CN101676233B - Method for preparing block functional glass - Google Patents
Method for preparing block functional glass Download PDFInfo
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- CN101676233B CN101676233B CN2008102001732A CN200810200173A CN101676233B CN 101676233 B CN101676233 B CN 101676233B CN 2008102001732 A CN2008102001732 A CN 2008102001732A CN 200810200173 A CN200810200173 A CN 200810200173A CN 101676233 B CN101676233 B CN 101676233B
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Abstract
The invention relates to a process for preparing block functional glass, belonging to the technical field of block functional glass material preparation. The method for preparing the block functional glass comprises the following steps: (1) synthesizing a molecular sieve, a mesoporous or macroporous material, or a composite molecular sieve, a mesoporous or macroporous material containing rare-earth ion doping, semiconductor compounds or metal nanoparticles by adopting a chemical method; and (2) quickly sintering a powder body to prepare the block functional glass by taking the mesoporous or macroporous material as raw materials and adopting discharching plasma. The block functional glass prepared through the processes can play an important role in luminescent materials, information processing, integration, communication and other aspects.
Description
Technical field
The present invention relates to the preparation technology of block functional glass, belong to the block functional glass technical field of material.
Background technology
Glass is seen everywhere in daily life, for example building glass, glassware, mirror or the like, the functional glass of using from a lot of up till now fields of above-mentioned glass used in everyday, for example splinter-proof glass of fluorescent glass, fast-ionic conductor glass, strong mechanical performance, bio-vitric or the like.
Called function glass is meant by methods such as design chemical constitution, preparation technology and following process processes, obtains to have the glass of special physics, chemistry or biological property, distinguishes simple glass used in everyday.Functional glass can roughly be divided into seven classes according to the function that is had: optical functional glass, magnetic functional glass, mechanical function glass, chemical functional glass, electric work energy glass, biological function glass, hot merit energy glass.
The glass technology for making has 5000 years of development history, up to modern age in order to adapt to the development of military optical instrument, the originator Otto Schott of SCH OTT company has developed contemporary optics glass melting technology in 1884, since the first block of high-quality opticglass in the world that has produced, the glass preparation technology has had very big development, mainly contains traditional high melt technology, colloidal sol-gel technique, ion implantation, radio frequency sputtering method, CVD method and PCVD method etc.
High melt is that scorification is the most frequently used method, adopts usually raw material is prepared glass by high-temperature fusion and thermal treatment.But there is the problem that melt temperature is high and smelting time is long in scorification, causes the easy decomposition or the problems such as volatilization and crystallite dimension skewness such as semiconductor compound of mixing.Generally wait at present and alleviate the problem that the high-temperature fusion technology exists by the decomposition of selecting raw material, strict control fusion and inhibition semiconductor compounds such as thermal treatment process, interpolation inhibitor.Colloidal sol-gel technique is a common method of preparation nano material, owing to can avoid high-temperature operation, thus avoided volatilization, decomposition and the oxidation of semiconductor compound, so adopt this technology can prepare the semiconductor doping devitrified glass.It is the scope that how to enlarge the semiconductor nano compound that but sol-gel processing prepares the subject matter of semiconductor doping devitrified glass existence, so that select semiconductor microcrystallite.Ion implantation is to utilize to have the ion bombardment glass of kiloelectron volt to the million-electron-volt energy region, and wherein a part of ion is owing to glass is left in the reflection of glass, and another part ion is injected the top layer of glass, promptly so-called injection ion.Radio frequency sputtering method is to be sputtering source bombardment target with the argon ion, and target atom is sputtered out attached to basic surface.So the high melt technology is a main method for preparing block functional glass at present, but the problem of its existence also is conspicuous, for example the temperature height, energy consumption is big, the time is long, problem such as the function ingredients that causes adding volatilizees easily, decomposition, segregation.
