CN105478791A - Composite nanometer material with palladium coated with aluminum oxide and preparing method of composite nanometer material - Google Patents
Composite nanometer material with palladium coated with aluminum oxide and preparing method of composite nanometer material Download PDFInfo
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- CN105478791A CN105478791A CN201510883364.3A CN201510883364A CN105478791A CN 105478791 A CN105478791 A CN 105478791A CN 201510883364 A CN201510883364 A CN 201510883364A CN 105478791 A CN105478791 A CN 105478791A
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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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- 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
- B22F1/17—Metallic particles coated with metal
Abstract
The invention discloses a composite nanometer material with palladium coated with aluminum oxide and a preparing method of the composite nanometer material. A nanometer particle two-dimensional chain serves as the material, and the particle size of nanometer particles forming the nanometer particle two-dimensional chain is 6-80 nm. The nanometer particle two-dimensional chain is formed by coating palladium nanometer particles with aluminum oxide, wherein the particle size of the palladium nanometer particles is 5-50 nm, and the thickness of an aluminum oxide layer is 1-30 nm. The method includes the steps that a palladium target material is put into a stirred aluminum nitrate solution, lasers with the wavelength being 532 nm or 1064 nm, the repetition frequency being 1-20 Hz, the pulse width being 5-15 ns and the power being 40-120 mJ/pulse are used for irradiating the palladium target material for at least 20 min, and a mixed colloidal solution is obtained; and afterwards, the mixed colloidal solution is subjected to solid-liquid separation, washing and drying in sequence, and a target product is prepared. The composite nanometer material is long in hydrogenation and polymerization reaction service life and high in structure stability and can be extremely easily and widely applied to the fields of hydrogenation and polymerization reactions, gas sensors and surface enhanced Raman scattering in a commercialized manner.
Description
Technical field
The present invention relates to a kind of composite nano materials and preparation method, composite nano materials of especially a kind of alumina-coated palladium and preparation method thereof.
Background technology
Palladium (Pd), as a kind of metal, is the indispensable critical material of the high-tech area such as space flight, aviation and auto manufacturing.In field of nanometer material technology, palladium is typically used as catalyst, has important using value in fields such as gas sensing, photocatalysis, electrochemistry.But palladium also also exists the problem that life cycle is short, regeneration frequency is high in the practical application of various hydrogenation, polymerisation.For addressing this problem, people have made unremitting effort, as at " nano Pd particle/Al
2o
3the sign of catalyst and selective hydrogenation performance thereof ", disclose a kind of nano Pd particle/Al in volume the 3rd phase in " petroleum journal (PETROLEUM PROCESSING) " June the 23rd in 2007 13rd ~ 19 pages
2o
3catalyst and its preparation method.Nano Pd particle/the Al mentioned in this article
2o
3the formation of catalyst is at cellular Al
2o
3the area load Pd nano particle of carrier; Nano-Palladium high-pressure inert gas for first to obtain Nano-Palladium by H_2+Ar arc plasma method, then is made current-carrying gas, by nozzle at Al by preparation method
2o
3after upper deposition film forming, be processed into product through a series of common process.Though this catalyst has higher catalytic activity, still have weak point, first, exposed Nano-Palladium still very easily " poisoning ", makes its service life shorter; Secondly, preparation method is very complicated both, again time-consuming power consumption, can't obtain the product with higher hydrogenation, polymerisation service life.
Summary of the invention
The technical problem to be solved in the present invention, for overcoming weak point of the prior art, provides a kind of rational in infrastructure, has the composite nano materials of higher hydrogenation, the alumina-coated palladium in polymerisation service life.
Another technical problem that the present invention will solve is for providing a kind of preparation method of composite nano materials of above-mentioned alumina-coated palladium.
For solving technical problem of the present invention, the technical scheme adopted is: the composite nano materials of alumina-coated palladium comprises palladium nano-particles, particularly,
Described composite nano materials is nano particle two dimension chain, and the particle diameter of the nano particle of described composition nano particle two dimension chain is 6 ~ 80nm;
Described nano particle is by palladium nano-particles outer cladding aluminium oxide (Al
2o
3) form;
The particle diameter of described palladium nano-particles is 5 ~ 50nm;
The thickness of described alumina layer is 1 ~ 30nm.
Further improvement as the composite nano materials of alumina-coated palladium:
Preferably, aluminium oxide is amorphous alumina.
