CN102877094A - Ordered hole array with gold-nanoparticle-based micro-nanometer composite structure and preparation method for ordered hole array - Google Patents
Ordered hole array with gold-nanoparticle-based micro-nanometer composite structure and preparation method for ordered hole array Download PDFInfo
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Abstract
The invention discloses an ordered hole array with a gold-nanoparticle-based micro-nanometer composite structure and a preparation method for the ordered hole array. According to the array, gold particles which form a wall of the ordered hole array are accumulated on a conducting substrate, the spacing of ordered holes is 0.1 to 30mu m, the particle size of each gold particle is 10 to 100nm, and 1 to 300 layers of gold particles are accumulated. The method comprises the following steps of: putting a single-layer colloidal crystal template on the conducting substrate; putting the conducting substrate into a gold electrolyte and electrodepositing to obtain a complex array; dissolving polystyrene colloidal spheres in the complex array to obtain a gold body array; and putting the gold body array into a potassium chloride solution for electrochemical oxidation-reduction circulation treatment, wherein the process of the electrochemical oxidation-reduction circulation treatment is that: the voltage begins from -0.3V, linearly rises to 1.2V at the rate of 1V/s, remains for 1.2s, and linearly drops to -0.3V at the rate of 0.5V/s, and the operation is circulated for 5 to 35 times to obtain a target product. The target product can be widely used for catalysis, electrochemistry and surface-enhanced Raman scattering active substrates.
Description
Technical field
The present invention relates to a kind of little-nano compound structure orderly hole array and preparation method, especially a kind of gold nano grain base is little-the orderly hole of nano compound structure array and preparation method thereof.
Background technology
The orderly hole of gold nano array has important using value in fields such as catalysis, electrochemistry and surface-enhanced Raman scattering activity substrates.Little-nano compound structure is the another kind of material structure system that causes extensive concern, it has advantages of micrometer structure and nano structural material simultaneously, coupling effect is strong, surfactivity is high, Stability Analysis of Structures, have important using value, can be widely used in high reactivity, high stability and repeatable device.Based on above factor, people are for obtaining golden micro-nano structure material, made unremitting effort, as at date of publication being a kind of " two-dimensional and double-cycle ordered structure array and preparation method thereof " of mentioning among the applicant's a Chinese invention patent application file CN 101891141A on November 24th, 2010.This two-dimensional and double-cycle ordered structure array contains a series of ordered porous thin-films that are made of the poroid and poroid metallic gold of nanometer of microparticle that place on the conductive substrates, and the pattern of one of them is that nanoporous is arranged in the microparticle hole, and is heaped-up; Its preparation method is template for adopting polystyrene colloid monolayer and aluminum oxide, uses electrodip process in conductive substrates, has obtained final product---the nanoporous that is heaped-up is arranged in the two-dimensional and double-cycle ordered structure array in microparticle hole.But, no matter be array, or its preparation method, all exist the shortcoming part, at first, final product is only for being equipped with the gold nano hole of heaped-up in the microparticle hole, and form two-dimensional and double-cycle ordered structure array with this, though it has possessed little-nano compound structure had both had the not good enough problem of microstructure hole array stability, be faced with again active not enough difficult problem when it is used as surface enhanced Raman scattering substrate; Secondly, the preparation method can not make stable, the active high final product of microstructure hole array.
Summary of the invention
The technical problem to be solved in the present invention is for overcoming shortcoming part of the prior art, provide a kind of good stability, active high gold nano grain base little-the orderly hole of nano compound structure array.
Another technical problem that the present invention will solve for provide a kind of above-mentioned gold nano grain base little-preparation method of the orderly hole of nano compound structure array.
For solving technical problem of the present invention, the technical scheme that adopts is: and the gold nano grain base is little-and the orderly hole of nano compound structure array comprises conductive substrates, particularly,
Piling up on the described conductive substrates has the gold grain that consists of orderly hole array wall;
The pitch of holes in described orderly hole is 0.1～30 μ m;
The particle diameter of described gold grain is 10～100nm, and the number of plies of its accumulation is 1～300 layer.
