CN1415650A - Method for continuous preparing nano oxide or its reactant collosol as well as hybridization material of polymer - Google Patents
Method for continuous preparing nano oxide or its reactant collosol as well as hybridization material of polymer Download PDFInfo
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- CN1415650A CN1415650A CN 02143661 CN02143661A CN1415650A CN 1415650 A CN1415650 A CN 1415650A CN 02143661 CN02143661 CN 02143661 CN 02143661 A CN02143661 A CN 02143661A CN 1415650 A CN1415650 A CN 1415650A
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Abstract
A process for continuous preparing nano oxide or its reactant sol and its polymer hybridized material features that under the protection of inert gas, N2, H2, or CO2 gas, the oxide or its mixture and doping substance immersed in inert liquid compound, solution or liquid mixture is bombarded by laser beams to generate a high-temp and -pressure microarea on solid-liquid interface for forming oxide sol, and after the solvent is removed or in-situ polymerization takes place, the nano oxide-polymer hybridized material is obtained.
Description
The present invention relates to adopt laser bombardment (or corrode or sputter) solid-liquid interface to prepare the method for nano-oxide or its reactant colloidal sol and polymer hybrid material thereof.
Nano-oxide is because of its small-size effect, surface effects, quantum size effect and macro quanta tunnel effect, and have many and the visibly different special property of macro-size oxide compound of the same race, in every field application prospect of the utmost importance is arranged, cause the very big attention of countries in the world, especially have function nano oxide compounds such as superconduction, conduction, semi-conductor, magnetic, non-line optics, photochemical catalysis, photoelectricity, variable color, become the research focus in the nano material.
So far nano oxide powder mainly obtains by methods such as chemical precipitation method, sol-gel method, combustion flame method, chemical gas phase coacervation and laser chemistry reaction methods.Laser is used for the preparation of various nano-metal-oxides, carbide and nitride as heat source for reaction in the laser chemistry reaction method, and nano-oxide wherein is as TiO
2, Al
2O
3, r-Fe
2O
3, SiO
2Begin to move towards the industrialization Deng.Adopt the laser bombardment solid-liquid interface to prepare report (Yang Guowei etc., " Chinese Journal Of High Pressure Physics ", 1998,12 (4): 303-306 of the also existing diamond nano crystalline substance of nano material, carbonization nitrogen etc.; Zheng Lansun etc. " SCI "; 1997; 18 (4): 124-126), but do not see that so far laser bombardment is dipped in oxide solid target in the liquid phase that flows and prepares nano-oxide and boil off solvent or report that further in-situ polymerization obtains nano-oxide-polymer hybrid material.
The objective of the invention is to propose a kind of novel method that can prepare nano-oxide colloidal sol continuously that adopts the laser bombardment solid-liquid interface, make the nano-oxide colloidal sol for preparing need not purifying can directly use or boil off solvent or further in-situ polymerization or condensation obtain corresponding nano-oxide-polymer hybrid functional materials.Main technical schemes of the present invention is: at rare gas element and nitrogen; the protection of flowing gas such as hydrogen or carbonic acid gas down; adopting the pulse laser bombardment to be dipped in the continuous flow liquid phase (selects oxide compound or its mixture; hotchpotch is chemically inert; and the fluid cpds that meets application purpose; liquid substances such as solution and composition thereof) the continuous work in is oxide solid target (single oxide or its mixture of displacement relatively; hotchpotch; or under preparation condition, can resolve into the precursor substance of oxide compound or the oxide compound of chemical reaction can take place to each other) surface; produce high-temperature high-pressure microdmain hot spot reaction zone in solid-liquid interface; generate nano-oxide colloidal sol and flow out reaction zone, boil off solvent or further in-situ polymerization or condensation and obtain nano-oxide-polymer hybrid material.
Particular content comprises:
1, adopt the mobile liquid phase from the top of oxide solid target or side or below with certain flow rate Continuous Flow superoxide solid target by the surface of laser bombardment, the thin layer of liquid thickness that control continuous flow liquid phase is flooded superoxide solid target surface is 0.0 ~ 5.00 millimeter, and optimum thickness is the 1.0-3.0 millimeter.Liquid phase flow rate is 0.001 ~ 0.500 milliliters/second, and optimum flow velocity is 0.01 ~ 0.06 milliliters/second.Liquid phase Continuous Flow superoxide solid target is by the surface of laser bombardment, the very fast diffusion of heat that high-temperature high-pressure microdmain is produced is distributed on the one hand, the oxide sol of avoiding again on the other hand having generated is subjected to follow-up laser bombardment and destroys, therefore the entire reaction device maintains under macroscopical normal pressure and temperature all the time, and has realized the continuous preparation of oxide sol.
