CN104674539B - A kind of method for preparing luminescent fibre and fabric - Google Patents
A kind of method for preparing luminescent fibre and fabric Download PDFInfo
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- CN104674539B CN104674539B CN201310641778.6A CN201310641778A CN104674539B CN 104674539 B CN104674539 B CN 104674539B CN 201310641778 A CN201310641778 A CN 201310641778A CN 104674539 B CN104674539 B CN 104674539B
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- luminescent
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- fiber
- europium
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- 239000000835 fiber Substances 0.000 title claims abstract description 48
- 239000004744 fabric Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 27
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 14
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000005084 Strontium aluminate Substances 0.000 claims abstract description 12
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 11
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005516 engineering process Methods 0.000 claims abstract description 10
- FNWBQFMGIFLWII-UHFFFAOYSA-N strontium aluminate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Sr+2].[Sr+2] FNWBQFMGIFLWII-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 24
- 238000005477 sputtering target Methods 0.000 claims description 8
- 239000013077 target material Substances 0.000 claims description 8
- 229920000742 Cotton Polymers 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 229920004934 Dacron® Polymers 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 239000003365 glass fiber Substances 0.000 claims description 3
- 239000002241 glass-ceramic Substances 0.000 claims description 3
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 3
- 238000003980 solgel method Methods 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 abstract description 13
- 230000008569 process Effects 0.000 abstract description 9
- 238000000151 deposition Methods 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000005286 illumination Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- 230000008021 deposition Effects 0.000 description 5
- -1 europium ion Chemical class 0.000 description 4
- 230000002688 persistence Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 230000005283 ground state Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 230000005281 excited state Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention provides a kind of method for preparing luminescent fibre and fabric, the good europium of luminescent properties and dysprosium co-doped strontium aluminate luminescenjt powder are prepared for using sol-gal process, by radiofrequency magnetron sputtering technology, in the luminescent layer that fiber and web surface depositing homogeneous are fine and close.The present invention luminescent fibre and fabric preparation method process is simple it is convenient, workable, be easy to produce and control the scope of luminescent layer in batches, by the method preparation luminescent fibre and fabric illumination effect it is good, luminescent layer is firmly combined with substrate.
Description
Technical field
The present invention relates to functional fiber and fabric and coating technology field, are more particularly to one kind and prepare luminescent fibre
With the method for fabric.
Background technology
Luminescent fibre and luminescent fabric possess excellent luminescent properties, in ultraviolet lighting as new functional material
Luminous energy can be absorbed and is stored under penetrating, and after equal excitation stops, being released energy so as to light in dark surrounds in the form of visible ray,
Or luminescent fibre and luminescent fabric also can continuous illumination several minutes even a few hours after connection power supply.Luminescent fibre and
Luminescent fabric is applied to night time operation industry, military industry and navigation operation, is also applied to civil area to provide safe photograph
Bright and decoration functions.
At present, both at home and abroad for the research emphasis of luminescent textile material be mostly focused in spinning liquid add luminescent powder with
Luminescent fibre is prepared, however, this operation is in aqueous environments, the luminescent properties of luminescent powder can be affected by steam and decline,
And complex process efficiency is low, automaticity is low and it is not easy to operate, the subsequent treatment of fiber will also decrease sending out for luminescent fibre
Optical property, the binding ability of luminescent powder and fiber is poor in addition, and controllability is low thus be difficult in adapt to the production of personalized product.
It is at present less to see the relevant report that luminescent fibre and luminescent fabric are prepared using coating technology, and there is not yet
The research of luminescent fibre and luminescent fabric is prepared using radiofrequency magnetron sputtering technology.
, under the irradiation of daylight, ultraviolet light or artificial light, luminescent material exists for europium and dysprosium co-doped strontium aluminate luminescent powder
There is energy level transition between ground state and excited state（4f65d1→4f7）, hole is left in ground state level, additionally, hole can also
Captured by the dysprosium ion of codope；After light excites stopping, electronics releases energy from excited state transition time ground state and lights, or
Hole is recombined and is lighted with electronics.Due to the addition of the second excitation ion --- the dysprosium ion beyond europium ion, therefore
The luminescent properties of luminescent material can be significantly improved, its persistence is also substantially strengthened.Which has excellent photism
Can, its luminous intensity is high, and persistence is long, and stable chemical performance, environmental pollution are few, are deposited onto fiber and fabric
On, the good luminescent properties of fiber and fabric and decoration functions will be given.However, with fiber and fabric as substrate, sending out
Luminescent material is sputtering target material, and the research for preparing luminescent fibre and fabric using rf magnetron sputtering is less, and deposition technique is to luminous
The influence research of the luminescent properties of fiber and fabric is less.Therefore, using radiofrequency magnetron sputtering technology, with fiber and fabric as base
Bottom, luminescent material prepares luminescent fibre for sputtering target material and fabric is the innovation area and weight of current luminescent textile developing material
Want one of research topic.
