CN107761366A - The preparation method of the electrospun fibers of gold nanorods load - Google Patents
The preparation method of the electrospun fibers of gold nanorods load Download PDFInfo
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- CN107761366A CN107761366A CN201711166010.2A CN201711166010A CN107761366A CN 107761366 A CN107761366 A CN 107761366A CN 201711166010 A CN201711166010 A CN 201711166010A CN 107761366 A CN107761366 A CN 107761366A
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- gold nanorods
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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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
- D06M11/83—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 metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/24—Polymers or copolymers of alkenylalcohols or esters thereof; Polymers or copolymers of alkenylethers, acetals or ketones
-
- 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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Artificial Filaments (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The present invention relates to synthetic fiber industry technical field, and in particular to a kind of preparation method of the electrospun fibers of gold nanorods load.A kind of preparation method of the electrospun fibers of gold nanorods load, comprises the following steps：（1）The preparation of gold nanorods；（2）The preparation of PVA/PAA electrospinning fibres；（3）Self assembly of the gold nanorods in fiber surface.As the method for the electrospun fibers that the gold nanorods that prepare of the present invention load it is simple, obtained by tunica fibrosa SERS substrates enhancing effect it is good, soft and can cut, can be advantageously used in conventional SERS detections.
Description
Technical field
The present invention relates to synthetic fiber industry technical field, and in particular to a kind of electrospun fibers of gold nanorods load
Preparation method.
Background technology
SERS with its high sensitivity, sample nondestructive is hindered and abundant molecular information can be provided
The features such as and be widely used in the fields such as material analysis, environment measuring and life science.The design of rational SERS substrates
It is to obtain the key point of high sensitivity SERS signal with preparation.In recent years, with electro spinning nano fiber carried noble metal nanoparticle
Son turns into the focus of research as SERS substrates.On the one hand, high activity SERS materials are usually noble metal nanometer material, but are received
Rice corpuscles due to unstability itself and assembling makes SERS performances drastically decline, simple noble metal nano particles are difficult to meet normal
The requirement of SERS substrates is advised, solves the problems, such as nanoparticle aggregation by carrier of electrospinning fibre.On the other hand, due to electricity
The high-specific surface area and high porosity of spinning fiber film and the 3D structures of itself so that more nano-particles can be with detection point
Son combines, there is provided stronger Raman signal.The polyvinyl alcohol containing Nano silver grain is prepared for from the method for first passage blending
After electrospun fiber membrane SERS substrates, noble metal nano particles by a variety of methods and electro spinning nano fiber it is compound and by with
Make SERS substrates.By silver nitrate/agar/polyacrylonitrile solution blending, by the electrospinning fibre of gained under ultraviolet light it is former
Position reduction, has obtained the composite electrospun fiber of Nano silver grain load, and the fiber can detect as little as 0.1 μ as SERS substrates
The presence of mol/L malachite green.Fiber surface, profit are modified in electrospinning polyacrylonitrile fibre surface aggregate by m-phenylene diamine (MPD)
Nano silver grain is supported on the hydrogen bond action between the fiber surface after modification and the citrate on Nano silver grain surface
Fiber surface, the 3D SERS substrates that enhancing effect is better than 2D substrates are obtained.Outside, plating, chemical plating and growth in situ etc.
Method is also widely used in the preparation of nano-particle/electrospinning composite fibre.
In numerous nano-particles, gold nanorods construct list as a kind of anisotropy nanometer being widely studied
Member.Because it has two different surface plasmon absorption peaks, and longitudinal SPR absworption peaks visible ray with
The ideal material that near infrared light region is adjustable and is applied as SERS.Gold nanorods are assembled using electrospun fibers as carrier to be used as
The related work of SERS substrates has been reported.However, prepared gold nanorods/electrospinning composite fibre is due to gold nanorods blending
In fibrous inside, in detection probe molecule, probe molecule needs to be seeped into fibrous inside and could combined with gold nanorods, so as to subtract
Weak SERS signal；Electrospinning fibre is modified by the method for LBL self-assembly, using after modification between fiber and gold nanorods
Electrostatic force load gold nano rod, it is prepared for the SERS substrates that gold nanorods are assembled in electrospun fibrous surface, but the method used in it
Need to carry out electrospinning fibre multiple modification, preparation process is excessively cumbersome.How surface prepared by simple effective method
One of the problem of composite electrospun fiber of load gold nano rod is current urgent need to resolve.
