CN105458247A - Gold-tin oxide core shell structure composite nano material and preparing method thereof - Google Patents
Gold-tin oxide core shell structure composite nano material and preparing method thereof Download PDFInfo
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- CN105458247A CN105458247A CN201510860023.4A CN201510860023A CN105458247A CN 105458247 A CN105458247 A CN 105458247A CN 201510860023 A CN201510860023 A CN 201510860023A CN 105458247 A CN105458247 A CN 105458247A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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Abstract
The invention discloses a gold-tin oxide core shell structure composite nano material and a preparing method thereof. The material is formed in the manner that gold nano particles are coated with tin oxide. The particle size of the material is 12-26 nm, the particle size of the gold nano particles is 10-20 nm, the thickness of a tin oxide layer is 1-3 nm, and the tin oxide layer is composed of oxide tin particles with the particle size of 1-3 nm. The method includes the steps that a gold target is put in a stirred stannic chloride aqueous solution, lasers with the wavelength of 532 nm or 1064 nm, the repetition frequency of 1-20 Hz, the pulse width of 5-15 ns and the power of 40-120 mJ/pulse are used for irradiating the gold target for at least one minute, and a mixed colloidal solution is obtained; and then, the mixed colloidal solution is subjected to solid-liquid separation, washing and drying in sequence, and the target product is obtained. The gold-tin oxide core shell structure composite nano material has higher gas sensitivity and is extremely easily and widely applied to the field of detection of poisonous and harmful gas and flammable and combustible gas in a commercialized manner.
Description
Technical field
The present invention relates to a kind of core-shell structure composite nano material and preparation method, especially a kind of gold-tin oxide core-shell structure composite nano material and preparation method thereof.
Background technology
Tin ash (SnO
2) be a kind of typical broad stopband (3.5eV-3.6eV) N-type semiconductor, be widely used in the aspects such as gas sensing, photocatalysis, solar cell and surface enhanced Raman scattering substrate.At present, tin dioxide nanometer material, as studying the most popular gas sensitive, has wide using value in the context of detection of poisonous and harmful and flammable explosive gas.But tin ash sensor still also exists poor stability, selective bad, the problem such as operating temperature is high in actual applications.For addressing this problem, people attempt to improve the air-sensitive performance of tin ash sensor by the adulterate method of a certain proportion of metal especially precious metal material of finishing or body, as at " AuSnO
2the research of the preparation of core/core/shell nanoparticles and oxygen air-sensitive performance thereof ", " material Leader B: a research section " in September, 2011 (under) disclose in the 25th volume the 9th phase 41st ~ 43 pages a kind of take gold nano grain as core, tin oxide be shell core/core/shell nanoparticles and its preparation method.The particle diameter of the core/core/shell nanoparticles mentioned in this article mostly is 50nm; Preparation method for reducing SnO in previously prepared Au nano-particle solution
2synthesis AuSn nano particle, then adopts interim heating and oxidation to obtain product.But, no matter be core/core/shell nanoparticles, or its preparation method, all there is shortcoming part, first, the tin oxide shell of coated gold nano grain is thicker, and is fine and close crystallizing layer, makes the efficient catalytic activity of gold nano grain be difficult to play; Secondly, preparation method is very complicated both, again time-consuming power consumption, can't obtain the product with higher air-sensitive effect.
Summary of the invention
The technical problem to be solved in the present invention, for overcoming shortcoming part of the prior art, provides a kind of rational in infrastructure, has the gold-tin oxide core-shell structure composite nano material of higher air-sensitive effect.
Another technical problem that the present invention will solve is for providing a kind of preparation method of above-mentioned gold-tin oxide core-shell structure composite nano material.
For solving technical problem of the present invention, the technical scheme adopted is: gold-tin oxide core-shell structure composite nano material is made up of the coated gold nano grain of tin oxide, particularly,
Described composite nano materials is graininess, and its particle diameter is 12 ~ 26nm;
The described particle diameter being coated with the gold nano grain of tin oxide is 10 ~ 20nm;
The thickness of described stannic oxide layer is 1 ~ 3nm, and its granules of stannic oxide being 1 ~ 3nm by particle diameter forms.
Further improvement as gold-tin oxide core-shell structure composite nano material:
Preferably, graininess composite nano materials is spherical.
