CN102330083A - Preparation method for metal nanoparticle monomolecular layer capable of copying complex surface - Google Patents
Preparation method for metal nanoparticle monomolecular layer capable of copying complex surface Download PDFInfo
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- CN102330083A CN102330083A CN 201110212440 CN201110212440A CN102330083A CN 102330083 A CN102330083 A CN 102330083A CN 201110212440 CN201110212440 CN 201110212440 CN 201110212440 A CN201110212440 A CN 201110212440A CN 102330083 A CN102330083 A CN 102330083A
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- complex surface
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Abstract
The invention relates to a preparation method for a metal nanoparticle monomolecular layer capable of copying a complex surface, which is characterized in that a method that an organic micromolecule self-assembling layer serves as a template, and flowing gas airflow helps spraying is utilized to prepare the metal nanoparticle monomolecular layer. The preparation method comprises the following steps of: putting a sample with a complex surface into a vacuum chamber, and slowly rotating; depositing an organic micromolecule capable of increasing a surface adhesive force onto the surface of the sample with a low-temperature fumigation method to form one layer of micromolecule layer; spraying an organic solution containing the metal nanoparticles from a nozzle above the sample, and depositing on the surface of the sample; introducing lateral airflow into a vacuum chamber, regulating airflow speed, and controlling the deposition density of the metal nanoparticle monomolecular layer on a complex surface; slowing filling gas into the vacuum chamber; and taking out the sample.
Description
Technical field
The present invention relates to a kind of preparation method who is used on complex surface, obtaining the metal nanoparticle unimolecular layer, especially on complex surface, obtain the preparation method of even metal nano particle unimolecular layer, have the characteristic of duplicating complex surface.
Background technology
Diameter has purposes very widely at the metal nanoparticle of about 1-50 nanometer (nm) at aspects such as semiconductor technology, light/magneticstorage, electronic devices and components manufacturing and catalysis.Metal nanoparticle has unique optical property.Particularly metal nanoparticle demonstrates tangible optical resonance, promptly so-called surface plasmon resonance.Cause is between conduction electron and the incident EM field of metal nanoparticle resonance coupling to take place.This resonance can depend on the wavelength of incident electromagnetic wave and the proportionlity between the nano particle radius by absorbing or scatter control.Utilize these special optical properties, can prepare various useful device or device.For example, based on the optically filtering chemical sensor of surperficial enhanced Raman scattering.Provided among the patent CN 101866961 metal nanoparticle directly has been prepared in the thin film silicon/crystalline silicon heterojunction solar battery to strengthen photoabsorption.
Metal nanoparticle is by multiple preparation method: gas evaporation; Mechanicalness grinds; Sputter; Electron beam evaporation; Thermal evaporation; The reversed micelle technology; Laser ablation; The pyrolysis of organometallic compound etc.And in actual the use, need metal nanoparticle evenly be covered on the complex surface of equipment or device.But when utilizing aforesaid method to be deposited on metal nanoparticle on the complex surface; Can't obtain the unimolecular layer of an even metal nano particle; The unfavorable condition that occurs is: there is the existence of a large amount of gathering metal nanoparticles the part of complex surface, and other part of complex surface possibly not cover any metal nanoparticle.Earlier the metal nanoparticle for preparing is configured to colloid or resin coating if adopt; Be coated in complex surface; Then because the leveling characteristics of colloid or resin layer still can appear at recess and assemble a large amount of metal nanoparticles, convex part then can't be covered by metal nanoparticle.This non-homogeneous coverage mode can greatly weaken the surface plasmons effect of metal nanoparticle, and the distinctive optical property of metal nanoparticle can't be embodied.
So, how on complex surface, evenly to cover one deck nano-metal particle unimolecular layer, most important to the surface plasmons effect that makes full use of nano-metal particle.
Summary of the invention
The present invention seeks in order to overcome the deficiency of prior art, a kind of method that can prepare layer of even metal nanoparticle unimolecular layer at complex surface is provided, and the controllable density of the metal nanoparticle unimolecular layer in this method.
The present invention is for realizing above-mentioned purpose; Designed a kind of preparation method who utilizes organic molecule self-assembly layer as template and the auxiliary spraying of flowing gas air-flow; It may further comprise the steps: the sample that will have complex surface is positioned in the Vakuumkammer; When slowly rotating; To have the organic molecule that increases surface adhesion force and be deposited on sample surfaces, form one deck unimolecular layer: contain of the spout ejection of the organic solution of metal nanoparticle, be deposited on sample surfaces from the sample top through the low temperature fumigation and steaming method; Simultaneously, in Vakuumkammer, introduce lateral airflow,, obtain the controlled metal nanoparticle unimolecular layer of settled density through the adjustment gas velocity; In Vakuumkammer, slowly charge into gas, take out sample.