As the gold nano grain base little-the further improvement of the orderly hole of nano compound structure array, described conductive substrates is conductive glass, or conductive rubber, or tinsel; Described orderly hole array is orderly Hexagonal array.
For solving another technical problem of the present invention, another technical scheme that adopts is: and above-mentioned gold nano grain base is little-and the preparation method of the orderly hole of nano compound structure array comprises electrodip process, and particularly completing steps is as follows:
Step 1, to be that the colloid monolayer crystal template that the polystyrene colloid ball of 0.1～30 μ m forms places on the conductive substrates by spherical diameter first, again the conductive substrates that is equipped with colloid monolayer crystal template on it being placed golden electrolytic solution, take it as working electrode, is 0.1～5mA/cm in current density
2Lower employing three-electrode method galvanic deposit 5～60min obtains the complex body array;
Step 2; first the complex body array is placed dichloromethane solvent to remove the polystyrene colloid ball; obtain golden volume array; place Klorvess Liquid to carry out electrochemical oxidation-reduction circular treatment golden volume array again; wherein; the process of electrochemical oxidation-reduction circular treatment is; voltage begins from-0.3V; to stop 1.2s behind the linear 1.2V of rising to of the speed of 1V/s; drop to-0.3V so that the speed of 0.5V/s is linear more subsequently; so move in circles 5～35 times, make the gold nano grain base little-the orderly hole of nano compound structure array.
As the gold nano grain base little-preparation method's of the orderly hole of nano compound structure array further improvement, described conductive substrates is conductive glass, or conductive rubber, or tinsel; Described golden electrolytic solution is that the hydrochloro-auric acid of 12g/L, the disodium ethylene diamine tetraacetate of 5g/L, the S-WAT of 160g/L and the dipotassium hydrogen phosphate of 30g/L mix mutually by concentration; During described galvanic deposit is Graphite Electrodes to electrode, and reference electrode is saturated calomel electrode; The concentration of described Klorvess Liquid is 0.05～0.5mol/L.
Beneficial effect with respect to prior art is, one uses respectively scanning electron microscope and X-ray diffractometer to characterize to the target product that makes, and by its result as can be known, target product is to pile up on the substrate granular substance that consists of orderly hole array wall is arranged; Wherein, the pitch of holes in hole is 0.1～30 μ m in order, and the particle diameter of granular substance is 10～100nm, and the number of plies of its accumulation is 1～300 layer.The hole array is orderly Hexagonal array in order.Substrate is conductive substrates, and granular substance is gold grain.Its two, target product had both possessed micro-nano structure, had strengthened widely again the stability of microstructure hole array, a large amount of gaps because existing between the gold nano grain also, and greatly increased activity when it is used as surface enhanced Raman scattering substrate; In addition, target product little-Na complex effect also will make its performance that has structural reinforcing at catalysis and electrochemistry microelectrode, can give full play to the double effects of portal array structure and little-nano compound structure.Its three, the preparation method is few, pollution-free except materials, belong to green synthesis techniques, and production efficiency is high, is suitable for outside the large-scale industrial production, also has universality, can promote for the synthesis of other material little-nano compound structure hole array.
As the further embodiment of beneficial effect, the one, conductive substrates is preferably conductive glass, or conductive rubber, or tinsel, not only makes conductive substrates that larger choice is arranged, and preparation technology is more easily implemented and flexibly; The 2nd, orderly hole array is preferably orderly Hexagonal array, is convenient to make the array in the target product more uniform; The 3rd, golden electrolytic solution is that the hydrochloro-auric acid of 12g/L, the disodium ethylene diamine tetraacetate of 5g/L, the S-WAT of 160g/L and the dipotassium hydrogen phosphate of 30g/L mix mutually by concentration preferably, except laying a good foundation for making target product, also makes galvanic deposit easy to implement; The 4th, during galvanic deposit electrode is preferably Graphite Electrodes, reference electrode is preferably saturated calomel electrode, is convenient to effective implementation of galvanic deposit; The 5th, the concentration of Klorvess Liquid is preferably 0.05～0.5mol/L, is beneficial to the fine quality of guaranteeing target product.
