CN107747212A - A kind of preparation method of the fluorescent fiber based on perovskite quantum dot - Google Patents
A kind of preparation method of the fluorescent fiber based on perovskite quantum dot Download PDFInfo
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- CN107747212A CN107747212A CN201711192580.9A CN201711192580A CN107747212A CN 107747212 A CN107747212 A CN 107747212A CN 201711192580 A CN201711192580 A CN 201711192580A CN 107747212 A CN107747212 A CN 107747212A
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- 239000000835 fiber Substances 0.000 title claims abstract description 83
- 239000002096 quantum dot Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 7
- 238000005538 encapsulation Methods 0.000 claims abstract description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- -1 halide ion Chemical group 0.000 claims description 13
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 9
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 4
- GSNUFIFRDBKVIE-UHFFFAOYSA-N DMF Natural products CC1=CC=C(C)O1 GSNUFIFRDBKVIE-UHFFFAOYSA-N 0.000 claims description 3
- 229930188620 butyrolactone Natural products 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 239000003086 colorant Substances 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 229910021645 metal ion Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- CMXPERZAMAQXSF-UHFFFAOYSA-M sodium;1,4-bis(2-ethylhexoxy)-1,4-dioxobutane-2-sulfonate;1,8-dihydroxyanthracene-9,10-dione Chemical compound [Na+].O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=CC=C2O.CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC CMXPERZAMAQXSF-UHFFFAOYSA-M 0.000 claims description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 2
- 239000011707 mineral Substances 0.000 claims description 2
- 239000002798 polar solvent Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000002657 fibrous material Substances 0.000 abstract 1
- 238000002604 ultrasonography Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 12
- 238000000151 deposition Methods 0.000 description 3
- BAVYZALUXZFZLV-UHFFFAOYSA-N mono-methylamine Natural products NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 3
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical group CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 1
- 229960000074 biopharmaceutical Drugs 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 125000000250 methylamino group Chemical group [H]N(*)C([H])([H])[H] 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
- C09K11/664—Halogenides
- C09K11/665—Halogenides with alkali or alkaline earth metals
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/02—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
- D06M13/03—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons with unsaturated hydrocarbons, e.g. alkenes, or alkynes
- D06M13/07—Aromatic hydrocarbons
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Textile Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses a kind of preparation method of the fluorescent fiber based on perovskite quantum dot, it is to prepare certain density perovskite precursor solution using good solvent, then appropriate surface end-capping reagent is added, porous fibre is soaked in the solution, ultrasound is pulled out after standing, poor solvent is coated on gained porous fibre surface again, the fluorescent fiber based on perovskite quantum dot is made in vacuum dried, encapsulation process.The present invention uses solwution method, large area prepares the perovskite quantum dot fluorescence fiber with high fluorescence efficiency under cryogenic, it has widened the preparation space of fluorescent fiber material, enormously simplify the preparation flow of fluorescent fiber, is advantageous to industrial volume production fluorescent fiber.
Description
Technical field
The invention belongs to perovskite quantum dot light emitting technical field, and in particular to a kind of fluorescence based on perovskite quantum dot
The preparation method of fiber.
Background technology
In the modern life, the application of fiber is ubiquitous.Be woven into military clothes from daily, from biologics to
Medical safety, it can be seen that the figure of fiber.Wherein fluorescent fiber is also known as safety fibre, and it can under the irradiation of ultraviolet light
To launch different colors, and after ultraviolet light disappears, fluorescent fiber reverts to the color of itself again, false proof so as to play
Effect.At present, fluorescent fiber is as a kind of most basic anti-fake material, the bank note of countries in the world, passport, stamp, security and
It is used widely in all kinds of cheque papers.In addition, the clothing not only antiwear heat resisting woven with fluorescent fiber, can be also used for military affairs
Protective garment, play hidden effect.But the performance of traditional fluorescent fiber is not excellent enough, its glow color is single, stability
Difference and the ultraviolet excitation that can only use single wavelength, which has limited application of the fluorescent fiber in real life.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the fluorescent fiber based on perovskite quantum dot, pass through the party
Method can with large area, low cost prepare fluorescent fiber, greatly simplify the process of synthesis fluorescent fiber, and optimize fluorescence
The fluorescence efficiency stability of fiber.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of the fluorescent fiber based on perovskite quantum dot, it comprises the following steps：
1）Certain density perovskite precursor solution is prepared using good solvent；
2）Appropriate surface end-capping reagent is added in gained perovskite precursor solution；
3）By porous fibre in step 2）Ultrasonic immersing in resulting solution；
4）Poor solvent is coated on step 3）Porous fibre surface after processing；
5）By step 4）Perovskite fluorescent fiber is obtained after the vacuum drying of gained porous fibre；
6）Gained perovskite fluorescent fiber is packaged processing, obtains the fluorescent fiber based on perovskite quantum dot.
