CN105112897A - Preparation method for porous copper-gold composite nanometer film material - Google Patents
Preparation method for porous copper-gold composite nanometer film material Download PDFInfo
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Abstract
The invention discloses a preparation method for a porous copper-gold composite nanometer film material. Under the action of acid, a solid alloy substrate material reacts under temperature control to remove one component, so that a porous solid copper substrate is formed, then a gold nanometer material reacts, and the porous copper-gold composite nanometer film material is formed. By the utilization of the reaction between active metal atoms in the alloy and the acid and the reaction in which inactive metal replaces active metal, the porous copper-gold composite nanometer film material capable of being used for filtration is obtained; design is reasonable; raw materials used in the preparation method are cheap; operation is simple; the reaction is easy to control; repeatability is good; pollution is avoided; safety is good; mass production is facilitated; the obtained porous copper-gold composite nanometer film material is high in content of holes and uniform in hole diameter, and has good permeability. The gold nanometer particles are uniform in size and large in distribution density, and keep a good optical property. The porous copper-gold composite nanometer film material can be used in the fields like surface enhanced Raman spectrums combined with filtration.
Description
Technical field
The present invention relates to the preparation method of a kind of Porous Cu gold composite Nano mould material, belong to technical field of inorganic nano-material preparation.
Background technology
Gold nano-material, due to the optics of its uniqueness and photo-thermal character, has huge application potential in every field such as biology, medical science.But it is expensive, shortage of resources, and also GOLD FROM PLATING SOLUTION aggregates of nanoparticles instability easily precipitates thus causes the poor reproducibility of Raman signal, significantly limit the range of application of aggregates of nanoparticles in solution.And the low price of copper, excellent conductivity, its composite nanometer film has high stability, is widely used in Raman detection field as good propping material.
In order to obtain better character, material should have larger surface-area.From this point, having just becomes one compared with large specific surface and the vesicular structure of not easily assembling character and well selects.Nowadays, porous film material has been widely used in fuel sensitization solar battery, photocatalytic degradation, gas sensor, biosensor and SERS sensor aspect.For solid porous film substrate, active substance by filtering fast enriching and can effectively covering whole substrate surface, therefore, can improve time of response and strength of signal simultaneously.The present invention selects solid copper alloy substrates, reaction removing wherein a kind of component thus form the substrate of porosu solid copper, the upper gold nano-material of reaction forms Porous Cu gold composite Nano mould material again, this Porous Cu gold composite nanometer film stability of material is good, can filter operation, Raman detection field can be applied to.
Summary of the invention
For above-mentioned prior art, the invention provides the preparation method of a kind of Porous Cu gold composite Nano mould material, the Porous Cu prepared by the method gold composite Nano mould material, good stability, can filter operation, Raman detection field can be applied to.
The present invention is achieved by the following technical solutions:
A preparation method for Porous Cu gold composite Nano mould material, step is as follows:
1) by thickness be the disk that the copper alloy solid substrate material slicing machine of 10 ~ 40 microns is cut into diameter 10 ~ 16 millimeters, then supersound washing 30 minutes respectively in ethanol, acetone, water successively.
2) at 25 ~ 80 DEG C, be soak 6 ~ 24 hours in the dilute acid soln of 0.5 ~ 5mol/L in concentration by the copper alloy solid substrate material after above-mentioned section, obtain the substrate of porosu solid copper.
3) by step 2) the porosu solid copper substrate ultrapure water of gained cleans.
4) by step 3) the porosu solid copper substrate of gained to be immersed in 1% ~ 10% (mass percent) aqueous solution of chloraurate 1 minute, and obtain Porous Cu gold composite Nano mould material, with ultrapure water cleaning, and store in ethanol.
Described step 1) in, copper alloy solid substrate material be selected from cupromanganese, copper zinc alloy, cupronickel, copper-iron alloy, gunmetal or Kufil any one, its existence form can be any one in paper tinsel, sheet, net.
Described step 2) in, diluted acid is the one in sulfuric acid, HCl, nitric acid, acetic acid, perchloric acid, phosphoric acid, oxalic acid.
Preferably, described step 2) in, the concentration of dilute acid soln is preferably 3 ~ 5mol/L, and soak time is preferably 6 ~ 12 hours, and the consumption of dilute acid soln is preferably: every sheet disk 20 ~ 50 milliliters of dilute acid solns.
