diallyl dimethyl ammoniumchloride) solution, make
It obtains PDDA molecule and is uniformly assembled in Au substrate surface, make the surface Au uniformly positively charged, then go the immersion of Au interdigital electrode
In ionized water 5 minutes to remove the PDDA molecule on unattached, the positively charged Au interdigital electrode in surface is immersed in
Graphene oxide solution, since GO lamella is uniformly negatively charged, and the surface Au is positively charged, so GO lamella can due to Electrostatic Absorption and
One layer of self assembly on Au substrate.Form graphene layer.
Graphene oxide and the mixed solution of carbon nanotube are sprayed on the graphene layer with spray gun, the purpose of this step is
The contact area for increasing surface, further sprays carbon nano-tube solution, spraying concentration and spraying again on the mixed solution
Depending on amount is according to required CNT thickness;
After drying at room temperature, the insulating materials after spraying is annealed in the lehr, so that the oxidation stone of the graphene layer
Black alkene becomes redox graphene, obtains low-impedance electrode.
The preparation method of bottom-resistive electrode provided in an embodiment of the present invention is increased using between current collector layer and active layer
One layer of graphene layer, is consequently formed the bottom-resistive electrode, reduces the contact berrier between current collector layer and active layer, reduces
Contact impedance.
Optionally, described to be immersed in graphene oxide solution in the insulating materials for being covered with metal layer, and before taking out cleaning,
Further include:
A layer photoresist is applied on the insulating material, is exposed together with figuratum mask plate, is removed uncured light
Photoresist;
The splash-proofing sputtering metal layer on the mask plate.
Optionally, the splash-proofing sputtering metal layer on the mask plate, specifically:
The layers of chrome that the first preset thickness is first sputtered on the mask plate, then sputters the layer gold of the second preset thickness.
Specifically, on that basi of the above embodiments, it is illustrated below with a specific example:
1) uniformly thermal oxide a layer thickness is the silicon oxide layer of 50-100nm on clean silicon wafer;
2) a layer thickness is got rid of on silicon oxide layer not less than 1 micron of thick photoresist, is exposed together with mask plate, is exposed
Depending on dosage is according to photoresist model and thickness.Then using the photoresist of corresponding developer solution removal uncured portion, wherein light
Depending on the model of photoresist and positive negativity foundation required thickness and mask plate;
3) the Cr layer for sputtering 5nm thickness, then sputters the Au layer of 50nm thickness, using oxygen plasma treatment five minutes,
So that layer gold has better hydrophily;
Optionally, the concentration of the graphene oxide solution is 1g/L.
Optionally, the graphene oxide and the mixed solution of carbon nanotube are by graphene oxide solution and carbon nanotube
Solution is mixed according to the ratio of 1:1.
On the basis of the above embodiments,
4) PDDA (diallyl dimethyl ammoniumchloride) for the silicon wafer for having sputtered Cr/Au layers being immersed 0.01mol/L is molten
5 minutes in liquid, then silicon chip extracting is immersed in deionized water 5 minutes, to wash the PDDA point for being not attached to the surface Au
Son;
5) attachment is immersed in GO (graphene oxide) solution of 1g/L 5 minutes with the silicon wafer of PDDA, then takes silicon wafer
It immerses in deionized water 5 minutes out, to wash the GO for being not attached to the surface Au;
6) it uses spray gun spraying in silicon wafer 1mLGO and the mixed solution (1:1wt/wt) of CNT (carbon nanotube), then sprays
The evenly dispersed CNT solution of 0.1g/L, depending on thickness of the quantity for spray according to required carbon nanotube electrode;
Optionally, before the insulating materials after the spraying is annealed in the lehr further include:
Insulating materials after the spraying is placed in acetone soln, residual photoresist is removed and is deposited on the spraying
The metal and carbon nanotube on insulating materials afterwards forms the structure of pattern on mask plate.
Optionally, pattern is interdigital pattern or annulus pattern on the mask plate.
7) silicon wafer is placed in acetone soln, jiggle with the metal that removes residual photoresist and be deposited thereon and
Carbon nanotube, at the structure of pattern on mask plate;Wherein, the pattern on mask plate can sets itself, in the embodiment of the present invention
In preferably interdigital pattern or annulus pattern.
Optionally, the insulating materials after the spraying is annealed in the lehr, and the temperature used is 900 degree.
8) at room temperature that silicon wafer is dry, subsequent 900 degree annealing 1 minute in the lehr, GO is reduced into rGO
(redox graphene).So far, the required carbon nanotube electrode with small impedance is obtained.
Optionally, the graphene layer with a thickness of 1nm.
On the basis of the above embodiments, Fig. 3 be electrode preparation method provided in an embodiment of the present invention and schematic illustration,
Using above-mentioned preparation method, obtained graphene layer is with a thickness of 1nm, as shown in Figure 2.
The embodiment of the present invention also provides a kind of bottom-resistive electrode, is made using the preparation method of above-mentioned bottom-resistive electrode,
Specific phenogram is as shown in Fig. 4 a-4f.
Fig. 5 is the impedance spectrum test comparison curve graph for the bottom-resistive electrode that one embodiment of the invention provides;It is received by pure carbon
The intersection point of the impedance spectrum curve and X-axis of mitron electrode and the carbon nanotube electrode with graphene interlayers, which is evident that, to be drawn
The contact impedance for having entered supercapacitor after graphene interlayers is substantially reduced;
Fig. 6 is the cyclic voltammetry comparison diagram for the bottom-resistive electrode that one embodiment of the invention provides, it is seen that due to having
Compared with Low ESR, device provided in an embodiment of the present invention can work normally under the up to scanning speed of 2000V/s.
