CN101993201B - Cellular glass containing iron nano particles and preparation method thereof - Google Patents
Cellular glass containing iron nano particles and preparation method thereof Download PDFInfo
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- CN101993201B CN101993201B CN 200910109550 CN200910109550A CN101993201B CN 101993201 B CN101993201 B CN 101993201B CN 200910109550 CN200910109550 CN 200910109550 CN 200910109550 A CN200910109550 A CN 200910109550A CN 101993201 B CN101993201 B CN 101993201B
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- micropore
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Abstract
The invention relates to a cellular glass containing iron nano particles and a preparation method thereof. The preparation method of cellular glass containing iron nano particles comprises the following steps: dissolving a compound containing iron ions into a solvent to prepare a solution the concentration of which ranges from 1mol/L-1*10<-6>mol/L; placing cellular glass into the prepared solution containing the iron ions, fully soaking the glass to obtain a semi-product of the glass; and heating the obtained semi-product of the glass to 150-550DEG C, preserving heat for 1-5h, then cooling to room temperature to prepare the cellular glass containing iron nano particles. The invention also relates to the cellular glass containing iron nano particles prepared by using the method. In the preparation method of the invention, cellular glass distributed with nanoscale micropores is adopted, and the iron nano particles are prepared in the micropores; and the process is simple, the preparation period is short, and the iron nano particles of the obtained cellular glass containing iron nano particles are evenly distributed.
Description
Technical field
The present invention relates to the preparation field of glass, more particularly, relate to sintered glass of a kind of ferri nano 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 complex process, production cycle provide a kind of preparation method of sintered glass of ferri nano particle than long shortcoming; Fe nanometer particles 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 of ferri nano particle is provided, and it adopts above-mentioned preparation method to make, and the Fe nanometer particles in the glass is evenly distributed.
The present invention solves the technical scheme that its technical problem adopts: a kind of preparation method of sintered glass of ferri nano particle is provided, comprises the steps:
Step 1: iron content ionic compound dissolution in solvent, is mixed with concentration range in 1mol/L～1 * 10
-6The iron content ion solution of mol/L;
Step 2: sintered glass is positioned in the iron content ion solution that step 1 prepares, after fully soaking, obtains parison;
Step 3: the resulting parison of step 2 is warmed up to 150 ℃～550 ℃, insulation 1h～5h, cool to room temperature is prepared the sintered glass of said ferri nano particle again.
In the preparation method of the sintered glass of ferri nano particle of the present invention, said iron content ionic compound is iron nitrate or iron(ic)chloride; Said solvent is water or ethanol.
In the preparation method of the sintered glass of ferri nano particle of the present invention; Said step 2 is: sintered glass is positioned in the iron content ion solution that step 1 prepares; Soak more than the 0.5h, take out sintered glass then, clean sintered glass with zero(ppm) water; And be put into dry 2h～3h in 80 ℃～120 ℃ the baking oven, obtain said parison.
In the preparation method of the sintered glass of ferri nano particle of the present invention; Said step 3 is: the prepared parison of step 2 is put into tube furnace under the environment of reducing atmosphere; Speed with 2 ℃～3 ℃/min is warmed up to 150 ℃～550 ℃; Insulation 1h～5h, cool to room temperature is prepared the sintered glass of said ferri nano particle again.
In the preparation method of the sintered glass of ferri nano particle of the present invention, said reducing atmosphere is CO, H
2, or N
2And H
2The atmosphere that exists of mixed gas.
In the preparation method of the sintered glass of ferri nano particle of the present invention, for the content that makes the contained Fe nanometer particles of sintered glass increases, said step 1～three can repeat.
In the preparation method of the sintered glass of ferri nano particle of the present invention, be distributed with micropore in the said sintered glass, the pore size of micropore is 4～100 nanometers, the volume of micropore accounts for 25～40% of glass TV.
In the preparation method of the sintered glass of ferri nano particle of the present invention, 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: the sintered glass that a kind of ferri nano particle is provided; Adopt aforesaid method preparation; Comprise: the micropore of sintered glass and interior distribution thereof; The pore size of micropore is 4～100 nanometers, and the volume of micropore accounts for 25～40% of glass TV, is evenly distributed with Fe nanometer particles in the micropore.
In the sintered glass of ferri nano 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 of the sintered glass of ferri nano particle of the present invention; Employing is distributed with nanometer level microporous sintered glass, in micropore, prepares Fe nanometer particles, can effectively limit the size of particle; And making Fe nanometer particles in glass, have good dispersiveness, its technology is simple, preparation cycle is lacked, can effectively be saved production cost; The sintered glass of prepared ferri nano particle, the Fe nanometer particles 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 1～7 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 micropore is 4～100 nanometers, and the volume of micropore accounts for 25～40% of glass TV.