For solving another technical problem of the present invention, another technical scheme adopted is: the preparation method of above-mentioned gold-tin oxide core-shell structure composite nano material comprises liquid phase method, and particularly completing steps is as follows:
Step 1, first gold target material is placed in the stannic chloride aqueous solution of 0.05 ~ 0.5mol/L under stirring, re-use the laser that wavelength is 532nm or 1064nm, repetition rate is 1 ~ 20Hz, pulse width is 5 ~ 15ns, power is 40 ~ 120mJ/pulse and irradiate gold target material at least 1min, obtain mixed colloidal solution;
Step 2, carries out the process of Separation of Solid and Liquid, washing and drying successively to mixed colloidal solution, obtained gold-tin oxide core-shell structure composite nano material.
Further improvement as the preparation method of gold-tin oxide core-shell structure composite nano material:
Preferably, the spot diameter of laser is 0.5 ~ 2.5mm.
Preferably, emission wavelength is the laser instrument of 532nm or 1064nm is Nd:YAG solid state laser.
Preferably, Separation of Solid and Liquid is treated to centrifugation, and its rotating speed is 1000 ~ 12000r/min, the time is 1 ~ 20min.
Preferably, carrying out washing treatment is use deionized water or ethanol or acetone to carry out the cleaning of 2 ~ 3 times to the solid that separation obtains, and being separated solid during cleaning is centrifugation.
Preferably, drying is treated at the solid after by cleaning is placed in 30 ~ 80 DEG C and dries, or is placed in natural drying under room temperature.
Relative to the beneficial effect of prior art be:
One, use ESEM, transmission electron microscope and X-ray diffractometer to characterize respectively to obtained object product, from its result, object product is granular nucleocapsid structure.Wherein, the particle diameter of core-shell structure particles is 12 ~ 26nm; Nucleocapsid structure is made up of the coated core nano particle of shell, and the particle diameter of core nano particle is wherein 10 ~ 20nm, and the thickness of shell is 1 ~ 3nm, and its particle being 1 ~ 3nm by particle diameter forms.The nano particle forming core is gold nano grain, the particle of shell is granules of stannic oxide.This object product be assembled into by the coated gold nano grain of granules of stannic oxide, based on the excellent gas-sensitive property that tin oxide possesses, and have efficient catalytic activity in the process that gas responded at tin oxide of gold nano grain, the significantly very thin thickness of stannic oxide layer, and stannic oxide layer is made up of the granules of stannic oxide that there is a large amount of hole each other, this not only drastically increases the specific area of tin oxide, also the efficient catalytic activity of gold nano grain is made to be given full play to, and mutual in air-sensitive response process of granules of stannic oxide layer and gold nano grain core, acting in conjunction, thus make selective as during gas sensor of object product, sensitivity and stability obtain great lifting.
Its two, preparation method is simple, science, efficient.Not only obtain rational in infrastructure, there is the object product of higher air-sensitive effect---gold-tin oxide core-shell structure composite nano material; Also make it have higher air-sensitive performance; More have that technique is simple, energy-and time-economizing, feature that cost of manufacture is low; And then make object product very easily in commercial applications widely in the detection field of poisonous and harmful and flammable explosive gas.
Accompanying drawing explanation
Fig. 1 is one of the object product obtained preparation method result of using ESEM (SEM) to characterize.It is dispersed good, numerous granular substance that SEM image demonstrates object product.
Fig. 2 is to one of result that the object product shown in Fig. 1 uses transmission electron microscope (TEM) to characterize.It is nucleocapsid structure that TEM image indicates object product.
Fig. 3 is to one of result that the object product shown in Fig. 1 uses X-ray diffraction (XRD) instrument to characterize.The XRD spectral line of product for the purpose of curve a in XRD spectra, curve b and curve c is respectively the standard spectral line of gold, tin ash; Fig. 3 confirms that object product is made up of golden core and tin oxide shell.
Detailed description of the invention
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
First buy from market or obtain voluntarily:
Gold target material; The stannic chloride aqueous solution; Nd:YAG solid state laser; Deionized water; Ethanol; Acetone.
Then,
Embodiment 1
The concrete steps of preparation are:
Step 1, is first placed in the stannic chloride aqueous solution of the 0.05mol/L under stirring by gold target material.Re-use the laser that wavelength is 532nm (or 1064nm), repetition rate is 1Hz, pulse width is 15ns, power is 40mJ/pulse and irradiate gold target material 20min; Wherein, the spot diameter of laser is 0.5mm, and emission wavelength is the laser instrument of 532nm (or 1064nm) is Nd:YAG solid state laser, obtains mixed colloidal solution.
