CN107761194A - A kind of multiple nanometer carbon filament composite carbon fiber and preparation method thereof - Google Patents
A kind of multiple nanometer carbon filament composite carbon fiber and preparation method thereof Download PDFInfo
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- CN107761194A CN107761194A CN201711027199.7A CN201711027199A CN107761194A CN 107761194 A CN107761194 A CN 107761194A CN 201711027199 A CN201711027199 A CN 201711027199A CN 107761194 A CN107761194 A CN 107761194A
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- carbon fiber
- carbon
- circumvolution
- multiple nanometer
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
- D01F9/1273—Alkenes, alkynes
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
- D01F9/1271—Alkanes or cycloalkanes
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
- D01F9/1273—Alkenes, alkynes
- D01F9/1275—Acetylene
Abstract
The invention discloses a kind of multiple nanometer carbon filament composite carbon fiber, the multiple nanometer carbon filament composite carbon fiber is the compound circumvolution shape carbon fiber of multiple nanometer carbon filament, and its expansion performance meets Hooke's law, and modulus of rigidity is more than 9.8Gpa.A diameter of 0.1~10 μm of the circumvolution of the compound carbon fiber, pitch are 0.1~5.5 μm, form a diameter of 0.05~1.5 μm of the carbon subfiber of the compound carbon fiber, the subfiber is combined by a diameter of 50 500 nanometers of carbon filament multiply;The compound carbon fiber is along circumvolution axle with constant circumvolution diameter and pitch regularly circumvolution.Using above-mentioned technical proposal, the present invention has advantages below relative to prior art:Preparation is simple, multiple nanometer carbon filament composite carbon fiber of the invention not only well-regulated circumvolution form, there is certain pitch dimension, and simultaneously flexible and rigid, suitable for used aloned as micromechanical component.
Description
Technical field
The present invention relates to a kind of multiple nanometer carbon filament composite carbon fiber, i.e., the multiple compound circumvolution shape carbon fiber of nanometer carbon filament
Preparation method, belong to multifunctional carbon fiber field of material technology.
Background technology
The carbon fiber of carbon fibre material field inward turning web-like has the premium properties of carbon material and the uniqueness of circumvolution shape because of it
Shape, make it that there are bright prospects in the application of electromagnetic material, composite additives etc..Therefore, its prepare and itself
The optimization of characteristic is the primary study object in such carbon fibre material field.
The method of current synthesis circumvolution shape carbon fiber is to use nickel catalytic chemical vapor deposition technique (Chemical Vapor
Deposition, abbreviation CVD), what can largely be obtained is micro- screwed pipe that the close circumvolution of double carbon filament forms, or interior through for zero
Torsion rope form micron (nanometer) grade carbon fiber.And with a constant pitch, the rigid big micro- carbon fiber of regular circumvolution compares screwed pipe
Or torsion rope form Nano/micron carbon fiber has more preferable micromechanics characteristic, but still lack the good synthesis technique of repeatability at present.
Therefore, in order to applied to microelectromechanical systems, exploitation rigidity is big and flexible micro- circumvolution shape carbon fiber it is steady
It is the technical problem that this area is badly in need of solving to determine technology of preparing.
Bibliography:
①CN 200410065511
②CN 200610148006.9
③CN 201310636461
④CN 201410424026
The content of the invention
The object of the present invention is to overcome the problems of the prior art point, is conceived to that to provide a kind of its own shape rule even
Claim, the good compound circumvolution shape carbon fiber of multiple nanometer carbon filament of retractility.
Based on foregoing invention purpose, the application provides multiple nanometer carbon filament composite carbon fiber, and the multiple nanometer carbon filament is compound
Carbon fiber is the compound circumvolution shape carbon fiber of multiple nanometer carbon filament, and its expansion performance meets Hooke's law, modulus of rigidity be 9.8Gpa with
On.
In order to preferably realize goal of the invention, in some embodiments, the circumvolution a diameter of 0.1 of the compound carbon fiber~
10 μm, pitch is 0.1~5.5 μm, forms a diameter of 0.05~1.5 μm of the carbon subfiber of the compound carbon fiber, the subfiber by
The carbon filament multiply of a diameter of 50-500 nanometers is combined;The compound carbon fiber is along circumvolution axle with constant circumvolution diameter and spiral shell
Away from regularly circumvolution.