Specifically; A kind of preparation method of metal nanoparticle unimolecular layer of reproducible complex surface is characterized in that, utilizes the method for organic molecule self-assembly layer as template and the auxiliary spraying of flowing gas air-flow; Preparation metal nanoparticle unimolecular layer; May further comprise the steps: the sample that will have complex surface is positioned in the Vakuumkammer, and slowly rotation, and speed of rotation is 100-500rpm: will have the organic small molecule material that increases surface adhesion force and be deposited on sample surfaces through the low temperature fumigation and steaming method; Form one deck unimolecular layer; This organic molecule can be organosilane, but is not limited to organosilane, so long as this area organic small molecule material that can increase surface adhesion force commonly used can; Spray the organic solution that contains metal nanoparticle from the spout of sample top, be deposited on sample surfaces; Simultaneously, in Vakuumkammer, introduce lateral airflow, the adjustment gas velocity is 10
-4-10Pa/s, control metal nanoparticle unimolecular layer is at the settled density of complex surface; In Vakuumkammer, slowly charge into gas, take out sample.The vacuum tightness of Vakuumkammer is 10
-1-10
-3Pa: be deposited on sample surfaces through the stifling organic molecule that increases surface adhesion force of low temperature, the fumigation temperature that forms one deck unimolecular layer is 320-355 Kelvin (K).Contain the organic solution of metal nanoparticle from the spout ejection of sample top, be deposited on sample surfaces, the processing parameter in this step does, contains the organic solution of metal nanoparticle, and volumetric molar concentration is 10
-4-10
-2Mol, organic solvent are low boiling point organic solvent: spraying rate, 10-100ml/min; Nozzle distance sample surfaces degree degree, 20-50cm: in Vakuumkammer, slowly charge into gas, when taking out sample, gases used is high pure nitrogen.
Advantage of the present invention is: adopt and utilize the preparation method of organic molecule self-assembly layer as template and the auxiliary spraying of flowing gas air-flow; And the flow velocity through strict control direction finding air-flow and airflow nozzle have overcome the shortcoming that can not prepare even metal nano particle unimolecular layer at complex surface apart from the height of sample.And, because the auxiliary characteristics of air flow can be controlled the settled density of metal nanoparticle on organic molecule self-assembly layer.
Description of drawings
Fig. 1 is the preparing method's synoptic diagram that utilizes organic molecule self-assembly layer as template and the auxiliary spraying of flowing gas air-flow of the present invention.
Among the figure: 1 nozzle, 2 Vakuumkammers, 3 direction finding air-flows feed and extract out pipe, 4 universal stages, 5 samples, 6 organic molecule steam feed and extract out pipe.
Embodiment
Embodiment 1
To the uniform nano-Ag particles unimolecular layer of deposition on cadmium sulfide nano-stick array, the substrate that is grown in cadmium sulfide nano-stick array is put into Vakuumkammer, vacuum degree control is 10
-2Pa; Slow rotary sample, the hot steam with hexamethyldisilane slowly feeds Vakuumkammer under the sample table of placing substrate simultaneously, and vapor temperature is controlled at 335K; Fumigate and stop after 30 minutes: in Vakuumkammer, feed high pure nitrogen simultaneously, gas velocity is controlled at 1Pa/s.The chloroformic solution of the nano-Ag particles of surface-treated is sprayed on the cadmium sulfide nano-stick array surface, spraying rate 20ml/min, nozzle distance sample surfaces height, 40cm, lateral airflow speed, 5Pa/s.Spray after 60 seconds and take out.
To the uniform nm gold particles unimolecular layer of deposition on traditional monocrystalline silicon battery sheet, the monocrystalline silicon battery sheet before the electrode printing is put into Vakuumkammer, vacuum degree control is 10
-2Pa; Slow rotary sample, the hot steam with the octyl triethoxyl silane slowly feeds Vakuumkammer under the sample table of placing the battery sheet simultaneously, and vapor temperature is controlled at 345L; Fumigate and stop after 20 minutes: in Vakuumkammer, feed high pure nitrogen simultaneously, gas velocity is controlled at 10
-1Pa/s.The alcohol suspending liquid of the nm gold particles of surface-treated is sprayed on battery sheet surface, spraying rate 10ml/min, nozzle distance sample surfaces height, 30cm, lateral airflow speed, 1Pa/s.Spray after 60 seconds and take out.
To the uniform nm gold particles unimolecular layer of deposition on traditional monocrystalline silicon battery sheet, the monocrystalline silicon battery sheet before the electrode printing is put into Vakuumkammer, vacuum degree control is 10
-2Pa, slow rotary sample, the hot steam with the octyl triethoxyl silane slowly feeds Vakuumkammer under the sample table of placing the battery sheet simultaneously, and vapor temperature is controlled at 345K, fumigates to stop after 20 minutes; In Vakuumkammer, feed high pure nitrogen simultaneously, gas velocity is controlled at 10
-4Pa/s.The alcohol suspending liquid of the nm gold particles of surface-treated is sprayed on battery sheet surface, spraying rate 10m/min, nozzle distance sample surfaces height, 30cm, lateral airflow speed, 1Pa/s.Spray after 60 seconds and take out.
