CN101774763B - Porous glass containing platinum nano-particle and preparation method thereof - Google Patents
Porous glass containing platinum nano-particle and preparation method thereof Download PDFInfo
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- CN101774763B CN101774763B CN2009101896805A CN200910189680A CN101774763B CN 101774763 B CN101774763 B CN 101774763B CN 2009101896805 A CN2009101896805 A CN 2009101896805A CN 200910189680 A CN200910189680 A CN 200910189680A CN 101774763 B CN101774763 B CN 101774763B
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Abstract
The invention relates to porous glass containing platinum nano-particles and a preparation method thereof, wherein the preparation method of the porous glass containing the platinum nano-particles comprises the following steps of: preparing a solution containing platinum ions; preparing a reducer solution; and soaking: alternately placing the porous glass into the solution containing the platinum ions and the reducer solution and respectively soaking to prepare the porous glass containing the platinum nano-particles. The invention also relates to the porous glass containing the platinum nano-particles, which is prepared by adopting the method. In the preparation method of the invention, the porous glass distributed with nano-scale millipores is adopted, the platinum nano-particles are prepared in the millipores, the process is simple, and the preparation period is short; and the prepared porous glass containing the platinum nano-particles has uniform distribution of the platinum nano-particles.
Description
Technical field
The present invention relates to the preparation field of glass, more particularly, relate to a kind of sintered glass that contains nano platinum particle and preparation method thereof.
Background technology
It is a kind of functional materials that vital role is arranged in fields such as optics, electronics, antibiotic and catalysis that gold doping belongs to matrix material that particle obtains.As far back as 4th century of Christian era, the Rome glazier just understood at metallic particles such as glass doping gold and silver, prepares to have glasswork abundant, beautiful color.Nowadays, along with the development of nonlinear optics, especially after the third-order non-linear performance after nineteen eighty-three U.S. scientist Jian and Lind have studied the glass doped nanoparticle, people begin to bias toward its optical property aspect to the research that gold doping in the glass belongs to particle.When metal nanoparticle was impregnated in glass, glass matrix was isolated from each other particle, formed quantum dot, made the locality of electronics and coherency strengthen, and caused quantum confined effect.Simultaneously, when the size of metal nanoparticle during much smaller than the light field wavelength, act on electric field on the particle medium macroscopic field around also obviously being different from, its polarization process will change the specific inductivity of local, thus generation dielectric confinement effect.These effects all can cause the significantly improving of non-linear optical property of glass; Make matrix material the important use advantage arranged in fields such as optical storage, transmission and switches with non-linear optical property; For example: compare with electronic switching device; Full light photon switch device has short, energy-conservation and life-span switching time and advantage such as grows, and will become the important composition parts of following optoelectronic device.
At present, in glass matrix, prepare the significant effort direction that equally distributed metal nanoparticle has become international physics, chemical boundary.Preparing method commonly used has: scorification, ion implantation and sol-gel method etc., these technologies are relatively ripe.But; These methods also all exist the some shortcomings part; For example: scorification need with metal-salt with at high temperature carry out fusion after frit mixes because the viscosity of glass system is bigger, metallic particles will realize in glass matrix that homodisperse is not the easy thing of part; Ion implantation is that metal is injected in the glass matrix with ionic species; Obtain metal nanoparticle through thermal treatment again; This method need be used expensive ion implantation device, and it is limited to inject the degree of depth, and metal nanoparticle can only be distributed in the glass matrix surface; Also having a kind of method is to utilize sol-gel method will contain metal-salt in preparation glass solution to mix with glass colloidal sol; Can access the glass that contains metal nanoparticle through aftertreatment; The dispersion of metal nanoparticle is also relatively even, but this method prepares glass, and complex process, production cycle are longer; And the intensity of glasswork is lower, does not reach practical requirement.
Summary of the invention
The technical problem that the present invention will solve is; To the existing preparation method who contains the glass of metal nanoparticle; The dispersion of metal nanoparticle in glass is inhomogeneous, and perhaps long shortcoming of complex process, production cycle provides a kind of preparation method who contains the sintered glass of nano platinum particle; Nano platinum particle in its glass of preparing is evenly distributed, and technology is simple, preparation is convenient.
The another technical problem that the present invention will solve is; To the existing glass that contains metal nanoparticle; Metal nanoparticle in the glass disperses uneven shortcoming; A kind of sintered glass that contains nano platinum particle is provided, and it adopts above-mentioned preparation method to make, and the nano platinum particle in the glass is evenly distributed.