Description of drawings
Below in conjunction with accompanying drawing optimal way of the present invention is described in further detail.
Fig. 1 is the route schematic diagram of preparation target product of the present invention.Figure 1A is the colloid monolayer crystal template that is comprised of the polystyrene colloid ball that places on the conductive substrates; Figure 1B is the complex body array through obtaining behind the electrochemical deposition; Fig. 1 C is for removing the golden volume array that obtains behind the polystyrene colloid ball; Fig. 1 D is through after electrochemical oxidation-reduction circular treatment, the target product that makes.
Fig. 2 uses one of result that field emission scanning electron microscope (SEM) characterizes to the target product that makes.Can be found out by the SEM photo, be equipped with micron-sized orderly hole array on the substrate, the hole wall that consists of the orderly hole of this orderly hole array is formed by nano level particle packing.
Embodiment
At first buy from market or make with ordinary method:
Spherical diameter is the colloid monolayer crystal template that the polystyrene colloid ball of 0.1～30 μ m forms;
Conductive glass, conductive rubber and tinsel as conductive substrates;
Be the golden electrolytic solution that the dipotassium hydrogen phosphate of the S-WAT of disodium ethylene diamine tetraacetate, 160g/L of hydrochloro-auric acid, the 5g/L of 12g/L and 30g/L mixes mutually by concentration;
Concentration is the Klorvess Liquid of 0.05～0.5mol/L.
Then,
Embodiment 1
The concrete steps of preparation are:
Step 1 will be that the colloid monolayer crystal template that the polystyrene colloid ball of 0.3 μ m forms places on the conductive substrates by spherical diameter first; Wherein, conductive substrates is conductive glass.Again the conductive substrates that is equipped with colloid monolayer crystal template on it being placed golden electrolytic solution, take it as working electrode, is 0.1mA/cm in current density
2Lower employing three-electrode method galvanic deposit 60min; Wherein, during galvanic deposit is Graphite Electrodes to electrode, and reference electrode is saturated calomel electrode, obtains the complex body array.
Step 2 places the complex body array first dichloromethane solvent to remove the polystyrene colloid ball, obtains golden volume array.Golden volume array being placed concentration is that the Klorvess Liquid of 0.05mol/L carries out electrochemical oxidation-reduction circular treatment again; wherein; the process of electrochemical oxidation-reduction circular treatment is; voltage begins from-0.3V; to stop 1.2s behind the linear 1.2V of rising to of the speed of 1V/s; drop to-0.3V so that the speed of 0.5V/s is linear more subsequently, so move in circles 35 times, make be similar to gold nano grain base shown in Figure 2 little-the orderly hole of nano compound structure array.
Embodiment 2
The concrete steps of preparation are:
Step 1 will be that the colloid monolayer crystal template that the polystyrene colloid ball of 0.3 μ m forms places on the conductive substrates by spherical diameter first; Wherein, conductive substrates is conductive glass.Again the conductive substrates that is equipped with colloid monolayer crystal template on it being placed golden electrolytic solution, take it as working electrode, is 0.5mA/cm in current density
2Lower employing three-electrode method galvanic deposit 45min; Wherein, during galvanic deposit is Graphite Electrodes to electrode, and reference electrode is saturated calomel electrode, obtains the complex body array.
Step 2 places the complex body array first dichloromethane solvent to remove the polystyrene colloid ball, obtains golden volume array.Golden volume array being placed concentration is that the Klorvess Liquid of 0.1mol/L carries out electrochemical oxidation-reduction circular treatment again; wherein; the process of electrochemical oxidation-reduction circular treatment is; voltage begins from-0.3V; to stop 1.2s behind the linear 1.2V of rising to of the speed of 1V/s; drop to-0.3V so that the speed of 0.5V/s is linear more subsequently, so move in circles 28 times, make be similar to gold nano grain base shown in Figure 2 little-the orderly hole of nano compound structure array.