Further, step 1）The concentration of middle perovskite precursor solution is 0.01-4mmol/mL；The perovskite can be with
For the mixing perovskite of organic perovskite, inorganic perovskite or organic-inorganic, its structural formula is ABX3, wherein, X is halogen
Ion, including Cl-、Br-、I-In any one or a few；B is Pb2+Or Sn2+；A is the amine organic groups such as methylamine, ethamine,
Or Cs+Deng inorganic metal ion, or both mixture.Step 1）Described in good solvent be the pole such as DMF, DMSO, butyrolactone
Any one or a few in property solvent.
Further, step 2）Described in surface end-capping reagent can be matched somebody with somebody using amino alkane, carboxyl alkane etc. as surface
The organic material of body, its addition are the 0.5%-15% of perovskite precursor solution volume.
Further, step 3）Described in the aperture of porous fibre be 1nm-50000nm, it can be string, dynamic
Any one or a few in fibres, mineral fibres, organic fiber, inorfil.
Further, step 4）Described in poor solvent be any one in the non-polar solven such as chlorobenzene, toluene；It is adopted
Porous fibre surface is coated on spray gun method or fumigating system, coating thickness is in 1nm-100 μ ms.
Further, step 5）In vacuum drying temperature control in the range of 20 DEG C -150 DEG C.
Further, step 6）Described in encapsulation process method include ALD, vacuum vapour deposition, solwution method.
Further, gained fluorescent fiber is transparent, has draftability；By changing the species of halide ion in perovskite, ratio
The aperture of example and porous fibre, can make gained fluorescent fiber can be sent under ultraviolet irradiation red, green, blueness,
The orange light for waiting different colours, and it is adjustable in visible-range.
Compared with prior art, the present invention can be in low temperature based on fluorescent fiber prepared by perovskite quantum dot（0℃-80
℃）Lower synthesis, its building-up process is fast and effective, technological operation is simple, beneficial to large-scale production, low manufacture cost, and prepares
The fluorescence efficiency of the perovskite quantum dot gone out is high, stability is good, fluorescent fiber has certain protective effect to quantum dot, has
Beneficial to the life-span for extending quantum dot, it is easy to carry out the popularization and use for being commercialized large area, there is great application prospect and city
Field value.
Brief description of the drawings
Fig. 1 is the schematic flow sheet of the inventive method；
Fig. 2 is the PL spectrograms of the perovskite fluorescent fiber prepared by embodiment 1.
Embodiment
The present invention provides a kind of preparation method of the fluorescent fiber based on perovskite quantum dot, and it comprises the following steps：
1）0.01-4mmol/mL perovskite precursor solution is configured to using good solvent；
2）Its volume 0.5%-15% surface end-capping reagent is added in gained perovskite precursor solution；
3）By porous fibre in step 2）Ultrasonic immersing in resulting solution；
4）Poor solvent is coated on by step 3 using spray gun method or fumigating system）Porous fibre surface after processing, its coating thickness
For 1nm-100 μm；
5）By step 4）After gained porous fibre is dried in vacuo under the conditions of 20 DEG C -150 DEG C, perovskite fluorescent fiber is obtained；
6）Gained perovskite fluorescent fiber is packaged processing, obtains the fluorescent fiber based on perovskite quantum dot.