Molecular sieve, mesoporous or large pore material are the novel porous materials of a class that occurs in recent years, its aperture is micropore (micropores) or molecular sieve (zeolite) less than 2nm, greater than 50nm is large pore material (macropores), and the aperture is commonly referred to as mesoporous material (mesopores) between 2nm and 50nm.Utilize the method for chemosynthesis can synthesize the assembling preparation and contain rare earth ion doped, semiconductor compound or nano metal particles composite molecular screen, mesoporous or large pore material, thereby realize new function such as photoelectricity.(SparkPlas ma Sintering-SPS) is nearly ten years a kind of new sintering technologies that occur to the discharge plasma sintering, have characteristics such as heat-up rate is fast, sintering temperature is low, sintering time is short, now become a kind of important sintering means, be successfully applied to preparation Functionally Graded Materials, biomaterial, nano material, Wimet, electromagnetic material etc.The present invention proposes to utilize discharge plasma Fast Sintering technology (SPS) sintering molecular sieve, mesoporous or large pore material, or contain rare earth ion doped, semiconductor compound or nano metal particles composite molecular screen, mesoporous or large pore material, can realize low temperature, quick, the generation of situations such as the function ingredients volatilization that inhibition is added, decomposition, prepare function bulk glass, set up a kind of preparation method or perhaps novel process of block functional glass with premium properties.
Summary of the invention
The object of the present invention is to provide a kind of worker who prepares block functional glass, it is characterized in that chemical process synthetic molecular sieve, mesoporous or large pore material, or contain rare earth ion doped, semiconductor compound or nano metal particles composite molecular screen, mesoporous or large pore material is a raw material, adopt discharge plasma Fast Sintering technology (SPS) then, prepare the function bulk glass with premium properties, this method has solved the problem that exists among the above-mentioned present preparation method.
Key problem in technology of the present invention is the chemical process synthesis of molecular sieve, mesoporous or large pore material, or contain rare earth ion doped, semiconductor compound or nano metal particles composite molecular screen, mesoporous or large pore material is a raw material, promptly come the design alternative raw material to form according to functional requirement, proportioning etc., utilize the chemical process synthesis of molecular sieve, mesoporous or large pore material, or contain rare earth ion doped, semiconductor compound or nano metal particles composite molecular screen, mesoporous or large pore material composite granule, then the synthetic powder is heat-treated, adopt discharge plasma Fast Sintering technology (SPS) sintering at last, main by control SPS sintering process parameter, comprise sintering temperature, pressure, temperature rise rate, soaking time etc., concrete enforcement can be divided into for two steps:
The preparation of the first step raw material composite granule
To adopt chemical process synthesis material powder, the rare earth ion that can select to contain according to the function needs can be Y, Gd, and La, Lu, Yb, Eu, Er, Dy, Pr, Tb, Sm, Ce, Nd, Ho, at least a among the Tm etc.; Semiconductor compound can be CdS, CdSeS
(1-x), ZnS, PbS, PbSe, Bi
2S
3, Sb
2S
3, CeO
2, ZnSe, ZnO, TiO
2Deng at least a; Nano metal particles can be at least a among Au, Ag, Cu, Pt, Pd, Ti, Nb, the Pb etc., utilizes that chemical process is mixed, assembling or compound, the synthesis material powder.With the synthetic composite granule, adopt a kind of in vacuum, inert atmosphere or the reducing atmosphere to heat-treat or do not heat-treat according to the characteristic of powder, thermal treatment temp is between 300～1200 ℃, and heat treatment time was at 1～6 hour.
The second step discharge plasma Fast Sintering (SPS)
This process is carried out under vacuum, inert atmosphere or reducing atmosphere, can select graphite jig for use.In sintering process, need strict control process parameters, comprise sintering temperature, pressure, temperature rise rate, soaking time etc.Wherein, sintering temperature and temperature rise rate are regulated by the size of pulsed current and voltage.The agglomerating temperature range is 500～1500 ℃; The temperature rise rate scope is 50～200 ℃/min; Pressure range is 10～100Mpa; The soaking time scope is 1～10 minute.