2. keeping focusing pulse laser bombardment point can drop under the condition on oxide solid target surface, make laser bombardment press that certain way is done on oxide solid target surface back and forth continuously or round-robin scans entirely, perhaps fixed laser bombarded point position is rotated or back and forth translation the oxide solid target continuously.In a word, adopt any purpose in above two kinds of methods, all be that the position that makes the pulse laser bombardment be dipped in the high-temperature high-pressure microdmain hot spot of the oxide solid target surface generation in the continuous flow liquid phase is brought in constant renewal in, create more favourable space environment for the generation of nano-oxide colloidal sol, improved the utilization ratio of oxide solid target simultaneously.
3. the component of oxide solid target is single oxide or its mixture, hotchpotch, the oxide compound of concrete can be Li, Be, B, Mg, Al, Si, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, Y, Zr, Nb, Mo, Tc, Ru, Rh, Pd, Ag, Cd, In, Sn, Sb, Ba, Hf, Ta, W, Re, Os, Ir, Pt, Hg, Pb, Bi and rare earth metal or its mixture, hotchpotch.
4. the solid target component also can adopt the precursor substance that can resolve into oxide compound under preparation condition, and it is carbonate, acid or subcarbonate, oxalate, carboxylate salt etc. normally, or its stoichiometry or non-stoichiometric mixture.
5. the solid target component can also adopt the oxide component that combination reaction can take place mutually under preparation condition, stoichiometry or nonstoichiometry mixture as acidic oxide and basic oxide, the stoichiometry of oxidisability oxide compound and reductibility oxide compound or nonstoichiometry mixture, normally carbonate, acid or subcarbonate, oxalate, phosphoric acid salt etc.The nano-oxide that obtains or its reactant or nano hybridization polymkeric substance are adulterated nano-oxide, or its reactant or hotchpotch nano hybridization polymer materials
6. the solid target component can add a small amount of or trace doped thing except oxide compound or its precursor and composition thereof, or behind preparation nano-oxide or its mixture colloidal sol, adds a small amount of hotchpotch immediately, and these hotchpotchs are simple substance and halogenide normally.
7. adopt rare gas element such as helium, argon and shielding gas such as nitrogen, hydrogen or carbonic acid gas to inject direction and feed reactor along pulse laser; from the oxide target side to blowing out; in air in discharging reactor, the oxygen etc.; take steam and the issuable gaseous product of preparation process that liquid phase produces out of reactor; after condensation, isolating phlegma, shielding gas recycles or emptying.
8. can in the liquid phase that flows, add an amount of polymkeric substance or polymerizable monomer in advance, adopt laser bombardment to be dipped in after oxide solid target in the continuous flow liquid phase obtains the Nano sol of oxide compound or its mixture, hotchpotch, can boil off solvent or further carry out in-situ polymerization or condensation and obtain nano-oxide-polymer hybrid material.
9. it is chemically inert can selecting oxide compound or its mixture, hotchpotch, have proper viscosity, boiling point and vapour pressure, and the liquid substances such as fluid cpds, solution and composition thereof that meet application purpose are as flowing liquid phase, its liquid substance can be water, lower alcohol, hydrocarbon, ether, ester, oligo-ether, liquid organosilicon compound, liquid terpenes, liquid polymer monomer etc., and the most frequently used is water, ethanol, normal hexane, sherwood oil, silicone oil, turps, acrylate, vinylbenzene, organosilane monomer etc. and solution or mixture.
As mentioned above, the invention has the advantages that:
1. can prepare oxide compound (comprising its mixture, hotchpotch, reactant) colloidal sol continuously, method is easy, is easy to control, and the liquid phase range of choice that flows is wide, and the scope of application is wide.
2. can make pure nano-oxide or its reactant colloidal sol; except containing nano-oxide, selected solvent and using required and the specific components that adds; no precursors reaction thing, protective material, dispersion agent etc. are an impediment to the unwanted component of application purpose, thereby need not repurity can directly use.
3. nano-oxide of Huo Deing or reactant colloidal sol can add polymkeric substance in advance in the liquid phase that flows, then the Nano sol that obtains is boiled off solvent or further in-situ polymerization obtain nano-oxide-polymer hybrid material.
4. can be when preparing nano-oxide colloidal sol in the liquid phase that flows or prepare the method that then in Nano sol, adds the required specific components of metrology applications immediately, it is required both to have satisfied application purpose, reach regulation and control nano-oxide particle diameter and distribution thereof again, and make it more stable purpose.
