CN113675006A - Preparation method of manganese-based oxide micro supercapacitor - Google Patents
Preparation method of manganese-based oxide micro supercapacitor Download PDFInfo
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- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 34
- 239000011572 manganese Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000000758 substrate Substances 0.000 claims abstract description 28
- 238000001704 evaporation Methods 0.000 claims abstract description 15
- 238000004544 sputter deposition Methods 0.000 claims abstract description 12
- 230000008020 evaporation Effects 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 7
- 238000001259 photo etching Methods 0.000 claims abstract description 7
- 229920002120 photoresistant polymer Polymers 0.000 claims abstract description 7
- 238000004528 spin coating Methods 0.000 claims abstract description 7
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000010931 gold Substances 0.000 claims abstract description 6
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 238000000576 coating method Methods 0.000 claims abstract description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052737 gold Inorganic materials 0.000 claims abstract description 4
- 238000002791 soaking Methods 0.000 claims abstract description 4
- 239000013077 target material Substances 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 239000007772 electrode material Substances 0.000 claims description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical group [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000003599 detergent Substances 0.000 claims description 2
- 239000011810 insulating material Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 230000000737 periodic effect Effects 0.000 claims description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 2
- 238000007740 vapor deposition Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 5
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims 1
- 239000012459 cleaning agent Substances 0.000 claims 1
- 229910001882 dioxygen Inorganic materials 0.000 claims 1
- 239000006210 lotion Substances 0.000 claims 1
- 239000010408 film Substances 0.000 abstract description 12
- 239000000853 adhesive Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 239000010409 thin film Substances 0.000 abstract description 2
- 239000003990 capacitor Substances 0.000 description 8
- 238000012512 characterization method Methods 0.000 description 3
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000011245 gel electrolyte Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000000233 ultraviolet lithography Methods 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention relates to a preparation method of a manganese-based oxide micro supercapacitor, which comprises the following steps: spin coating: spin-coating a photoresist on the surface of the clean substrate; photoetching: exposing and developing the surface of the substrate after spin coating; evaporation: carrying out evaporation on the surface of the substrate after photoetching treatment, firstly evaporating a chromium metal film, and then evaporating a gold metal film; sputtering: sputtering the interdigital pattern area on the surface of the substrate after the evaporation treatment by adopting a magnetron sputtering coating system, wherein the target material is manganese-based oxide; stripping: and soaking the sputtered device in an organic solvent to remove the film except the interdigital structural pattern. The invention has the beneficial effects that: the thin film electrode with compact structure and strong adhesive force is prepared by utilizing a magnetron sputtering process, the liquid phase stripping process is simple, the shape of the obtained interdigital electrode is kept complete, the gap width of adjacent interdigital electrodes is favorably reduced, the number of interdigital electrodes is increased, the effective area of the electrode is increased, and the capacity of a micro device is improved.
Description
Technical Field
The invention belongs to the field of super capacitors, and particularly relates to a preparation method of a manganese-based oxide micro super capacitor.
Background
The super capacitor is a power type energy storage device and is composed of electrode, electrolyte, diaphragm and other key components. The electrode materials of super capacitor are mainly classified into capacitance materials represented by activated carbon and metal oxides (such as RuO) according to the difference of energy storage mechanism2、MnO2Etc.) and a conductive polymer.
The miniature super capacitor is a miniaturized super capacitor device with the area not exceeding a few square millimeters, and the performance of the miniature super capacitor not only depends on electrode materials, but also is influenced by the structure of the device. In the conventional flat plate structure scheme, an upper electrode and a lower electrode respectively use a supporting substrate, and a liquid or gel electrolyte is arranged between the two electrode plates. This stacked design will result in increased thickness, somewhat limiting its planar integration applications. The interdigital structure arranges the two electrodes on the same plane, effectively reduces the thickness of the device, is convenient to integrate with various micro electronic devices, and has good application prospect.
Manganese-based oxide micro-supercapacitors typically employ electrochemical deposition methods to fabricate interdigitated electrodes. Despite the simple process, the prepared electrode is not dense enough and has weak adhesion. In order to avoid short circuit of the device caused by contact of adjacent interdigital electrodes, the distance between the interdigital electrodes is generally wide. Considering the limited planar area, the width of the inactive gap between adjacent crossing electrodes increases, which results in a decrease in the effective electrode area. Therefore, an effective method for preparing the manganese-based oxide interdigital electrode with a compact structure and strong adhesion is needed, and the area of an area without an active gap is reduced, so that the capacity of a device is improved.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a manganese-based oxide micro supercapacitor.