By the block functional glass of said process preparation, can play an important role at aspects such as luminescent material, information processing, integrated, communications, at aspects such as photomodulator, all-optical switch and optical storage extremely vast potential for future development is arranged.In the glass display of the semiconductor microcrystallite that contains nano-scale good optical non-linear.Generally speaking, the crystallite dimension that mixes in the semiconductor microcrystallite doped-glass is more little, and its optical nonlinearity polarizability is high more, and fast response time is short more.For example contain semi-conductor (semi-conductors such as ZnSe, CdS, PbS) quantum dot or devitrified glass, metal (Au, Ag, Ti, Nb, Pb etc.) Quantum Dot Glass etc.Rear-earth-doped long-afterglow luminescent glass can have important use in fields such as building, aviation, national defence, art decorations.Er doped silica glasses laser apparatus, up-conversion luminescent glass etc. have huge application potential in technical fields such as information demonstration, HIGH-DENSITY OPTICAL STORAGE, photoelectron and biologic medical diagnosis.The block functional glass preparation method that the present invention proposes can low temperature (well below the fusing point of glass), the short period of time (dozens of minutes even several minutes) prepares block functional glass, effectively avoids mixing problems such as volatilization in traditional preparation process glasswork pyroprocess such as semiconductor microcrystallite or quantum dot, metallics, rare earth ion, decomposition, skewness.Owing to can obtain high performance block functional glass, and the workability of glass basis, therefore adopt the preparation method or perhaps the novel process of this invention foundation, be easy to realize the transition process from the high performance material to the device, have using value.
Description of drawings
Fig. 1 is X light diffracting analysis (XRD) figure of embodiment 1;
Fig. 2 is fluorescence emission spectrum (PL) figure of embodiment 3;
Fig. 3 is fracture scanning electron microscope (SEM) photo of embodiment 6;
Embodiment
Embodiment 1
With the ZSM-5 molecular sieve is that the feedstock production silicate glass is an example.Earlier with the NaOH, white carbon black, the Al that mix
2(SO
4)
318H
2O and N aF calcine 20h at 5300C, adsorb quadrol then.Crystallization 100h under 1800C at last.After crystallization finishes, will still be the product washing of dry powder, heat-treat at 5500C and remove template.At last heat treated powder is packed into behind the graphite jig, put into SPS equipment and carry out sintering.The SPS preparation process is carried out under vacuum condition.Temperature rise rate is 100 ℃/min; Sintering temperature is 1300 ℃; Soaking time is 3min; Institute's applied pressure is 10MPa during sintering, and holding stage institute applied pressure is 50MPa.Prepared bulk glass XRD analysis result as shown in Figure 1.
Embodiment 2
To contain the adulterated silicate glass of 1.5at%Er is example.At first with Er
2O
3Join in the hydrochloric acid, then solution and molecular sieve powder are mixed, 75 ℃ are stirred down 2h, carry out the secondary ions exchange behind vacuum filtration, washing, vacuum filtration, heat-treat after overanxious, and thermal treatment temp is 500 ℃, and heat treatment time was at 1 hour.At last heat treated powder is packed into behind the graphite jig, put into SPS equipment and carry out sintering.The SPS preparation process is carried out under vacuum condition.Temperature rise rate is 100 ℃/min; Sintering temperature is 1350 ℃; Soaking time is 5min; Institute's applied pressure is 10M Pa during sintering, and holding stage institute applied pressure is 75MPa.Prepared bulk glass can be sent the fluorescence about 1.54 μ m at ambient temperature.
Embodiment 3
With the silicate glass that contains the 2.0at%Er/Yb codoped is example.At first with Er
2O
3/ Yb
2O
3(the certain atomic ratio of Er and Yb, for example be 1:1) join in rare nitric acid, then solution and molecular sieve powder are mixed, at magnetic agitation 3h, dropping ammonia, keep powerful the stirring in the dropping process, up to precipitation fully, continue to stir 50min, still aging 20h, heat-treat after overanxious through suction filtration, washing then, thermal treatment temp is 500 ℃, and heat treatment time is at 3h.At last heat treated powder is packed into behind the graphite jig, put into SPS equipment and carry out sintering.The SPS preparation process is carried out under vacuum condition.Temperature rise rate is 100 ℃/min; Sintering temperature is 1270 ℃; Soaking time is 5min; Institute's applied pressure is 10MPa during sintering, and holding stage institute applied pressure is 75MPa.Prepared bulk glass can be sent the fluorescence about 1.54 μ m at ambient temperature.