Embodiment 1: under room temperature environment, iron nitrate is dissolved in the water, compound concentration is the iron nitrate aqueous solution 10mL of 1mol/L; Sintered glass is put into soaks 0.5h in the iron nitrate aqueous solution, take out sintered glass,, and be put into 80 ℃ oven drying 2h with distilled water flushing 3 times; Then sintered glass is put in the tube furnace, in tube furnace, feeds CO gas, beginning is warmed up to 200 ℃ with the speed of 2 ℃/min, and insulation 3h, is cooled to room temperature afterwards, prepares the sintered glass of ferri nano particle.
Embodiment 2: under room temperature environment, iron nitrate is dissolved in the water, compound concentration is 1 * 10
-1The iron nitrate aqueous solution 10mL of mol/L; Sintered glass is put into soaks 1h in the iron nitrate aqueous solution, take out sintered glass,, and be put into 90 ℃ oven drying 2h with distilled water flushing 3 times; Then sintered glass is put in the tube furnace, in tube furnace, feeds H
2Gas, beginning is warmed up to 150 ℃ with the speed of 3 ℃/min, and insulation 5h, is cooled to room temperature afterwards, prepares the sintered glass of ferri nano particle.
Embodiment 3: under room temperature environment, iron(ic)chloride is dissolved in the water, compound concentration is 1 * 10
-2The ferric chloride in aqueous solution 10mL of mol/L; Sintered glass is put into soaks 1h in the ferric chloride in aqueous solution, take out sintered glass,, and be put into 100 ℃ oven drying 2h with distilled water flushing 3 times; Then sintered glass is put in the tube furnace, in tube furnace, feeds N
2And H
2Volume ratio is 95: 5 a mixed gas, and beginning is warmed up to 500 ℃ with the speed of 3 ℃/min, and insulation 2h, is cooled to room temperature afterwards, prepares the sintered glass of ferri nano particle.
Embodiment 4: under room temperature environment, iron nitrate is dissolved in the ethanol, compound concentration is 1 * 10
-3The iron nitrate ethanolic soln 10mL of mol/L is put into sintered glass in the iron nitrate ethanolic soln and soaks 1.5h, takes out sintered glass, with distilled water flushing 3 times, and is put into 80 ℃ oven drying 3h; Then sintered glass is put in the tube furnace, in tube furnace, feeds CO gas, beginning is warmed up to 210 ℃ with the speed of 2 ℃/min, and insulation 3h, is cooled to room temperature afterwards, prepares the sintered glass of ferri nano particle.
Embodiment 5: under room temperature environment, iron(ic)chloride is dissolved in the water, compound concentration is 1 * 10
-4The ferric chloride in aqueous solution 10mL of mol/L; Sintered glass is put into soaks 2h in the ferric chloride in aqueous solution, take out sintered glass,, and be put into 120 ℃ oven drying 3h with distilled water flushing 3 times; Then sintered glass is put in the tube furnace, in tube furnace, feeds N
2And H
2Volume ratio is 95: 5 a mixed gas, and beginning is warmed up to 500 ℃ with the speed of 3 ℃/min, and insulation 1h, is cooled to room temperature afterwards, prepares the sintered glass of ferri nano particle.
Embodiment 6: under room temperature environment, iron(ic)chloride is dissolved in the water, compound concentration is 1 * 10
-5The ferric chloride in aqueous solution 10mL of mol/L; Sintered glass is put into soaks 2h in the ferric chloride in aqueous solution, take out sintered glass,, and be put into 85 ℃ oven drying 3h with distilled water flushing 3 times; Then sintered glass is put in the tube furnace, in tube furnace, feeds N
2And H
2Volume ratio is 95: 5 a mixed gas, and beginning is warmed up to 550 ℃ with the speed of 3 ℃/min, and insulation 2h, is cooled to room temperature afterwards, prepares the sintered glass of ferri nano particle; For the content that makes the contained Fe nanometer particles of sintered glass increases, can the aforesaid operations step be repeated 3 times.
Embodiment 7: under room temperature environment, iron nitrate is dissolved in the water, compound concentration is 1 * 10
-6The iron nitrate aqueous solution 10mL of mol/L; Sintered glass is put into soaks 2h in the iron nitrate aqueous solution, take out sintered glass,, and be put into 105 ℃ oven drying 3h with distilled water flushing 3 times; Then sintered glass is put in the tube furnace, in tube furnace, feeds N
2And H
2Volume ratio is 95: 5 a mixed gas, and beginning is warmed up to 450 ℃ with the speed of 3 ℃/min, and insulation 5h, is cooled to the sintered glass that room temperature preparation goes out the ferri nano particle afterwards; For the content that makes the contained Fe nanometer particles of sintered glass increases, can the aforesaid operations step be repeated 5 times.
