CN106044703B - A kind of pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material patterning microelectrode and its micro fabrication - Google Patents
A kind of pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material patterning microelectrode and its micro fabrication Download PDFInfo
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Abstract
The present invention relates to the micro fabrication that a kind of pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material patterns microelectrode, including：1) graphene, Sodium Molybdate Dihydrate, thiocarbamide, water are pressed 1~10：400：600~700：After 10000~30000 mass ratio is well mixed, carry out hydrothermal synthesis reaction in a kettle., hydrothermal synthesis reaction finish after by centrifugation, be dried to obtain solid product, solid product ground, obtain molybdenum disulfide nano sheet/grapheme material；2) photoresist is well mixed with molybdenum disulfide nano sheet/grapheme material and be then coated with drying on substrate, ultraviolet photolithographic, development and rinse are carried out again, are finally carried out high temperature pyrolysis reaction and are obtained pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material patterning microelectrode.The microelectrode of gained has good chemical property, has good application prospect in the field such as microsensor and miniature energy storage device.
Description
Technical field
The present invention relates to nano material and micro fabrication crossing domain, more specifically to a kind of sulphur of pyrolytic carbon/bis-
Change molybdenum nanometer sheet/graphene composite material patterning microelectrode and its micro fabrication.
Background technology
MEMS (MEMS, Micro the Electro Mechanical grown up based on micro ＆ nano technology
Systems in the every field for) being widely used in society, wherein, based on the carbon-based micro-system made by pyrolysis photoresist
(C-MEMS, carbon Micro Electro Mechanical Systems) because its micro-structural controllable precise, environmental protection and economy,
Equipment requirement is low, technique can with existing semiconductor microactuator processing technology it is fully-integrated the features such as and be widely studied and be applied to various
In microdevice and system.Molybdenum disulfide stratiform nano material has high-specific surface area, fake capacitance activity, compared to oxide tool
There is highly electron conductive and there is high electrochemistry capacitance, therefore the high-performance electric as researcher's extensive concern relative to graphite
One of container material.Chinese invention patent (Authorization Notice No. CN104226337, authorized announcement date 2016.05.04) discloses one
Graphene-supported sheet molybdenum disulfide nano compound and preparation method thereof is planted, the invention is used as starting using ammonium molybdate and thiocarbamide
Thing, can load the nanometer titanium dioxide molybdenum of sheet in surface of graphene oxide under hydrothermal conditions；By calcination process
The sheet molybdenum disulfide that graphene is loaded afterwards has higher crystallinity, and photocatalysis efficiency exceedes commercial nano-titanium oxide
More than 1.7 times, but the compound is more difficult compatible with micro fabrication, is difficult to realize this composite in micro element and micro- system
The effective integration of system.
The content of the invention
The technical problem to be solved in the present invention is, more difficult in micro- device for the molybdenum disulfide nano compound of prior art
The defect of the effective integration of part and micro-system is simple there is provided a kind of technique, and with good chemical property, larger area
Pyrolytic carbon/molybdenum disulfide nano sheet of specific capacity/graphene composite material patterns the processing technology of microelectrode.
The technical solution adopted for the present invention to solve the technical problems is：Using the photoresist of photoresist, and with light
Photosensitive resin in photoresist is that carbon source and molybdenum disulfide nano sheet/grapheme material of Hydrothermal Synthesiss are mutually combined, obtained pyrolytic carbon/
Molybdenum disulfide nano sheet/graphene composite material microelectrode, has been made pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite wood
The micro-patterning microelectrode of material.
According to above scheme, a kind of pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material patterning microelectrode
Micro fabrication, specifically include following steps：
1) it is 1~10 by graphene, Sodium Molybdate Dihydrate, thiocarbamide, water：400：600~700：10000~30000 quality
Than carrying out hydrothermal synthesis reaction after being well mixed in a kettle., the temperature of hydrothermal synthesis reaction is 150~250 DEG C, during reaction
Between be 20~30h.Hydrothermal synthesis reaction washes hydrothermal product for several times with centrifugally operated cooperation ethanol after finishing, and centrifugal rotational speed is
10000r/min, centrifugation time is 3min, and the hydrothermal product after washes clean is centrifuged, solid is obtained after taking solids, drying
Product, solid product is ground, and obtains molybdenum disulfide nano sheet/grapheme material；The molybdenum disulfide obtained in this way
In nanometer sheet/grapheme material molybdenum disulfide receive with graphene uniform component, using the graphene of this proportioning, molybdate dihydrate acid
Molybdenum disulfide nano sheet/grapheme material that sodium, thiocarbamide, water are obtained, mutually its dissolubility, sign are optimal.