Embodiment 4
With the SBA-15 mesoporous material is that the feedstock production functional glass is an example.With tensio-active agent P123, distilled water, mixed in hydrochloric acid, the dissolving back adds tetraethoxy (TEOS) through stirring fully, 40 ℃ of stirred in water bath after 24 hours, resulting mixture is transferred in the stainless steel cauldron that liner is a tetrafluoroethylene, puts into baking oven and under 100 ℃ of conditions, reacted 50 hours.After filtration, washing, dry back removed tensio-active agent P123 in 5 hours 550 ℃ of thermal treatments, obtains the SBA-15 powder of white at last.The SBA-15 powder is packed into behind the graphite jig, put into SPS equipment and carry out sintering.The SPS preparation process is carried out under vacuum condition.Temperature rise rate is 100 ℃/min; Sintering temperature is 1000 ℃; Soaking time is 10min; Institute's applied pressure is 10MPa during sintering, and holding stage institute applied pressure is 50MPa.There are two luminescence peaks in prepared bulk glass, as shown in Figure 2 at ambient temperature simultaneously in 410nm～430nm scope.
Embodiment 5
With the 3%ZnS/MCM-41 complex mesoporous material is that the feedstock production functional glass is an example.Anhydrous Zn (CH with weighing
3COO)
2Be dissolved in dehydrated alcohol, after treating to dissolve fully, add the MCM-41 powder, violent stirring 5h places 130 ℃ of crystallization 10h of stainless steel cauldron with the mixed solution that obtains, and obtains the mesoporous assembled material of ZnO/MCM-41 of different ZnO contents.The mesoporous assembled material of synthetic ZnO/MCM-41 is placed in the tube furnace, under 120 ℃ of conditions, feeds hydrogen sulfide, carry out vulcanization reaction and prepare the mesoporous assembled material of ZnS/MCM-41.At last composite granule is packed into behind the graphite jig, put into SPS equipment and carry out sintering.The SPS preparation process is carried out under vacuum condition.Temperature rise rate is 100 ℃/min; Sintering temperature is 1000 ℃; Soaking time is 5min; Institute's applied pressure is 10MPa during sintering, and holding stage institute applied pressure is 100MPa.Prepared bulk glass sem analysis result as shown in Figure 3.
Embodiment 6
To contain the 1.5%CdS functional glass is example.With a certain amount of Cd (CH
3COO)
2Join in the methanol solution, after stirring dissolving fully, a certain amount of mesoporous powder is added in the solution, after stirring 10h, soak, again through after filtration, the drying, powder is placed in the tube furnace, under 120 ℃ of conditions, feeds hydrogen sulfide, carry out reduction reaction and prepare the mesoporous assembled material of CdS/SBA-15.At last composite granule is packed into behind the graphite jig, put into SPS equipment and carry out sintering.The SPS preparation process is carried out under vacuum condition.Temperature rise rate is 100 ℃/min; Sintering temperature is 1100 ℃; Soaking time is 3min; Institute's applied pressure is 10MPa during sintering, and holding stage institute applied pressure is 100MPa.There is luminous spectrum in prepared bulk glass at ambient temperature in 400nm～450nm scope.
Embodiment 7
To contain the 1.5%PbS functional glass is example.A certain amount of molecular sieve powder is joined AgNO
3In the solution, process stirs 10 backs and soaks about a week, through after filtration, the drying, powder is placed in the tube furnace again, feeds hydrogen under 300 ℃ of conditions, carries out reduction reaction and prepares the mesoporous assembled material of Ag/SBA-15.At last composite granule is packed into behind the graphite jig, put into SPS equipment and carry out sintering.The SPS preparation process is carried out under vacuum condition.Temperature rise rate is 100 ℃/min; Sintering temperature is 1100 ℃; Soaking time is 5min; Applied force is 10MPa during sintering, and holding stage institute applied pressure is 75MPa.
Embodiment 8
To contain the 1.0%Au functional glass is example.A certain amount of mesoporous powder is joined HAuCl
4In the solution, soak about a week, under 80 ℃ of temperature, add Trisodium Citrate stirring reaction 5h, again through filtering, after the drying, powder being placed on heat-treating the mesoporous assembled material of preparation Au/SBA-15 in the tube furnace through stirring 10 backs.At last composite granule is packed into behind the graphite jig, put into SPS equipment and carry out sintering.The SPS preparation process is carried out under vacuum condition.Temperature rise rate is 100 ℃/min; Sintering temperature is 1100 ℃; Soaking time is 5min; Applied force is 10MPa during sintering, and holding stage institute applied pressure is 75MPa.Third-order nonlinear susceptibility (the χ of prepared bulk glass
(3)) 10
-8～10
-12About the esu order of magnitude.