For solving another technical problem of the present invention, another technical scheme adopted is: the preparation method of the composite nano materials of above-mentioned alumina-coated palladium comprises liquid phase method, and particularly completing steps is as follows:
Step 1, first palladium target is placed in the aluminum nitrate solution of 0.01 ~ 2mol/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 palladium target at least 20min, obtain mixed colloidal solution;
Step 2, carries out the process of Separation of Solid and Liquid, washing and drying successively to mixed colloidal solution, the composite nano materials of obtained alumina-coated palladium.
Further improvement as the preparation method of the composite nano materials of alumina-coated palladium:
Preferably, aluminum nitrate solution is aluminum nitrate aqueous solution, or aluminum nitrate ethanolic solution, or aluminum nitrate acetone soln.
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, uses transmission electron microscope and X-ray diffractometer to characterize to obtained object product respectively, and from its result, object product is by numerous, that interconnective Core-shell Structure Nanoparticles forms two-dimentional chain; Wherein, the particle diameter of Core-shell Structure Nanoparticles is 6 ~ 80nm, and the particle diameter of core nano particle is wherein 5 ~ 50nm, and the thickness of shell is 1 ~ 30nm.Core nano particle is palladium nano-particles, and shell is amorphous alumina layer.This object product being assembled chaining by palladium nano-particles outer cladding aluminium oxide, both because palladium has high selective and sensitivity response as catalyst to reducibility gas, again because aluminium oxide has extraordinary surfacecti proteon effect, also owing to both to be integrated into effectively the highly stable two-dimentional chain of structure, thus the hydrogenation of object product, polymerisation service life and structural stability is made all to obtain great lifting.
Its two, preparation method is simple, science, efficient.Not only obtain rational in infrastructure, there is object product---the composite nano materials of alumina-coated palladium in higher hydrogenation, polymerisation service life; Also because of surface coated Al
2o
3layer serves the adsorption capacity strengthened object gas or fluid molecule, makes it greatly increase performance in gas sensor, SERS field; 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 hydrogenation, polymerisation, gas sensor, SERS field.
Accompanying drawing explanation
Fig. 1 is one of the object product obtained preparation method result of using transmission electron microscope (TEM) to characterize.It is the Core-shell Structure Nanoparticles being interconnected to two-dimentional chain that TEM image demonstrates object product.
Fig. 2 is to one of result that the object product shown in Fig. 1 uses high magnification transmission electron microscope to characterize.TEM image shows, the nucleocapsid structure of object product is that palladium nano-particles is coated with amorphous alumina.
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 is the standard x RD spectral line of palladium, because aluminium oxide is amorphous state, therefore does not record corresponding spectral line; Fig. 3 composition graphs 2 confirms that object product is made up of palladium core and aluminium 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:
Palladium target; As the aluminum nitrate aqueous solution of aluminum nitrate solution, aluminum nitrate ethanolic solution and aluminum nitrate acetone soln; 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 aluminum nitrate solution of the 0.01mol/L under stirring by palladium target; Wherein, aluminum nitrate solution is aluminum nitrate aqueous solution.Re-use the laser that wavelength is 532nm (or 1064nm), repetition rate is 1Hz, pulse width is 15ns, power is 40mJ/pulse and irradiate palladium target 60min; 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 use deionized water or ethanol or acetone to carry out the cleaning of 2 times to the solid that separation obtains, 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).Obtained to be similar to shown in Fig. 1 and Fig. 2, and the composite nano materials of alumina-coated palladium as shown in the curve in Fig. 3.
Embodiment 2
The concrete steps of preparation are:
Step 1, is first placed in the aluminum nitrate solution of the 0.05mol/L under stirring by palladium target; Wherein, aluminum nitrate solution is aluminum nitrate aqueous solution.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 palladium target 50min; 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 use deionized water or ethanol or acetone to carry out the cleaning of 2 times to the solid that separation obtains, 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).Obtained to be similar to shown in Fig. 1 and Fig. 2, and the composite nano materials of alumina-coated palladium as shown in the curve in Fig. 3.
