CN1063774C - Prepn of in-situ synthetic inorganic metal base organic composite optical function material - Google Patents
Prepn of in-situ synthetic inorganic metal base organic composite optical function material Download PDFInfo
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- CN1063774C CN1063774C CN96107833A CN96107833A CN1063774C CN 1063774 C CN1063774 C CN 1063774C CN 96107833 A CN96107833 A CN 96107833A CN 96107833 A CN96107833 A CN 96107833A CN 1063774 C CN1063774 C CN 1063774C
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Abstract
The present invention discloses a preparation method of a compound light function material of an inorganic base metallic organic coordination compound synthesized in situ. The present invention is characterized in that the required metallic organic coordination compound is synthesized in situ in the organic-inorganic nanometer compound process or in the formation process of inorganic gel or in subsequent processing processes; the dispersing and the compounding of the metallic organic coordination compound in an inorganic base material in nanometer level are achieved to prepare the inorganic base compound light function material. The present invention can decrease the absorption loss of the base material to pumping light, enhance the effective doping concentration of organic optical active substances in the inorganic base material in large amplitude, enhance quenching concentration by one order of magnitude, and enhance light function performance and service life.
Description
The present invention relates to a kind of in-situ synthetic inorganic metal base organic composite optical function material preparation method.
In recent years, along with the fast development of modern high technology,, and be subjected to countries in the world and greatly pay attention to as a new branch of science in the information science---" photon and photoelectronics " emerges.It will make and utilize the electric field controls electrical signal to an electric optical modulation and light one optical modulation development in the electronics, thereby overcome the restriction of " electronic bottleneck " of conditional electronic technology, realization is based on the ultrafast full optical information processing of photoelectron technology, and this is the another new great leap of information technology.Therefore, the laser in the Materials science, light demonstration and nonlinear optical material have become most important photon and photoelectronics material.Except gas and liquid-dye laser, the laser of practicability, light demonstration and nonlinear optical material all are mineral crystal basically, as gallium arsenide, quartz, potassium primary phosphate (KDP), Lithium niobium trioxide etc. but up to now.
The electron delocalization degree height of some organic compound, its luminous efficiency and second order, third-order non-linear coefficient are all much higher than inorganic materials, higher electro-optic coefficient, super fast response time are arranged, to environment sensitive and good building-up properties be easy to characteristics such as low-dimensionalization.A metal-organic complex is the important optically active substance of a class, particularly as highly efficient luminous substance, understands for people more for a long time.Early sixties, people such as American scholar H.J.Scimitschek find that rare earth-beta diketone title complex can produce laser effect in solution, are the upsurge of the visible waveband laser apparatus of working-laser material with research rare earth-beta diketone title complex for a moment thereby start.But very fast people absorbed strong owing to organism to pump light with regard to discovery and the organic group vibration causes that the nonradiative transition power loss is excessive, thereby there are two shortcomings that are difficult to overcome in the laser apparatus made from it, and promptly laser threshold is too high and need work down and can't practicability at＜100K low temperature.From the eighties initial stage, along with going deep into of organic optical function material research, all kinds of have the organic of excellent in performance and polymkeric substance optical function material report arranged successively, many challenging new developments have been obtained, make organic materials demonstrate the advantage of performance and wide potential application day by day, attracted the extensive concern and the intervention of various countries academia and industry member.But compare with inorganic materials, organic materials and device be because its material structure stability and data are repeatable poor, and low and life-span of working temperature limits it and moves towards practicability than shortcoming such as weak point.
Since the nineties, people begin to utilize sol-gel (sol-gel) wet-chemical technique, it is compound that organic photoactive species and inorganic matrix are carried out homodisperse, may have the research of the composite optical function material of organic and inorganic materials characteristic concurrently with preparation, and obtain some progress.For example, compound with various organic dye and inorganic gel glass, in the hope of obtaining can be used as (R.Reisfeld:Optical Materials, 4 (1994) 1-3 etc.) such as full curing, tunable laser operation material and inorganic based composite non-linear optical materials.But relevant organic inorganic compounding optical function material technology of preparing both at home and abroad of report mostly is so-called pre-the doping (pre-doped) and back doping (post-doped) two kinds of methods of employing so far.The former after pure dissolubility or water miscible organic photoactive species are made specific pioneer's liquid, directly is dispersed in the inorganic matrix, utilizes the so-gel technology to make the composite solid material; The latter is dissolved in superpolymer or monomer with organic photoactive species, utilize impregnation technology to make it directly to immerse and filling in porous, inorganic matrix.These two kinds of methods all exist essential defective and limitation, with dipping (then mix) technology prepared come down to a kind of composite diphase material, owing to existing tangible interface to influence its optical homogeneity.And for those in alcohol or water insoluble and under the sol-gel processing condition unsettled organic photoactive species, then can not adopt traditional sol-gel technology to prepare the uniform inorganic based composite optical function material of optics.For example, a metal-organic complex of great majority with outstanding smooth functional performance will produce decomposition and be difficult to realize and mix under traditional sol-gel processing condition.At this problem of solvent medium, for many years, carrying out extensive work aspect the research and development polymer-based carbon optical function material, but still failing to overcome the key issue that existing stability of organic materials and circulation ratio etc. influence its practicability.