When oxide solid target component when the oxide compound of chemical reaction or its precursor mixture can take place for, also can obtain the Nano sol of its reactant (inorganics) or its mixture.
6. work as the solid target component except oxide compound or its precursor or its mixture, also can add an amount of hotchpotch, or after making nano-oxide or its mixture colloidal sol, add an amount of hotchpotch immediately, these hotchpotchs are simple substance or halogenide normally, and the colloidal sol of acquisition or nano hybridization polymkeric substance are adulterated nano-oxide or adulterated nano hybridization polymer materials.
Below with non-limiting example to laser bombardment of the present invention continuously the method for the pure oxide sol of preparation be described further; to help understanding to the present invention and advantage thereof; and not as a limitation of the invention, protection scope of the present invention is decided by claims.
Embodiment 1
By Nd: the double-frequency laser bundle (pulsewidth 10ns, pulse-repetition is 10) of YAG solid statelaser output 532nm focuses on the ferric oxide (Fe that is immersed in surging mutually
2O
3) the solid target surface.Mobile liquid phase is the analytical pure normal hexane that newly heavily steamed, and the control liquid phase flow rate is 0.02ml/ second.Slowly pure nitrogen gas is fed reactor, effusive nitrogen gas stream through cooling jacket cooling, isolate phlegma after emptying.Preparation is one hour continuously, obtains the lurid nanometer Fe of about 60ml
2O
3-normal hexane sol liquid.
Embodiment 2
In preparation facilities with embodiment 1, change the liquid phase that flows for removing the analytical pure methyl methacrylate of stopper, dry and new underpressure distillation, solid target is the titanium dioxide compressing tablet, slowly pure argon is fed reactor, effusive argon gas stream recycles through cooling jacket cooling, after isolating phlegma.Pulse laser is the one hour time of bombardment continuously.Obtain the transparent nano titanium oxide of the shallow oyster white of about 65ml/methyl methacrylate colloidal sol, add 0.10% azo isobutyronitrile initiator, in 60 ℃ of polymerizations two hours, be warming up to 100 ℃ one hour, obtain water white nano-TiO
2-PMMA hydridization solid material.
Embodiment 3
In the preparation facilities with embodiment 1, changing the liquid phase that flows is the analytical pure ethanol that dewaters and newly heavily steamed, and solid target is that purity is 99.99% europiumsesquioxide (Eu
2O
3) the powder compressing tablet, the control liquid phase flow rate is 0.04ml/ second, slowly pure nitrogen gas is fed reactor, effusive nitrogen gas stream through cooling jacket cooling, isolate phlegma after emptying.Pulse laser bombarded one hour continuously, obtained the transparent nano europium oxide of the shallow white of about 130ml-ethanol colloidal sol.
Embodiment 4
In the preparation facilities with embodiment 1, changing the liquid phase that flows is the analytical pure benzole soln that dewaters and reduce pressure and heavily steamed that contains 0.5% polystyrene, and solid target is 99.99% spectroscopically pure SiO
2The powder compressing tablet, the control liquid phase flow rate is 0.02ml/ second, slowly pure nitrogen gas is fed reactor, the emptying after cooling jacket cools and isolates phlegma of effusive nitrogen gas stream.Pulse laser bombarded one hour, obtained the nanometer SiO of about 60ml clear, colorless
2-polystyrene colloidal sol, pressure reducing and steaming benzene obtains water white nanometer SiO
2-polystyrene hybrid material.
Embodiment 5 is in the preparation facilities with embodiment 1, and the liquid phase that change to flow is to contain the analytical pure ethyl acetate solution that the new decompression of 0.5% polymethylmethacrylate was heavily steamed, and solid target is that purity is 99.9%PbO and TiO
2By weight 1: 1 mole ratio mixture compressing tablet.The control liquid phase flow rate is 0.02 milliliters/second, slowly pure nitrogen gas is fed reactor, and effusive nitrogen cools off through cooling jacket, isolates emptying behind the phlegma, and pulse laser bombarded one hour continuously, obtains the clear, colorless nanometer PbTiO of about 60ml
3-polymethylmethacrylate-ethyl acetate colloidal sol, be poured on treat that ethyl acetate is volatilized voluntarily on the horizontal positioned glass plate after, water white nanometer PbTiO
3-polymethyl methacrylate hybrid thin-film material.