Embodiment 3
The concrete steps of preparation are:
Step 1 will be that the colloid monolayer crystal template that the polystyrene colloid ball of 0.3 μ m forms places on the conductive substrates by spherical diameter first; Wherein, conductive substrates is conductive glass.Again the conductive substrates that is equipped with colloid monolayer crystal template on it being placed golden electrolytic solution, take it as working electrode, is 1mA/cm in current density
2Lower employing three-electrode method galvanic deposit 30min; Wherein, during galvanic deposit is Graphite Electrodes to electrode, and reference electrode is saturated calomel electrode, obtains the complex body array.
Step 2 places the complex body array first dichloromethane solvent to remove the polystyrene colloid ball, obtains golden volume array.Golden volume array being placed concentration is that the Klorvess Liquid of 0.15mol/L carries out electrochemical oxidation-reduction circular treatment again; wherein; the process of electrochemical oxidation-reduction circular treatment is; voltage begins from-0.3V; to stop 1.2s behind the linear 1.2V of rising to of the speed of 1V/s; drop to-0.3V so that the speed of 0.5V/s is linear more subsequently, so move in circles 20 times, make as shown in Figure 2 gold nano grain base little-the orderly hole of nano compound structure array.
Embodiment 4
The concrete steps of preparation are:
Step 1 will be that the colloid monolayer crystal template that the polystyrene colloid ball of 0.3 μ m forms places on the conductive substrates by spherical diameter first; Wherein, conductive substrates is conductive glass.Again the conductive substrates that is equipped with colloid monolayer crystal template on it being placed golden electrolytic solution, take it as working electrode, is 3mA/cm in current density
2Lower employing three-electrode method galvanic deposit 20min; Wherein, during galvanic deposit is Graphite Electrodes to electrode, and reference electrode is saturated calomel electrode, obtains the complex body array.
Step 2 places the complex body array first dichloromethane solvent to remove the polystyrene colloid ball, obtains golden volume array.Golden volume array being placed concentration is that the Klorvess Liquid of 0.35mol/L carries out electrochemical oxidation-reduction circular treatment again; wherein; the process of electrochemical oxidation-reduction circular treatment is; voltage begins from-0.3V; to stop 1.2s behind the linear 1.2V of rising to of the speed of 1V/s; drop to-0.3V so that the speed of 0.5V/s is linear more subsequently, so move in circles 13 times, make be similar to gold nano grain base shown in Figure 2 little-the orderly hole of nano compound structure array.
Embodiment 5
The concrete steps of preparation are:
Step 1 will be that the colloid monolayer crystal template that the polystyrene colloid ball of 0.3 μ m forms places on the conductive substrates by spherical diameter first; Wherein, conductive substrates is conductive glass.Again the conductive substrates that is equipped with colloid monolayer crystal template on it being placed golden electrolytic solution, take it as working electrode, is 5mA/cm in current density
2Lower employing three-electrode method galvanic deposit 5min; Wherein, during galvanic deposit is Graphite Electrodes to electrode, and reference electrode is saturated calomel electrode, obtains the complex body array.
Step 2 places the complex body array first dichloromethane solvent to remove the polystyrene colloid ball, obtains golden volume array.Golden volume array being placed concentration is that the Klorvess Liquid of 0.5mol/L carries out electrochemical oxidation-reduction circular treatment again; wherein; the process of electrochemical oxidation-reduction circular treatment is; voltage begins from-0.3V; to stop 1.2s behind the linear 1.2V of rising to of the speed of 1V/s; drop to-0.3V so that the speed of 0.5V/s is linear more subsequently, so move in circles 5 times, make be similar to gold nano grain base shown in Figure 2 little-the orderly hole of nano compound structure array.
The colloid monolayer crystal template of selecting respectively again the polystyrene colloid ball of arbitrary spherical diameter of 0.1～30 μ m to form; conductive glass or conductive rubber or tinsel as conductive substrates; repeat above-described embodiment 1～5, made equally as or be similar to gold nano grain base shown in Figure 2 little-the orderly hole of nano compound structure array.
Obviously, those skilled in the art can-nano compound structure orderly hole array little to gold nano grain base of the present invention and preparation method thereof carries out various changes and modification and does not break away from the spirit and scope of the present invention.Like this, if of the present invention these are revised and modification belongs within the scope of claim of the present invention and equivalent technologies thereof, then the present invention also is intended to comprise these changes and modification interior.