Embodiment 9
To contain the 0.5%Ag functional glass is example.A certain amount of SBA-15 powder is joined AgNO
3In the solution, process stirs 10 backs and soaks about a week, through after filtration, the drying, powder is placed in the tube furnace again, feeds hydrogen under 300 ℃ of conditions, carries out reduction reaction and prepares the mesoporous assembled material of Ag/SBA-15.At last composite granule is packed into behind the graphite jig, put into SPS equipment and carry out sintering.The SPS preparation process is carried out under vacuum condition.Temperature rise rate is 100 ℃/min; Sintering temperature is 1100 ℃; Soaking time is 5min; Applied force is 10MPa during sintering, and holding stage institute applied pressure is 75MPa.The time of response of prepared bulk glass is in picosecond level.
Claims (7)
1. the preparation method of block functional glass, this method comprises step:
(1) adopt chemical process syntheticly to contain rare earth ion doped, semiconductor compound composite molecular screen, mesoporous or large pore material is a material powder;
(2) adopt discharge plasma Fast Sintering powder preparing block functional glass.
2. by the preparation method of the block functional glass described in the claim 1, it is characterized in that described chemical process comprises sol-gel method, even coprecipitation method, microemulsion method, hydrothermal method, template, Organometallic Chemistry method, chemical gas-phase reaction method, chemical gas phase coacervation, spray pyrolysis, electrospinning weave.
3. by the preparation method of the block functional glass described in the claim 1, it is characterized in that described rare earth ion doped, semiconductor compound composite molecular screen, the mesoporous or large pore material of containing, the rare earth ion that wherein contains comprises Y, Gd, La, Lu, Yb, Eu, Er, Dy, Pr, Tb, Sm, Ce, Nd, Ho, at least a among the Tm; Semiconductor compound comprises CdS, CdSeS
(1-x), ZnS, PbS, PbSe, Bi
2S
3, Sb
2S
3, CeO
2, ZnSe, ZnO, TiO
2In at least a.
4. by the preparation method of the block functional glass described in the claim 1 or 2 or 3, it is characterized in that the synthetic material powder need be through Overheating Treatment, heat-treatment temperature range is at 300～1000 ℃.
5. by the preparation method of the block functional glass described in the claim 1 or 2 or 3, it is characterized in that synthetic contains rare earth ion doped, semiconductor compound composite molecular screen, mesoporous or large pore material comprises in crystalline phase or the amorphous phase at least a.
6. press the preparation method of the block functional glass described in the claim 1 or 2 or 3, it is characterized in that adopting discharge plasma raw materials for sintering powder, wherein temperature rise rate is 50～200 ℃/min in the discharge plasma sintering process, sintering temperature is 500～1400 ℃, pressure is 10～100MPa, and soaking time is 1～10 minute.
7. by the preparation method of the block functional glass described in the claim 1 or 2 or 3, when it is characterized in that adopting discharge plasma raw materials for sintering powder, adopt sintering under a kind of condition in vacuum, inert atmosphere or the reducing atmosphere.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104310784A (en) * | 2014-10-17 | 2015-01-28 | 东华大学 | Quantum dot LED light emitting glass and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP5749792B2 (en) * | 2010-04-22 | 2015-07-15 | オーシャンズ キング ライティング サイエンスアンドテクノロジー カンパニー リミテッド | Quantum dot / glass composite light emitting material and method for producing the same |
| CN103274597B (en) * | 2013-05-21 | 2015-08-12 | 东华大学 | The method of the near-infrared luminous glass of a kind of bismuth ion doped micropore molecular sieve |
| CN106588015A (en) * | 2016-12-23 | 2017-04-26 | 东华大学 | Method for preparing yttrium oxide ceramic based on mesoporous yttrium oxide |
| RU171679U1 (en) * | 2017-02-21 | 2017-06-09 | Автономная некоммерческая организация высшего образования "Белгородский университет кооперации, экономики и права" | DEVICE FOR OBTAINING BLOCK FOAM GLASS |
| CN114345401B (en) * | 2022-01-10 | 2023-06-02 | 万华化学集团股份有限公司 | Preparation method of p-hydroxyphenoxyethanol |
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| CN104310784A (en) * | 2014-10-17 | 2015-01-28 | 东华大学 | Quantum dot LED light emitting glass and preparation method thereof |
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