CN103359935A - Silver nano-doped tellurate glass and preparation method thereof - Google Patents
Silver nano-doped tellurate glass and preparation method thereof Download PDFInfo
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- CN103359935A CN103359935A CN2012100832757A CN201210083275A CN103359935A CN 103359935 A CN103359935 A CN 103359935A CN 2012100832757 A CN2012100832757 A CN 2012100832757A CN 201210083275 A CN201210083275 A CN 201210083275A CN 103359935 A CN103359935 A CN 103359935A
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- 239000011521 glass Substances 0.000 title claims abstract description 90
- XHGGEBRKUWZHEK-UHFFFAOYSA-L tellurate Chemical compound [O-][Te]([O-])(=O)=O XHGGEBRKUWZHEK-UHFFFAOYSA-L 0.000 title claims abstract description 58
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 53
- 239000004332 silver Substances 0.000 title claims abstract description 53
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 15
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002105 nanoparticle Substances 0.000 claims description 46
- 239000000203 mixture Substances 0.000 claims description 12
- 238000002844 melting Methods 0.000 claims description 11
- 230000008018 melting Effects 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- 101710134784 Agnoprotein Proteins 0.000 claims description 9
- 238000000137 annealing Methods 0.000 claims description 8
- OVMJVEMNBCGDGM-UHFFFAOYSA-N iron silver Chemical compound [Fe].[Ag] OVMJVEMNBCGDGM-UHFFFAOYSA-N 0.000 claims description 8
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 7
- 229910001882 dioxygen Inorganic materials 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 238000010583 slow cooling Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229940100890 silver compound Drugs 0.000 claims description 2
- 150000003379 silver compounds Chemical class 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 230000004044 response Effects 0.000 abstract description 22
- 239000000463 material Substances 0.000 abstract description 12
- 239000005304 optical glass Substances 0.000 abstract description 5
- -1 silver ion compound Chemical class 0.000 abstract description 4
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract 1
- 229910003069 TeO2 Inorganic materials 0.000 abstract 1
- 238000010309 melting process Methods 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 description 19
- 238000012360 testing method Methods 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 238000004891 communication Methods 0.000 description 7
- 239000011734 sodium Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 230000009022 nonlinear effect Effects 0.000 description 6
- 239000002082 metal nanoparticle Substances 0.000 description 5
- 229910000510 noble metal Inorganic materials 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 238000002156 mixing Methods 0.000 description 3
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 150000003378 silver Chemical class 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000005365 phosphate glass Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
The invention relates to silver nano-doped tellurate glass and a preparation method thereof, wherein the silver nano-doped tellurate glass is prepared from 65-90 mol% of TeO25 to 25 mol% of ZnO, 1 to 20 mol% of Na2O and silver ion compound with the mass percentage concentration of 2-10 percent. The invention provides the tellurate glass doped with silver nano-particles, which has simple melting process and can obtain the optical glass material with high nonlinearity and high response time according to the principle that the silver nano-particles are doped with silver and have better physical propertiesAnd a method for preparing the same.
Description
Technical field
The invention belongs to optical field, relate to a kind of glass and preparation method thereof, relate in particular to tellurate glass that a kind of silver nanoparticle for non-linear optical field mixes and preparation method thereof.
Background technology
In the development of photon technology, the raising of data rate is very crucial problem.Switch with Tbit/s transmission speed is the key of mechanics of communication of future generation, and such communication speed is very difficult for electron device.All-optical switch as the Primary Component of Tbit/s communication in future, need to have the nonlinear material of high non-linearity and fast time of response.Noble metal nano particles, such as gold and silver and copper, caused people for they the huge interest as the all-optical switch material, this is because when their doping enter the substrate material the inside, have very large non-linearly, time of response of Ps magnitude is arranged simultaneously.Because the response type of noble metal nano particles is non-linear, the non-linear of the glass that noble metal nano particles mixes can strengthen at surface plasma body resonant vibration wavelength place seven orders of magnitude.