The content of the invention
It is contemplated that in view of the above-mentioned problems, propose a kind of preparation method of the electrospun fibers of gold nanorods load.
Technical program of the present invention lies in：
A kind of preparation method of the electrospun fibers of gold nanorods load, comprises the following steps：
（1）The preparation of gold nanorods；
（2）The preparation of PVA/PAA electrospinning fibres；
（3）Self assembly of the gold nanorods in fiber surface.
The preparation method of described gold nanorods is as described below：It is first that 103 μ L mass fractions are molten for 1% gold chloride
Drop is added in 8mL0.1mol/L CTAB solution, after stirring 2min, adds 0.6mL Fresh
0.01mol/L sodium borohydride solutions, continue to obtain seed solution after stirring 3 min.The solution can be used for growing in 2 ~ 5h
The seed of gold nanorods;Then configuration growth solution, growth solution are configured to sequentially add 47. 5mL 0.1mol/L's
The CTAB aqueous solution, 1.03 mL 1% aqueous solution of chloraurate, 200 μ L silver nitrate aqueous solutions and 400 μ L ascorbic acid
The aqueous solution；Finally, 60 μ L seed solutions are added in growth solution, growth 10h is stood after jog 30s, it is molten to obtain gold nanorods
Liquid.
The preparation method of described PVA/PAA electrospinning fibres is as described below：0.5g PVA powder is weighed, adds 4.5g water,
Stirring 4h obtains PVA solution at room temperature；The 2g 25%PAA aqueous solution then is weighed, is diluted with water to 5g；Finally by both the above
The mass mixings such as solution, continuing stirring 2h makes it well mixed, obtains spinning solution；Gained spinning solution is subjected to electrostatic spinning,
Obtain PVA/PAA electrospun fiber membranes；Tunica fibrosa is then heat-treated 30min in 145 DEG C, makes tunica fibrosa not soluble in water.
Described gold nanorods are as described below in the process of the self assembly of fiber surface：By the PVA/PAA electricity after heat treatment
Spinning fiber film soaks 3h in deionized water, is adequately ionized the carboxyl in fiber；Then the tunica fibrosa after immersion is immersed in
In gold nanorods solution；Tunica fibrosa is taken out after 12h and with deionized water rinsing 3 times, removing fiber surface solid gold not strong for load
Nanometer rods, drying at room temperature.
The spinning voltage of described electrostatic spinning is 15kV, and charging rate is 300 μ L/h, and it is 20cm to receive distance, is spun
The silk time is 2h.
The technical effects of the invention are that：
The methods of the electrospun fibers loaded as the gold nanorods that prepare of the present invention is simple, obtained by tunica fibrosa SERS substrates
Enhancing effect is good, soft and can cut, and can be advantageously used in conventional SERS detections.
Embodiment
A kind of preparation method of the electrospun fibers of gold nanorods load, comprises the following steps：
（1）The preparation of gold nanorods；
（2）The preparation of PVA/PAA electrospinning fibres；
（3）Self assembly of the gold nanorods in fiber surface.
Wherein, the preparation method of described gold nanorods is as described below：It is first that 103 μ L mass fractions are golden for 1% chlorine
Acid solution is added drop-wise in 8mL0.1mol/L CTAB solution, after stirring 2min, adds 0.6mL Fresh
0.01mol/L sodium borohydride solutions, continue to obtain seed solution after stirring 3 min.The solution can be used for growing in 2 ~ 5h
The seed of gold nanorods;Then configuration growth solution, growth solution are configured to sequentially add 47. 5mL 0.1mol/L's
The CTAB aqueous solution, 1.03 mL 1% aqueous solution of chloraurate, 200 μ L silver nitrate aqueous solutions and 400 μ L ascorbic acid
The aqueous solution；Finally, 60 μ L seed solutions are added in growth solution, growth 10h is stood after jog 30s, it is molten to obtain gold nanorods
Liquid.
The preparation method of described PVA/PAA electrospinning fibres is as described below：0.5g PVA powder is weighed, adds 4.5g water,
Stirring 4h obtains PVA solution at room temperature；The 2g 25%PAA aqueous solution then is weighed, is diluted with water to 5g；Finally by both the above
The mass mixings such as solution, continuing stirring 2h makes it well mixed, obtains spinning solution；Gained spinning solution is subjected to electrostatic spinning,
Obtain PVA/PAA electrospun fiber membranes；Tunica fibrosa is then heat-treated 30min in 145 DEG C, makes tunica fibrosa not soluble in water.It is described
The spinning voltage of electrostatic spinning be 15kV, charging rate is 300 μ L/h, and it is 20cm to receive distance, and the spinning time is 2h.