The nanometer carbon filament composite carbon fiber of the present invention is supported on conduct on carrier including the catalyst fines containing copper and mickel
Supported catalyst, making hydrocarbon, catalytic pyrolysis is compound into carbon particulate deposition into multiple nanometer carbon filament in a hydrogen atmosphere
Circumvolution shape carbon fiber;Loaded catalyst containing copper and mickel use containing nitrate and catalyst it is compound, copper is in composite catalyst
Content and the ratio between nickel content be no less than 10% (count by weight percentage);The particle diameter of carrier is between 0.5~5 μm, carrier
Specific surface area be not less than 20m2The mass ratio of/g, catalyst and carrier is 0.05~0.2:1.The dosage of supported catalyst is
React substrate 10~50mg/cm of upper berth2。
The present invention is hydrocarbon is cracked in hydrogen atmosphere high temperature by using anisotropy supported catalyst
For carbon particle, deposition growing is realized into micron circumvolution shape carbon fiber.Carbon is micro- after hydrocarbon oxidation catalyst cracking in the present invention
Grain deposition growing, reaction time preferably 1~3h.Catalyst containing copper is obtained by powder load on carrier.
Present invention also offers a kind of multiple nanometer carbon filament composite carbon fiber producing processes, comprise the following steps:
1) substrate surface, being laid in catalyst in reactor;
2), 700~850 DEG C will be heated in reactor in a nitrogen atmosphere;
3) hydrocarbon gas and hydrogen, are imported, while imports the catalytic promoter containing sulphur;
4), maintenance reaction 0.5-5 hours;
5) the compound circumvolution shape carbon fiber of multiple nanometer carbon filament is obtained after, cooling down.
In order to preferably realize goal of the invention, in some embodiments, the import volume of catalytic promoter is to ensure in gas
The volumetric concentration of sulphur is 0.01~5% in phase.
In order to preferably realize goal of the invention, in some embodiments, hydrocarbon is ethene, acetylene or third
Alkane, the importing flow of hydrocarbon is 0.5~5sccm of substrate area every square centimeter.
In order to preferably realize goal of the invention, in some embodiments, the multiple compound circumvolution shape carbon fiber of nanometer carbon filament
Preparation method, the ratio between import volume of hydrogen and hydrocarbon is 0.5~2 in this method:1, the import volume of nitrogen and hydrogen
The ratio between be 0.5~3:1.
In order to preferably realize goal of the invention, in some embodiments, supported catalyst is laid in reactor
Substrate surface, make to be heated to 700~850 DEG C in reactor in a nitrogen atmosphere, import hydrocarbon gas and hydrogen, simultaneously
Little power shape catalytic promoter, maintenance reaction 30 minutes to some hours are imported with nitrogen stream.The process of reaction is to make carbon
Process of the hydrogen compound catalytic pyrolysis into carbon particulate deposition growing.
In order to preferably realize goal of the invention, in some embodiments, by the nitrate and catalyst carrier of copper and mickel
Mixing, under a hydrogen atmosphere in 700 DEG C of calcinings;For the particle diameter of carrier between 0.5~5 μm, the specific surface area of carrier is not less than 20m2/
G, the present invention in catalyst and carrier mass ratio be 0.05~0.2:1.
The dosage of supported catalyst is reaction substrate 10~50mg/cm of upper berth in the present invention2, reduce catalyst usage amount
Being advantageous to avoid the multiple nano combined circumvolution shape carbon fiber of product from winding mutually so that operation is easy when picking single circumvolution, but
Usage amount is too low to influence catalytic effect;Catalyst granules can be caused to be gathered into bulky grain and cannot get on the contrary, usage amount is too high
Multiple nano combined circumvolution shape carbon fiber.Reaction substrate in reactor is graphite or metal substrate, and reactor is preferably horizontal
Reaction tube, in order to the multiple nano combined circumvolution shape carbon fiber of large area deposition;The top of reaction tube sets airway tube, to lead to
Enter to crack and obtain the unstrpped gas of carbon, being continuously passed through nitrogen from reaction tube both ends prevents large quantity of air from entering in pipe, reaction
Pressure in pipe is atmospheric pressure.
The hydrocarbon imported in the present invention is ethene, acetylene or propane, preferably acetylene;Sulfur-bearing catalytic promoter is too
Height can cause to be catalyzed crystal seed poisoning and stop growing, and content is too low, can have to straight line carbon fiber.Hydrocarbon is led
Inbound traffics are 0.5~5sccm of substrate area flow every square centimeter, the ratio between import volume of hydrogen and hydrocarbon for 0.5~
2:1, the ratio between import volume of nitrogen and hydrogen is 0.5~3:1.