In the exploratory stage of highly-nonlinear material, glass is extensively selected, and mainly is because they have the higher time of response.In present research, be used for the glass matrix of doped precious metal nano particle to be limited in traditional silicate, phosphate glass the inside.Yet they are but facing to non-linear or relatively low problem.According to the Miller rule, there is the glass of higher linear refractive index to have than higher non-linear of traditional glass.But the glass of high refractive index itself also possesses a lot of shortcomings, such as frangible, can not see through at visible light part, is difficult for bulk processing etc., so select the glass of suitable high refractive index to become a developing direction.
In the melting technology of the non-linear glass of research, how preparing suitable glass is crucial part, the process of founding, and the temperature and time of the return of goods all exerts an influence to last result.So select suitable melting technology, become important content in the materials preparation.
Summary of the invention
In order to solve the above-mentioned technical problem that exists in the background technology, the present invention provides a kind of melting technology tellurate glass that silver nanoparticle simple, that can obtain high non-linearity and high time of response optical glass material is mixed and preparation method thereof according to the silver nanoparticle principle with better physical properties of mixing.
Technical solution of the present invention is: the invention provides the tellurate glass that a kind of silver nanoparticle is mixed, its special character is: the tellurate glass that described silver nanoparticle is mixed is the TeO by 65～90mol%
2, the ZnO of 5～25mol%, the Na of 1～20mol%
2O and mass percent concentration are that 2%～10% silver iron compound is prepared from.
The tellurate glass that above-mentioned silver nanoparticle is mixed is the TeO by 70～85mol%
2, the ZnO of 10～23mol%, the Na of 2～15mol%
2O and mass percent concentration are that 3%～9% silver iron compound is prepared from.
The tellurate glass that above-mentioned silver nanoparticle is mixed is the TeO by 72～82mol%
2, the ZnO of 18～20mol%, the Na of 2～5mol%
2O and mass percent concentration are that the silver iron compound of 5wt%～8wt% is prepared from.
Above-mentioned silver compound is AgNO
3, AgCl, Ag
2SO
4, Ag
2CO
3, Ag
3PO
4, Ag
2Other introduce the compound of silver ions O or AgI etc.
The preparation method of the tellurate glass that a kind of silver nanoparticle is mixed, its special character is: said method comprising the steps of:
1) according to proportioning raw materials raw material is mixed; Described raw material comprises TeO
2, ZnO, Na
2O is with silver iron compound;
3) with step 1) resulting mixture founds;
4) annealing;
5) heat-treat the tellurate glass sample that obtains the silver nanoparticle doping after the cooling.
The preparation method of the tellurate glass that above-mentioned silver nanoparticle is mixed is in step 1) and step 3) between also comprise:
2) to step 1) raw mix that obtains carries out physics and dewaters.
Above-mentioned steps 2) specific implementation is:
2.1) under vacuum environment, raw mix heated stage by stage dewater, be used for removing the moisture on chemical surface;
2.2) with step 2.1) carry out under the condition of the dry high purity oxygen gas of the raw material rapid moving excess of imports after the vacuum-drying and positive high voltage, and in 200～400 ℃ of scopes, carry out the gradient increased temperature drying, be used for removing most of mechanical water molecule of chemical inside;
The condition of described vacuum environment is: the vacuum environment of 1～2Pa; The condition of described super dry high purity oxygen gas is P 〉=4N and H
2The super dry high purity oxygen gas condition of O≤2ppm; The condition of described positive high voltage is 4～12kPa positive high voltage.
Above-mentioned steps 3) specific implementation is: be warming up to 800～900 ℃, melting time is founded and is passed into high purity oxygen in the process always for being not less than 3 hours, under the condition of positive high voltage 4～12kPa, and the glass metal that obtains melting.
