CN104233511A - Method for preparing gold-silver alloy fiber by coaxially electrostatic spinning - Google Patents
Method for preparing gold-silver alloy fiber by coaxially electrostatic spinning Download PDFInfo
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- CN104233511A CN104233511A CN201410546060.3A CN201410546060A CN104233511A CN 104233511 A CN104233511 A CN 104233511A CN 201410546060 A CN201410546060 A CN 201410546060A CN 104233511 A CN104233511 A CN 104233511A
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Abstract
The invention discloses a method for preparing gold-silver alloy nanofiber by coaxially electrostatic spinning, relates to the preparation method of metal nanofiber, and overcomes the problem that metallics in the gold-silver alloy nanofiber prepared by using the existing method are not enough close in arrangement. The preparation method comprises the steps of: 1, dissolving polyvinyl alcohol in solvent to prepare shell layer spinning solution; 2, dissolving spinning solution in solvent, then adding chloroauric acid, heating to boil, then adding reductant, dialyzing after distilling for concentration, and thereby obtaining nuclear layer spinning solution; 3, adopting the polyvinyl alcohol solution as outer shaft solution and the gold-silver alloy nano particle solution as inner shaft solution, and adjusting spinning parameters to perform coaxially electrostatic spinning; 4, placing nuclear nanofiber in a muffle furnace to perform heating and annealing process, and thereby completing preparation of the gold-silver alloy nanofiber. The gold-silver alloy nanofiber prepared by the method provided by the invention is smooth in surface, and the gold-silver alloy nano particles are closely arranged.
Description
Technical field
The present invention relates to a kind of preparation method of alloy fiber, be specifically related to the method utilizing coaxial electrostatic spinning legal system for electrum fiber.
Background technology
Nearly ten years, one-dimensional nano structure material is as alloy nano fiber, nanotube, nanobelt, nano wire and nano-cable etc., they due to show in electricity, light, magnetic etc. the novel feature that is different from corresponding body material and other form nanometer material structure and they basic research and high-technology field application aspect important value and receive much concern, in the nano structure devices such as following Novel electric, magnetic, occupy important strategic status.
At present, what utilize electrostatic spinning to prepare has copper nano-wire, cobalt nanowire and SiC/C nano fibrous membrane etc., existing method such as template assisting growth solvent-thermal process and melt spinning and dry spinning etc. are used for design and synthesizing magnetic nano structural material by development, but there is complex process in these preparation methods, or the nanofiber of preparation is short, metallic arranges the shortcomings such as defective tightness, thus causes the reduction of nanofiber electric conductivity.Coaxial electrostatic spinning be utilize high polymeric solution or melt for shell layer spinning solution and alloy nano particle solution be sandwich layer spinning solution, its principle is in electrospinning process, shell viscosity solution drives sandwich layer solution to form coaxial jet by forming " frictional shearing " to sandwich layer solution in high voltage electric field, this coaxial jet flow deformation in high-voltage electrostatic field, solidify through solvent evaporates cooling or melt cooling, thus obtain a kind of method of core-shell nano fiber.
Summary of the invention
The present invention seeks to the problem in order to solve metallic arrangement defective tightness in metallic alloy fiber that existing method prepares, and provide a kind of coaxial electrostatic spinning to prepare the method for electrum fiber.
The method that coaxial electrostatic spinning of the present invention prepares electrum fiber follows these steps to realize:
One, polyvinyl alcohol is dissolved in solvent a, is heated to 50 ~ 100 DEG C, be stirred to dissolving and obtain shell layer spinning solution;
Two, the silver nitrate of 0.0037g ~ 0.0222g is dissolved in the solvent b of 10 ~ 60mL, the chlorauric acid solution that 2 ~ 6mL mass concentration is 1% is added after abundant dissolving, add solvent b after stirring again and reactant liquor is diluted to 90 ~ 540mL, reactant liquor is placed in reaction vessel and is heated to seethe with excitement at oil bath pan and keeps 2 ~ 10min, then the reductant that 10 ~ 100mL mass concentration is 1% is added, continue to maintain boiling 30 ~ 50min, adding 5 ~ 20ml mass concentration is again distillation and concentration to 10 ~ 50mL after 5% ~ 10%PVA solution, concentrate bag filter dialysis 22 ~ 26h, repeatedly change water 3 ~ 4 times, obtain stratum nucleare spinning solution,
Three, the shell layer spinning solution that step one obtains is placed in the outer tube of coaxial electrostatic spinning silk device, stratum nucleare spinning solution step 2 obtained is placed in pipe in coaxial electrostatic spinning silk device, adjustment spinning voltage is 13 ~ 25kv, relative humidity is 10% ~ 30%, indoor temperature is 15 ~ 25 DEG C, receiving range is 10 ~ 25cm, and stratum nucleare spinning solution is (1 ~ 0.1) with the ratio of shell layer spinning solution fltting speed: 1 carries out coaxial electrostatic spinning, obtains electrum-PVA core-shell nano fiber;
Four, electrum-PVA core-shell nano fiber step 3 obtained is placed in Muffle furnace, is warming up to 300 DEG C and is incubated 6 ~ 7h, then continuing to be warming up to 400 ~ 600 DEG C, naturally cools to room temperature, obtain electrum nanofiber after insulation 1 ~ 2h with body of heater.