Carbon fiber vapor growth mechanism is as follows in present invention reaction:Reaction starting stage catalyst granules tends to reacting
Bulky grain is gathered on substrate, after being passed through accelerator and remaining gas, catalyst crystal seed is formed from bulky grain, is emerged upwards,
Hydrocarbon decomposes in the presence of catalyst crystal seed, and the hydrocarbon further imported decomposes on each crystal face, expands
Symmetrical crystal face is scattered to deposit as multiple nano combined circumvolution shape carbon fiber.
Under suitable reaction temperature and reactant concentration, due to the anisotropy of crystal plane, the three of catalyst crystal grain are brilliant
On face, the speed that carbon separates out is different and grows carbon filament circumvolution.Specifically because more subfibers close caused by multiple faces
Into one carbon filament (single line), the subfiber that the crystal plane small from activity is formed is in inner side, the Asia of the crystal plane formation big from activity
Fiber causes carbon filament internal stress in outside, therefore carbon filament is had to grow up into circumvolution the multiple nanometer of form rule and answered
Close circumvolution shape carbon fiber.
From using merely unlike metallic catalyst nickel, the present invention is assisted due to the importing of copper, and with sulfur containing promoter
Same-action, within induction period, unstable alloy carbide and gas molecular action, nickel sheet is produced in alloy surface, but Cu,
S covering inhibits the reconstruction of particle, it is suppressed that the formation of Ni (111) crystal face, as a result, being produced from catalyst granules many
Small crystal face, carbon filament from these crystal faces grow and go out, under those gas flows and assigned temperature under the conditions of with regard to multiple receive can be obtained
The circumvolution shape carbon fiber that rice carbon filament is combined.Temperature control is at 700 to 850 DEG C during present invention reaction inner reaction tube, preferably
750-800 DEG C, temperature is too high or too low all cannot get multiple nano combined circumvolution shape carbon fiber.
Heretofore described modulus of rigidity method of testing includes:
1st, the computational methods of spring constant:Fracture strength is the bigger the better, and micro- circumvolution carbon crystallinity of the invention is sent out than Japan
Carbon fiber involved by bright open JPA_2006083494 is high, is because growth conditions is optimized, particulate accumulation construction lacks
Fall into and reduce, so fracture strength is high, average fracture strength 63Mpa, fracture strength here:Determined with microoperation robotic arm
One section of obtained micro- carbon circumvolution (spring) tensile strength.Microoperation robotic arm and micro electronic balance are combined, micro- carbon circumvolution
One end and be placed on the loading of micro electronic balance and be connected, the other end and microoperation robotic arm, specific practice is day
Heibei provincial opera zero, then the micro- carbon circumvolution of measure object is passed through by axial tension of the micro-mechanical arm along micro- carbon circumvolution or compression
The elongation z of loading F and spring when micro- carbon circumvolution is disconnected, spring constant k is calculated based on Hooke's law (F=k × z).
Balance loading when being broken from micro- carbon circumvolution calculates fracture strength.Spring constant is calculated according to Hooke's law.
2nd, modulus of rigidity:Micro- carbon circumvolution modulus of rigidity G calculates from following equation
Wherein k, G, d, N and D are represented as follows respectively:
k:Spring constant (N/mm)
G:Modulus of rigidity (MPa (=N/mm2)〕
d:Fibre diameter (mm)
N:Active spring coils number
D:Spring (mm)
3rd, active spring coils number N computational methods are as follows:
Wherein L:Microspring length (mm), P:Spring pitch (mm)
Using above-mentioned technical proposal, the present invention has advantages below relative to prior art:Preparation is simple,
Although the compound circumvolution shape carbon fiber productivity ratio of multiple nanometer carbon filament of the present invention is relatively low, not only well-regulated circumvolution form and height
Crystallinity, there is bigger pitch, and it is flexible and rigid, suitable for used aloned as micromechanical component.
Brief description of the drawings
Fig. 1 is the growth tip scanning electron microscopy of the multiple compound circumvolution shape carbon fiber of nanometer carbon filament of the present invention.
Fig. 2 is the scanning electron microscopy of the corpus fibrosum of the multiple compound circumvolution shape carbon fiber of nanometer carbon filament of the present invention.