2) photoresist and molybdenum disulfide nano sheet/grapheme material are pressed 10~200：After 1 mass ratio is well mixed
To composite, composite is coated on substrate and dried, then carries out ultraviolet photolithographic, development and rinse obtains sample, finally
Sample is carried out to high temperature pyrolysis reaction under an inert atmosphere and obtains pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material figure
Case microelectrode；Being reached by controlling the content of photoresist and molybdenum disulfide nano sheet/grapheme material improves the mesh of component
, it is shown good chemical property, area specific capacity is significantly improved.
The reactor is inner liner polytetrafluoroethylene reactor, and the compactedness of the reactor is 50~70%；Control is anti-
Answering the compactedness of reaction solution in kettle prevents reaction solution from excessively being overflowed during reaction.
The high temperature pyrolysis reaction process is：200~400 DEG C are heated the sample to first, are incubated 15~45min, then
500~600 DEG C are heated to, 15~45min is incubated, continues to be heated to 700~1000 DEG C, is incubated 0.5~1.5h, is finally cooled to
Room temperature.The intensity of micro-structural is improved by the way of this three steps heat stepwise, prevents micro-structural from occurring fracture at high temperature existing
As.
The substrate is silicon substrate or glass substrate；
Preferably, the substrate is the polishing silicon substrate that surface carries silica oxide layer.This substrate has preferable
Flatness, be conveniently coated process.
Preferably, the step 2) in, to photoresist and the mixed composite wood of molybdenum disulfide nano sheet/grapheme material
Ethanol is added in material, the mass ratio of the ethanol and composite is 1：5~20；When the molybdenum disulfide nano in composite
When the content of piece/grapheme material is higher, composite is too sticky to be difficult to be coated process, reduces sticky by adding ethanol
Degree facilitates working procedure of coating.
The invention has the advantages that：
1) pyrolytic carbon/molybdenum disulfide nano sheet/graphene pattern microelectrode obtained by the present invention, with good electrification
Performance is learned, area specific capacity is significantly improved, and has good application in the field such as microsensor and miniature energy storage device
Prospect.
2) micro fabrication of the present invention is simple, raw material sources are wide, equipment requirement is low, producing efficiency is high, is adapted to push away
Wide application.
Brief description of the drawings
Fig. 1 is pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material patterning microelectrode of the embodiment of the present invention 1
Micro fabrication schematic flow sheet；
Fig. 2 is pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material patterning microelectrode in the embodiment of the present invention 1
Morphology characterization sem image；
Fig. 3 is pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material patterning microelectrode in the embodiment of the present invention 2
Morphology characterization sem image；
Fig. 4 is molybdenum disulfide nano sheet/grapheme material (MoS to gained in the embodiment of the present invention 12), forge at 900 DEG C
Burn molybdenum disulfide nano sheet/grapheme material (MoS2- 900 DEG C), photoresist/molybdenum disulfide nano sheet/graphene composite material
Through the product (C/MoS after 900 DEG C of pyrolysis carbonizations2- 900 DEG C) carry out X-ray diffraction thing phase characterization result；
Fig. 5 is 1 pyrolytic carbon of the embodiment of the present invention/molybdenum disulfide nano sheet/graphene composite material patterning microelectrode
Optical microscope image；
Embodiment
Technical scheme is illustrated with embodiment below in conjunction with the accompanying drawings.