The present invention solves the technical scheme that its technical problem adopts: a kind of preparation method who contains the sintered glass of nano platinum particle is provided, comprises the steps:
Preparation platiniferous ion solution;
The preparation reductant solution;
Soak: with sintered glass alternately be positioned in the said platiniferous ion solution with said reductant solution in soak respectively after, prepare the said sintered glass that contains nano platinum particle.
In the preparation method of the sintered glass that contains nano platinum particle of the present invention, the step of said preparation platiniferous ion solution is: platiniferous ionic compound dissolution in solvent, is mixed with concentration range in 1mol/L～1 * 10
-6The platiniferous ion solution of mol/L, said platiniferous ionic compound is Platinic chloride, sodium platinichloride or potassium platinichloride, said solvent is water or ethanol.
In the preparation method of the sintered glass that contains nano platinum particle of the present invention, the step of said preparation reductant solution is: reductive agent is dissolved in the solvent, is mixed with concentration range in 1mol/L～1 * 10
-3The reductant solution of mol/L, said reductive agent are inferior sodium phosphate, Hydrazine Hydrate 80, xitix, POTASSIUM BOROHYDRIDE 97MIN, Peng Qinghuana or Trisodium Citrate, and said solvent is water or ethanol.
In the preparation method of the sintered glass that contains nano platinum particle of the present invention, said reductive agent is Hydrazine Hydrate 80, Trisodium Citrate, POTASSIUM BOROHYDRIDE 97MIN or Peng Qinghuana.
In the preparation method of the sintered glass that contains nano platinum particle of the present invention, said soaking step is: sintered glass is positioned in the said platiniferous ion solution, soaks more than the 0.5h; Make the platiniferous ion solution fully enter into the micropore of sintered glass, then sintered glass is taken out, clean with zero(ppm) water; Be positioned over again in the said reductant solution; Soak reaction 10min～20h, the platinum ion reduction in the sintered glass obtains platinum simple substance, then sintered glass is taken out; Clean after drying with zero(ppm) water, prepare the said sintered glass that contains nano platinum particle.
In the preparation method of the sintered glass that contains nano platinum particle of the present invention, said soaking step is: sintered glass is positioned in the said reductant solution, soaks more than the 0.5h; Make reductant solution fully enter into the micropore of sintered glass, then sintered glass is taken out, clean with zero(ppm) water; Be positioned over again in the said platiniferous ion solution; Soak reaction 10min～20h, the platinum ion reduction in the sintered glass obtains platinum simple substance, then sintered glass is taken out; Clean after drying with zero(ppm) water, prepare the said sintered glass that contains nano platinum particle.
In the preparation method of the sintered glass that contains nano platinum particle of the present invention, said soaking step repeats to carry out for several times.
In the preparation method of the sintered glass that contains nano platinum particle of the present invention, be distributed with micropore in the said sintered glass, the pore size of single micropore is 4～100 nanometers, the volume of micropore accounts for 25～40% of sintered glass TV in the sintered glass; The staple of the raw material of said sintered glass is calculated by weight, comprises: SiO
294～98 parts; B
2O
31～3 part; Al
2O
31～3 part; Na
20～1 part of O; ZrO
20～1 part.
The present invention solves another technical scheme that its technical problem adopts: a kind of sintered glass that contains nano platinum particle is provided; Adopt aforesaid method preparation; Comprise: the micropore of sintered glass and interior distribution thereof; The pore size of single micropore is 4～100 nanometers, and the volume of micropore accounts for 25～40% of sintered glass TV in the sintered glass, is distributed with nano platinum particle in the micropore.
In the sintered glass that contains nano platinum particle of the present invention, the staple of said sintered glass is calculated by weight, comprises: SiO
294～98 parts; B
2O
31～3 part; Al
2O
31～3 part; Na
20～1 part of O; ZrO
20～1 part.
Embodiment of the present invention; Has following beneficial effect: the preparation method who contains the sintered glass of nano platinum particle of the present invention; Employing is distributed with nanometer level microporous sintered glass, in micropore, prepares nano platinum particle, can effectively limit the size of particle; And making nano platinum particle in glass, have good dispersiveness, its technology is simple, preparation cycle is lacked, can effectively be saved production cost; The prepared sintered glass that contains nano platinum particle, the nano platinum particle in the glass is evenly distributed, and the non-linear optical property of glass is significantly improved.
Embodiment
The sintered glass that is adopted among the following embodiment 1～11 is in type sintered glass, can making in laboratory, also can directly use the commercially available Vycor of Corning Incorporated series sintered glass, and the staple of its raw material is calculated by weight, comprises: SiO
294～98 parts; B
2O
31～3 part; Al
2O
31～3 part; Can also contain other composition, as: Na
20～1 part of O; ZrO
20～1 part; Be distributed with micropore in the prepared sintered glass, the pore size of single micropore is 4～100 nanometers, and the volume of micropore accounts for 25～40% of sintered glass TV in the sintered glass.