The purpose of this invention is to provide a kind of in-situ synthetic inorganic metal base organic composite optical function material preparation method.
Be illustrated below in conjunction with embodiment
The present invention provides a kind of improved so-gel (sol-gel) technology, its major technique characteristics are, in organic one inorganic nano combined process, make required a metal-organic complex in no face gel formation process or its position, last handling process Central Plains synthetic, reach the nanoscopic level dispersion of a metal-organic complex in inorganic matrix and compound, with the new technology of preparation inorganic based composite optical function material, develop novel nano combined luminous, the demonstration of a class and nonlinear optical material and device thereof.The present invention includes: pioneer's fluid component design and preparation method thereof; The method of the synthetic a metal-organic complex of original position in the so-gel process; The method of an organic inorganic compounding xerogel synthetic a metal-organic complex of original position in the control heat treatment process.
1. pioneer's fluid component design and preparation thereof: select inorganic salt (as the phosphoric acid salt of sodium, barium, titanium, vanadium etc., borate, nitrate etc.) or mineral acid (as phosphoric acid, boric acid etc.) or metal alkoxide (as tetraethoxy, tetramethoxysilance, butyl (tetra) titanate, sodium methylate etc.) as precursor, water-soluble and organic solvent, under 20 ℃～90 ℃ temperature, acid catalysis and intense agitation, through hydrolysis one polycondensation, obtain uniform inorganic matrix so-gel pioneer liquid.
2. original position is synthesized a metal-organic complex in the sol-gel process: the aqueous solution and the organic ligand solution that add metal (transition metal or rare earth) salt in sol-gel pioneer liquid, pioneer's liquid is formed (molar fraction): inorganic salt (as the phosphoric acid salt of sodium, barium, titanium, vanadium etc., borate, nitrate etc.) or mineral acid (as phosphoric acid, boric acid etc.) or metal alkoxide (as tetraethoxy, methyl silicate, butyl (tetra) titanate, sodium methylate etc.) 5-20, organic solvent 25-50, deionized water 30-55.Organic ligand is respectively 0.2～2.0mol% and 0.1-1.0mol% with the central metal ion add-on of title complex (molar fraction of relative inorganic gel glass matrix).It is 1.0～6.5 with the pH value that the temperature of regulating mixed solution is 20 ℃～90 ℃, mixing the back leaves standstill under 30 ℃ of-80 ℃ of environment, through 3-15 days dryings, make the transparent and uniform composite xerogel, make a metal-organic complex original position in the mixed system gelation process synthetic, make the uniform composite optical function material of optics.
3. original position is synthesized a metal-organic complex in the xerogel heat treatment process: the aqueous solution and the organic ligand solution that add metal (transition metal or rare earth) salt in sol-gel pioneer liquid, pioneer's liquid is formed (molar fraction): inorganic salt (as the phosphoric acid salt of sodium, barium, titanium, vanadium etc., borate, nitrate etc.) or mineral acid (as phosphoric acid, boric acid etc.) or metal alkoxide (as tetraethoxy, methyl silicate, butyl (tetra) titanate, sodium methylate etc.) 5-15, organic solvent 35-50, deionized water 30-45.Organic ligand is respectively 0.2-1.5mol% and 0.3-0.8mol% with the central metal ion add-on of title complex (molar fraction of relative inorganic gel glass matrix).The temperature of regulating mixed solution is 20-90 ℃ and pH value 1.0-6.0, mixes the back and leaves standstill under 30 ℃ of-80 ℃ of environment, through 3-15 days dryings, makes the transparent and uniform composite xerogel.Xerogel heats up with 20 ℃ of-40 ℃ of/hour speed, heat-treats successively through 90 ℃-300 ℃, makes a metal-organic complex original position in the inorganic gel glass matrix synthetic, makes the uniform composite optical function material of optics.
