CN1394882A - Preparation method of CdTe nano crystal transparent polymer body phase material with high visible luminescent efficiency - Google Patents
Preparation method of CdTe nano crystal transparent polymer body phase material with high visible luminescent efficiency Download PDFInfo
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Abstract
The preparation method of transparent polymer body phase material containing CdTe semiconductor nano crystal with high luminescent efficiency includes three steps of preparing water soluble CdTe semiconductor nano crystal and polymerizable surfactant, nano crystal phase transfer and adding initiator to make self-body polymerization. The water soluble CdTe semiconductor nano crystal can be obtained by using colloid chemical process, its reflux time is 0.5 hr to three days; the phase transfer of semiconductor nano crystal can be implemented by means of adding oil-soluble polymerizable cation surfactant. The ratio of polymerizable surfactant and CdTe water sol is 1-5 mg/1ml, its initiator is 0.1 wt%-0.3wt% of monomer, its self-body polymerization temp. is 55-130 deg.c and its reaction time is 20-30 hr.
Description
Technical field:
The present invention relates to the compound of a kind of inorganic particles and polymer materials and hydridization reaction method, particularly relate to a kind of by the long-chain polymerisable surfactant to water-soluble CdTe semiconductor nano surface modification, add original positions such as organic monomer, initiator and carry out mass polymerization, preparation contains the body phase material method of the transparent polymer of high-luminous-efficiency CdTe semiconductor nano.
Background technology:
Owing to there is quantum size effect, the photoluminescence of semiconductor nano, electroluminescent color rely on particle size strongly.For CdTe is nanocrystalline, when mean particle dia when 2.5nm is increased to 4.0nm, its glow color changes to ruddiness from green glow.In addition, the method synthetic is nanocrystalline compares with other, aqueous phase with the direct synthetic of sulfydryl stablizer nanocrystallinely have that cost is low, toxicity is little, good reproducibility, advantage such as easy to operate.As a kind of type material, the semiconductor nano with high-luminous-efficiency can be used in fields such as photodiode, laser apparatus, biological fluorescent labelling, anti-false sign.Realize luminescence nanocrystalline practicability, must transfer to the inert media from colloidal solution, thereby improve nanocrystalline stability and workability nanocrystalline.Being fixed in the polymer materials nanocrystalline, is a feasible route, but the consistency that how to improve between nanocrystalline/polymkeric substance is the key issue of this method.If what solve is bad, nano composite material can be separated, and causes that material is opaque, luminous efficiency descends.Previous methods is nanocrystalline with what prepare in the oil phase, be distributed in the special construction monomer (methacrylic acid bay alcohol ester) that contains 5% high boiling solvent, initiated polymerization (Adv.Mater., 2000,12,333～337, full color emissionfrom II-VI semiconductor quantum dot-polymer composites).This method shortcoming has two: the first, because the existence of solvent, the gained material hardness is low, poor stability; The second, the monomer of special construction is synthetic complicated, the cost height.It is that nano material is put to key in application that the body of nano functional particulate is changed mutually, because most polymers and polymerisable monomer all are oil-soluble, it is one not have the difficult problem of solution all the time that water-soluble semiconductor nano is compounded in the polymer body phase material.
Summary of the invention:
Purpose of the present invention just provides a kind of preparation method: from water-soluble high-luminous-efficiency semiconductor nano, modify through the long-chain polymerisable surfactant, transfer to the monomer oil phase from water, through the last efficiently luminous inorganic semiconductor/organic polymer transparent nano matrix material that obtains of free radical polymerization.Its key is that polymerisable surfactant coats water-solubility nanocrystalline and realizes the transfer of water to oil phase.
The present invention includes following steps: 1, preparation water-soluble CdTe semiconductor nano; 2, polymerisable surfactant synthetic; 3, nanocrystalline phase transition and mass polymerization.
The objective of the invention is to be achieved through the following technical solutions: the present invention adopts the colloid chemistry method to prepare the CdTe semiconductor nano in the aqueous solution, nanocrystalline glow color is controlled by the return time to colloidal solution, is beneficial to the polymer materials that next step constructs different glow colors; Polymerisable surfactant has multiple synthetic route, and its basic structure should have oil soluble and polymerizable groups concurrently; Nanocrystalline can transferring to earlier in the common organic solvent behind the surface modification, evaporate to dryness obtains the oil soluble powder, also can directly transfer in the polymer monomer; Add initiator in the nanocrystalline monomer solution of CdTe, carry out mass polymerization, polymerisate is typical mass polymerization product, and appearance transparent is easy to carry out mechanical workout.
Above-mentioned water-soluble CdTe nano crystal synthesis phase is raw materials used to be cadmium salt, ionic tellurium source, mercaptan carboxylic acid.Cadmium salt can be CdCl
2, Cd (ClO
4)
2Deng; Ionic tellurium source can be H
2Te, NaHTe etc.; The mercaptan carboxylic acid can be a Thiovanic acid, thiohydracrylic acid, Gelucystine etc.With raw material CdCl
2, NaHTe, thiohydracrylic acid are example, general employing once feeds intake and forms CdCl
2With the aqueous solution of thiohydracrylic acid, the pH value is transferred to neutrality or weakly alkaline with NaOH and HCl, at N
2Will be under the gas shiled by Te powder and NaBH
4The NaHTe of prepared in reaction joins CdCl
2In the thiohydracrylic acid mixing solutions.CdCl
2Concentration be controlled at 3.0 * 10
-2N to 1.0 * 10
-3Between the N, CdCl
2, NaHTe, the ratio of thiohydracrylic acid is 1: 0.5: 2.4.The colloidal solution of new system is refluxed for some time (0.5 hour to 2 days) down at 100 ℃, control nanocrystalline particle diameter, along with the prolongation of return time, particle diameter constantly increases, and the different steps sampling obtains all samples from the green glow to ruddiness.