The content of the invention
For disadvantages mentioned above, a kind of side for preparing illumination effect is good, binding force of cladding material is good luminescent fibre and fabric is developed
Method.
Further, in addition it is also necessary to develop that a kind of process is simple is convenient, workable, be easy to batch production, and adapt to
The preparation method of the luminescent fibre and fabric of personalized product production.
The invention provides a kind of method for preparing luminescent fibre and fabric, methods described with fiber and fabric as substrate,
With luminescent material as sputtering target material, luminescent material is sputtered and is deposited to fiber and web surface using radiofrequency magnetron sputtering technology
Method.
Preferably, according in the method for preparing luminescent fibre and fabric of the present invention, luminescent material is that europium and dysprosium are common
The strontium aluminate luminescent powder of doping.
Preferably, according in the method for preparing luminescent fibre and fabric of the present invention, europium and dysprosium co-doped aluminic acid
The chemical formula of strontium is SrAl2O4:Eu2+,Dy3+。
Preferably, according in the method for preparing luminescent fibre and fabric of the present invention, luminescent material is by sol-gel
It is prepared by method.
Preferably, according in the method for preparing luminescent fibre and fabric of the present invention, cotton, woven dacron, rustless steel,
Glass fibre and ceramic fiber cloth etc..
The present invention is prepared for the good europium of luminescent properties and dysprosium co-doped strontium aluminate luminous material using sol-gel process
Powder, by radiofrequency magnetron sputtering technology, in the luminescent layer that fiber and web surface depositing homogeneous are fine and close.The present invention's is luminous
The preparation method process is simple of fiber and fabric is convenient, workable, be easy to produce and control the scope of luminescent layer in batches, by
Luminescent fibre and the illumination effect of fabric prepared by the method is good, and luminescent layer is firmly combined with substrate.
Below by embodiment, the present invention will be further described.
Specific embodiment
The concrete technology flow process of the present embodiment is as follows：
(1) europium and dysprosium co-doped strontium aluminate luminous material of powder are prepared by sol-gel process：
A. Sr (the NO of 0.94mol are weighed3)2With the Al (NO of 2mol3)3·9H2O, and it is dissolved in a small amount of deionized water；Weigh
The Eu of 0.01mol2O3With the Dy of 0.02mol2O3It is dissolved in dilute HNO of 500mL3Nitrate solution is prepared into, then by two kinds of nitric acid
Saline solution is mixed into compound nitrate solution in case stand-by.
B. the citric acid for weighing 20g is dissolved in 50mL deionized waters, is prepared into citric acid solution.
C. above-mentioned citric acid solution is slowly added in above-mentioned composite solution, is then stirred in 80 DEG C of waters bath with thermostatic control and magnetic control
Under the conditions of mixing, the pH value for adjusting the composite solution with ammonia is 7.0, and stirring 5h obtains gel.
D. above-mentioned gel is dried into 11.5h in 105 DEG C of calorstat to remove excessive moisture, so as to obtain luminescent material
Precursor powder.
E. the SX3-3L-1400 types intelligence Muffle furnace for above-mentioned precursor powder being produced in Hangzhou Zhuo Chi Instrument Ltd.
In, after pre-burning 1h at 450 DEG C, 1200 DEG C are risen to the heating rate of 10 DEG C/min, in the reducing atmosphere that activated carbon powder is provided
Lower calcining 3h, obtains chemical formula for Sr0.94Eu0.02Dy0.04Al2O4Powdered luminescent materials.
When calcining under the reducing atmosphere that activated carbon powder is provided, the europium ion of trivalent is reduced into the europium ion of bivalence, most
Europium and dysprosium co-doped strontium aluminate luminescent powder are obtained eventually.The europium in this way preparing and dysprosium co-doped strontium aluminate luminous material
Luminous intensity is high, luminous efficiency is high, persistence is long.