Original position synthesizing inorganic Base Metal machine title complex composite luminescent material can prepare as follows:
1. pioneer's fluid component design and preparation thereof: select inorganic salt (as the phosphoric acid salt of sodium, barium, titanium, vanadium etc., borate, nitrate etc.) or mineral acid (as phosphoric acid, boric acid etc.) or metal alkoxide (as tetraethoxy, methyl silicate, butyl (tetra) titanate, sodium methylate etc.) as precursor, water-soluble and organic solvent (as alcohol, acetone etc.), under 20 ℃ of-90 ℃ of temperature, acid catalysis and intense agitation, through hydrolysis-condensation reaction, obtain uniform inorganic matrix sol-gel pioneer liquid.
2. original position is synthesized a metal-organic complex in the sol-gel process: add metal (transition metal or rare earth) salt brine solution and organic ligand solution in sol-gel pioneer liquid, pioneer's liquid is formed (molar fraction): inorganic salt (as the phosphoric acid salt of sodium, barium, titanium, vanadium etc., borate, nitrate etc.) or mineral acid (as phosphoric acid, boric acid etc.) or metal alkoxide (as tetraethoxy, methyl silicate, butyl (tetra) titanate, sodium methylate etc.) 8-15, organic solvent (as alcohol, acetone etc.) 35-45, deionized water 35-45.The add-on (molar fraction of relative inorganic gel glass matrix) of the central metallic ions (as transition metal ion or rare earth ions such as manganese, chromium, titanium, zinc) of organic ligand (as carboxylic acid, beta diketone and various Lewis bases etc.) and title complex is respectively 0.5-1.5mol% and 0.4-0.7mol%.It is 1.0-6.5 with the pH value that the mixed degree of regulating mixed solution is 20 ℃-90 ℃, mixing the back leaves standstill under 30 ℃ of-70 ℃ of environment, through 3-10 days dryings, make a metal-organic complex original position in the mixed system gelation process synthetic, make the uniform composite luminescent material of optics.
3. original position is synthesized a metal-organic complex in the xerogel heat treatment process: the aqueous solution and the organic ligand solution that add metal (transition metal) salt in sol-gel pioneer liquid, pioneer's liquid is formed (molar fraction): inorganic salt (as the phosphoric acid salt of sodium, barium, titanium, vanadium etc., borate, nitrate etc.) or mineral acid (as phosphoric acid, boric acid etc.) or metal alkoxide (as tetraethoxy, methyl silicate, butyl (tetra) titanate, sodium methylate etc.) 10-15, organic solvent (as alcohol, acetone etc.) 35-45, deionized water 35-45.The add-on (molar fraction of relative inorganic gel glass matrix) of the central metallic ions (as transition metal ion or rare earth ions such as manganese, chromium, titanium, zinc) of organic accessory (as carboxylic acid, beta diketone and various Lewis bases etc.) and title complex is respectively 1.0-1.5mol% and 0.4-0.6mol%.The temperature of regulating mixed solution is 20-90 ℃ and pH value 1.0-3.0, mixes the back and leaves standstill under 30 ℃ of-50 ℃ of environment, through 3-10 days dryings, makes the transparent and uniform composite xerogel.Xerogel heats up with 20 ℃-30 ℃/hour speed, heat-treats successively through 90 ℃-300 ℃, makes a metal-organic complex original position in the inorganic gel glass matrix synthetic, makes the uniform composite luminescent material of optics.
Pioneer's liquid that embodiment 1. adopts is formed (molar fraction): tetraethoxy 10 ± 2, ethanol 42 ± 3, deionized water 42 ± 3.Dipyridyl alcoholic solution and terbium trichloride (Tb-Cl
3) add-on (relatively tetraethoxy molar fraction) of the aqueous solution is respectively 1.00 ± 0.10mol% and 0.50 ± 0.05mol%.The temperature of regulating mixed solution is 25 ± 5 ℃ and pH value 1.5 ± 0.5, mixes the back and leaves standstill under 30 ℃ of-50 ℃ of environment, through 3-7 days dryings, makes the transparent and uniform composite xerogel.Xerogel heats up with 20 ℃/hour speed, heat-treats successively through 90 ℃-250 ℃, then obtains at the uniform SiO of optics
2The composite luminescent material of original position synthesis nano Tb (III)-dipyridyl title complex in the gel glass matrix.Terbium ion (Tb in this gel glass
3+) the characteristic fluorescence emissive porwer is than the Tb that singly mixes same concentrations
3+, and through the same heat treated SiO of temperature schedule
2The terbium ion fluorescent emission intensity of gel glass is high more than 15 times.