The manganese-based oxide micro supercapacitor comprises: the device comprises a substrate, a current collector and interdigital electrodes; wherein the current collector is deposited on the substrate, and the interdigital electrode is deposited on the current collector; the current collector is of an interdigital structure, and the interdigital structure is a structure in which a periodic pattern is formed in a finger-shaped or comb-shaped surface; the electrode material of the interdigital electrode is manganese oxide and a mixture thereof.
Preferably, the substrate has a flat surface and is made of an insulating material, such as optical glass, surface-coated with SiO2Silicon wafers for insulating layers, etc.
Preferably, the width range of the interdigital electrode is 5-100 micrometers, and the width range of the gap between adjacent interdigital electrodes is 3-200 micrometers.
Preferably, the thickness of the interdigital electrode is 0.05-0.3 micron.
The preparation method of the manganese-based oxide micro supercapacitor specifically comprises the following steps:
step 1) spin coating: spin-coating photoresist on the surface of a clean substrate, and baking on a hot plate;
step 2) photoetching: exposing the substrate surface treated in the step 1 by adopting an ultraviolet photoetching machine, then baking on a hot plate, cooling, developing by using a developer, immediately washing by using a flowing detergent after developing, and then drying by using high-purity nitrogen;
step 3) evaporation: evaporating the substrate surface treated in the step 2 by using a metal film evaporator, wherein a chromium metal film is evaporated firstly, and then a gold metal film is evaporated;
step 4), sputtering: sputtering the interdigital pattern area on the substrate surface treated in the step 3 by adopting a magnetron sputtering coating system, wherein the target material is manganese-based oxide;
step 5) stripping: and (4) soaking the device processed in the step (4) in an organic solvent, removing the film outside the interdigital structural pattern, cleaning, and finally drying by using high-purity nitrogen.
Preferably, the photoresist in step 1 is a negative photoresist.
Preferably, the developer in step 2 is 2.28% NMD-3, the development time is 45 seconds, and the rinse is deionized water.
Preferably, the thickness of the chromium metal film evaporated in the step 3 is 10-20 nm, and the evaporation rate is 0.01-0.03 nm/s; the thickness of the gold-vapor-deposited metal film is 80-100 nm, and the vapor deposition rate is 0.03-0.05 nm/s.
Preferably, the working gas used in sputtering in step 4 is argon, or argon and oxygen are used simultaneously; and when argon and oxygen are adopted, the flow rate of the argon is 20-40 sccm, and the flow rate of the oxygen is 1-8 sccm.
Preferably, the organic solvent used in the stripping in step 5 is acetone, and the washing agents used in the washing are acetone and deionized water in sequence.
The invention has the beneficial effects that: the invention provides a preparation method of a manganese-based oxide micro supercapacitor, which is characterized in that a thin film electrode with a compact structure and strong adhesive force is prepared by utilizing a magnetron sputtering process, a liquid phase stripping process is simple, the shape of the obtained interdigital electrode is kept complete, the reduction of the gap width of adjacent interdigital electrodes is facilitated, the number of interdigital electrodes is increased, the effective area of the electrode is increased, and the capacity of a micro device is improved.
Drawings
FIG. 1 is an optical picture of a manganese-based oxide micro supercapacitor; wherein the electrode width in fig. 1(a) is 20 microns and the gap width between adjacent interdigitated electrodes is 200 microns; the width of the interdigital electrode in fig. 1(b) is 20 micrometers, and the gap width between adjacent interdigital electrodes is 100 micrometers; the width of the interdigital electrode in fig. 1(c) is 20 micrometers, and the gap width between adjacent interdigital electrodes is 50 micrometers; the width of the interdigital electrode in fig. 1(d) is 20 micrometers, and the gap width between adjacent interdigital electrodes is 10 micrometers; the width of the interdigital electrode in fig. 1(e) is 5 micrometers, and the gap width between adjacent interdigital electrodes is 200 micrometers; the interdigital electrode width of fig. 1(f) is 5 micrometers, and the gap width between adjacent interdigital electrodes is 10 micrometers; the width of the interdigital electrode in fig. 1(g) and 1(h) is 5 micrometers, and the gap width between adjacent interdigital electrodes is 5 micrometers;
FIG. 2 is a thickness characterization graph of a manganese-based oxide micro supercapacitor; fig. 2(a) is a thickness characterization of the current collector (Cr/Au), and fig. 2(b) is a thickness characterization of the current collector and the interdigital electrode.
FIG. 3 is a cyclic voltammogram of the manganese-based oxide micro-supercapacitors of example 2 and example 3.
Detailed Description
The present invention will be further described with reference to the following examples. The following examples are set forth merely to aid in the understanding of the invention. It should be noted that, for a person skilled in the art, several modifications can be made to the invention without departing from the principle of the invention, and these modifications and modifications also fall within the protection scope of the claims of the present invention.