Above-mentioned steps 4) specific implementation is: with step 3) in the quick placement of glass metal that melts be warmed up in 220～260 ℃ the annealing furnace, be incubated after three hours, slow cooling is to room temperature, the glass of tentatively being made.
Above-mentioned steps 5) specific implementation is: the glass that will tentatively make slowly is warmed up in 260～295 ℃ the annealing furnace, is incubated after 3～12 hours, and slow cooling obtains the tellurate glass that silver nanoparticle is mixed to room temperature.
Advantage of the present invention is:
1, can prepare the optical glass material that has uniformly than high non-linearity.High non-linear of the present invention's non-linear and tellurate glass that just noble metal nano particles is high first combines to prepare the optical glass material that has than high non-linearity, its nonlinear refractive index strengthens 27 times than conventional quartz, strengthens 3 times than common tellurate glass.
2, can prepare the optical glass material that has uniformly the very fast time of response.Because the time of response that noble metal nano particles has the ps level, and the time of response of tellurate glass material itself also can reach the ps magnitude, the time of response that the tellurate glass liquid that silver nanoparticle is mixed also has the ps level, this communication for T bit/s level is suitable.On high nonlinear basis, corresponding time shorten.
3, preparation method of the present invention is simple, and is effective.The present invention and other ion implantation, the modes such as solution infiltration are compared, doping content is large, the preparation method is easy, preparation cycle is short, for commercialization provide preferably early stage condition.
Description of drawings
Fig. 1 is the making schema of the tellurate glass of silver nanoparticle doping provided by the present invention;
Fig. 2 is physics dewatering process and the glass melting temperature graphic representation of the tellurate glass of silver nanoparticle doping provided by the present invention;
Fig. 3-the 1st, the 17th embodiment of tellurate glass provided by the present invention is at the absorption figure of visible light wave range;
Fig. 3-the 2nd, the 17th embodiment of tellurate glass provided by the present invention is in the non-linear test result at 800nm place;
Fig. 4-the 1st, the 18th embodiment of tellurate glass provided by the present invention is at the absorption figure of visible light wave range;
Fig. 4-the 2nd, the 18th embodiment of tellurate glass provided by the present invention is in the non-linear test result at 800nm place;
Fig. 5-the 1st, the 7th embodiment of tellurate glass provided by the present invention is at the absorption figure of visible light wave range;
Fig. 5-the 2nd, the 7th embodiment of tellurate glass provided by the present invention is in the non-linear test result at 1500nm place;
Fig. 6-the 1st, the 9th embodiment of tellurate glass provided by the present invention is at the absorption figure of visible light wave range;
Fig. 6-the 2nd, the 9th embodiment of tellurate glass provided by the present invention is in the non-linear test result at 1500nm place;
Fig. 7 is the 7th embodiment and near the relatively traditional nonlinear enhancing synoptic diagram of silica glass 1500nm of the 9th embodiment of tellurate glass provided by the present invention.
Embodiment
The invention provides the tellurate glass that a kind of silver nanoparticle is mixed, the component of the tellurate glass that this silver nanoparticle is mixed comprises: the TeO of 65～90mol%
2, the ZnO of 5～25mol%, the Na of 3～20mol%
2Mix the in addition AgNO of 2wt%～10wt% of O
3Be prepared from.
The TeO of the component 68～86mol% of the tellurate glass that silver nanoparticle is mixed
2, 7～22mol% ZnO with the Na of 5～15mol%
2Mix the in addition AgNO of 3wt%-9wt% of O
3Be prepared from.
The component of the tellurate glass that silver nanoparticle is mixed comprises the TeO of 70～85mol%
2, 8～19mol% ZnO, the Na of 6～14mol%
2Mix the in addition AgNO of 5wt%-8wt% of O
3Be prepared from.
