CN115974159A - Preparation method and application of patterned manganese oxide array - Google Patents
Preparation method and application of patterned manganese oxide array Download PDFInfo
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- CN115974159A CN115974159A CN202211555103.5A CN202211555103A CN115974159A CN 115974159 A CN115974159 A CN 115974159A CN 202211555103 A CN202211555103 A CN 202211555103A CN 115974159 A CN115974159 A CN 115974159A
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- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 title claims abstract description 150
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 39
- 239000011521 glass Substances 0.000 claims abstract description 38
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 23
- 239000007864 aqueous solution Substances 0.000 claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 239000011229 interlayer Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 22
- 239000002070 nanowire Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000004146 energy storage Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000010410 layer Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims 1
- 239000002243 precursor Substances 0.000 abstract description 9
- 239000002086 nanomaterial Substances 0.000 abstract description 6
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 16
- 239000006059 cover glass Substances 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001259 photo etching Methods 0.000 description 3
- 238000007540 photo-reduction reaction Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000003491 array Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 229940071125 manganese acetate Drugs 0.000 description 2
- 229940093474 manganese carbonate Drugs 0.000 description 2
- 235000006748 manganese carbonate Nutrition 0.000 description 2
- 239000011656 manganese carbonate Substances 0.000 description 2
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 2
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 2
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920002120 photoresistant polymer Polymers 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- -1 manganese salt Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention belongs to the technical field of micro-nano material preparation, and discloses a preparation method and application of a patterned manganese oxide array. The preparation method of the manganese oxide array comprises the following steps: (1) Adding a potassium permanganate aqueous solution into the upper glass substrate and the lower glass substrate to form an interlayer; (2) Adjusting laser to focus the laser on the junction of the upper glass substrate and the potassium permanganate aqueous solution, wherein the power of the laser is adjusted to be not more than 100mW, the wavelength of the laser is 500-515nm, and the pulse width is 200-260fs; and (3) moving the laser to obtain the manganese oxide array. The invention takes potassium permanganate as a precursor solution, takes a glass substrate as a substrate, only needs single-step laser irradiation, has the laser power of not more than 100mW, the laser wavelength of 500-515nm and the pulse width of 200-260fs, and can prepare the high-precision patterned manganese oxide array. Greatly reducing the laser power and simplifying the manufacturing process.
Description
Technical Field
The invention belongs to the technical field of micro-nano material preparation, and particularly relates to a preparation method and application of a patterned manganese oxide array.
Background
Patterned fabrication is increasingly important in the fabrication of micro-integrated circuits. At present, the patterning preparation of the metal oxide electrode is mainly realized by the photoetching technology. The photoetching technology needs to cover a layer of photoresist on the surface of a material, then carries out structure etching, then is soaked in a developing solution to remove the redundant photoresist, and finally carries out etching to write the structure on the surface of the material. The patterned micro-nano circuit is prepared by photoetching, the process is complex, the cost is high, and the preparation of the complex patterned circuit is difficult.
In the field of nanotechnology, manganese dioxide (MnO) 2 ) It is of great interest because of its low toxicity. Compared with a bulk material, the manganese oxide nano material has higher electron mobility and larger specific surface area, and has huge application potential on energy storage devices, photoelectric devices and gas sensitive devices. At present, manganese oxide nanomaterials with various morphologies, including nanowires, nanorods, nanotubes, nanosheets, nanoarrays, and the like, have been prepared. Common manganese oxide nanomaterial wet chemical synthesis methods, such as a hydrothermal method, a sol-gel method, a redox method and the like, can realize size control of the manganese oxide nanomaterial in the synthesis process. Manganese dioxide nanoparticles are synthesized in a variety of ways, but challenges remain in obtaining the desired nanoparticles. When the existing synthesis method is used for preparing the manganese oxide nano particles, the phase and the appearance of the nano particles can be influenced by the change of temperature and reaction time. In addition, the reaction temperature of the existing synthesis method is generally hundreds of ℃, the reaction time is often more than ten hours, and a large amount of energy is consumed.