The present invention utilizes coaxial electrostatic spinning method to prepare electrum-PVA nuclear fibre, the stratum nucleare of electrum-PVA core-shell nano fiber is gold-silver alloy nanoparticles solution, shell is PVA solution, and core-shell nano fiber obtains single shaft electrum fiber after roasting.The single favorable dispersibility of electrum fiber that the present invention prepares, gold-silver alloy nanoparticles is close-packed arrays in stratum nucleare, and in electrum fiber, the content of gold is higher.This electrum fiber is mainly used in wire device, filters barrier material etc.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the gold-silver alloy nanoparticles that embodiment one step 2 obtains;
Fig. 2 is the TEM figure of the electrum-PVA nuclear fibre that embodiment one step 3 obtains;
Fig. 3 is the SEM figure of the electrum-PVA nuclear fibre that embodiment one step 3 obtains;
Fig. 4 is the ultraviolet absorption curve figure of the electrum fiber that embodiment one step 4 obtains;
Fig. 5 is the XRD spectra of the electrum fiber that embodiment one step 4 obtains;
Fig. 6 is the Ag3d energy spectrogram of the electrum fiber XPS that embodiment one step 4 obtains;
Fig. 7 is the Au4f energy spectrogram of the electrum fiber XPS that embodiment one step 4 obtains;
Fig. 8 is the Raman spectrum of the electrum fiber that embodiment one prepares;
Fig. 9 is the scanning electron microscope (SEM) photograph of the electrum fiber that embodiment one prepares.
Detailed description of the invention
Detailed description of the invention one: the method that present embodiment coaxial electrostatic spinning prepares electrum fiber follows these steps to implement:
One, polyvinyl alcohol is dissolved in solvent a, is heated to 50 ~ 100 DEG C, be stirred to dissolving and obtain shell layer spinning solution;
Two, the silver nitrate of 0.0037g ~ 0.0222g is dissolved in the solvent b of 10 ~ 60mL, the chlorauric acid solution that 2 ~ 6mL mass concentration is 1% is added after abundant dissolving, add solvent b after stirring again and reactant liquor is diluted to 90 ~ 540mL, reactant liquor is placed in reaction vessel and is heated to seethe with excitement at oil bath pan and keeps 2 ~ 10min, then the reductant that 10 ~ 100mL mass concentration is 1% is added, continue to maintain boiling 30 ~ 50min, adding 5 ~ 20ml mass concentration is again distillation and concentration to 10 ~ 50mL after 5% ~ 10%PVA solution, concentrate bag filter dialysis 22 ~ 26h, repeatedly change water 3 ~ 4 times, obtain stratum nucleare spinning solution,
Three, the shell layer spinning solution that step one obtains is placed in the outer tube of coaxial electrostatic spinning silk device, stratum nucleare spinning solution step 2 obtained is placed in pipe in coaxial electrostatic spinning silk device, adjustment spinning voltage is 13 ~ 25kv, relative humidity is 10% ~ 30%, indoor temperature is 15 ~ 25 DEG C, receiving range is 10 ~ 25cm, and stratum nucleare spinning solution is (1 ~ 0.1) with the ratio of shell layer spinning solution fltting speed: 1 carries out coaxial electrostatic spinning, obtains electrum-PVA nuclear fibre;
Four, electrum-PVA nuclear fibre step 3 obtained is placed in Muffle furnace, is warming up to 300 DEG C and is incubated 6 ~ 7h, then continues to be warming up to 400 ~ 600 DEG C, naturally cools to room temperature, obtain electrum fiber after insulation 1 ~ 2h with body of heater.
When present embodiment utilizes coaxial electrostatic spinning to prepare nuclear fibre, the velocity ratio of the composition of the kind of raw material, the molecular weight of chelating polymer template level, stratum nucleare and sandwich layer spinning solution, stratum nucleare and sandwich layer spinning solution, spinning process parameter and Technology for Heating Processing have material impact to the pattern of final products and size.Present embodiment adopts coaxial electrostatic spinning method, with the mixed liquor of polyvinyl alcohol and deionized water for shell solution, with the mixed liquor of gold-silver alloy nanoparticles, polyvinyl alcohol and deionized water for sandwich layer solution, control the viscosity of shell and sandwich layer solution, control the velocity ratio of stratum nucleare and sandwich layer spinning solution, spinning process parameter under the spinning condition of optimum, prepare electrum-PVA nuclear fibre, then after high-temperature process, obtain electrum fiber.