Embodiment 3
The concrete steps of preparation are:
Step 1, is first placed in the aluminum nitrate solution of the 0.2mol/L under stirring by palladium target; Wherein, aluminum nitrate solution is aluminum nitrate aqueous solution.Re-use the laser that wavelength is 532nm (or 1064nm), repetition rate is 10Hz, pulse width is 10ns, power is 80mJ/pulse and irradiate palladium target 40min; 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 use deionized water or ethanol or acetone to carry out the cleaning of 3 times to the solid that separation obtains, 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).Obtained as depicted in figs. 1 and 2, and the composite nano materials of alumina-coated palladium as shown in the curve in Fig. 3.
Embodiment 4
The concrete steps of preparation are:
Step 1, is first placed in the aluminum nitrate solution of the 1mol/L under stirring by palladium target; Wherein, aluminum nitrate solution is aluminum nitrate aqueous solution.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 palladium target 30min; 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 use deionized water or ethanol or acetone to carry out the cleaning of 3 times to the solid that separation obtains, 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).Obtained to be similar to shown in Fig. 1 and Fig. 2, and the composite nano materials of alumina-coated palladium as shown in the curve in Fig. 3.
Embodiment 5
The concrete steps of preparation are:
Step 1, is first placed in the aluminum nitrate solution of the 2mol/L under stirring by palladium target; Wherein, aluminum nitrate solution is aluminum nitrate aqueous solution.Re-use the laser that wavelength is 532nm (or 1064nm), repetition rate is 20Hz, pulse width is 5ns, power is 120mJ/pulse and irradiate palladium target 20min; 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 use deionized water or ethanol or acetone to carry out the cleaning of 3 times to the solid that separation obtains, 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).Obtained to be similar to shown in Fig. 1 and Fig. 2, and the composite nano materials of alumina-coated palladium as shown in the curve in Fig. 3.
Select the aluminum nitrate aqueous solution as aluminum nitrate solution more respectively, or aluminum nitrate ethanolic solution, or aluminum nitrate acetone soln; Repeat above-described embodiment 1 ~ 5, obtained equally as or be similar to shown in Fig. 1 and Fig. 2, and the composite nano materials of alumina-coated palladium as shown in the curve in Fig. 3.
Obviously, those skilled in the art can carry out various change and modification to composite nano materials of alumina-coated palladium of the present invention 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 (9)
1. a composite nano materials for alumina-coated palladium, comprises palladium nano-particles, it is characterized in that:
Described composite nano materials is nano particle two dimension chain, and the particle diameter of the nano particle of described composition nano particle two dimension chain is 6 ~ 80nm;
Described nano particle is made up of palladium nano-particles outer cladding aluminium oxide;
The particle diameter of described palladium nano-particles is 5 ~ 50nm;
The thickness of described alumina layer is 1 ~ 30nm.
2. the composite nano materials of alumina-coated palladium according to claim 1, is characterized in that aluminium oxide is amorphous alumina.
3. a preparation method for the composite nano materials of alumina-coated palladium described in claim 1, comprises liquid phase method, it is characterized in that completing steps is as follows:
Step 1, first palladium target is placed in the aluminum nitrate solution of 0.01 ~ 2mol/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 palladium target at least 20min, obtain mixed colloidal solution;
Step 2, carries out the process of Separation of Solid and Liquid, washing and drying successively to mixed colloidal solution, the composite nano materials of obtained alumina-coated palladium.
4. the preparation method of the composite nano materials of alumina-coated palladium according to claim 3, is characterized in that aluminum nitrate solution is aluminum nitrate aqueous solution, or aluminum nitrate ethanolic solution, or aluminum nitrate acetone soln.
5. the preparation method of the composite nano materials of alumina-coated palladium according to claim 3, is characterized in that the spot diameter of laser is 0.5 ~ 2.5mm.
6. the preparation method of the composite nano materials of alumina-coated palladium according to claim 3, is characterized in that emission wavelength be the laser instrument of 532nm or 1064nm is Nd:YAG solid state laser.
7. the preparation method of the composite nano materials of alumina-coated palladium according to claim 3, 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.
8. the preparation method of the composite nano materials of alumina-coated palladium according to claim 3, 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.
9. the preparation method of the composite nano materials of alumina-coated palladium according to claim 3, 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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CN109569589A (en) * | 2018-12-10 | 2019-04-05 | 郑州师范学院 | A kind of levulic acid adds hydrogen gamma-valerolactone M-B@Al2O3Catalyst and its preparation method and application |
CN109612976A (en) * | 2018-12-24 | 2019-04-12 | 北华大学 | A kind of 3-dimensional multi-layered body structure surface enhancing Raman substrate and preparation method thereof |
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