Embodiment 1
1) preparation of molybdenum disulfide nano sheet/grapheme material：
1.1,0.8g Sodium Molybdate Dihydrates are dissolved in 30g deionized waters, clear solution is stirred to obtain, 6mg stones are added thereto
Black alkene powder, ultrasonically treated 1h obtains uniform dark solution；
1.2, added into dark solution after 1.26g thiocarbamides, stirring 30min, then ultrasound 30min obtains mixed liquor；
1.3, mixed liquor is transferred to volume in 50ml polytetrafluoroethyllining lining reactors, the Hydrothermal Synthesiss at 200 DEG C
React 24h；
1.4, coordinate ethanol to wash 6 times with centrifugally operated the product of Hydrothermal Synthesiss, each centrifugal rotational speed is 10000r/min,
Centrifugation time is 3min, is then centrifuged the hydrothermal product after washes clean, rotating speed is 10000r/min, centrifuges 3min, then
Sediment after centrifugation is positioned in drying box at 70 DEG C and dries 24h, product solid is obtained；
1.5, solid product is ground, molybdenum disulfide nano sheet/grapheme material is obtained.
2) preparation of photoresist/molybdenum disulfide nano sheet/graphene composite material：
2.1) obtained molybdenum disulfide nano sheet/grapheme material is weighed into 0.15g, and with 1.5g PR1-9000A just
Property photoresist be mixed to get composite, then into composite add 0.33g ethanol, then simultaneously carry out mechanical agitation and
Ultrasonically treated 6h, obtains photoresist/molybdenum disulfide nano sheet/graphene composite material；
3) pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material patterns the preparation of microelectrode：
3.1) using the single-sided polishing silicon substrate of RCA standard cleaning method cleaning tape oxide layers；
3.2) enter obtained photoresist/molybdenum disulfide nano sheet/graphene composite material in the burnishing surface of silicon substrate
Row coats process, and rotating speed is：The first step, 10s, 1000rpm；Second step, 40s, 6000rpm；It is subsequently placed in 100 DEG C of baking ovens and dries
15min is obtained applying silicon-covered substrate, and the painting silicon-covered substrate that surface scribbles the silicon substrate of composite must be arrived as shown in Figure 1a；
3.3) after coating is finished, ultraviolet photolithographic processing is carried out to silicon substrate after coating, it is 90s to control the time for exposure, then
Develop 60s in immersion RD6 developer solutions, then the rinse 30s in 1 grade of deionized water, finally the rinse 30s in 2 grades of deionized waters,
Rinse, which is placed in after finishing in 100 DEG C of baking ovens, dries 15min, obtains sample, as shown in Figure 1 b, carries out ultraviolet photolithographic, development, after rinse
Sample；
3.4) sample is placed under nitrogen atmosphere, carries out high temperature pyrolysis reaction, the process of high temperature pyrolysis reaction is：Tube furnace
With 2 DEG C of min-1Speed be warming up to 300 DEG C and be incubated 30min, then with 2 DEG C of min-1Speed be warming up to 600 DEG C and be incubated
After 30min, then with 2 DEG C of min-1Speed be warming up to 900 DEG C and be incubated 1h, be subsequently cooled to room temperature and obtain the sulphur of pyrolytic carbon/bis-
Change molybdenum nanometer sheet/graphene composite material patterning microelectrode, as illustrated in figure 1 c, carry out the pyrolysis obtained after high temperature pyrolysis reaction
Carbon/molybdenum disulfide nano sheet/graphene composite material patterning microelectrode.
Step 3.3 in embodiment 1) gained sample observe its pattern using SEM, be shown as continuously receiving
Rice piece (such as Fig. 2).To gained photoresist/molybdenum disulfide nano sheet/graphene composite material (C/MoS2- 900 DEG C) carry out X-ray
Diffraction is characterized, and finds photoresist/molybdenum disulfide nano sheet/graphene composite material after pyrolysis, molybdenum disulfide nano sheet/graphite
Alkene material composition is unchanged (such as Fig. 4).To the pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite wood obtained in the present embodiment
Material patterning microelectrode carries out light microscope and taken pictures, and image is as shown in Figure 5.Pass through Autolab electrochemical workstations and low temperature
The chemical property that probe station patterns microelectrode to pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material is tested：
Gained pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material patterning microelectrode is in sulfuric acid/PVA gels electricity in embodiment 1
Solve in liquid, in 0-0.8V voltage windows and 5mVs-1Sweep under speed its area specific capacity up to 9.53mF cm-2, 500mVs-1
It is 93.7% to sweep under speed capability retention after the circle of circulation 10000, is above most of molybdenum disulfide microsupers electricity reported
Container.