Detailed description of the invention two: present embodiment and detailed description of the invention one are deionized water, dimethyl sulfoxide (DMSO) or DMF unlike the solvent a described in step one.Other step and parameter identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment and detailed description of the invention one or two are 5% ~ 10% unlike the mass percent of polyvinyl alcohol in step one shell layer spinning solution.Other step and parameter identical with detailed description of the invention one or two.
Present embodiment controls the concentration of shell layer spinning solution, and when avoiding shell solution concentration too low, shell viscosity solution passes through too low to stratum nucleare solution formation " frictional shearing " and stratum nucleare solution cannot be driven to form coaxial jet in high voltage electric field.When avoiding shell solution concentration too high, shell solution viscosity is high, and in high voltage electric field, enhanced stretch resistance increases and is difficult to form stable coaxial jet with stratum nucleare solution.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three are deionized water, dimethyl sulfoxide (DMSO) or DMF unlike the solvent b described in step 2.Other step and parameter identical with one of detailed description of the invention one to three.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to four are natrium citricum, sodium borohydride, hydrazine hydrate or formic acid unlike the reductant described in step 2.Other step and parameter identical with one of detailed description of the invention one to four.
Detailed description of the invention six: one of present embodiment and detailed description of the invention one to five are 0.1 ~ 5mL/h unlike the fltting speed of stratum nucleare spinning solution in step 3, the fltting speed of shell layer spinning solution is 2 ~ 10mL/h.Other step and parameter identical with one of detailed description of the invention one to five.
Detailed description of the invention seven: one of present embodiment and detailed description of the invention one to six are incubated 6 ~ 7h unlike step 4 with the ramp to 300 of 1 ~ 6 DEG C/min DEG C, then with the ramp to 400 DEG C of 1 ~ 2 DEG C/min, after insulation 1 ~ 2h, room temperature is naturally cooled to body of heater.Other step and parameter identical with one of detailed description of the invention one to six.
Embodiment one: the method that the present embodiment coaxial electrostatic spinning prepares electrum fiber follows these steps to implement:
One, 1.2022g polyvinyl alcohol (PVA, n=1750 ± 50) is dissolved in 10.8198ml deionized water, is heated to 90 DEG C and is stirred to dissolving, obtain shell layer spinning solution;
Two, the silver nitrate of 0.0222g is dissolved in the deionized water of 60mL, the chlorauric acid solution that 6mL mass concentration is 1% is added after abundant dissolving, add deionized water after stirring again and reactant liquor is diluted to 540mL, reactant liquor is placed in reaction vessel and is heated to seethe with excitement at oil bath pan and keeps 5min, then the natrium citricum that 60mL mass concentration is 1% is added, continue to maintain boiling 30min, add 0.411g mass concentration be after 5%PVA solution distillation and concentration to 30mL, concentrate bag filter is dialysed 24h, repeatedly change water 3 times, obtain stratum nucleare spinning solution;
Three, the shell layer spinning solution that step one obtains is placed in the outer tube of coaxial electrostatic spinning silk device, stratum nucleare spinning solution step 2 obtained is placed in pipe in coaxial electrostatic spinning silk device, adjustment spinning voltage is 18kv, relative humidity is 30%, indoor temperature is 20 DEG C, and receiving range is 18cm, and stratum nucleare spinning solution fltting speed is 2.5mL/h, shell layer spinning solution fltting speed is that 7.5mL/h carries out coaxial electrostatic spinning, obtains electrum-PVA nuclear fibre;
Four, nuclear fibre is placed in Muffle furnace, is incubated 7h with the ramp to 300 of 4 DEG C/min DEG C, then with the ramp to 400 DEG C of 1.5 DEG C/min, naturally cools to room temperature with body of heater after insulation 1h, obtain electrum fiber.
The average diameter of the electrum fiber that the present embodiment obtains is 50 ~ 100nm.
Gold and silver nano particle diameter is more homogeneous as can be seen from Figure 1, and agglomeration is few.Scheme known gold-silver alloy nanoparticles in stratum nucleare arrangement closely by the TEM of Fig. 2 electrum-PVA nuclear fibre, the SEM figure of Fig. 3 shows the continuous fibers structure that fiber morphology keeps good, and single good dispersion, has larger specific area.