Step 1）The perovskite can be the mixing perovskite of organic calcium titanium ore, inorganic perovskite or organic-inorganic, its
Structural formula is ABX3, wherein, X is halide ion, including Cl-、Br-、I-In any one or a few；B is Pb2+Or Sn2 +；A is the amine organic group such as methylamine, ethamine, or Cs+Deng inorganic metal ion, or both mixture.The good solvent is
Any one or a few in DMF, DMSO, butyrolactone polar solvent.
Step 2）Described in surface end-capping reagent can be as organic material of surface ligand using amino alkane, carboxyl alkane etc.
Material,.
Step 3）Described in the aperture of porous fibre be 1nm-50000nm, it can be string, animal origin, ore deposit
Any one or a few in fibres, organic fiber, inorfil.
Step 4）Described in poor solvent be any one in the non-polar solven such as chlorobenzene, toluene.
Step 6）Described in encapsulation process method include ALD, vacuum vapour deposition, solwution method.
Below in conjunction with the accompanying drawings and specifically the present invention is further described for embodiment, and the present invention provides preferred embodiment,
But it should not be considered limited to embodiment set forth herein.It should be appreciated that following descriptions for embodiment are more detailed
Carefully, the limitation to invention patent protection scope therefore can not be considered, one of ordinary skill in the art is the present invention's
Under enlightenment, in the case where not departing from the ambit that the claims in the present invention are protected, it is a variety of that replacement, simple combination etc. can also be made
Deformation.
Embodiment 1
A kind of preparation method of the fluorescent fiber based on perovskite quantum dot, is concretely comprised the following steps：
The first step：By 0.4mmol PbBr2It is dissolved in 0.4mmol CsBr in 10mLDMF and is configured to precursor solution；
Second step：1mL OA are added in precursor solution（Dodecyl amine-oxides）With 0.5mL Oam（N- octadecyl propylene
Acid amides）, stirring standing；
3rd step：Take porous fibre ultrasonic immersing in above-mentioned mixed solution；
4th step：10mL toluene is placed in spray gun, porous fibre surface after treatment, institute are sprayed using spraying process
Obtain the fluorescence that fiber sends green immediately under the irradiation of ultraviolet light；
5th step：Perovskite fluorescent fiber can be obtained after gained porous fibre is dried in vacuo；
6th step：Perovskite fluorescent fiber is packaged using ALD；
7th step：Fluorescent fiber after encapsulation process is woven into article.
Embodiment 2
A kind of preparation method of the fluorescent fiber based on perovskite quantum dot, is concretely comprised the following steps：
The first step：By 0.4mmol PbI2It is dissolved in 0.4mmol CsI in 10mLDMSO and is configured to precursor solution；
Second step：1mL OA and 0.5mL OAm are added in precursor solution, stirring is stood；
3rd step：Take porous fibre ultrasonic immersing in above-mentioned mixed solution；
4th step：10mL toluene is placed in spray gun, porous fibre surface after treatment, institute are sprayed using spraying process
Obtain the fluorescence that fiber sends red immediately under the irradiation of ultraviolet light；
5th step：Perovskite fluorescent fiber can be obtained after gained porous fibre is dried in vacuo；
6th step：Perovskite fluorescent fiber is packaged using vapour deposition method；
7th step：Fluorescent fiber after encapsulation process is woven into article.
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, it should all belong to the covering scope of the present invention.
Claims (9)
- A kind of 1. preparation method of the fluorescent fiber based on perovskite quantum dot, it is characterised in that：Comprise the following steps：1）Certain density perovskite precursor solution is prepared using good solvent；2）Surface end-capping reagent is added in gained perovskite precursor solution；3）By porous fibre in step 2）Ultrasonic immersing in resulting solution；4）Poor solvent is coated on step 3）Porous fibre surface after processing；5）By step 4）Perovskite fluorescent fiber is obtained after the vacuum drying of gained porous fibre；6）Gained perovskite fluorescent fiber is packaged processing, obtains the fluorescent fiber based on perovskite quantum dot.