Pioneer's liquid that embodiment 2. adopts is formed (molar fraction): tetraethoxy 10 ± 2, ethanol 42 ± 2, deionized water 42 ± 2.α-thenoyltrifluoroacetone (TTA) alcoholic solution, triphenyl phosphorus oxide (TPPO) alcoholic solution and europium chloride (EuCl
3) add-on (relatively tetraethoxy molar fraction) of the aqueous solution be respectively 1.5 ± 0.15mol%, 1.00 native 0.10mol% and, 0.50 ± 0.05mol%.It is 3.0 ± 0.5 with the pH value that the temperature of regulating mixed solution is 25 ± 5 ℃, mixes under 30 ℃～50 ℃ environment and leaves standstill, and through 3-7 days dryings, obtains at the uniform SiO of optics
2The composite luminescent material of original position synthesis nano Eu (III)-TTA-TPO title complex in the gel glass matrix.This gel glass europium ion (Eu
3+) the characteristic fluorescence emissive porwer is than the Eu that singly mixes same concentrations
3+SiO
2The europium ion fluorescent emission intensity Senior Three of gel glass is more than the order of magnitude.
The present invention compares with employing porous, inorganic matrix impregnation organic polymer soln (rear doping) method with traditional sol-gel (the pre-doping) method of existing domestic and international research and employing, has following outstanding advantages:
1. overcome the most metals organic coordination compound at traditional sol-gel technology bar Can not stable existence or homodisperse shortcoming under the part, it is multiple to be implemented in organic-inorganic nano Close in the process in-situ synthetic inorganic metal base organic composite optical function material.
2. can utilize rigidity " cage " effect of inert inorganic matrix, avoid organic optical to live The property molecule between and and inorganic matrix between various photochemical reactions, effectively improve The service life of composite optical function material.
3. can reduce matrix to the absorption loss water of pump light, increase substantially organic optical and live The Effective Doping concentration of property material in inorganic matrix makes its quenching concentration improve a number More than the magnitude.
4. can increase substantially the exhibiting optical function energy of composite, take composite luminescent material as Example, original position synthesizing inorganic base rare earth organic complex composite luminescent material, rare earth ion feature The high 1-3 of the rare-earth-ion-doped material of a fluorescence intensity ratio list order of magnitude.
5. can be by control gel process and heat-treat condition, effectively to composite Exhibiting optical function can be adjusted and optimize.
6. the present invention has wider adaptability, and it is organic to prepare a series of inorganic metal bases Complex recombination luminescence, multicolor displaying and nonlinear optical material.
Claims (6)
1. an in-situ synthetic inorganic metal base organic composite optical function material preparation method is characterized in that its step is:
1) pioneer's liquid preparation: select inorganic salt or mineral acid or metal alkoxide as precursor, water-soluble and organic solvent 20～90 ℃ of temperature, under acid catalysis and the agitation condition, through hydrolysis one polycondensation, obtains uniform inorganic matrix sol-gel pioneer liquid;
2) the synthetic a metal-organic complex of original position in the so-gel process: the aqueous solution and the organic ligand solution that in sol-gel pioneer liquid, add transition metal or rare-earth salts, pioneer's liquid is formed molar fraction: inorganic salt or mineral acid or metal alkoxide 5～20, organic solvent 25～50, deionized water 20～55; Organic ligand is respectively 0.2～2.0mol% and 0.1～1.0mol% with the molar fraction of the relative inorganic gel glass matrix of the central metal ion add-on of title complex; It is 1.0～6.5 with pH that the temperature of regulating mixed solution is 20～90 ℃, mixing the back leaves standstill under 30～80 ℃ of environment, through 3～15 days dryings, make the transparent and uniform composite xerogel, make a metal-organic complex original position in the mixed system gelation process synthetic, make the even composite optical function material of optics.