The ultraviolet absorption curve figure of the electrum fiber of preparation as shown in Figure 4, can find out in electrum fiber along with the increase that the content of gold increases, the ultraviolet absorption peak of electrum fiber moves to long wave direction, can judge that products therefrom is gold-silver alloy nanoparticles, instead of the mixture of golden nanometer particle and Nano silver grain.Fig. 5 is XRD spectra, 2 θ=38.2 ° in figure, 44.2 °, 64.4 ° and 77.5 °, corresponding (111), (200), (220) and (311), further demonstrate that the fiber of synthesis is electrum fiber respectively; X-ray photoelectron spectroscopy analysis is carried out to obtained electrum fiber, electrum fiber XPS schemes as shown in Figure 6, Fig. 6 is the energy spectrogram of Ag3d, can find out that from figure two peaks of silver element appear on the position of 368eV and 374eV, judge that silver is reduced and is present in electrum fiber by consulting XPS handbook, and exist with stable element form; What Fig. 7 represented is Au4f's can spectrogram, two peaks are respectively on the position of 84eV and 88eV as we can see from the figure, can be defined as gold according to XPS handbook, can infer containing gold in electrum fiber, this just means that gold is completely reduced and exists with stable form.Fig. 8 is the SERS of electrum fiber (1) and PVA-alloy composite fibre (2), can see that electrum fiber Raman phenomenon is obviously enhanced.
Claims (7)
1. coaxial electrostatic spinning prepares a method for electrum nanofiber, it is characterized in that following these steps to realize:
One, polyvinyl alcohol is dissolved in solvent a, is heated to 50 ~ 100 DEG C, be stirred to dissolving and obtain shell layer spinning solution;
Two, the silver nitrate of 0.0037g ~ 0.0222g is dissolved in the solvent b of 10 ~ 60mL, the chlorauric acid solution that 2 ~ 6mL mass concentration is 1% is added after abundant dissolving, add solvent b after stirring again and reactant liquor is diluted to 90 ~ 540mL, reactant liquor is placed in reaction vessel and is heated to seethe with excitement at oil bath pan and keeps 2 ~ 10min, then the reductant that 10 ~ 100mL mass concentration is 1% is added, continue to maintain boiling 30 ~ 50min, adding 5 ~ 20ml mass concentration is again distillation and concentration to 10 ~ 50mL after 5% ~ 10%PVA solution, concentrate bag filter dialysis 22 ~ 26h, repeatedly change water 3 ~ 4 times, obtain stratum nucleare spinning solution,
Three, the shell layer spinning solution that step one obtains is placed in the outer tube of coaxial electrostatic spinning silk device, stratum nucleare spinning solution step 2 obtained is placed in pipe in coaxial electrostatic spinning silk device, adjustment spinning voltage is 13 ~ 25kv, relative humidity is 10% ~ 30%, indoor temperature is 15 ~ 25 DEG C, receiving range is 10 ~ 25cm, and stratum nucleare spinning solution is (1 ~ 0.1) with the ratio of shell layer spinning solution fltting speed: 1 carries out coaxial electrostatic spinning, obtains electrum-PVA core-shell nano fiber;
Four, electrum-PVA core-shell nano fiber step 3 obtained is placed in Muffle furnace, is warming up to 300 DEG C and is incubated 6 ~ 7h, then continuing to be warming up to 400 ~ 600 DEG C, naturally cools to room temperature, obtain electrum nanofiber after insulation 1 ~ 2h with body of heater.
2. a kind of coaxial electrostatic spinning according to claim 1 prepares the method for electrum nanofiber, it is characterized in that the solvent a described in step one is deionized water, dimethyl sulfoxide (DMSO) or DMF.
3. a kind of coaxial electrostatic spinning according to claim 1 prepares the method for electrum nanofiber, it is characterized in that the mass percent of polyvinyl alcohol in step one shell layer spinning solution is 5% ~ 10%.
4. a kind of coaxial electrostatic spinning according to claim 1 prepares the method for electrum nanofiber, it is characterized in that the solvent b described in step 2 is deionized water, dimethyl sulfoxide (DMSO) or DMF.
5. a kind of coaxial electrostatic spinning according to claim 1 prepares the method for electrum nanofiber, it is characterized in that the reductant described in step 2 is natrium citricum, sodium borohydride, hydrazine hydrate or formic acid.
6. a kind of coaxial electrostatic spinning according to claim 1 prepares the method for electrum nanofiber, it is characterized in that the fltting speed of stratum nucleare spinning solution in step 3 is 0.1 ~ 5mL/h, and the fltting speed of shell layer spinning solution is 2 ~ 10mL/h.
7. a kind of coaxial electrostatic spinning according to claim 1 prepares the method for electrum nanofiber, it is characterized in that step 4 is incubated 6 ~ 7h with the ramp to 300 of 1 ~ 6 DEG C/min DEG C, then with the ramp to 400 DEG C of 1 ~ 2 DEG C/min, after insulation 1 ~ 2h, room temperature is naturally cooled to body of heater.
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