Step 2, carries out the process of Separation of Solid and Liquid, washing and drying successively to mixed colloidal solution; Wherein, Separation of Solid and Liquid is treated to centrifugation, its rotating speed is 1000r/min, the time is 20min, carrying out washing treatment is for using deionized water (or ethanol or acetone) to the cleaning being separated the solid obtained and carrying out 2 times, being separated solid during cleaning is centrifugation, and drying is treated at the solid after by cleaning is placed in 30 DEG C and dries (or be placed in room temperature under natural drying).Obtain and be similar to shown in Fig. 1 and Fig. 2, and the gold-tin oxide core-shell structure composite nano material as shown in the curve in Fig. 3.
Embodiment 2
The concrete steps of preparation are:
Step 1, is first placed in the stannic chloride aqueous solution of the 0.08mol/L under stirring by gold target material.Re-use the laser that wavelength is 532nm (or 1064nm), repetition rate is 5Hz, pulse width is 12.5ns, power is 60mJ/pulse and irradiate gold target material 15min; Wherein, the spot diameter of laser is 1mm, and emission wavelength is the laser instrument of 532nm (or 1064nm) is Nd:YAG solid state laser, obtains mixed colloidal solution.
Step 2, carries out the process of Separation of Solid and Liquid, washing and drying successively to mixed colloidal solution; Wherein, Separation of Solid and Liquid is treated to centrifugation, its rotating speed is 3000r/min, the time is 15min, carrying out washing treatment is for using deionized water (or ethanol or acetone) to the cleaning being separated the solid obtained and carrying out 2 times, being separated solid during cleaning is centrifugation, and drying is treated at the solid after by cleaning is placed in 44 DEG C and dries (or be placed in room temperature under natural drying).Obtain and be similar to shown in Fig. 1 and Fig. 2, and the gold-tin oxide core-shell structure composite nano material as shown in the curve in Fig. 3.
Embodiment 3
The concrete steps of preparation are:
Step 1, is first placed in the stannic chloride aqueous solution of the 0.1mol/L under stirring by gold target material.Re-use the laser that wavelength is 532nm (or 1064nm), repetition rate is 10Hz, pulse width is 10ns, power is 80mJ/pulse and irradiate gold target material 10min; Wherein, the spot diameter of laser is 1.5mm, and emission wavelength is the laser instrument of 532nm (or 1064nm) is Nd:YAG solid state laser, obtains mixed colloidal solution.
Step 2, carries out the process of Separation of Solid and Liquid, washing and drying successively to mixed colloidal solution; Wherein, Separation of Solid and Liquid is treated to centrifugation, its rotating speed is 6000r/min, the time is 10min, carrying out washing treatment is for using deionized water (or ethanol or acetone) to the cleaning being separated the solid obtained and carrying out 3 times, being separated solid during cleaning is centrifugation, and drying is treated at the solid after by cleaning is placed in 55 DEG C and dries (or be placed in room temperature under natural drying).Obtain as depicted in figs. 1 and 2, and the gold-tin oxide core-shell structure composite nano material as shown in the curve in Fig. 3.
Embodiment 4
The concrete steps of preparation are:
Step 1, is first placed in the stannic chloride aqueous solution of the 0.3mol/L under stirring by gold target material.Re-use the laser that wavelength is 532nm (or 1064nm), repetition rate is 15Hz, pulse width is 7.5ns, power is 100mJ/pulse and irradiate gold target material 5min; Wherein, the spot diameter of laser is 2mm, and emission wavelength is the laser instrument of 532nm (or 1064nm) is Nd:YAG solid state laser, obtains mixed colloidal solution.
Step 2, carries out the process of Separation of Solid and Liquid, washing and drying successively to mixed colloidal solution; Wherein, Separation of Solid and Liquid is treated to centrifugation, its rotating speed is 9000r/min, the time is 5min, carrying out washing treatment is for using deionized water (or ethanol or acetone) to the cleaning being separated the solid obtained and carrying out 3 times, being separated solid during cleaning is centrifugation, and drying is treated at the solid after by cleaning is placed in 68 DEG C and dries (or be placed in room temperature under natural drying).Obtain and be similar to shown in Fig. 1 and Fig. 2, and the gold-tin oxide core-shell structure composite nano material as shown in the curve in Fig. 3.