(2) prepare sputtering target material：
Pour the europium of the powder of preparation and dysprosium co-doped strontium aluminate luminous material into mould that size is Φ 90mm × 8mm
In tool, above-mentioned luminescent material is suppressed under 19 tons of static pressures with the manual standard type tablet machine of 3855 type U.S. CARVER and obtain after 1h
To the sputtering target material of round pie, its thickness is about 6mm.
The sputtering target material in this way preparing, due to the press time it is long, it is not necessary to make by carrying out annealing sintering processes
With process is simple, efficiency high.
(3) weaving face fabric pre-treatment：
By the stainless steel fibre cloth of 60mm × 60mm sizes, 40min is respectively washed with dehydrated alcohol and acetone successively, then is used
Deionized water is clean by unnecessary solvent clean, is then placed in being dried 24h in 80 DEG C of baking oven to remove unnecessary moisture.
The stainless steel fibre cloth clean surface in this way cleaned and be dried, residual moisture are few, are especially suitable for radio frequency
Control sputtering, can obtain preferable luminescent layer.
（4）Magnetron sputtering deposition：
A. the stainless steel fibre cloth of drying is arranged on into the POLED/ that Shenyang Institute Of Ultra-High Vacuum Applications are developed
On the substrate frame of the vacuum chamber of PET- magnetron sputtering deposition vacuum systems, sputtering target material is arranged in target support, and is protected
The distance for holding base material and target is 10cm.
B. background vacuum be 0.0001Pa, deposition pressure be 0.6Pa, argon ventilation be 40sccm, sample rotating speed
Under the conditions of the technological parameter of 100r/min, deposition power for 500W, pre-sputtering deposition 5min, the sputtering sedimentation time is 15min,
The luminescent powder thickness for being sputtered is about 2um.
The luminescent fabric luminous intensity prepared under the process conditions of the present embodiment is high, and persistence is long, and luminous efficiency is high,
The associativity of luminescent layer and fabric is good, and the luminescent layer distribution of shapes for obtaining is controllable, and the adaptation of product is high.
In the present invention, textile fabric and fabric are not limited to cotton, woven dacron, rustless steel, glass fibre and ceramic fibre
Cloth, can also such as be common polyester-mixed cotton cloth, silk cloth, and carbon fiber, the specialty fibers cloth such as graphitized carbon fibre.
Above-described embodiment is interpreted as being merely to illustrate the present invention rather than limits the scope of the invention.Readding
After having read the content of record of the present invention, those skilled in the art can be made various changes or modifications to the present invention, and these are equivalent
Change and modification equally fall into the scope of the claims in the present invention.
Claims (1)
1. a kind of method for preparing luminescent fibre and fabric, it is characterised in that methods described with fiber and fabric as substrate, to send out
Luminescent material is sputtering target material, luminescent material is sputtered and deposited to the side of fiber and web surface using radiofrequency magnetron sputtering technology
Method；
The fiber and fabric are cotton, woven dacron, rustless steel, glass fibre or ceramic fiber cloth；
The luminescent material is europium and dysprosium co-doped strontium aluminate；The chemical formula of the europium and dysprosium co-doped strontium aluminate is
SrAl2O4:Eu2+,Dy3+；
The luminescent material is prepared by sol-gel process.
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|---|---|---|---|
| CN201310641778.6A CN104674539B (en) | 2013-12-03 | 2013-12-03 | A kind of method for preparing luminescent fibre and fabric |
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| CN201310641778.6A CN104674539B (en) | 2013-12-03 | 2013-12-03 | A kind of method for preparing luminescent fibre and fabric |
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| Publication Number | Publication Date |
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| CN104674539A CN104674539A (en) | 2015-06-03 |
| CN104674539B true CN104674539B (en) | 2017-04-05 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107287879B (en) * | 2016-03-31 | 2020-03-10 | 香港理工大学 | Preparation method of luminous textile fabric based on laser annealing process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102337671A (en) * | 2010-07-27 | 2012-02-01 | 五邑大学 | Preparation method of intelligent anti-ultraviolet fabric |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102337671A (en) * | 2010-07-27 | 2012-02-01 | 五邑大学 | Preparation method of intelligent anti-ultraviolet fabric |
Non-Patent Citations (1)
| Title |
|---|
| 射频磁控溅射制备铝酸锶长余辉发光薄膜;谢伟 等;《材料研究与应用》;20130930;第7卷(第3期);第188-192页 * |
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