At present, the general steps for preparing the manganese oxide micro-nano device by using laser are as follows: the method comprises the steps of preparing an organic solution of manganese salt/manganese oxide nanoparticles as a precursor, coating the precursor on a substrate by various methods (such as silk-screen printing) by taking an organic film as the substrate, and irradiating by high-flux laser to realize the generation of laser-induced graphene and the preparation of manganese oxide on a laser irradiation path at the same time, thereby synthesizing the manganese oxide nano-array in situ. The technology of preparing manganese oxide nano-arrays by laser direct writing can simply prepare patterned manganese oxide arrays, but the use of organic solvents (such as PAA) and organic substrates (such as polyimide films) limits the power threshold of lasers. Namely, the process of preparing the patterned manganese oxide array in the prior art often requires high laser power (power of 0.2-0.8W), and the excessively high laser power is easy to damage the region which does not need to be patterned. In the prior art, multiple times of laser irradiation are often required for preparing the patterned manganese oxide array, so that the complexity of the process is increased.
Therefore, it is desirable to provide a new method for preparing a patterned manganese oxide array, which simplifies the process and reduces the laser power.
Disclosure of Invention
The present invention has been made to solve at least one of the above-mentioned problems occurring in the prior art. Therefore, the invention provides a preparation method of a patterned manganese oxide array and application thereof, the laser power used in the preparation method is not more than 100mW, even not more than 50mW, multi-step laser irradiation is not required, the process is simplified, and the high-precision patterned manganese oxide array can be prepared.
The invention conception of the invention is as follows: according to the invention, potassium permanganate is used as a precursor solution, a glass substrate is used as a substrate, single-step laser irradiation is only needed, the laser power is not more than 100mW, even not more than 50mW, the wavelength of the laser is 500-515nm, and the pulse width is 200-260fs, so that the high-precision patterned manganese oxide array can be prepared. Greatly reduces the laser power and simplifies the manufacturing process.
A first aspect of the invention provides a method of preparing a patterned manganese oxide array.
Specifically, the preparation method of the patterned manganese oxide array comprises the following steps:
(1) Adding a potassium permanganate aqueous solution into the upper glass substrate and the lower glass substrate to form an interlayer;
(2) Adjusting laser to focus on the junction of the upper glass substrate and the potassium permanganate aqueous solution, wherein the power of the laser is adjusted to be not more than 100mW, the wavelength of the laser is 500-515nm, and the pulse width of the laser is 200-260fs;
(3) And moving the laser to obtain the patterned manganese oxide array.
Preferably, in the step (1), the glass substrate is cleaned by using ultrasonic waves and then by using UV light. The purpose of this washing is to clean the surface of the glass substrate and to adjust the hydrophilicity and hydrophobicity of the surface of the glass substrate. And a manganese oxide array with good adhesive force is formed on the lower surface of the upper glass substrate.
Preferably, in the step (1), the glass substrate is SiO 2 A glass substrate.
Preferably, in the step (1), the thickness of the glass substrate is 0.1-0.8mm; further preferably, the thickness of the glass substrate is 0.1 to 0.5mm.
Preferably, in the step (1), the length and width of the glass substrate are (1-4) cm x (1-4) cm; further preferably, the thickness of the glass substrate is (1-2) cm × (1-2) cm.
Preferably, in the step (1), the concentration of the potassium permanganate aqueous solution is 0.05-0.5mol/L; further preferably, the concentration of the potassium permanganate aqueous solution is 0.05-0.2mol/L.
Preferably, in the interlayer in the step (1), the liquid layer formed by the potassium permanganate solution has a thickness of 2-30 μm; preferably 10-15 μm.
Preferably, in the step (2), the power of the laser is 10-100mW, preferably 20-50mW. The laser is femtosecond laser, and irradiation is carried out in a pulse mode to obtain a patterned manganese oxide array.
Preferably, in step (2), the repetition frequency of the laser is 100-200KHz, preferably 150-200KHz, and more preferably 200KHz.
The laser irradiation point generates the reduction reaction of potassium permanganate, and the reduction product is separated out and deposited on the glass substrate.
Preferably, in the step (2), the means for adjusting the laser comprises a femtosecond laser, an attenuation sheet, a diaphragm, an electrically controlled shutter, a pulse shaper, a reflecting mirror, a dichroic mirror, a focusing objective, a translation stage, a convex lens, a charge-coupled device and a computer. The femtosecond laser generated by the femtosecond laser adjusts laser power through the attenuation sheet, adjusts the diameter of a femtosecond laser spot through the diaphragm, then enters the pulse shaper through the electric control shutter, the laser emitted from the shaper is reflected by the reflector and one side of the dichroic mirror, and the focusing of a light beam is realized through the focusing objective lens. The means for adjusting the laser is one of the prior art.