Silver ions herein, the doping way of sodium ion can be other variety of ways, for example can be Silver Nitrate, silver chloride etc., as long as can add silver ions and the sodium ion of equivalent, all be considered as repeating the proportioning implementation when following table is the silver-doped ion under the selected different mass percentage concentration with the present invention:
Referring to Fig. 1, in the tellurate glass that the invention provides a kind of silver nanoparticle doping, also provide the preparation method of the tellurate glass of this silver nanoparticle doping, the method may further comprise the steps:
1) according to the proportioning raw materials relation raw material is mixed;
Referring to Fig. 2, be physics dewatering process and the glass melting temperature graphic representation that the present invention adopts; 2) to step 1) raw mix that obtains carries out physics and dewaters, and this physics dewaters and comprises two aspects:
2.1) under 1～2Pa vacuum environment, raw mix heated stage by stage dewater, being used for removing the moisture on chemical surface, this is the first step that physics dewaters, and also is the simplest step;
2.2) with step 2.1) carry out the excess of imports of raw material rapid moving dry high purity oxygen gas (P 〉=4N and H after the vacuum-drying
2Under the condition of O≤2ppm) and 4～12kPa positive high voltage, and carry out the gradient increased temperature drying in 200～400 ℃ of scopes, be used for removing most of mechanical water molecule of chemical inside, this is the second step that physics dewaters;
3) be warmed up to 800～900 ℃, melting time is founded and is passed into high purity oxygen in the process always for being not less than 3 hours, under the condition of positive high voltage 4～12kPa, and the glass metal that obtains melting.
4) glass metal that melts is poured on the mould that is preheating to 200 ℃, put into fast and be warmed up to 220～260 ℃ annealing furnace, be incubated after three hours, slow cooling is to room temperature.The glass of tentatively being made.
5) heat-treated after the cooling.The glasswork of tentatively making put into be preheating on the mould, slowly be warmed up in 260～295 ℃ the annealing furnace, be incubated after 3～12 hours, slow cooling is to room temperature.Obtain the tellurate glass that silver nanoparticle is mixed.
Absorption figure and non-linear test result referring to Fig. 3-Fig. 5 tellurate glass visible light wave range that to be the present invention mix according to different proportionings and the different silver nanoparticles of utilizing method provided by the present invention to form, the solid evidence that the absorption figure of visible light wave range forms and exists as silver nanoparticle, wherein, among Fig. 3, be absorption figure and the non-linear test result of the present invention's the 17th embodiment visible light wave range, glass ingredient is 6.0Ag-TZN78 (78TeO
2-14ZnO-8Na
2O (mol%)+6.0wt%AgNO
3Abbreviation).Can see that glass has absorption peak at visible light wave range, peak value is at the 553nm place, and the absorption peak of this position is regarded as the evidence that silver nanoparticle exists.The non-linear result that Fig. 3-2 records for the method for 6.0Ag-TZN78 sample by the Ke Er signal, nonlinear test result sees that the nonlinear properties strength ratio of 6.0Ag-TZN78 is about 100 times of silica glass, and nonlinear refractive index is converted into 17.2 times of silica glass.And the time of response is the full width at half maximum of nonlinear properties, is calculated as 256.2fs, this time of response that represents this sample at 256.2fs with interior (the tested person condition influence can not be more accurate).The so fast time of response is so that the application of photoswitch becomes possibility.
Fig. 4 is the present invention the 18th embodiment 7.0Ag-TZN78 (78TeO
2-14ZnO-8Na
2O (mol%)+6.0wt%AgNO
3Abbreviation) absorption figure and the non-linear test result of the tellurate glass visible light wave range that mixes of silver nanoparticle; Can see that glass has absorption peak at visible light wave range, peak value is at the 553nm place, and the absorption peak of this position is regarded as the evidence that silver nanoparticle exists.The non-linear result that Fig. 4-2 records for the method for 7.0Ag-TZN78 sample by the Ke Er signal, nonlinear test result sees that the nonlinear properties strength ratio of 7.0Ag-TZN78 is about 100 times of silica glass, and nonlinear refractive index is converted into 18.1 times of silica glass.And the time of response is the full width at half maximum of nonlinear properties, is calculated as 246fs, this time of response that represents this sample at 246fs with interior (the tested person condition influence can not be more accurate).The so fast time of response is so that the application in the ultrafast optical communication becomes possibility.