Embodiment 6
In preparation facilities with embodiment 1, be moving phase with the analytical pure toluene that dewaters and newly heavily steamed, solid target is the WO of content 99%
3Compressing tablet, control toluene flow velocity is 0.01ml/ second.Flooded WO
3The liquid level on solid target surface is 2.00mm, slowly purity nitrogen is fed reactor, and effusive pure argon is isolated phlegma and forced to flow in preparation facilities by recycle pump after the cooling jacket cooling.The continuous bombardment time of pulse laser one hour obtains the transparent nanometer WO of the shallow oyster white of about 30ml
3-toluene colloidal sol, add 0.5 gram and just heavily steamed the analytical pure aniline and the metering hydrogen peroxide of purifying, dripping 0.1ml concentrated hydrochloric acid adjusting PH is 2, in three mouthfuls of beakers of Zhuan You rotation flow condenser and electric mixer, stir polymerization two hours down in 120 ℃, be warming up to 110 ℃ then and continued stirring reaction one hour, filter, wash, get 0.40 gram black nano WO
3-polyaniline hybridized material.
Embodiment 7:
In preparation facilities with embodiment 1, be moving phase with the analytical pure ethyl acetate that dewaters and just heavily steamed that contains 1% polymethylmethacrylate, the solid target composition is the spectroscopically pure SiO that contains 1%Si
2Compressing tablet, the control flow rate of mobile phase is 0.01ml/ second, and flooding solid target surface liquid level is 2.0mm, and as protection gas, pulse laser bombarded one hour continuously with pure helium, must about 30ml water white transparency mixes the nanometer SiO of Si
2-polymethylmethacrylate-ethyl acetate colloidal sol falls on the glass plate of horizontal positioned, treats that ethyl acetate volatilizees naturally, must the adulterated nanometer SiO of Si
2-polymethyl methacrylate hybrid thin-film material.
Embodiment 8:
In preparation facilities, be moving phase with the benzole soln that contains 0.1% polystyrene, to mix 10%Ln with embodiment 1
2O
3SnO
2Compressing tablet is a solid target, and all the other conditions must the water white nanometer Ln of about 30ml with embodiment 7
2O
3-SnO
2-polystyrene-benzene sol falls in the glass plate of horizontal positioned, benzene is volatilized naturally after, must contain nanometer Ln
2O
3-SnO
2-polystyrene hybrid film.
Claims (10)
1. the present invention relates to adopt laser bombardment (corrode or sputter) solid-liquid interface to prepare the method for nano-oxide colloidal sol and polymer hybrid material thereof; it is characterized in that under the protection of flowing gas such as rare gas element and nitrogen, hydrogen or carbonic acid gas; the continuous work that liquid phase Continuous Flow such as fluid cpds, solution and composition thereof is crossed be excited the light beam bombardment is the solid target surface that is made of single oxide or its mixture, hotchpotch or its reacting precursor of displacement relatively, thereby realizes continuously preparation nano-oxide colloidal sol and further obtain the purpose of its polymer hybrid material.
2. preparation method according to claim 1, it is characterized in that making below or side or the top Continuous Flow superoxide solid target surface of the liquid phase of continuous flow from the oxide solid target, the thin layer of liquid thickness that superoxide solid target surface is flooded in control is the 0.01-5.00 millimeter, optimum thickness is the 1.0-3.0 millimeter, liquid phase flow rate is 0.001-0.500 milliliter/second, and optimum flow velocity is the 0.01-0.06 milliliters/second.
3. preparation method according to claim 1, it is characterized in that keeping focusing pulse laser bombardment point to drop under the prerequisite on oxide solid target surface, fixedly the oxide compound solid target makes the laser beam focus point scan the whole surface of oxide solid target continuously, perhaps fixed laser beam focusing point position and make oxide solid target constantly rotation or back and forth translation, adopt above two kinds of laser bombardment points and oxide solid target constantly to make the mode of relative displacement, purpose is the position continual renovation that produces high-temperature high-pressure microdmain when making pulse laser bombard the oxide solid target that is dipped in the continuous flow liquid phase in solid-liquid interface.
4. preparation method according to claim 1; it is characterized in that shielding gas such as rare gas element such as helium, argon gas or nitrogen, hydrogen, carbonic acid gas feed reactor along the pulse laser incident direction; blow out from oxide solid target side direction; take air, oxygen etc. in the reactor and liquid phase steam and issuable gaseous product out of reactor simultaneously; after condensation, isolating phlegma, gas circulation is used or emptying.
5. preparation method according to claim 1, the component that it is characterized in that the oxide solid target is to be chemically inert single oxide and composition thereof or hotchpotch for the liquid phase that specify to flow, oxide compound of concrete is Li, Be, B, Mg, Al, Si, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, Sr, Y, Zr, Nb, Mo, Tc, Ru, Rh, Pd, Ag, Cd, In, Sn, Sb, Ba, Hf, Ta, W, Re, Os, Ir, Pt, Hg, Pb, Bi and rare earth metal and composition thereof or hotchpotch.