Example 1:
a symmetrical micro super capacitor and a preparation method thereof are disclosed, wherein the preparation method comprises the following steps:
1) gluing: the negative glue 5200 is uniformly spin-coated on the surface of the glass by using clean high-temperature glass as a substrate, and then the glass is placed on a hot plate at 110 ℃ for 90 minutes.
2) Photoetching: and (2) exposing the surface of the substrate treated in the step (1) for 8s by adopting an ultraviolet lithography machine, drying the substrate for 90 minutes at a hot plate at 110 ℃, cooling the substrate, developing the substrate by using NMD-32.28% developer for 45 seconds, immediately washing the substrate by using flowing deionized water after developing, drying the substrate by using high-purity nitrogen, and observing whether the pattern is complete and the edge is clear under a microscope. The electrode width of the interdigital structure pattern is 20 micrometers, and the gap width between adjacent interdigital electrodes is 200 micrometers.
3) Evaporation: and (3) performing evaporation on the surface of the substrate treated in the step (2) by using a metal film evaporator, firstly plating a chromium metal film at the evaporation rate of 0.02nm/s and the thickness of 10nm, and then plating a gold metal film at the evaporation rate of 0.04nm/s and the thickness of 90 nm.
4) Sputtering: and 3, sputtering the interdigital pattern region on the surface of the substrate treated in the step 3 by adopting a magnetron sputtering coating system, wherein the target material is manganese-based oxide, the working gas is argon, the flow rate of the argon is 40sccm, and the sputtering thickness is 0.15 micrometer.
5) Stripping: and (4) putting the device treated in the step (4) into an acetone solution for soaking for 8 hours, carrying out ultrasonic treatment for 5 minutes, then sequentially washing with acetone and deionized water, and finally blowing with high-purity nitrogen for drying.
The manganese-based oxide micro supercapacitor shown in FIG. 1(a) was prepared.
Example 2:
this embodiment is substantially the same as embodiment 1, and is characterized in that: the electrode width of the interdigital structure pattern is 20 micrometers, and the gap width between adjacent interdigital electrodes is 100 micrometers. The manganese-based oxide micro supercapacitor shown in FIG. 1(b) was prepared.
Example 3:
this embodiment is substantially the same as embodiment 1, and is characterized in that: the electrode width of the interdigital structure pattern is 20 micrometers, and the gap width between adjacent interdigital electrodes is 50 micrometers. The manganese-based oxide micro supercapacitor was obtained as shown in FIG. 1 (c).
Example 4:
this embodiment is substantially the same as embodiment 1, and is characterized in that: the electrode width of the interdigital structure pattern is 20 micrometers, and the gap width between adjacent interdigital electrodes is 10 micrometers. The manganese-based oxide micro supercapacitor was obtained as shown in FIG. 1 (d).
Example 5:
this embodiment is substantially the same as embodiment 1, and is characterized in that: the electrode width of the interdigital structure pattern is 5 micrometers, and the gap width between adjacent interdigital electrodes is 200 micrometers. The manganese-based oxide micro supercapacitor was obtained as shown in FIG. 1 (e).
Example 6:
this embodiment is substantially the same as embodiment 1, and is characterized in that: the electrode width of the interdigital structure pattern is 5 micrometers, and the gap width between adjacent interdigital electrodes is 10 micrometers. The manganese-based oxide micro supercapacitor was obtained as shown in FIG. 1 (f).
Example 7:
this embodiment is substantially the same as embodiment 1, and is characterized in that: the electrode width of the interdigital structure pattern is 5 micrometers, the gap width of the adjacent interdigital electrodes is 5 micrometers, and the sputtering thickness is 0.1 micrometer. Manganese-based oxide micro supercapacitors as shown in FIGS. 1(g) and 1(h) were produced.
The experimental results are as follows:
compared with fig. 1(a) to 1(d), as the inter-digital electrode gap width is reduced, the number of inter-digital electrodes is increased, and the area of the inter-digital electrodes is gradually increased.
The sample prepared in example 4 was tested by using a step profiler, and the result is shown in fig. 2, wherein the thickness of the current collector (Cr/Au) is 0.1 micrometer, the total thickness of the interdigital electrode and the current collector is 0.25 micrometer, and the thickness of the interdigital electrode prepared by magnetron sputtering is 0.15 micrometer.
Using 1M sodium sulfate aqueous solution as electrolyte, and using an electrochemical workstation to represent the micro-supercapacitors prepared in examples 2 and 3, so as to obtain cyclic voltammetry curves of the symmetrical micro-supercapacitors shown in FIG. 3; as can be seen from the observation of the curve, the area of the cyclic voltammetry curved surface of the device with the narrow gap between the adjacent interdigital electrodes (example 3) is larger under the same scanning rate, indicating that the capacity is higher.