Claims (8)
- A gold nano grain base little-the orderly hole of nano compound structure array, comprise conductive substrates, it is characterized in that:Piling up on the described conductive substrates has the gold grain that consists of orderly hole array wall;The pitch of holes in described orderly hole is 0.1～30 μ m;The particle diameter of described gold grain is 10～100nm, and the number of plies of its accumulation is 1～300 layer.
- Gold nano grain base according to claim 1 little-the orderly hole of nano compound structure array, it is characterized in that conductive substrates is conductive glass, or conductive rubber, or tinsel.
- Gold nano grain base according to claim 1 little-the orderly hole of nano compound structure array, it is characterized in that orderly hole array is orderly Hexagonal array.
- The described gold nano grain base of claim 1 little-preparation method of the orderly hole of nano compound structure array, comprise electrodip process, it is characterized in that completing steps is as follows:Step 1, to be that the colloid monolayer crystal template that the polystyrene colloid ball of 0.1～30 μ m forms places on the conductive substrates by spherical diameter first, again the conductive substrates that is equipped with colloid monolayer crystal template on it being placed golden electrolytic solution, take it as working electrode, is 0.1～5mA/cm in current density 2Lower employing three-electrode method galvanic deposit 5～60min obtains the complex body array;Step 2; first the complex body array is placed dichloromethane solvent to remove the polystyrene colloid ball; obtain golden volume array; place Klorvess Liquid to carry out electrochemical oxidation-reduction circular treatment golden volume array again; wherein; the process of electrochemical oxidation-reduction circular treatment is; voltage begins from-0.3V; to stop 1.2s behind the linear 1.2V of rising to of the speed of 1V/s; drop to-0.3V so that the speed of 0.5V/s is linear more subsequently; so move in circles 5～35 times, make the gold nano grain base little-the orderly hole of nano compound structure array.
- Gold nano grain base according to claim 4 little-preparation method of the orderly hole of nano compound structure array, it is characterized in that conductive substrates is conductive glass, or conductive rubber, or tinsel.
- Gold nano grain base according to claim 4 little-preparation method of the orderly hole of nano compound structure array, it is characterized in that golden electrolytic solution is that the hydrochloro-auric acid of 12g/L, the disodium ethylene diamine tetraacetate of 5g/L, the S-WAT of 160g/L and the dipotassium hydrogen phosphate of 30g/L mix mutually by concentration.
- Gold nano grain base according to claim 4 little-preparation method of the orderly hole of nano compound structure array, when it is characterized in that galvanic deposit is Graphite Electrodes to electrode, reference electrode is saturated calomel electrode.
- Gold nano grain base according to claim 4 little-preparation method of the orderly hole of nano compound structure array, the concentration that it is characterized in that Klorvess Liquid is 0.05～0.5mol/L.
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| CN104576925A (en) * | 2013-10-22 | 2015-04-29 | 吉林师范大学 | Method for preparing nano bowl-shaped phase change memory unit |
| CN107400909A (en) * | 2017-06-20 | 2017-11-28 | 广东工业大学 | A kind of three-D nano-porous copper and its preparation method and application |
| CN108103534A (en) * | 2017-12-25 | 2018-06-01 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of preparation method of metal grill film |
| CN108871026A (en) * | 2018-08-30 | 2018-11-23 | 桂林电子科技大学 | A kind of ultrathin heat pipe capillary structure and preparation method thereof |
| CN112795963A (en) * | 2020-12-28 | 2021-05-14 | 青岛大学 | Method for simply and rapidly preparing ultramicro electrode array |
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| CN104576925A (en) * | 2013-10-22 | 2015-04-29 | 吉林师范大学 | Method for preparing nano bowl-shaped phase change memory unit |
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| CN112795963A (en) * | 2020-12-28 | 2021-05-14 | 青岛大学 | Method for simply and rapidly preparing ultramicro electrode array |
| CN112795963B (en) * | 2020-12-28 | 2022-05-27 | 青岛大学 | Method for simply and rapidly preparing ultramicro electrode array |
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Application publication date: 20130116 |