Embodiment 1: under room temperature environment, Platinic chloride is dissolved in the water, compound concentration is the chloroplatinic acid aqueous solution 5mL of 1mol/L, and in water, compound concentration is 1 * 10 with dissolution of ascorbic acid
-1The aqueous ascorbic acid 10mL of mol/L, and chloroplatinic acid aqueous solution refrigeration deposited; Sintered glass is put into soaks 0.5h in the chloroplatinic acid aqueous solution; So that chloroplatinic acid aqueous solution fully enters into the micropore of sintered glass; Take out sintered glass,, and then sintered glass is put into to soak in the aqueous ascorbic acid reacts 3h with distilled water flushing 3 times; Take out the back and clean and drying, prepare the sintered glass that contains nano platinum particle with zero(ppm) water.
Embodiment 2: under room temperature environment, Platinic chloride is dissolved in the water, compound concentration is 1 * 10
-1The chloroplatinic acid aqueous solution 5mL of mol/L is dissolved in water with inferior sodium phosphate, and compound concentration is 1 * 10
-2The ortho phosphorous acid sodium water solution 10mL of mol/L, and chloroplatinic acid aqueous solution refrigeration deposited; Sintered glass is put into soaks 1h in the chloroplatinic acid aqueous solution; So that chloroplatinic acid aqueous solution fully enters into the micropore of sintered glass; Take out sintered glass,, and then sintered glass is put into to soak in the ortho phosphorous acid sodium water solution reacts 20h with distilled water flushing 3 times; Take out the back and clean and drying, prepare the sintered glass that contains nano platinum particle with zero(ppm) water.
Embodiment 3: under room temperature environment, Platinic chloride is dissolved in the water, compound concentration is 1 * 10
-2The chloroplatinic acid aqueous solution 5mL of mol/L is dissolved in water with Peng Qinghuana, and compound concentration is 1 * 10
-2The sodium borohydride aqueous solution 10mL of mol/L, and chloroplatinic acid aqueous solution refrigeration deposited; Sintered glass is put into soaks 1h in the chloroplatinic acid aqueous solution; So that chloroplatinic acid aqueous solution fully enters into the micropore of sintered glass; Take out sintered glass,, and then sintered glass is put into to soak in the sodium borohydride aqueous solution reacts 10min with distilled water flushing 3 times; Take out the back and clean and drying, prepare the sintered glass that contains nano platinum particle with zero(ppm) water.
Embodiment 4: under room temperature environment, Platinic chloride is dissolved in the ethanol, compound concentration is 1 * 10
-3The Platinic chloride ethanolic soln 5mL of mol/L is dissolved in water with POTASSIUM BOROHYDRIDE 97MIN, and compound concentration is the POTASSIUM BOROHYDRIDE 97MIN aqueous solution 10mL of 1mol/L, and the refrigeration of Platinic chloride ethanolic soln is deposited; Sintered glass is put in the POTASSIUM BOROHYDRIDE 97MIN aqueous solution soaks 1h; So that the POTASSIUM BOROHYDRIDE 97MIN aqueous solution fully enters into the micropore of sintered glass; Take out sintered glass,, and then sintered glass is put into to soak in the Platinic chloride ethanolic soln reacts 10min with distilled water flushing 3 times; Take out the back and clean and drying, prepare the sintered glass that contains nano platinum particle with zero(ppm) water.
Embodiment 5: under room temperature environment, Platinic chloride is dissolved in the water, compound concentration is 1 * 10
-4The chloroplatinic acid aqueous solution 5mL of mol/L is dissolved in water with Trisodium Citrate, and compound concentration is 1 * 10
-2The sodium citrate aqueous solution 10mL of mol/L, and chloroplatinic acid aqueous solution refrigeration deposited; Sintered glass is put into soaks 1h in the chloroplatinic acid aqueous solution; So that chloroplatinic acid aqueous solution fully enters into the micropore of sintered glass; Take out sintered glass,, and then sintered glass is put into to soak in the sodium citrate aqueous solution reacts 18h with distilled water flushing 3 times; Take out the back and clean and drying, prepare the sintered glass that contains nano platinum particle with zero(ppm) water.