The preparation method of bottom-resistive electrode provided in an embodiment of the present invention, first by Au interdigital electrode oxygen plasma obtained
Body handles 5 minutes so that negative electricity on the homogeneous band of the surface Au.Au substrate is then immersed to the PDDA of ready 0.01mol/L
5 minutes in (diallyl dimethyl ammoniumchloride) solution, so that PDDA molecule is uniformly assembled in Au substrate surface, the surface Au is allowed
It can be uniformly positively charged.Then by 5 minutes in Au interdigital electrode immersion deionized water to remove the PDDA molecule on unattached.
The positively charged Au interdigital electrode in surface is immersed in GO (graphene oxide) solution of 1g/L in next step, since GO lamella is uniform
It is negatively charged, and the surface Au is positively charged, so GO lamella can be due to Electrostatic Absorption and one layer of self assembly on Au substrate.
In addition, uniform whirl coating, exposure and development on the silicon wafer of silicon oxide layer, to obtain the light with interdigitated configuration
Photoresist layer, Cr/Au layers of uniform sputter on silicon wafer, then use one layer of GO film of the uniform self assembly of preceding method.It uses in next step
The purpose of mixed solution of a small amount of GO/CNT of spray gun spraying, this step is the contact area for increasing surface.It is molten that CNT is then sprayed again
Depending on liquid, spraying concentration and quantity for spray are according to required CNT thickness.Finally, obtained device is placed in after drying at room temperature
It anneals 1 minute in Muffle furnace in 900 degree, GO is reduced into rGO (redox graphene).
The method provided according to embodiments of the present invention, the GO layer of self assembly is with a thickness of 1nm in prepared bottom-resistive electrode
Left and right, can be confirmed as single layer two-dimensional material.It is tested according to impedance spectrum, the contact resistance of device obtained does not have graphene interlayers
When reduce about half, be down to about 2 ohms.According to test, the cyclic voltammetric rate of device is up to 2000V/s.
The preparation method and bottom-resistive electrode of bottom-resistive electrode provided in an embodiment of the present invention, using in current collector layer and activity
One layer of graphene layer is increased between layer, the bottom-resistive electrode is consequently formed, reduces connecing between current collector layer and active layer
Potential barrier is touched, contact impedance is reduced.
The apparatus embodiments described above are merely exemplary, wherein described, unit can as illustrated by the separation member
It is physically separated with being or may not be, component shown as a unit may or may not be physics list
Member, it can it is in one place, or may be distributed over multiple network units.It can be selected according to the actual needs
In some or all of the modules achieve the purpose of the solution of this embodiment.Those of ordinary skill in the art are not paying creativeness
Labour in the case where, it can understand and implement.
Through the above description of the embodiments, those skilled in the art can be understood that each embodiment can
It realizes by means of software and necessary general hardware platform, naturally it is also possible to pass through hardware.Based on this understanding, on
Stating technical solution, substantially the part that contributes to existing technology can be embodied in the form of software products in other words, should
Computer software product may be stored in a computer readable storage medium, such as ROM/RAM, magnetic disk, CD, including several fingers
It enables and using so that a computer equipment (can be personal computer, server or the network equipment etc.) executes each implementation
Method described in certain parts of example or embodiment.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features;
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (10)
1. a kind of preparation method of bottom-resistive electrode characterized by comprising
The insulating materials for being covered with metal layer is immersed in graphene oxide solution, forms graphene layer;
The mixed solution that graphene oxide and carbon nanotube are sprayed on the graphene layer, sprays carbon on the mixed solution again
Nanotube solution;
Insulating materials after spraying is annealed in the lehr, so that the graphene oxide of the graphene layer becomes oxygen reduction fossil
Black alkene obtains low-impedance electrode.
2. the method according to claim 1, wherein described be immersed in oxidation in the insulating materials for being covered with metal layer
Graphene solution, and before taking out cleaning, further includes:
A layer photoresist is applied on the insulating material, is exposed together with figuratum mask plate, is removed uncured photoresist;
The splash-proofing sputtering metal layer on the mask plate.
3. according to the method described in claim 2, it is characterized in that, the splash-proofing sputtering metal layer on the mask plate, specifically:
The layers of chrome that the first preset thickness is first sputtered on the mask plate, then sputters the layer gold of the second preset thickness.
4. the method according to claim 1, wherein the concentration of the graphene oxide solution is 1g/L.
5. the method according to claim 1, wherein the graphene oxide and the mixed solution of carbon nanotube are
Graphene oxide solution and carbon nano-tube solution are mixed according to the ratio of 1:1.
6. the method according to claim 1, wherein the graphene layer with a thickness of 1nm.
7. according to the method described in claim 2, it is characterized in that, the insulating materials after the spraying is annealed in the lehr
Before further include:
Insulating materials after the spraying is placed in acetone soln, after removing residual photoresist and being deposited on the spraying
Metal and carbon nanotube on insulating materials form the structure of pattern on mask plate.
8. the method according to the description of claim 7 is characterized in that pattern is interdigital pattern or doughnut on the mask plate
Case.
9. the method according to claim 1, wherein the insulating materials after the spraying is annealed in the lehr,
The temperature used is 900 degree.
10. a kind of bottom-resistive electrode, which is characterized in that including the use of the preparation of any one of the claim 1-9 plane electrode
Method is made.
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