Embodiment 2
1) preparation of molybdenum disulfide nano sheet/grapheme material：
1.1,0.8g Sodium Molybdate Dihydrates are dissolved in 60g deionized waters, clear solution is stirred to obtain；2mg stones are added thereto
Black alkene powder, ultrasonically treated 1h obtains uniform dark solution；
1.2, added into dark solution after 1.2g thiocarbamides, stirring 30min, then ultrasound 30min obtains mixed liquor；
1.3, mixed liquor is transferred to volume in 100ml polytetrafluoroethyllining lining reactors, the Hydrothermal Synthesiss at 200 DEG C
React 24h；
1.4, coordinate ethanol to wash 6 times with centrifugally operated the product of Hydrothermal Synthesiss, each centrifugal rotational speed is 10000r/min,
Centrifugation time is 3min, is then centrifuged the hydrothermal product after washes clean, rotating speed is 10000r/min, centrifuges 3min, then
Sediment after centrifugation is positioned in drying box at 70 DEG C and dries 24h, product solid is obtained；
1.5, solid product is ground, final product molybdenum disulfide nano sheet/grapheme material is obtained.
2) preparation of photoresist/molybdenum disulfide nano sheet/graphene composite material：
2.1) obtained molybdenum disulfide nano sheet/grapheme material is weighed into 0.15g, and with 30g PR1-9000A just
Property photoresist be mixed to get composite, mechanical agitation and ultrasonically treated 6h are then carried out simultaneously, photoresist/molybdenum disulfide is obtained
Nanometer sheet/graphene composite material；
3) pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material patterns the preparation of microelectrode：
3.1) using the single-sided polishing silicon substrate of RCA standard cleaning method cleaning tape oxide layers；
3.2) enter obtained photoresist/molybdenum disulfide nano sheet/graphene composite material in the burnishing surface of silicon substrate
Row coats process, and rotating speed is：The first step, 10s, 1000rpm；Second step, 40s, 6000rpm；It is subsequently placed in 100 DEG C of baking ovens and dries
15min obtains applying silicon-covered substrate.
3.3) after coating is finished, ultraviolet photolithographic processing is carried out to applying silicon-covered substrate, it is 90s to control the time for exposure, is then soaked
Enter the 60s that develops in RD6 developer solutions, then the rinse 30s in 1 grade of deionized water, finally the rinse 30s in 2 grades of deionized waters, moisten
Wash to be placed in 100 DEG C of baking ovens after finishing and dry 15min, obtain sample.
3.4) sample is placed under nitrogen atmosphere, carries out high temperature pyrolysis reaction, the process of high temperature pyrolysis reaction is：Tube furnace
With 2 DEG C of min-1Speed be warming up to 200 DEG C and be incubated 15min, then with 2 DEG C of min-1Speed be warming up to 500 DEG C and be incubated
After 15min, then with 2 DEG C of min-1Speed be warming up to 700 DEG C and be incubated 0.5h, be subsequently cooled to room temperature and obtain pyrolytic carbon/bis-
Molybdenum sulfide nanometer sheet/graphene composite material patterning microelectrode.
Step 3.3 in embodiment 2) gained sample using SEM observes its pattern, shows it by separating
Nanometer sheet bead constitutes (such as Fig. 3).Pyrolytic carbon/molybdenum disulfide is received by Autolab electrochemical workstations and cold probe platform
The chemical property of rice piece/graphene composite material patterning microelectrode is tested：The gained sulphur of pyrolytic carbon/bis- in embodiment 2
Change molybdenum nanometer sheet/graphene composite material and pattern microelectrode in sulfuric acid/PVA gel electrolytes, in 0-0.8V voltage windows
And 5mVs-1Sweep under speed, its area specific capacity is up to 3.4mF cm-2。
Embodiment 3
1) preparation of molybdenum disulfide nano sheet/grapheme material：
1.1,0.8g Sodium Molybdate Dihydrates are dissolved in 20g deionized waters, clear solution is stirred to obtain；20mg is added thereto
Graphene powder, ultrasonically treated 1h obtains uniform dark solution；
1.2, added into dark solution after 1.4g thiocarbamides, stirring 30min, then ultrasound 30min obtains mixed liquor；
1.3, mixed liquor is transferred to volume in 50ml polytetrafluoroethyllining lining reactors, the Hydrothermal Synthesiss at 200 DEG C
React 24h；
1.4, coordinate ethanol to wash 6 times with centrifugally operated the product of Hydrothermal Synthesiss, each centrifugal rotational speed is 10000r/min,
Centrifugation time is 3min, is then centrifuged the hydrothermal product after washes clean, rotating speed is 10000r/min, centrifuges 3min, then
Sediment after centrifugation is positioned in drying box at 70 DEG C and dries 24h, product solid is obtained；
1.5, solid product is ground, final product molybdenum disulfide nano sheet/grapheme material is obtained.