Embodiment
The invention will now be described in further detail with reference to the accompanying drawings.
With reference to Fig. 1,2, copper nitrate, nickel nitrate and ultra-fine alumina carrier are sufficiently mixed, copper and mickel weight ratio is 6:4,
The weight of carrier is 10 times of copper and nickel element gross weight;Hydrogen gas of the calcining furnace at 700 DEG C is moved into after being dried in 80 DEG C
Calcined 3 hours in atmosphere and obtain carrier model composite catalyst, synthesized as follows:
Synthetic example one:Supported catalyst is pressed into 30mg/cm2Amount be laid in the substrate table being flat in reactor
Face, for constant temperature at 700~750 DEG C, it is substrate area 1sccm every square centimeter to import acetylene flow to reactor in a nitrogen atmosphere,
The ratio between import volume of hydrogen and hydrocarbon is 1.5:1, the ratio between import volume of nitrogen and hydrogen is 0.5:1, while use hydrogen
Sulphur-containing substance thiophene is carried and imports reaction system, controls the content of sulphur in gas to account for 0.5%, makes hydrocarbon in hydrogen gas
Catalytic pyrolysis is deposited on composite catalyst crystal face into carbon particulate under atmosphere, and reaction obtains multiple nanometer carbon filament in two hours and is combined
Circumvolution shape carbon fiber, as depicted in figs. 1 and 2, it is 10.7Gpa to measure modulus of rigidity to its microscopic pattern.
Synthetic example two:Supported catalyst is pressed into 50mg/cm2Amount be laid in the substrate table being flat in reactor
Face, for constant temperature at 760~790 DEG C, it is substrate area 5sccm every square centimeter to import acetylene flow to reactor in a nitrogen atmosphere,
The ratio between import volume of hydrogen and hydrocarbon is 2:1, the ratio between import volume of nitrogen and hydrogen is 3:1, while with the hydrogen
Sulphur-containing substance thiophene is carried and imports reaction system, controls the content of sulphur in gas to account for 0.9%, makes hydrocarbon in hydrogen gas
Catalytic pyrolysis is deposited on composite catalyst crystal face into carbon particulate under atmosphere, and reaction obtains multiple nanometer carbon filament in two hours and is combined
Circumvolution shape carbon fiber, a diameter of 4.2 μm of circumvolution, pitch be 1.2 μm, it is 10.3Gpa to measure modulus of rigidity.
Synthetic example three:Supported catalyst is pressed into 10mg/cm2Amount be laid in the substrate table being flat in reactor
Face, constant temperature at 800~850 DEG C, imports hydrocarbon gas and hydrogen to reactor in a nitrogen atmosphere, and importing acetylene flow is
The ratio between import volume of substrate area 0.5sccm every square centimeter, hydrogen and hydrocarbon is 0.5:1, nitrogen and hydrogen are led
Enter the ratio between amount for 0.5:1, while sulphur-containing substance thiophene is carried with the hydrogen and imports reaction system, sulphur contains in control gas
Amount accounts for 0.1%, and making hydrocarbon, catalytic pyrolysis is deposited on composite catalyst crystal face into carbon particulate in a hydrogen atmosphere, reaction
The circumvolution shape carbon fiber that multiple nanometer carbon filament is combined, a diameter of 1.9 μm of circumvolution are obtained within two hours, pitch is 0.5 μm, is measured
Modulus of rigidity is 11.7Gpa.
Above-described is only some embodiments of the present invention.For the person of ordinary skill of the art, not
On the premise of departing from the invention design, various modifications and improvements can be made, these belong to the protection model of the present invention
Enclose.
Claims (8)
- A kind of 1. multiple nanometer carbon filament composite carbon fiber, it is characterised in that:Described multiple nanometer carbon filament composite carbon fiber is more The compound circumvolution shape carbon fiber of weight nanometer carbon filament, its expansion performance meet Hooke's law, and modulus of rigidity is more than 9.8Gpa.
- 2. multiple nanometer carbon filament composite carbon fiber according to claim 1, it is characterised in that:Described multiple nanometer carbon filament A diameter of 0.1~10 μm of the circumvolution of compound carbon fiber, pitch are 0.1~5.5 μm, form described multiple nanometer carbon filament composite carbon A diameter of 0.05~1.5 μm of the carbon subfiber of fiber, the carbon subfiber is compound by the carbon filament multiply of a diameter of 50-500 nanometers Form;Described multiple nanometer carbon filament composite carbon fiber circumvolution is regularly revolved along circumvolution axle with constant circumvolution diameter and pitch Volume.