Described step 3) in, the concentration of chlorauric acid solution is preferably 5%.
The hole copper gold composite Nano mould material prepared by aforesaid method, thing, mutually by X-ray diffraction spectra (XRD) test, adopts BrukerD8X-x ray diffractometer x with Cu-K alpha-ray (wavelength
) X light diffracting analysis is done to product for diffraction light sources.The pattern of Porous Cu gold composite Nano mould material is by electron scanning micrograph (SEM) display, and adopt JEOLJSM-7600F cold field emission scanning electronic microscope, acceleration voltage is 3.0kV.
Reaction principle of the present invention is: under the action of an acid, with reaction removing wherein a kind of component under solid alloy base material temperature control, thus form the substrate of porosu solid copper, the upper gold nano-material of reaction again, thus form good stability, can be used for the Porous Cu gold composite Nano mould material that filter operation has very high SERS-Activity.
The present invention utilizes the reaction of reaction between atoms metal active in alloy and acid and torpescence metal replacement active metal, has obtained the Porous Cu gold composite Nano mould material that can be used for filtering.This novel material not only has excellent stability, and has very high SERS-Activity.Compare ordinary solid Raman substrate, this Porous Cu gold composite Nano mould material has the advantage that can be combined with solid phase extraction techniques.
Excellent results of the present invention is as follows:
1, the present invention utilizes the reaction of reaction between atoms metal active in alloy and acid and torpescence metal replacement active metal, has obtained the Porous Cu gold composite Nano mould material with high stability and high Raman reinforced effects that can be used for filtering.
2, the present invention is reasonable in design, raw materials used low price, simple to operate, and easy control of reaction is reproducible, pollution-free, and security is good, is easy to scale operation.
Accompanying drawing explanation
Fig. 1: the X-ray diffraction spectrum (XRD) of Porous Cu gold composite Nano mould material prepared by the present invention.
Fig. 2: the scanning electronic microscope of Porous Cu gold composite Nano mould material prepared by the present invention is according to (SEM).
Fig. 3: the Porous Cu gold composite Nano mould material using the present invention to prepare is the advantageous effect figure (RAMAN) of filtrable Raman substrate.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, but be not limited thereto.
Instrument, reagent, material etc. involved in following embodiment, unless otherwise noted, be existing conventional instrument, reagent, material etc. in prior art, obtain by regular commercial sources.Experimental technique involved in following embodiment, detection method etc., unless otherwise noted, are existing normal experiment method in prior art, detection method etc.
Porous Cu gold composite Nano mould material prepared by following examples, by X-ray diffraction spectrum (XRD) test, adopts BrukerD8X-x ray diffractometer x with Cu-K alpha-ray (wavelength
) X light diffracting analysis is done to product for diffraction light sources.The pattern of product is by electron scanning micrograph (SEM) display, and adopt JEOLJSM-7600F cold field emission scanning electronic microscope, acceleration voltage is 3.0kV.
Embodiment 1 prepares Porous Cu gold composite Nano mould material
Step is as follows:
1) by thickness be the copper zinc alloy sheet (Cu of 10 microns
0.65zn
0.35) be cut into the disk of diameter 10 millimeters with slicing machine, then supersound washing 30 minutes respectively in ethanol, acetone, water successively.
2) at 80 DEG C, be soak 12 hours (every sheet copper zinc alloy sheet dilute acid soln 40 milliliters) in the dilution heat of sulfuric acid of 5mol/L in concentration by the copper zinc alloy sheet of above-mentioned section, obtain the substrate of porosu solid copper.
3) by step 2) the porosu solid copper substrate ultrapure water of gained cleans.
4) by step 3) the porosu solid copper substrate of gained to be immersed in 5% aqueous solution of chloraurate 1 minute, and obtain Porous Cu gold composite Nano mould material, with ultrapure water cleaning, and store in ethanol.
Embodiment 2: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 1) in the thickness of cupromanganese sheet be 20 microns.
Embodiment 3: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 1) in the thickness of cupromanganese sheet be 30 microns.
Embodiment 4: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 1) in the thickness of cupromanganese sheet be 40 microns.