6. preparation method according to claim 1, the component that it is characterized in that solid target also can adopt the precursor substance that can resolve into oxide compound under preparation condition, normally carbonate, acid or subcarbonate, oxalate, phosphoric acid salt etc., or its stoichiometry or non-stoichiometric mixture.
7. preparation method according to claim 1, it is characterized in that oxide solid target component can be the oxide compound that chemical reaction can take place to each other, they are acidic oxide and basic oxide, oxidisability oxide compound and reductibility oxide compound, and the Nano sol of acquisition or nano hybridization polymkeric substance are the Nano sol or the nano hybridization polymkeric substance of chemical combination resultant between its oxide compound.
8. preparation method according to claim 1, it is chemically inert it is characterized in that selecting oxide solid target component, liquid substance with proper viscosity, boiling point and vapour pressure is as the liquid phase that flows, they can be water, lower alcohol, hydrocarbon, ether, ester, oligo-ether, liquid organosilicon compound, liquid terpenes and liquid polymer monomer, and the most frequently used is solution or its mixtures such as water, ethanol, normal hexane, sherwood oil, silicone oil, turps, organosilane monomer, esters of acrylic acid and vinylbenzene.
9. preparation method according to claim 1, it is characterized in that in the liquid phase that flows, dissolving in an amount of polymkeric substance or polymerizable monomer in advance, after adopting laser bombardment to be dipped in that the oxide solid target obtains oxide compound or its mixture in the continuous flow liquid phase, mixing the Nano sol of thing, can boil off solvent and further carry out in-situ polymerization or condensation and obtain nano-oxide-polymer hybrid material.
10. preparation method according to claim 1 is characterized in that the solid target component except oxide compound or its reactant precursor and polymkeric substance thereof, mixes thing normally simple substance or halogenide.
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|---|---|---|---|
| CN 02143661 CN1252162C (en) | 2002-09-27 | 2002-09-27 | Method for continuous preparing nano oxide or its reactant collosol as well as hybridization material of polymer |
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| CN1252162C CN1252162C (en) | 2006-04-19 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103059491A (en) * | 2012-12-28 | 2013-04-24 | 中国科学院合肥物质科学研究院 | Liquid phase laser sputtering-based preparation method of inorganic-polymer nanocomposite material |
| CN106637104A (en) * | 2016-12-22 | 2017-05-10 | 天津大学 | Preparation method of black titanium dioxide composite film |
| CN106756788A (en) * | 2016-11-24 | 2017-05-31 | 天津大学 | A kind of method that Gas Sensor Films Deposited by Pulsed Laser Deposition prepares black titanium dioxide powder under subnormal ambient |
| CN110129109A (en) * | 2019-06-17 | 2019-08-16 | 中国科学院兰州化学物理研究所 | A kind of preparation method and applications of transient metal sulfide nanoparticle |
-
2002
- 2002-09-27 CN CN 02143661 patent/CN1252162C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103059491A (en) * | 2012-12-28 | 2013-04-24 | 中国科学院合肥物质科学研究院 | Liquid phase laser sputtering-based preparation method of inorganic-polymer nanocomposite material |
| CN103059491B (en) * | 2012-12-28 | 2015-04-08 | 中国科学院合肥物质科学研究院 | Liquid phase laser sputtering-based preparation method of inorganic-polymer nanocomposite material |
| CN106756788A (en) * | 2016-11-24 | 2017-05-31 | 天津大学 | A kind of method that Gas Sensor Films Deposited by Pulsed Laser Deposition prepares black titanium dioxide powder under subnormal ambient |
| CN106756788B (en) * | 2016-11-24 | 2019-05-21 | 天津大学 | A kind of method that Gas Sensor Films Deposited by Pulsed Laser Deposition prepares black titanium dioxide powder under subnormal ambient |
| CN106637104A (en) * | 2016-12-22 | 2017-05-10 | 天津大学 | Preparation method of black titanium dioxide composite film |
| CN106637104B (en) * | 2016-12-22 | 2019-04-12 | 天津大学 | The preparation method of black titanium dioxide laminated film |
| CN110129109A (en) * | 2019-06-17 | 2019-08-16 | 中国科学院兰州化学物理研究所 | A kind of preparation method and applications of transient metal sulfide nanoparticle |
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| CN1252162C (en) | 2006-04-19 |
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