Embodiment 6: under room temperature environment, Platinic chloride is dissolved in the water, compound concentration is 1 * 10
-5The chloroplatinic acid aqueous solution 5mL of mol/L dilutes hydrazine hydrate solution with zero(ppm) water, and compound concentration is 1 * 10
-3The hydrazine hydrate aqueous solution 10mL of mol/L, and chloroplatinic acid aqueous solution refrigeration deposited; Sintered glass is put into soaks 1h in the chloroplatinic acid aqueous solution; So that chloroplatinic acid aqueous solution fully enters into the micropore of sintered glass; Take out sintered glass,, and then sintered glass is put into to soak in the hydrazine hydrate aqueous solution reacts 3h with distilled water flushing 3 times; Take out the back and clean and drying, prepare the sintered glass that contains nano platinum particle with zero(ppm) water; For the content that makes the contained nano platinum particle of sintered glass increases, can above-mentioned dip operation step be repeated 5 times.
Embodiment 7: under room temperature environment, Platinic chloride is dissolved in the water, compound concentration is 1 * 10
-6The chloroplatinic acid aqueous solution 5mL of mol/L is dissolved in water with Peng Qinghuana, and compound concentration is 1 * 10
-3The sodium borohydride aqueous solution 10mL of mol/L, and chloroplatinic acid aqueous solution refrigeration deposited; Sintered glass is put into soaks 1h in the chloroplatinic acid aqueous solution; So that chloroplatinic acid aqueous solution fully enters into the micropore of sintered glass; Take out sintered glass,, and then sintered glass is put into to soak in the sodium borohydride aqueous solution reacts 0.5h with distilled water flushing 3 times; Take out the back and clean and drying, prepare the sintered glass that contains nano platinum particle with zero(ppm) water; For the content that makes the contained nano platinum particle of sintered glass increases, can above-mentioned dip operation step be repeated 10 times.
Embodiment 8: under room temperature environment, sodium platinichloride is dissolved in the water, compound concentration is 1 * 10
-2The sodium platinichloride aqueous solution 5mL of mol/L is dissolved in water with Peng Qinghuana, and compound concentration is 1 * 10
-1The sodium borohydride aqueous solution 10mL of mol/L, and sodium platinichloride aqueous solution refrigeration deposited; Sintered glass is put into soaks 0.5h in the sodium borohydride aqueous solution; So that sodium borohydride aqueous solution fully enters into the micropore of sintered glass; Take out sintered glass,, and then sintered glass is put into to soak in the sodium platinichloride aqueous solution reacts 1h with distilled water flushing 3 times; Take out the back and clean and drying, prepare the sintered glass that contains nano platinum particle with zero(ppm) water.
Embodiment 9: under room temperature environment, sodium platinichloride is dissolved in the water, compound concentration is 1 * 10
-4The sodium platinichloride aqueous solution 5mL of mol/L, in water, compound concentration is 1 * 10 with dissolution of ascorbic acid
-1The xitix ethanolic soln 10mL of mol/L, and sodium platinichloride aqueous solution refrigeration deposited; Sintered glass is put in the xitix ethanolic soln soaks 1h; So that the xitix ethanolic soln fully enters into the micropore of sintered glass; Take out sintered glass,, and then sintered glass is put into to soak in the sodium platinichloride aqueous solution reacts 1h with distilled water flushing 3 times; Take out the back and clean and drying, prepare the sintered glass that contains nano platinum particle with zero(ppm) water; For the content that makes the contained nano platinum particle of sintered glass increases, can above-mentioned dip operation step be repeated 8 times.
Embodiment 10: under room temperature environment, potassium platinichloride is dissolved in the water, compound concentration is the potassium platinichloride aqueous solution 5mL of 1mol/L, and in water, compound concentration is 1 * 10 with dissolution of ascorbic acid
-1The aqueous ascorbic acid 10mL of mol/L, and potassium platinichloride aqueous solution refrigeration deposited; Sintered glass is put in the potassium platinichloride aqueous solution soaks 0.5h; So that the potassium platinichloride aqueous solution fully enters into the micropore of sintered glass; Take out sintered glass,, and then sintered glass is put into to soak in the aqueous ascorbic acid reacts 3h with distilled water flushing 3 times; Take out the back and clean and drying, prepare the sintered glass that contains nano platinum particle with zero(ppm) water.