- 2. the preparation method of the fluorescent fiber according to claim 1 based on perovskite quantum dot, it is characterised in that：Step 1）The concentration of middle perovskite precursor solution is 0.01-4mmol/mL；The structural formula of the perovskite is ABX3, wherein, X is halide ion, including Cl-、Br-、I-In any one or It is several；B is Pb2+Or Sn2+；A is the mixture of amine organic group, inorganic metal ion or both.
- 3. the preparation method of the fluorescent fiber according to claim 1 based on perovskite quantum dot, it is characterised in that：Step 1）Described in good solvent be any one or a few in polar solvent, including DMF, DMSO, butyrolactone.
- 4. the preparation method of the fluorescent fiber according to claim 1 based on perovskite quantum dot, it is characterised in that：Step 2）Described in surface end-capping reagent be amino alkane or carboxyl alkane, it adds volume as perovskite precursor solution volume 0.5%-15%。
- 5. the preparation method of the fluorescent fiber according to claim 1 based on perovskite quantum dot, it is characterised in that：Step 3）Described in the aperture of porous fibre be 1nm-50000nm, its be string, animal origin, mineral fibres, organic fiber, Any one or a few in inorfil.
- 6. the preparation method of the fluorescent fiber according to claim 1 based on perovskite quantum dot, it is characterised in that：Step 4）Described in poor solvent be any one in non-polar solven, including chlorobenzene, toluene；It uses spray gun method or fumigating system to be coated on porous fibre surface, and coating thickness is in 1nm-100 μ ms.
- 7. the preparation method of the fluorescent fiber according to claim 1 based on perovskite quantum dot, it is characterised in that：Step 5）In vacuum drying temperature control in the range of 20 DEG C -150 DEG C.
- A kind of 8. preparation method of fluorescent fiber based on perovskite quantum dot according to claim 1, it is characterised in that： Step 6）Described in encapsulation process method include ALD, vacuum vapour deposition, solwution method.
- 9. the preparation method of the fluorescent fiber according to claim 1 based on perovskite quantum dot, it is characterised in that：Gained Fluorescent fiber is transparent, tool draftability, and it can send the light of different colours under ultraviolet irradiation.
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| CN201711192580.9A CN107747212B (en) | 2017-11-24 | 2017-11-24 | Preparation method of fluorescent fiber based on perovskite quantum dots |
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| CN201711192580.9A CN107747212B (en) | 2017-11-24 | 2017-11-24 | Preparation method of fluorescent fiber based on perovskite quantum dots |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108589287A (en) * | 2018-04-03 | 2018-09-28 | 四川大学 | A kind of in-situ preparation method of fluorescence cotton fiber |
| CN109736073A (en) * | 2019-01-10 | 2019-05-10 | 陕西科技大学 | A kind of height mould proof terylene and preparation method thereof quantum-dot modified using tin based perovskites |
| CN110288900A (en) * | 2019-06-27 | 2019-09-27 | 福州大学 | A kind of antifalsification label and preparation method thereof based on perovskite nanometer sheet |
| KR102184508B1 (en) * | 2019-07-30 | 2020-11-30 | 인하대학교 산학협력단 | Halogen censor comprising Cellulose-CsPbBr3 complex |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108589287A (en) * | 2018-04-03 | 2018-09-28 | 四川大学 | A kind of in-situ preparation method of fluorescence cotton fiber |
| CN109736073A (en) * | 2019-01-10 | 2019-05-10 | 陕西科技大学 | A kind of height mould proof terylene and preparation method thereof quantum-dot modified using tin based perovskites |
| CN110288900A (en) * | 2019-06-27 | 2019-09-27 | 福州大学 | A kind of antifalsification label and preparation method thereof based on perovskite nanometer sheet |
| KR102184508B1 (en) * | 2019-07-30 | 2020-11-30 | 인하대학교 산학협력단 | Halogen censor comprising Cellulose-CsPbBr3 complex |
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| Publication number | Publication date |
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| CN107747212B (en) | 2020-05-08 |
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