Claims (10)
1. A manganese-based oxide micro supercapacitor, comprising: the device comprises a substrate, a current collector and interdigital electrodes; wherein the current collector is deposited on the substrate, and the interdigital electrode is deposited on the current collector; the current collector is of an interdigital structure, and the interdigital structure is a structure in which a periodic pattern is formed in a finger-shaped or comb-shaped surface; the electrode material of the interdigital electrode is manganese oxide and a mixture thereof.
2. The manganese-based oxide micro-supercapacitor according to claim 1, wherein: the substrate has a flat surface and is made of an insulating material.
3. The manganese-based oxide micro-supercapacitor according to claim 1, wherein: the width range of the interdigital electrodes is 5-100 micrometers, and the width range of gaps between adjacent interdigital electrodes is 3-200 micrometers.
4. The manganese-based oxide micro-supercapacitor according to claim 1, wherein: the thickness of the interdigital electrode is 0.05-0.3 microns.
5. The method for preparing the manganese-based oxide micro supercapacitor according to claim 1, comprising the following steps:
step 1) spin coating: spin-coating photoresist on the surface of a clean substrate, and baking on a hot plate;
step 2) photoetching: exposing the substrate surface treated in the step 1 by adopting an ultraviolet photoetching machine, then baking on a hot plate, cooling, developing by using a developer, immediately washing by using a flowing detergent after developing, and then drying by using high-purity nitrogen;
step 3) evaporation: evaporating the substrate surface treated in the step 2 by using a metal film evaporator, wherein a chromium metal film is evaporated firstly, and then a gold metal film is evaporated;
step 4), sputtering: sputtering the interdigital pattern area on the substrate surface treated in the step 3 by adopting a magnetron sputtering coating system, wherein the target material is manganese-based oxide;
step 5) stripping: and (4) soaking the device processed in the step (4) in an organic solvent, removing the film outside the interdigital structural pattern, cleaning, and finally drying by using high-purity nitrogen.
6. The method of making a manganese-based oxide micro supercapacitor of claim 5, wherein: the photoresist in step 1 is a negative photoresist.
7. The method of making a manganese-based oxide micro supercapacitor of claim 5, wherein: in the step 2, the developer is 2.28 percent of NMD-3, the development time is 45 seconds, and the lotion is deionized water.
8. The method of making a manganese-based oxide micro supercapacitor of claim 5, wherein: in the step 3, the thickness of the evaporated chromium metal film is 10-20 nm, and the evaporation rate is 0.01-0.03 nm/s; the thickness of the gold-vapor-deposited metal film is 80-100 nm, and the vapor deposition rate is 0.03-0.05 nm/s.
9. The method of making a manganese-based oxide micro supercapacitor of claim 5, wherein: the working gas adopted in the sputtering in the step 4 is argon gas, or argon gas and oxygen gas are adopted simultaneously; and when argon and oxygen are adopted, the flow rate of the argon is 20-40 sccm, and the flow rate of the oxygen is 1-8 sccm.
10. The method of making a manganese-based oxide micro supercapacitor of claim 5, wherein: the organic solvent adopted in the stripping in the step 5 is acetone; the cleaning agent used in the cleaning process sequentially comprises acetone and deionized water.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114397333A (en) * | 2021-12-21 | 2022-04-26 | 海宁市产业技术研究院 | Electrolyte concentration sensor based on double electric layer principle, preparation method and application thereof |
| CN114883116A (en) * | 2022-05-23 | 2022-08-09 | 电子科技大学 | Porous MnO 2 Preparation method of nanotube array micro energy storage device |
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| US20130250483A1 (en) * | 2012-03-20 | 2013-09-26 | National Yunlin University Of Science And Technology | Electrodes And Their Fabrication Methods As Well As Applications |
| CN104465119A (en) * | 2014-11-28 | 2015-03-25 | 国家纳米科学中心 | Super capacitor based on three-dimensional ZnO@MnO2 composite nano array interdigital electrode and manufacturing method thereof |
| CN106057491A (en) * | 2016-08-17 | 2016-10-26 | 武汉理工大学 | High-performance asymmetric metal oxide-based miniature super capacitor and preparation method thereof |
| CN106158411A (en) * | 2016-08-17 | 2016-11-23 | 武汉理工大学 | A kind of high-performance symmetrical expression metal-oxide base micro super capacitor and preparation method thereof |
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| CN114397333A (en) * | 2021-12-21 | 2022-04-26 | 海宁市产业技术研究院 | Electrolyte concentration sensor based on double electric layer principle, preparation method and application thereof |
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