Fig. 5 is the present invention the 7th embodiment 5.0Ag-TZN75 (75TeO
2-20ZnO-5Na
2O (mol%)+5.0wt%AgNO
3Abbreviation) absorption figure and the non-linear test result of the tellurate glass visible light wave range that mixes of silver nanoparticle; Can see that glass has absorption peak at visible light wave range, peak value is at the 553nm place, and the absorption peak of this position is regarded as the evidence that silver nanoparticle exists.The non-linear result that Fig. 5-2 records for the method for 5.0Ag-TZN78 sample by four-wave mixing, the nonlinear refractive index of nonlinear test result 5.0Ag-TZN78 is 17.5 times of silica glass.And the time of response is the full width at half maximum of nonlinear properties, is calculated as 1.0839Ps, and this time of response that represents this sample is 1.0839Ps (the tested person condition influence can not be more accurate).The so fast time of response is so that the application in the ultrafast optical communication becomes possibility.
Fig. 6 is absorption figure and the non-linear test result of the tellurate glass visible light wave range that mixes of the silver nanoparticle of the present invention the 9th embodiment; 7.5Ag-TZN75 (75TeO
2-20ZnO-5Na
2O (mol%)+7.5wt%AgNO
3Abbreviation) absorption figure and the non-linear test result of the tellurate glass visible light wave range that mixes of silver nanoparticle; Can see that glass has absorption peak at visible light wave range, peak value is at the 553nm place, and the absorption peak of this position is regarded as the evidence that silver nanoparticle exists.The non-linear result that Fig. 6-2 records for the method for 7.5Ag-TZN78 sample by four-wave mixing, the nonlinear refractive index of nonlinear test result 7.5Ag-TZN78 is 27 times of silica glass.And the time of response is the full width at half maximum of nonlinear properties, is calculated as 0.9805Ps, and this time of response that represents this sample is 0.9805Ps (the tested person condition influence can not be more accurate).The so fast time of response is so that the application in the ultrafast optical communication becomes possibility.
Fig. 7 be among the 7 9th embodiment glass in the contrast of non-linear and silica glass and the TZN75 glass of 1500nm vicinity, can see that from figure the non-linear relative silica glass of glass can improve about 30 times, and with respect to general TZN75 glass, also have significantly improved, the material of the high non-linearity that this expression the present invention obtains has very large advantage.
Foregoing only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (10)
1. the tellurate glass that mixes of a silver nanoparticle, it is characterized in that: the tellurate glass that described silver nanoparticle is mixed is the TeO by 65～90mol%
2, the ZnO of 5～25mol%, the Na of 1～20mol%
2O and mass percent concentration are that 2%～10% silver iron compound is prepared from.
2. the tellurate glass that mixes of silver nanoparticle according to claim 1, it is characterized in that: the tellurate glass that described silver nanoparticle is mixed is the TeO by 70～85mol%
2, the ZnO of 10～23mol%, the Na of 2～15mol%
2O and mass percent concentration are that 3%～9% silver iron compound is prepared from.
3. the tellurate glass that mixes of silver nanoparticle according to claim 2, it is characterized in that: the tellurate glass that described silver nanoparticle is mixed is the TeO by 72～82mol%
2, the ZnO of 18～20mol%, the Na of 2～5mol%
2O and mass percent concentration are that the silver iron compound of 5wt%～8wt% is prepared from.
4. according to claim 1 and 2 or the tellurate glass that mixes of 3 described silver nanoparticles, it is characterized in that: described silver compound is AgNO
3, AgCl, Ag
2SO
4, Ag
2CO
3, Ag
3PO
4, Ag
2O or AgI.