Preferably, in the step (3), the moving laser can control the laser to move in the X-Y direction through a three-dimensional moving platform system, so that the preparation of the patterned manganese oxide array is realized.
Preferably, in the step (3), the patterned manganese oxide array is composed of manganese oxide nanowires, and the diameter of the manganese oxide nanowires is 100nm-10 μm.
Preferably, step (3) is carried out under air, nitrogen or vacuum conditions.
Preferably, in the step (3), after the patterned manganese oxide array is prepared, deionized water and ethanol are used for cleaning.
The method for preparing the patterned manganese oxide array by adopting the laser is characterized in that the manganese oxide lines are prepared by adopting the laser direct writing, and the manganese oxide lines further form the patterned manganese oxide array.
A second aspect of the invention provides the use of a method of making a patterned manganese oxide array.
In particular to the application of the preparation method in the preparation of energy storage devices, photoelectric devices or gas sensitive devices.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, potassium permanganate is used as a precursor solution, a glass substrate is used as a substrate, single-step laser irradiation is only needed, the laser power is not more than 100mW, even not more than 50mW, the wavelength of the laser is 500-515nm, and the pulse width is 200-260fs, so that the high-precision patterned manganese oxide array can be prepared. Greatly reducing the laser power and simplifying the manufacturing process.
Drawings
FIG. 1 is a schematic diagram of a femtosecond laser photoreduction method for preparing a patterned manganese oxide array in example 1 of the present invention;
FIG. 2 is a SEM (scanning electron microscope) and elemental distribution plot of manganese oxide in a manganese oxide array prepared in example 1 of the present invention;
FIG. 3 shows a manganese oxide line in a manganese oxide array according to example 1 of the present invention;
FIG. 4 shows a manganese oxide array prepared in example 1 of the present invention.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.
The starting materials, reagents or apparatuses used in the following examples are conventionally commercially available or can be obtained by conventionally known methods, unless otherwise specified.
Example 1
A method of making a patterned manganese oxide array, comprising the steps of:
(1) Ultrasonically cleaning two glass substrates (a cover glass and a glass slide respectively) by using ethanol and drying, cleaning the two glass substrates (the cleaning time is 1 hour) by using UV light, improving the hydrophilicity of the two glass substrates, fixing the glass slide on a moving platform as a substrate, dropwise adding a proper amount of potassium permanganate aqueous solution (the concentration is 0.05 mol/L) onto the glass slide, and covering liquid drops by using the cover glass to form an interlayer;
(2) Starting a laser, selecting a laser (namely a femtosecond laser) with the wavelength of 515nm and the pulse width of 260fs as an output light source, moving by using a program control platform to focus the laser to the junction of the cover glass and the potassium permanganate aqueous solution, adjusting the laser power to be 50mW, and beginning to precipitate manganese oxide at the interface;
(3) And controlling the platform to move the laser along the X-Y axis to obtain the patterned manganese oxide array.
Fig. 1 is a schematic diagram of a femtosecond laser photoreduction method for preparing a patterned manganese oxide array in example 1 of the present invention. In FIG. 1, 100 denotes a glass slide, 200 denotes an aqueous potassium permanganate solution, 300 denotes a cover glass, and 400 denotes a laser. Focusing laser on the boundary of the cover glass and the potassium permanganate aqueous solution to ensure that MnO in the solution is 4 - (as MnO) 4 - (aq)) photoreduction to solid MnO x (MnO x Represents manganese oxide, denoted MnO x (s)), thereby achieving the object of preparing a patterned manganese oxide array.
FIG. 2 is a SEM and elemental distribution plot of manganese oxide in a manganese oxide array made according to example 1 of the present invention; fig. 2 (a) is an SEM image of manganese oxide in the manganese oxide array prepared in example 1. Fig. 2 (b), (c) and (d) are element distribution diagrams of manganese oxide in the manganese oxide array obtained in example 1, and it can be seen from fig. 2 that the product prepared by the method of this example has no significant potassium enrichment and the main component is manganese oxide.