Embodiment 5: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 1) in be cut into the disk of diameter 12 millimeters.
Embodiment 6: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 1) in be cut into the disk of diameter 14 millimeters.
Embodiment 7: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 1) in be cut into the disk of diameter 16 millimeters.
Embodiment 8: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 2) in " at water-bath 80 DEG C " change into " at water-bath 40 DEG C ".
Embodiment 9: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 2) in " at water-bath 80 DEG C " change into " at water-bath 60 DEG C ".
Embodiment 10: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 2) in " at water-bath 80 DEG C " change into " at room temperature ".
Embodiment 11: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 2) in the concentration of dilute sulphuric acid be 0.5mol/L.
Embodiment 12: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 2) in the concentration of dilute sulphuric acid be 1mol/L.
Embodiment 13: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 2) in the concentration of dilute sulphuric acid be 3mol/L.
Embodiment 14: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 2) in soak time be 6 hours.
Embodiment 15: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 2) in soak time be 18 hours.
Embodiment 16: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 2) in soak time be 24 hours.
Embodiment 17: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 2) in " dilution heat of sulfuric acid " replace with " hydrochloric acid ".
Embodiment 18: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 2) in " dilution heat of sulfuric acid " replace with " salpeter solution ".
Embodiment 19: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 2) in " dilution heat of sulfuric acid " replace with " acetum ".
Embodiment 20: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 2) in " dilution heat of sulfuric acid " replace with " perchloric acid solution ".
Embodiment 21: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 2) in " dilution heat of sulfuric acid " replace with " phosphoric acid solution ".
Embodiment 22: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 2) in " dilution heat of sulfuric acid " replace with " oxalic acid solution ".
Embodiment 23: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 2) in every sheet disk dilute acid soln used be 20 milliliters.
Embodiment 24: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 2) in every sheet disk dilute acid soln used be 50 milliliters.
Embodiment 25: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 1) in " copper zinc alloy " replace with " cupromanganese ".
Embodiment 26: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 1) in " copper zinc alloy " replace with " cupronickel ".
Embodiment 27: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 1) in " copper zinc alloy " replace with " copper-iron alloy ".
Embodiment 28: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 1) in " copper zinc alloy " replace with " gunmetal ".
Embodiment 29: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 1) in " copper zinc alloy " replace with " Kufil ".
Embodiment 30: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 1) in " copper zinc alloy sheet " replace with " clutch gold ".
Embodiment 31: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 1) in " copper zinc alloy sheet " replace with " copper zinc alloy net ".
Embodiment 32: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 4) in the concentration of hydrochloro-auric acid be 1%.
Embodiment 33: the method preparing Porous Cu gold composite Nano mould material, step is with example 1, and difference is step 4) in the concentration of hydrochloro-auric acid be 10%.
Its X-ray diffraction spectrum (XRD) as shown in Figure 1, scanning electronic microscope according to (SEM) as shown in Figure 2, Raman reinforced effects (RAMAN) as shown in Figure 3, many, the uniform pore diameter of Porous Cu gold composite nanometer film material hole content, has good perviousness as seen from the figure.Size of nanometer gold grain is even, and distribution density is large, has very high SERS-Activity.Compared with the Raman signal of the mercaptoaniline after this Porous Cu gold composite nanometer film filtration of material of use is soaked the signal after same time with use copper metal/composite material, filtration method signal is stronger.
Claims (7)
1. a preparation method for Porous Cu gold composite Nano mould material, is characterized in that: step is as follows:
1) by thickness be the disk that the copper alloy solid substrate material of 10 ~ 40 microns is cut into diameter 10 ~ 16 millimeters, then supersound washing 30 minutes respectively in ethanol, acetone, water successively;
2) at 25 ~ 80 DEG C, be soak 1 ~ 24 hour in the dilute acid soln of 0.025 ~ 5mol/L in concentration by the copper alloy solid substrate material after above-mentioned section, obtain the substrate of porosu solid copper;
3) by step 2) the porosu solid copper substrate ultrapure water of gained cleans;
4) by step 3) the porosu solid copper substrate of gained to be immersed in 1% ~ 10% aqueous solution of chloraurate 1 minute, obtains Porous Cu gold composite Nano mould material.