Described gold nanorods are as described below in the process of the self assembly of fiber surface：By the PVA/PAA electricity after heat treatment
Spinning fiber film soaks 3h in deionized water, is adequately ionized the carboxyl in fiber；Then the tunica fibrosa after immersion is immersed in
In gold nanorods solution；Tunica fibrosa is taken out after 12h and with deionized water rinsing 3 times, removing fiber surface solid gold not strong for load
Nanometer rods, drying at room temperature.
Claims (5)
- A kind of 1. preparation method of the electrospun fibers of gold nanorods load, it is characterised in that：Comprise the following steps：（1）The preparation of gold nanorods；（2）The preparation of PVA/PAA electrospinning fibres；（3）Self assembly of the gold nanorods in fiber surface.
- 2. the preparation method of the electrospun fibers of gold nanorods load according to claim 1, it is characterised in that：It is described Gold nanorods preparation method it is as described below：The chlorauric acid solution that 103 μ L mass fractions are 1% is added drop-wise to 8mL first In 0.1mol/L CTAB solution, after stirring 2min, the 0.01mol/L sodium borohydrides of 0.6mL Fresh are added Solution, continue to obtain seed solution after stirring 3 min；The solution can be used for the seed of growth gold nanorods in 2 ~ 5h;With After configure growth solution, the CTAB aqueous solution for being configured to sequentially add 47. 5mL 0.1mol/L of growth solution, 1.03 mL 1% aqueous solution of chloraurate, 200 μ L silver nitrate aqueous solutions and 400 μ L aqueous ascorbic acids；Finally, will 60 μ L seed solutions are added in growth solution, and growth 10h is stood after jog 30s, obtains gold nanorods solution.
- 3. the preparation method of the electrospun fibers of gold nanorods load according to claim 2, it is characterised in that：It is described PVA/PAA electrospinning fibres preparation method it is as described below：0.5g PVA powder is weighed, 4.5g water is added, stirs 4h at room temperature Obtain PVA solution；The 2g 25%PAA aqueous solution then is weighed, is diluted with water to 5g；Finally the quality such as both the above solution are mixed Close, continuing stirring 2h makes it well mixed, obtains spinning solution；Gained spinning solution is subjected to electrostatic spinning, obtains PVA/PAA Electrospun fiber membrane；Tunica fibrosa is then heat-treated 30min in 145 DEG C, makes tunica fibrosa not soluble in water.
- 4. the preparation method of the electrospun fibers of gold nanorods load according to claim 3, it is characterised in that：It is described Gold nanorods it is as described below in the process of the self assembly of fiber surface：PVA/PAA electrospun fiber membranes after heat treatment are soaked 3h in deionized water, it is adequately ionized the carboxyl in fiber；Then the tunica fibrosa after immersion is immersed in gold nanorods solution In；Tunica fibrosa is taken out after 12h and is done with deionized water rinsing 3 times, removing fiber surface solid gold nanorods not strong for load, room temperature It is dry.
- 5. the preparation method of the electrospun fibers of gold nanorods load according to claim 3, it is characterised in that：It is described The spinning voltage of electrostatic spinning be 15kV, charging rate is 300 μ L/h, and it is 20cm to receive distance, and the spinning time is 2h.
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| CN201711166010.2A CN107761366A (en) | 2017-11-21 | 2017-11-21 | The preparation method of the electrospun fibers of gold nanorods load |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110699953A (en) * | 2019-10-10 | 2020-01-17 | 天津工业大学 | Preparation method of nano gold film anti-counterfeiting fabric |
| CN114538440A (en) * | 2022-03-10 | 2022-05-27 | 南京工业大学 | Activated carbon-loaded gold nanorod surface-enhanced Raman detection material and preparation method thereof |
-
2017
- 2017-11-21 CN CN201711166010.2A patent/CN107761366A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110699953A (en) * | 2019-10-10 | 2020-01-17 | 天津工业大学 | Preparation method of nano gold film anti-counterfeiting fabric |
| CN110699953B (en) * | 2019-10-10 | 2022-05-31 | 天津工业大学 | Preparation method of nano gold film anti-counterfeiting fabric |
| CN114538440A (en) * | 2022-03-10 | 2022-05-27 | 南京工业大学 | Activated carbon-loaded gold nanorod surface-enhanced Raman detection material and preparation method thereof |
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Application publication date: 20180306 |