Embodiment 4
To the uniform nm gold particles unimolecular layer of deposition on traditional monocrystalline silicon battery sheet, the monocrystalline silicon battery sheet before the electrode printing is put into Vakuumkammer, vacuum degree control is 10
-2Pa; Slow rotary sample, the hot steam with the octyl triethoxyl silane slowly feeds Vakuumkammer under the sample table of placing the battery sheet simultaneously, and vapor temperature is controlled at 345K; Fumigate and stop after 20 minutes: in Vakuumkammer, feed high pure nitrogen simultaneously, gas velocity is controlled at 10Pa/s.The alcohol suspending liquid of the nm gold particles of surface-treated is sprayed on battery sheet surface, spraying rate 10ml/min, nozzle distance sample surfaces height, 30cm, lateral airflow speed, 1Pa/s.Spray after 60 seconds and take out.
Claims (7)
1. the preparation method of the metal nanoparticle unimolecular layer of a reproducible complex surface; It is characterized in that; Utilize the method for organic molecule self-assembly layer as template and the auxiliary spraying of flowing gas air-flow, preparation metal nanoparticle unimolecular layer may further comprise the steps:
The sample that will have complex surface is positioned in the Vakuumkammer, and slowly rotation;
To have the organic molecule that increases surface adhesion force and be deposited on sample surfaces, form one deck unimolecular layer through the low temperature fumigation and steaming method;
Spray the organic solution that contains metal nanoparticle from the spout of sample top, be deposited on sample surfaces;
In Vakuumkammer, introduce lateral airflow, the adjustment gas velocity, control metal nanoparticle unimolecular layer is at the settled density of complex surface;
In Vakuumkammer, slowly charge into gas, take out sample.
2. the preparation method of the metal nanoparticle unimolecular layer of reproducible complex surface according to claim 1, it is characterized in that: the said sample that will have complex surface is positioned in the Vakuumkammer, and slowly rotation, and the processing parameter in this step does,
Vacuum degree in vacuum chamber, 10
-1-10
-3Pascal (Pa);
The sample speed of rotation, 100-500 rpm (rpm).
3. the preparation method of the metal nanoparticle unimolecular layer of reproducible complex surface according to claim 1 and 2; It is characterized in that: the said organic molecule that will have the increase surface adhesion force is deposited on sample surfaces through the low temperature fumigation and steaming method; Form one deck unimolecular layer; Processing parameter in this step does
The kind of organic molecule, organosilane:
Fumigation temperature, 320-355 Kelvin (K).
4. the preparation method of the metal nanoparticle unimolecular layer of reproducible complex surface according to claim 3; It is characterized in that: the said organic solution that contains metal nanoparticle from the spout ejection of sample top; Be deposited on sample surfaces, the processing parameter in this step does
Contain the organic solution of metal nanoparticle, volumetric molar concentration is 10
-1-10
-2Every liter (M/L) of mole, organic solvent is a low boiling point organic solvent;
Spraying rate, 10-100 milliliter PM (ml/min).
Nozzle distance sample surfaces height, 20-50 centimetre (cm)
5. the preparation method of the metal nanoparticle unimolecular layer of reproducible complex surface according to claim 3; It is characterized in that: the said lateral airflow of in Vakuumkammer, introducing; The adjustment gas velocity; Control metal nanoparticle unimolecular layer is at the settled density of complex surface, and the processing parameter in this step does
Lateral airflow speed, 10
-4-10 pascal's per seconds (Pa/s).
6. the preparation method of the metal nanoparticle unimolecular layer of reproducible complex surface according to claim 3 is characterized in that: the said gas that in Vakuumkammer, slowly charges into, take out sample, and be specially and in Vakuumkammer, charge into high pure nitrogen, take out sample then.
7. according to the preparation method of metal nanoparticle unimolecular layer of the reproducible complex surface of the described arbitrary or combination of claim 4-5, it is characterized in that: contain the organic solution of metal nanoparticle from the spout ejection of sample top, be deposited on sample surfaces; In Vakuumkammer, introduce lateral airflow, the adjustment gas velocity, control metal nanoparticle unimolecular layer is at the settled density of complex surface.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1458288A (en) * | 2002-05-17 | 2003-11-26 | 中国科学院金属研究所 | Nanolizing method for metal material surface |
| CN1696353A (en) * | 2005-05-16 | 2005-11-16 | 山东科技大学 | Method for making Nano surface of metal material |
| KR20110051812A (en) * | 2009-11-11 | 2011-05-18 | 한국생산기술연구원 | Method for treating the surface of steel welding joint |
-
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1458288A (en) * | 2002-05-17 | 2003-11-26 | 中国科学院金属研究所 | Nanolizing method for metal material surface |
| CN1696353A (en) * | 2005-05-16 | 2005-11-16 | 山东科技大学 | Method for making Nano surface of metal material |
| KR20110051812A (en) * | 2009-11-11 | 2011-05-18 | 한국생산기술연구원 | Method for treating the surface of steel welding joint |
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