Embodiment 5
The concrete steps of preparation are:
Step 1, is first placed in the stannic chloride aqueous solution of the 0.5mol/L under stirring by gold target material.Re-use the laser that wavelength is 532nm (or 1064nm), repetition rate is 20Hz, pulse width is 5ns, power is 120mJ/pulse and irradiate gold target material 1min; Wherein, the spot diameter of laser is 2.5mm, and emission wavelength is the laser instrument of 532nm (or 1064nm) is Nd:YAG solid state laser, obtains mixed colloidal solution.
Step 2, carries out the process of Separation of Solid and Liquid, washing and drying successively to mixed colloidal solution; Wherein, Separation of Solid and Liquid is treated to centrifugation, its rotating speed is 12000r/min, the time is 1min, carrying out washing treatment is for using deionized water (or ethanol or acetone) to the cleaning being separated the solid obtained and carrying out 3 times, being separated solid during cleaning is centrifugation, and drying is treated at the solid after by cleaning is placed in 80 DEG C and dries (or be placed in room temperature under natural drying).Obtain and be similar to shown in Fig. 1 and Fig. 2, and the gold-tin oxide core-shell structure composite nano material as shown in the curve in Fig. 3.
Obviously, those skilled in the art can carry out various change and modification to gold of the present invention-tin oxide core-shell structure composite nano material and preparation method thereof and not depart from the spirit and scope of the present invention.Like this, if belong within the scope of the claims in the present invention and equivalent technologies thereof to these amendments of the present invention and modification, then the present invention is also intended to comprise these change and modification.
Claims (8)
1. gold-tin oxide core-shell structure composite nano material, is made up of the coated gold nano grain of tin oxide, it is characterized in that:
Described composite nano materials is graininess, and its particle diameter is 12 ~ 26nm;
The described particle diameter being coated with the gold nano grain of tin oxide is 10 ~ 20nm;
The thickness of described stannic oxide layer is 1 ~ 3nm, and its granules of stannic oxide being 1 ~ 3nm by particle diameter forms.
2. gold according to claim 1-tin oxide core-shell structure composite nano material, is characterized in that graininess composite nano materials is spherical.
3. a preparation method for gold described in claim 1-tin oxide core-shell structure composite nano material, comprises liquid phase method, it is characterized in that completing steps is as follows:
Step 1, first gold target material is placed in the stannic chloride aqueous solution of 0.05 ~ 0.5mol/L under stirring, re-use the laser that wavelength is 532nm or 1064nm, repetition rate is 1 ~ 20Hz, pulse width is 5 ~ 15ns, power is 40 ~ 120mJ/pulse and irradiate gold target material at least 1min, obtain mixed colloidal solution;
Step 2, carries out the process of Separation of Solid and Liquid, washing and drying successively to mixed colloidal solution, obtained gold-tin oxide core-shell structure composite nano material.
4. the preparation method of gold according to claim 3-tin oxide core-shell structure composite nano material, is characterized in that the spot diameter of laser is 0.5 ~ 2.5mm.
5. the preparation method of gold according to claim 3-tin oxide core-shell structure composite nano material, is characterized in that emission wavelength be the laser instrument of 532nm or 1064nm is Nd:YAG solid state laser.
6. the preparation method of gold according to claim 3-tin oxide core-shell structure composite nano material, is characterized in that Separation of Solid and Liquid is treated to centrifugation, and its rotating speed is 1000 ~ 12000r/min, the time is 1 ~ 20min.
7. the preparation method of gold according to claim 3-tin oxide core-shell structure composite nano material, it is characterized in that carrying out washing treatment is use deionized water or ethanol or acetone to carry out the cleaning of 2 ~ 3 times to the solid that separation obtains, being separated solid during cleaning is centrifugation.
8. the preparation method of gold according to claim 3-tin oxide core-shell structure composite nano material, is characterized in that drying is treated at the solid after by cleaning is placed in 30 ~ 80 DEG C and dries, or be placed in natural drying under room temperature.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106041060A (en) * | 2016-05-31 | 2016-10-26 | 华中科技大学 | Method for preparing nanocomposite through laser welding in liquid phase |
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Cited By (2)
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| CN106041060A (en) * | 2016-05-31 | 2016-10-26 | 华中科技大学 | Method for preparing nanocomposite through laser welding in liquid phase |
| CN106041060B (en) * | 2016-05-31 | 2018-02-16 | 华中科技大学 | A kind of method for preparing nano composite material using laser welding in the liquid phase |
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