- 3. multiple nanometer carbon filament composite carbon fiber according to claim 1 or 2, it is characterised in that:Described nanometer carbon filament Compound carbon fiber is supported on carrier including the catalyst fines containing copper and mickel and is used as supported catalyst, makes hydrocarbon Catalytic pyrolysis forms the compound circumvolution shape carbon fiber of multiple nanometer carbon filament into carbon particulate deposition in a hydrogen atmosphere;It is described to contain copper and mickel Loaded catalyst use compound containing nitrate and catalyst carrier, the content of described copper in composite catalyst contains with nickel The ratio between amount is no less than 10%;For the particle diameter of the carrier between 0.5~5 μm, the specific surface area of carrier is not less than 20m2/ g, it is described The mass ratio of catalyst and carrier is 0.05~0.2:1.
- 4. multiple nanometer carbon filament composite carbon fiber according to claim 3, it is characterised in that:The supported catalyst Dosage is reaction substrate 10~50mg/cm of upper berth2。
- 5. the multiple nanometer carbon filament composite carbon fiber producing processes according to any one of Claims 1-4, it is characterised in that Comprise the following steps:1) substrate surface, being laid in the catalyst in reactor;2), 700~850 DEG C will be heated in reactor in a nitrogen atmosphere;3) hydrocarbon gas and hydrogen, are imported, while imports the catalytic promoter containing sulphur;4), maintenance reaction 0.5-5 hours;5) the compound circumvolution shape carbon fiber of multiple nanometer carbon filament is obtained after, cooling down.
- 6. the preparation method of multiple nanometer carbon filament composite carbon fiber according to claim 5, it is characterised in that:Catalysed promoted The import volume of agent is to ensure that the volumetric concentration of sulphur in the gas phase is 0.01~5%.
- 7. the preparation method of multiple nanometer carbon filament composite carbon fiber according to claim 5, it is characterised in that described carbon Hydrogen compound is ethene, acetylene or propane, the importing flow of the hydrocarbon be substrate area 0.5 every square centimeter~ 5sccm。
- 8. the preparation method of multiple nanometer carbon filament composite carbon fiber according to claim 5, it is characterised in that the hydrogen It is 0.5~2 with the ratio between the import volume of hydrocarbon:1, the ratio between import volume of nitrogen and hydrogen is 0.5~3:1.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109368615A (en) * | 2018-12-11 | 2019-02-22 | 广东双虹新材料科技有限公司 | A kind of composite Nano carbon material and preparation method thereof |
CN111586945A (en) * | 2020-05-29 | 2020-08-25 | 福建星宏新材料科技有限公司 | Single-key touch-press dimming switch and switch dimming method |
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CN1327093A (en) * | 2000-06-07 | 2001-12-19 | 华侨大学 | High elastic screw carbon fibre and its preparing method |
CN102745665A (en) * | 2012-01-06 | 2012-10-24 | 中国科学院成都有机化学有限公司 | Method for preparing helical structure carbon nanotubes |
CN104843672A (en) * | 2015-04-29 | 2015-08-19 | 广东双虹新材料科技有限公司 | Coiling micro-carbon spring and preparation method thereof |
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JPH02300323A (en) * | 1989-05-13 | 1990-12-12 | Tanaka Kikinzoku Kogyo Kk | Spinneret for carbon fiber |
CN1327093A (en) * | 2000-06-07 | 2001-12-19 | 华侨大学 | High elastic screw carbon fibre and its preparing method |
CN102745665A (en) * | 2012-01-06 | 2012-10-24 | 中国科学院成都有机化学有限公司 | Method for preparing helical structure carbon nanotubes |
CN104843672A (en) * | 2015-04-29 | 2015-08-19 | 广东双虹新材料科技有限公司 | Coiling micro-carbon spring and preparation method thereof |
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CN109368615A (en) * | 2018-12-11 | 2019-02-22 | 广东双虹新材料科技有限公司 | A kind of composite Nano carbon material and preparation method thereof |
CN111586945A (en) * | 2020-05-29 | 2020-08-25 | 福建星宏新材料科技有限公司 | Single-key touch-press dimming switch and switch dimming method |
CN111586945B (en) * | 2020-05-29 | 2023-04-21 | 福建星宏新材料科技有限公司 | Single-key touch-press light-adjusting switch |
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