2) preparation of photoresist/molybdenum disulfide nano sheet/graphene composite material：
2.1) obtained molybdenum disulfide nano sheet/grapheme material is weighed into 0.15g, and it is negative with 15g NR9-1000PY
Property photoresist be mixed to get composite, the dilution of 0.76g ethanol is then added into composite, machinery is then carried out simultaneously and is stirred
Ultrasonically treated 6h is mixed and stirred, photoresist/molybdenum disulfide nano sheet/graphene composite material is obtained；
3) pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material patterns the preparation of microelectrode：
3.1) using the single-sided polishing silicon substrate of RCA standard cleaning method cleaning tape oxide layers；
3.2) obtained photoresist/molybdenum disulfide nano sheet/graphene composite material is entered in the burnishing surface of silicon substrate
Row coats process, and rotating speed is：The first step, 10s, 1000rpm；Second step, 40s, 6000rpm；It is subsequently placed in 100 DEG C of baking ovens and dries
15min obtains applying silicon-covered substrate.
3.3) after coating is finished, ultraviolet photolithographic processing is carried out to applying silicon-covered substrate, it is 90s to control the time for exposure, is then soaked
Enter the 60s that develops in RD6 developer solutions, then the rinse 30s in 1 grade of deionized water, finally the rinse 30s in 2 grades of deionized waters, moisten
Wash to be placed in 100 DEG C of baking ovens after finishing and dry 15min, obtain sample.
3.4) sample is placed under nitrogen atmosphere, carries out high temperature pyrolysis reaction, the process of high temperature pyrolysis reaction is：Tube furnace
With 2 DEG C of min-1Speed be warming up to 400 DEG C and be incubated 45min, then with 2 DEG C of min-1Speed be warming up to 600 DEG C and be incubated
After 45min, then with 2 DEG C of min-1Speed be warming up to 1000 DEG C and be incubated 1.5h, be subsequently cooled to room temperature and obtain pyrolytic carbon/bis-
Molybdenum sulfide nanometer sheet/graphene composite material patterning microelectrode.
Step 3.3 in embodiment 3) gained sample observe its pattern using SEM, as a result show its for connect
Continuous nanometer sheet pattern.By Autolab electrochemical workstations and cold probe platform to pyrolytic carbon/molybdenum disulfide nano sheet/stone
The chemical property of black alkene composite patterning microelectrode is tested：Gained pyrolytic carbon/molybdenum disulfide nano in embodiment 3
Piece/graphene composite material patterns microelectrode in sulfuric acid/PVA gel electrolytes, in 0-0.8V voltage windows and 5mVs-1
Sweep under speed its area specific capacity up to 4.2mF cm-2。
Novel pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material microelectrode has preferable obtained by above example
Chemical property, can wide popularization and application in the field such as micro-nano device and system.
Embodiments of the invention are described above in conjunction with accompanying drawing, but the invention is not limited in above-mentioned specific
Embodiment, above-mentioned embodiment is only schematical, rather than restricted, one of ordinary skill in the art
Under the enlightenment of the present invention, in the case of present inventive concept and scope of the claimed protection is not departed from, it can also make a lot
Form, these are belonged within the protection of the present invention.
Claims (9)
1. a kind of pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material patterning microelectrode, including substrate and photoetching are in base
Composite on plate, it is characterised in that the composite is by photoresist and molybdenum disulfide nano sheet/grapheme material group
Into the mass ratio of the photoresist and molybdenum disulfide nano sheet/grapheme material is 10~200：1；The molybdenum disulfide nano
Piece/grapheme material is made up of graphene, Sodium Molybdate Dihydrate, thiocarbamide, water, the graphene, Sodium Molybdate Dihydrate, thiocarbamide, water
Mass ratio is 1~10：400：600~700：10000~30000.