The sintered glass of the prepared ferri nano particle that goes out of the foregoing description 1～7 is evenly distributed with Fe nanometer particles 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 (9)
1. the preparation method of the sintered glass of a ferri nano particle is characterized in that, comprises the steps:
Step 1: iron content ionic compound dissolution in solvent, is mixed with concentration range in 1mol/L～1 * 10
-6The iron content ion solution of mol/L;
Step 2: sintered glass is positioned in the iron content ion solution that step 1 prepares, after fully soaking, obtains parison;
Step 3: the resulting parison of step 2 is warmed up to 150 ℃～550 ℃, insulation 1h～5h, cool to room temperature is prepared the sintered glass of said ferri nano particle again;
Wherein, said iron content ionic compound is iron nitrate or iron(ic)chloride; Said solvent is water or ethanol.
2. the preparation method of the sintered glass of ferri nano particle as claimed in claim 1; It is characterized in that said step 2 is: sintered glass is positioned in the iron content ion solution that step 1 prepares, soaks more than the 0.5h; Take out sintered glass then; Clean sintered glass with zero(ppm) water, and be put into dry 2h～3h in 80 ℃～120 ℃ the baking oven, obtain said parison.
3. the preparation method of the sintered glass of ferri nano particle as claimed in claim 1; It is characterized in that; Said step 3 is: the prepared parison of step 2 is put into tube furnace under the environment of reducing atmosphere; Speed with 2 ℃～3 ℃/min is warmed up to 150 ℃～550 ℃, insulation 1h～5h, and cool to room temperature is prepared the sintered glass of said ferri nano particle again.
4. the preparation method of the sintered glass of ferri nano particle as claimed in claim 3 is characterized in that, said reducing atmosphere is CO, H
2, or N
2And H
2The atmosphere that exists of mixed gas.
5. the preparation method of the sintered glass of ferri nano particle as claimed in claim 1 is characterized in that, for the content that makes the contained Fe nanometer particles of sintered glass increases, said step 1～three can repeat.
6. the preparation method of the sintered glass of ferri nano particle as claimed in claim 1 is characterized in that, is distributed with micropore in the said sintered glass, and the pore size of micropore is 4～100 nanometers, and the volume of micropore accounts for 25～40% of glass TV.
7. the preparation method of the sintered glass of ferri nano particle as claimed in claim 1 is characterized in that, 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.
8. the sintered glass of a ferri nano particle; The preparation of employing the method for claim 1; It is characterized in that, comprising: the micropore of sintered glass and interior distribution thereof, the pore size of micropore are 4～100 nanometers; The volume of micropore accounts for 25～40% of glass TV, is evenly distributed with Fe nanometer particles in the micropore.
9. the sintered glass of ferri nano particle as claimed in claim 8 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910109550 CN101993201B (en) | 2009-08-10 | 2009-08-10 | Cellular glass containing iron nano particles and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910109550 CN101993201B (en) | 2009-08-10 | 2009-08-10 | Cellular glass containing iron nano particles and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101993201A CN101993201A (en) | 2011-03-30 |
| CN101993201B true CN101993201B (en) | 2012-03-28 |
Family
ID=43784028
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200910109550 Active CN101993201B (en) | 2009-08-10 | 2009-08-10 | Cellular glass containing iron nano particles and preparation method thereof |
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| Country | Link |
|---|---|
| CN (1) | CN101993201B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3867156A (en) * | 1972-02-21 | 1975-02-18 | Shikoku Kaken Kogyo Kk | Process for manufacturing granular foamed products of silica |
| CN1735562A (en) * | 2003-01-17 | 2006-02-15 | 西巴特殊化学品控股有限公司 | A process for the production of porous inorganic materials or a matrix material containing nanoparticles |
| CN1911845A (en) * | 2006-08-23 | 2007-02-14 | 陕西科技大学 | Preparation method of through hole foamed glass |
-
2009
- 2009-08-10 CN CN 200910109550 patent/CN101993201B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3867156A (en) * | 1972-02-21 | 1975-02-18 | Shikoku Kaken Kogyo Kk | Process for manufacturing granular foamed products of silica |
| CN1735562A (en) * | 2003-01-17 | 2006-02-15 | 西巴特殊化学品控股有限公司 | A process for the production of porous inorganic materials or a matrix material containing nanoparticles |
| CN1911845A (en) * | 2006-08-23 | 2007-02-14 | 陕西科技大学 | Preparation method of through hole foamed glass |
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| Publication number | Publication date |
|---|---|
| CN101993201A (en) | 2011-03-30 |
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