2. an in-situ synthetic inorganic metal base organic composite optical function material preparation method is characterized in that its step is:
1) pioneer's liquid preparation: select inorganic salt or mineral acid or metal alkoxide as precursor, water-soluble and organic solvent is 20～90 ℃ of temperature, under acid catalysis and the intense agitation, through hydrolysis one polycondensation, obtain uniform inorganic matrix so-gel pioneer liquid;
2) the synthetic a metal-organic complex of original position in the xerogel heat treatment process: the aqueous solution and the organic ligand solution that in so-gel pioneer liquid, add transition metal or rare-earth salts, pioneer's liquid is formed molar fraction: inorganic salt or mineral acid or metal alkoxide 5～15, organic solvent 35～50, deionized water 30～45, organic ligand is respectively 0.2～1.5mol% and 0.3～0.8mol% with the molar fraction of the relative inorganic gel glass matrix of the central metal ion add-on of title complex.The temperature of regulating mixed solution is 20～90 ℃ and pH value 1.0～6.0, mixing the back leaves standstill under 30～80 ℃ of environment, after dry 3～15 days, heat up with 20～40 ℃ of/hour speed, heat-treat through 90～300 ℃, make a metal-organic complex original position in the inorganic gel glass matrix synthetic, the uniform composite optical function material of system optics.
3. a kind of in-situ synthetic inorganic metal base organic composite optical function material preparation method according to claim 1 is characterized in that: said inorganic salt are: the phosphoric acid salt of sodium, barium, titanium, vanadium, borate, nitrate; Mineral acid is: phosphoric acid, boric acid; Metal alkoxide is: tetraethoxy, methyl silicate, butyl (tetra) titanate, sodium methylate; Organic solvent is: alcohol, acetone;
4. a kind of former chivalrous synthesizing inorganic Base Metal organic coordination compound composite optical function material preparation method according to claim 1 is characterized in that: said organic ligand is: carboxylic acid, beta diketone and Lewis base; The title complex central metallic ions is: manganese, chromium, titanium, zinc transition metal ion or rare earth ion.
5. a kind of in-situ synthetic inorganic metal base organic composite optical function material preparation method according to claim 2 is characterized in that: said inorganic salt are: the phosphoric acid salt of sodium, barium, titanium, vanadium, borate, nitrate; Mineral acid is: phosphoric acid, boric acid; Metal alkoxide is: tetraethoxy, methyl silicate, butyl (tetra) titanate, sodium methylate; Organic solvent is: alcohol, acetone;
6. a kind of former chivalrous synthesizing inorganic Base Metal organic coordination compound composite optical function material preparation method according to claim 2 is characterized in that: said organic ligand is: carboxylic acid, beta diketone and Lewis base; The title complex central metallic ions is: manganese, chromium, titanium, zinc transition metal ion or rare earth ion.
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| CN1063774C true CN1063774C (en) | 2001-03-28 |
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| CN100575450C (en) * | 2008-01-10 | 2009-12-30 | 同济大学 | A kind of preparation method of fluorescent powder used for plasma display |
| CN103497759A (en) * | 2013-09-03 | 2014-01-08 | 东莞上海大学纳米技术研究院 | Visible-light-sensitized rare-earth-complex-doped luminescent gel and preparation method thereof |
| CN103881005B (en) * | 2014-03-18 | 2016-05-04 | 陕西师范大学 | A kind of photocuring preparation method of rare earth bonding type fluorescence gel glass |
| CN115611259B (en) * | 2022-12-20 | 2023-04-07 | 江苏正力新能电池技术有限公司 | Polyanion electrode material, preparation method thereof and sodium-ion battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5132668A (en) * | 1974-09-13 | 1976-03-19 | Hitachi Ltd | DOITAIRYURYO SOKUTE ISOCHI |
| US5356667A (en) * | 1990-07-11 | 1994-10-18 | The University Of Florida | Laser dye impregnated silica sol-gel monoliths |
| JP4068077B2 (en) * | 2004-04-16 | 2008-03-26 | 三菱電機株式会社 | Disk unit |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5132668A (en) * | 1974-09-13 | 1976-03-19 | Hitachi Ltd | DOITAIRYURYO SOKUTE ISOCHI |
| US5356667A (en) * | 1990-07-11 | 1994-10-18 | The University Of Florida | Laser dye impregnated silica sol-gel monoliths |
| JP4068077B2 (en) * | 2004-04-16 | 2008-03-26 | 三菱電機株式会社 | Disk unit |
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