2. a kind of pyrolytic carbon/molybdenum disulfide nano sheet according to claim 1/graphene composite material patterns micro- electricity
Pole, it is characterised in that the substrate is silicon substrate or glass substrate.
3. a kind of pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material patterns the micro fabrication of microelectrode, its feature
It is, comprises the following steps：
1) graphene, Sodium Molybdate Dihydrate, thiocarbamide, water are pressed 1~10：400：600~700：10000~30000 mass ratio is mixed
Close it is uniform after, carry out hydrothermal synthesis reaction in a kettle., hydrothermal synthesis reaction finish after by centrifugation, be dried to obtain solid production
Thing, solid product is ground, and obtains molybdenum disulfide nano sheet/grapheme material；
2) photoresist and molybdenum disulfide nano sheet/grapheme material are pressed 10~200：Answered after 1 mass ratio is well mixed
Condensation material, composite is evenly applied to dry after substrate, then is carried out ultraviolet photolithographic, development and rinse and obtained sample, finally
High temperature pyrolysis reaction is carried out to sample under an inert atmosphere and obtains pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material figure
Case microelectrode.
4. a kind of pyrolytic carbon/molybdenum disulfide nano sheet according to claim 3/graphene composite material patterning microelectrode
Micro fabrication, it is characterised in that the reactor is inner liner polytetrafluoroethylene reactor, and the compactedness of the reactor is
50~70%.
5. a kind of pyrolytic carbon/molybdenum disulfide nano sheet according to claim 3/graphene composite material patterning microelectrode
Micro fabrication, it is characterised in that the high temperature pyrolysis reaction process is：The sample is heated to 200~400 first
DEG C, 15~45min is incubated, 500~600 DEG C are then heated to, 15~45min is incubated, continues to be heated to 700~1000 DEG C, guarantor
0.5~1.5h of temperature, is finally cooled to room temperature.
6. a kind of pyrolytic carbon/molybdenum disulfide nano sheet according to claim 3/graphene composite material patterning microelectrode
Micro fabrication, it is characterised in that the temperature of the hydrothermal synthesis reaction be 150~250 DEG C, the reaction time be 20~30h.
7. a kind of pyrolytic carbon/molybdenum disulfide nano sheet according to claim 3/graphene composite material patterning microelectrode
Micro fabrication, it is characterised in that the substrate be silicon substrate or glass substrate.
8. a kind of pyrolytic carbon/molybdenum disulfide nano sheet/graphene composite material patterning according to claim 3 or 7 is micro-
The micro fabrication of electrode, it is characterised in that the substrate is the polishing silicon substrate that surface carries silica oxide layer.
9. a kind of pyrolytic carbon/molybdenum disulfide nano sheet according to claim 3/graphene composite material patterning microelectrode
Micro fabrication, it is characterised in that the step 2) in, mixed to photoresist with molybdenum disulfide nano sheet/grapheme material
Ethanol is added in composite afterwards, the mass ratio of the ethanol and composite is 1：5~20.
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| CN107367905B (en) * | 2017-07-14 | 2019-04-12 | 北京师范大学 | The method for preparing photoresist-grapheme material compound system of high-specific surface area |
| CN107298442A (en) * | 2017-07-15 | 2017-10-27 | 中国海洋大学 | A kind of biomass carbon/molybdenum disulfide nano-composite material and preparation method thereof |
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| CN102142551B (en) * | 2011-02-25 | 2014-02-19 | 浙江大学 | Graphene nano sheet/MoS2 composite nano material and synthesis method thereof |
| CN102142538B (en) * | 2011-02-25 | 2014-04-09 | 浙江大学 | Lithium ion battery electrode made of graphene/ MoS2 and amorphous carbon and preparation method |
| KR102287343B1 (en) * | 2014-07-04 | 2021-08-06 | 삼성전자주식회사 | Hardmask composition and method of forming patterning using the hardmask composition |
| CN104226337B (en) * | 2014-09-16 | 2016-05-04 | 吉林大学 | A kind of graphene-supported sheet molybdenum disulfide nano compound and preparation method thereof |
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