2. the preparation method of Porous Cu gold composite Nano mould material according to claim 1, it is characterized in that: described step 1) in, copper alloy solid substrate material be selected from cupromanganese, copper zinc alloy, cupronickel, copper-iron alloy, gunmetal or Kufil any one, its existence form is any one in paper tinsel, sheet, net.
3. the preparation method of Porous Cu gold composite Nano mould material according to claim 1, is characterized in that: described step 2) in, diluted acid is the one in sulfuric acid, HCl, nitric acid, acetic acid, perchloric acid, phosphoric acid, oxalic acid.
4. the preparation method of the Porous Cu gold composite Nano mould material according to claim 1 or 3, it is characterized in that: described step 2) in, the concentration of dilute acid soln is 3 ~ 5mol/L, soak time is 6 ~ 12 hours, and the consumption of dilute acid soln is: every sheet disk 20 ~ 50 milliliters of dilute acid solns.
5. the preparation method of Porous Cu gold composite Nano mould material according to claim 1, is characterized in that: described step 3) in, the concentration of chlorauric acid solution is 5%.
6. utilize the Porous Cu gold composite Nano mould material that the preparation method of the gold of the Porous Cu according to any one of claim 1 ~ 5 composite Nano mould material prepares.
7. Porous Cu gold composite Nano mould material according to claim 6 is as the application of propping material in Raman detection.
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CN105734335A (en) * | 2016-03-15 | 2016-07-06 | 济南大学 | Copper-based nano porous film and preparation method thereof |
CN105928924A (en) * | 2016-04-25 | 2016-09-07 | 上海交通大学 | Preparation method for SERS substrate of gold-silver composite nanometer particles |
CN106521501A (en) * | 2016-12-05 | 2017-03-22 | 河北工业大学 | Brass alloy with macro-hole, micron-hole and nano-hole hierarchical hole structure and application thereof |
CN106731885A (en) * | 2016-12-19 | 2017-05-31 | 中国科学院宁波材料技术与工程研究所 | A kind of metal organic framework/metal nano ion composite filtering film and its preparation method and application |
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CN110029383A (en) * | 2019-03-15 | 2019-07-19 | 浙江工贸职业技术学院 | A kind of degradable zinc-copper foam biological material |
CN114657626A (en) * | 2022-03-30 | 2022-06-24 | 昆明理工大学 | Preparation method of nano porous copper |
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Cited By (11)
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CN105734335A (en) * | 2016-03-15 | 2016-07-06 | 济南大学 | Copper-based nano porous film and preparation method thereof |
CN105734335B (en) * | 2016-03-15 | 2018-01-30 | 济南大学 | A kind of copper-based nano porous membrane and preparation method thereof |
CN105928924A (en) * | 2016-04-25 | 2016-09-07 | 上海交通大学 | Preparation method for SERS substrate of gold-silver composite nanometer particles |
CN105928924B (en) * | 2016-04-25 | 2019-08-23 | 上海交通大学 | A kind of preparation method of gold and silver composite nanometer particle SERS substrate |
CN106521501A (en) * | 2016-12-05 | 2017-03-22 | 河北工业大学 | Brass alloy with macro-hole, micron-hole and nano-hole hierarchical hole structure and application thereof |
CN106731885A (en) * | 2016-12-19 | 2017-05-31 | 中国科学院宁波材料技术与工程研究所 | A kind of metal organic framework/metal nano ion composite filtering film and its preparation method and application |
CN107099787A (en) * | 2017-05-18 | 2017-08-29 | 江西师范大学 | A kind of surface enhanced Raman scattering substrate and preparation method thereof |
CN107099787B (en) * | 2017-05-18 | 2019-12-13 | 江西师范大学 | Surface-enhanced Raman scattering substrate and preparation method thereof |
CN110029383A (en) * | 2019-03-15 | 2019-07-19 | 浙江工贸职业技术学院 | A kind of degradable zinc-copper foam biological material |
CN110029383B (en) * | 2019-03-15 | 2020-08-18 | 浙江工贸职业技术学院 | Degradable zinc-copper foam biological material |
CN114657626A (en) * | 2022-03-30 | 2022-06-24 | 昆明理工大学 | Preparation method of nano porous copper |
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