5. the preparation method of a tellurate glass that mixes based on the described silver nanoparticle of the arbitrary claim of claim 1-4 is characterized in that: said method comprising the steps of:
1) according to the described proportioning raw materials of arbitrary claim among the claim 1-4 raw material is mixed; Described raw material comprises TeO
2, ZnO, Na
2O is with silver iron compound;
3) with step 1) resulting mixture founds;
4) annealing;
5) heat-treat the tellurate glass sample that obtains the silver nanoparticle doping after the cooling.
6. the preparation method of the tellurate glass that mixes of silver nanoparticle according to claim 5, it is characterized in that: the preparation method of the tellurate glass that described silver nanoparticle is mixed is in step 1) and step 3) between also comprise:
2) to step 1) raw mix that obtains carries out physics and dewaters.
7. the preparation method of the tellurate glass that mixes of silver nanoparticle according to claim 6, it is characterized in that: specific implementation described step 2) is:
2.1) under vacuum environment, raw mix heated stage by stage dewater, remove the moisture on chemical surface;
2.2) with step 2.1) carry out under the condition of the dry high purity oxygen gas of the raw material rapid moving excess of imports after the vacuum-drying and positive high voltage, and in 200～400 ℃ of scopes, carry out the gradient increased temperature drying, remove most of mechanical water molecule of chemical inside;
The condition of described vacuum environment is: the vacuum environment of 1～2Pa; The condition of described super dry high purity oxygen gas is P 〉=4N and H
2The super dry high purity oxygen gas condition of O≤2ppm; The condition of described positive high voltage is 4～12kPa positive high voltage.
8. according to claim 5 or the preparation method of the tellurate glass that mixes of 6 or 7 described silver nanoparticles, it is characterized in that: specific implementation described step 3) is: be warming up to 800～900 ℃, melting time is for being not less than 3 hours, found and pass into high purity oxygen in the process always, under the condition of positive high voltage 4～12kPa, the glass metal that obtains melting.
9. the preparation method of the tellurate glass that mixes of silver nanoparticle according to claim 8, it is characterized in that: specific implementation described step 4) is: with step 3) in the quick placement of glass metal that melts be warmed up in 220～260 ℃ the annealing furnace, be incubated after three hours, slow cooling is to room temperature, the glass of tentatively being made.
10. the preparation method of the tellurate glass that mixes of silver nanoparticle according to claim 9, it is characterized in that: specific implementation described step 5) is: the glass that will tentatively make slowly is warmed up in 260～295 ℃ the annealing furnace, be incubated after 3～12 hours, slow cooling obtains the tellurate glass that silver nanoparticle is mixed to room temperature.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104230168A (en) * | 2014-08-28 | 2014-12-24 | 华南理工大学 | Preparation method of transparent nanocrystal doped glass |
| CN106630655A (en) * | 2016-09-29 | 2017-05-10 | 中国科学院理化技术研究所 | High-transparency composite optical glass doped with stibene nano material and application |
| CN116375343A (en) * | 2023-03-28 | 2023-07-04 | 华南理工大学 | Silver-containing nanoparticle tellurate photo-functional glass ceramic material with photoinduced resistance enhancement characteristic, and preparation method and application thereof |
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|---|---|---|---|---|
| CN101219857A (en) * | 2008-01-30 | 2008-07-16 | 中国科学院上海光学精密机械研究所 | Tellurate glass and preparation method thereof |
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| CN106630655B (en) * | 2016-09-29 | 2019-04-05 | 中国科学院理化技术研究所 | High-transparency composite optical glass doped with stibene nano material and application |
| CN116375343A (en) * | 2023-03-28 | 2023-07-04 | 华南理工大学 | Silver-containing nanoparticle tellurate photo-functional glass ceramic material with photoinduced resistance enhancement characteristic, and preparation method and application thereof |
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