Embodiment 11: under room temperature environment, potassium platinichloride is dissolved in the ethanol, compound concentration is 1 * 10
-5The potassium platinichloride ethanolic soln 5mL of mol/L is dissolved in water with POTASSIUM BOROHYDRIDE 97MIN, and compound concentration is the POTASSIUM BOROHYDRIDE 97MIN aqueous solution 10mL of 1mol/L, and the refrigeration of potassium platinichloride ethanolic soln is deposited; Sintered glass is put in the POTASSIUM BOROHYDRIDE 97MIN aqueous solution soaks 1h; So that the POTASSIUM BOROHYDRIDE 97MIN aqueous solution fully enters into the micropore of sintered glass; Take out sintered glass,, and then sintered glass is put into to soak in the potassium platinichloride ethanolic soln reacts 20h with distilled water flushing 3 times; Take out the back and clean and drying, prepare the sintered glass that contains nano platinum particle with zero(ppm) water.
The prepared sintered glass that contains nano platinum particle that goes out of the foregoing description 1～11 is evenly distributed with nano platinum particle in the micropore of sintered glass.
The above; Be merely the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, any technician who is familiar with the present technique field is in the technical scope that the present invention discloses; The variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (6)
1. a preparation method who contains the sintered glass of nano platinum particle is characterized in that, comprises the steps:
Preparation platiniferous ion solution; The step of said preparation platiniferous ion solution is: platiniferous ionic compound dissolution in solvent, is mixed with concentration range in 1mol/L～1 * 10
-6The platiniferous ion solution of mol/L;
The preparation reductant solution; The step of said preparation reductant solution is: reductive agent is dissolved in the solvent, is mixed with concentration range in 1mol/L～1 * 10
-3The reductant solution of mol/L;
Soak: with sintered glass alternately be positioned in the said platiniferous ion solution with said reductant solution in soak respectively after, prepare the said sintered glass that contains nano platinum particle;
Said soaking step is: sintered glass is positioned in the said platiniferous ion solution, soaks more than the 0.5h, make the platiniferous ion solution fully enter into the micropore of sintered glass; Then sintered glass is taken out, clean, be positioned over again in the said reductant solution with zero(ppm) water; Soak reaction 10min～20h, the platinum ion reduction in the sintered glass obtains platinum simple substance, then sintered glass is taken out; Clean after drying with zero(ppm) water, prepare the said sintered glass that contains nano platinum particle; Perhaps sintered glass is positioned in the said reductant solution, soaks more than the 0.5h, make reductant solution fully enter into the micropore of sintered glass; Then sintered glass is taken out, clean, be positioned over again in the said platiniferous ion solution with zero(ppm) water; Soak reaction 10min～20h, the platinum ion reduction in the sintered glass obtains platinum simple substance, then sintered glass is taken out; Clean after drying with zero(ppm) water, prepare the said sintered glass that contains nano platinum particle;
Wherein, said platiniferous ionic compound is Platinic chloride, sodium platinichloride or potassium platinichloride, and said reductive agent is inferior sodium phosphate, Hydrazine Hydrate 80, xitix, POTASSIUM BOROHYDRIDE 97MIN, Peng Qinghuana or Trisodium Citrate, and said solvent is water or ethanol.
2. the preparation method who contains the sintered glass of nano platinum particle as claimed in claim 1 is characterized in that, said reductive agent is Hydrazine Hydrate 80, Trisodium Citrate, POTASSIUM BOROHYDRIDE 97MIN or Peng Qinghuana.
3. the preparation method who contains the sintered glass of nano platinum particle as claimed in claim 1 is characterized in that, said soaking step repeats to carry out for several times.
4. the preparation method who contains the sintered glass of nano platinum particle as claimed in claim 1; It is characterized in that; Be distributed with micropore in the said sintered glass, the pore size of single micropore is 4～100 nanometers, and the volume of micropore accounts for 25～40% of sintered glass TV in the sintered glass; The staple of the raw material of said sintered glass is calculated by weight, comprises: SiO
294～98 parts; B
2O
31～3 part; Al
2O
31～3 part; Na
2O0～1 part; ZrO
20～1 part.
5. sintered glass that contains nano platinum particle; The preparation of employing the method for claim 1; It is characterized in that: the micropore that comprises sintered glass and interior distribution thereof; The pore size of single micropore is 4～100 nanometers, and the volume of micropore accounts for 25～40% of sintered glass TV in the sintered glass, is distributed with nano platinum particle in the micropore.
6. the sintered glass that contains nano platinum particle as claimed in claim 5 is characterized in that, the staple of said sintered glass is calculated by weight, comprises: SiO
294～98 parts; B
2O
31～3 part; Al
2O
31～3 part; Na
20～1 part of O; ZrO
20～1 part.
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| CN2009101896805A CN101774763B (en) | 2009-08-31 | 2009-08-31 | Porous glass containing platinum nano-particle and preparation method thereof |
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| CN101774763B true CN101774763B (en) | 2012-01-04 |
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