Fig. 3 shows a manganese oxide line in a manganese oxide array prepared in example 1 of the present invention.
FIG. 4 is a manganese oxide array prepared in example 1 of the present invention. As can be seen from fig. 4, the patterned manganese oxide array prepared by the present invention has high definition.
Example 2
A method of making a patterned manganese oxide array, comprising the steps of:
(1) Ultrasonically cleaning two glass substrates (a cover glass and a glass slide respectively) by using ethanol, drying, cleaning the two glass substrates by using UV light to improve the hydrophilicity, fixing the glass slide on a moving platform as a substrate, dropwise adding a proper amount of precursor solution potassium permanganate aqueous solution (the concentration is 0.2 mol/L) onto the glass slide, and covering the droplets by using the cover glass to form an interlayer;
(2) Starting a laser, selecting laser with the wavelength of 515nm and the pulse width of 260fs as an output light source, controlling the platform to move through a program, focusing the laser to the junction of the cover glass and the precursor solution potassium permanganate aqueous solution, adjusting the laser power to be 20mW, and beginning to precipitate manganese oxide at the interface;
(3) And controlling the platform to move the laser along the X-Y axis to obtain the patterned manganese oxide array.
Comparative example 1
Compared with the embodiment 1, the manganese acetate aqueous solution with equal concentration is adopted in the comparative example 1 to replace the precursor solution potassium permanganate aqueous solution in the embodiment 1, and other processes are the same as the embodiment 1. Comparative example 1 failed to successfully produce a patterned manganese oxide array because the patterned manganese oxide array of example 1 could not be produced at a laser power of 50mW due to poor absorption of 515nm laser light by the aqueous solution of manganese acetate.
Comparative example 2
Compared with the example 2, the manganese carbonate aqueous solution with equal concentration is adopted in the comparative example 2 to replace the precursor solution potassium permanganate aqueous solution in the example 2, and other processes are the same as the example 2. Comparative example 2 failed to successfully produce a patterned manganese oxide array because the patterned manganese oxide array of example 2 could not be produced at a laser power of 20mW due to poor absorption of 515nm laser light by the aqueous solution of manganese carbonate.
Claims (10)
1. The preparation method of the manganese oxide array is characterized by comprising the following steps of:
(1) Adding a potassium permanganate aqueous solution into the upper glass substrate and the lower glass substrate to form an interlayer;
(2) Adjusting laser to focus the laser on the junction of the upper glass substrate and the potassium permanganate aqueous solution, wherein the power of the laser is adjusted to be not more than 100mW, the wavelength of the laser is 500-515nm, and the pulse width is 200-260fs;
(3) And moving the laser to obtain the manganese oxide array.
2. The production method according to claim 1, wherein in the step (1), the glass substrate is cleaned using ultrasonic cleaning and then cleaned using UV light.
3. The production method according to claim 1, wherein in the step (1), the glass substrate is SiO 2 A glass substrate.
4. The preparation method according to claim 1, wherein in the step (1), the concentration of the aqueous potassium permanganate solution is 0.05 to 0.5mol/L.
5. The production method according to claim 1, wherein in the interlayer, the liquid layer formed by the aqueous potassium permanganate solution has a thickness of 2 to 30 μm.
6. The production method according to claim 1, wherein in the step (2), the power of the laser is 20 to 50mW.
7. The method according to claim 1, wherein in the step (2), the repetition rate of the laser is 100 to 200KHz.
8. The method according to claim 1, wherein in the step (3), the manganese oxide array is composed of manganese oxide nanowires, and the diameter of the manganese oxide nanowires is 100nm to 10 μm.
9. The method according to claim 1, wherein the step (3) is carried out under air, nitrogen or vacuum.
10. Use of the production method according to any one of claims 1 to 9 for producing an energy storage device, a photovoltaic device or a gas-sensitive device.
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| JP7038455B1 (en) * | 2021-11-04 | 2022-03-18 | 日本重化学工業株式会社 | Manganese dioxide and its manufacturing method |
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| CN106098410A (en) * | 2016-06-25 | 2016-11-09 | 于有海 | Laser one-step method prepares ultracapacitor Graphene/manganese oxide flexible electrode |
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