Polymerisable surfactant is to have quaternary ammonium salt head, the alkyl chain of 18 above length of carbon, the cats product of at least one styrene group.Positively charged quaternary ammonium salt is used for and the effect of electronegative CdTe nanocrystal surface, and long alkyl chain is used for improving oil soluble, and styrene group is used for and the solvent monomer polymerization.
Polymerisable surfactant used in the present invention is an octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride, by N, and N-dimethyl stearyl ammonium and 4-Bian Ji chloro-styrene prepared in reaction.
In the phase transition stage, oil phase can be common organic solvents such as toluene, chloroform, vinylbenzene, and best organic solvent: the ratio of water is 1: 2-1: between 3.The ratio of the polymerisable surfactant and the CdTe water-sol should be more than or equal to 1 milligram of tensio-active agent/1 ml water colloidal sol (but being no more than 5 mg/ml).
Used monomer of bulk polymerization stage can be vinylbenzene, can also be styrene monomer and the monomeric mixture of methyl acrylic ester; CdTe is nanocrystalline to transfer in the various monomer solutions initiated polymerization organizer phase luminescent material after polymerisable surfactant coats.This kind transfer promptly can be direct extraction, also can be to obtain powder earlier to dissolve again.The nanocrystalline add-on of CdTe is no more than 20 wt% of reaction system total amount, initiator general BPO, AIBN or other oil-soluble initiators, and consumption is 0.1 wt%-0.3wt% of reaction total amount; The mass polymerization temperature generally is 55-130 ℃, after general process is the low temperature pre-polymerization, slowly heats up again, prevents sudden and violent gathering, and needing the time is 20-30 hour.
Behind the stopped reaction, obtain appearance transparent, the glow color nanocrystalline polymer body phase material of a series of CdTe of containing from the green glow to ruddiness.
Embodiment:
The present invention is further elaborated below in conjunction with embodiment, rather than will limit the invention with this.
Embodiment one: 1: with CdCl
2, NaHTe, thiohydracrylic acid are that the synthetic CdTe of raw material is nanocrystalline
The NaHTe aqueous solution is by Te powder and NaBH
4Prepared in reaction: earlier with 80mg NaBH
4Fully be dissolved in the 1ml deionized water, add 127.5mg Te powder then, only stay the hydrogen that produces in the pin hole discharging system, reaction is 8 hours in ice-water bath, obtains the 1N NaHTe aqueous solution.
In the 1000ml reaction system, add 1.25 * 10
-3The CdCl of M
2With 3 * 10
-3The thiohydracrylic acid of M is transferred to 9.0 with NaOH with pH, and logical N
2Gas shiled; Under agitation condition, add the 0.625ml 1N NaHTe aqueous solution; CdCl
2, NaHTe, the molar ratio of thiohydracrylic acid are 1: 0.5: 2.4.100 ℃ of backflows, nanocrystalline discharging time of various glow color CdTe and performance perameter are as shown in table 1 with the freshly prepd CdTe water-sol.
Table 1: discharging time and performance perameter table
2: polymerisable surfactant octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride (OVDAC) synthetic
| Glow color | Return time (hour) | Emission peak position (nanometer) | Median size (nanometer) | Quantum yield in the aqueous solution (%) | Quantum yield in the polymkeric substance (%) |
| Green | ???0.5～1 | ????525 | ????2.8 | ????18 | ????12 |
| Yellow | ???5.5～6 | ????562 | ????3.3 | ????38 | ????20 |
| Orange | ???17～20 | ????595 | ????3.6 | ????17 | ????15 |
| Red | ???30～36 | ????649 | ????4.0 | ????4 | ????8 |
With 4.2ml N, N-dimethyl stearyl ammonium and 1.87g 4-Bian Ji chloro-styrene are dissolved in the 5ml acetone, and 40 ℃ were heated two hours, after the product cooling, with acetone flush away unreacted reactant, vacuum-drying.Phase transition that 3:CdTe is nanocrystalline and mass polymerization
Get the nanocrystalline colloidal solution 30ml of the CdTe with green fluorescence, add 30mg octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride,, take out the vinylbenzene phase with 10ml vinylbenzene extraction 20min; Use anhydrous MgSO
4After the simple drying, add the initiator A IBN of 0.3% weight ratio.Adopt the tube sealing polymerization to prepare body phase material: vinylbenzene to be placed test tube mutually, seal; Reaction system is placed liquid nitrogen, vinylbenzene is solidified mutually; Take out the gas in the reaction system, again closed system; Vinylbenzene melts with water-bath, discharges entrap bubble in the vinylbenzene naturally; Repeat said process 3-5 time, fully remove the gas in the system.70 ℃ of oil baths 24 hours make the vinylbenzene phase-polymerization, then 120 ℃ constant temperature 2-4 hour, make the abundant polymerization of monomer, obtain transparent CdTe nanocrystalline/poly styrene composite material.The quantum yield of nano composite material is as shown in table 1.
Embodiment 21: the synthetic nanocrystalline method of CdTe is as described in the embodiment one 2: synthetic octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride method is as nanocrystalline phase transition and the mass polymerization of 3:CdTe as described in the embodiment one
Get the nanocrystalline colloidal solution 30ml of the CdTe with yellow fluorescence, add 30mg octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride,, take out the vinylbenzene phase with 10ml vinylbenzene extraction 20min; Use anhydrous MgSO
4After the simple drying, add the initiator A IBN of 0.3% weight ratio.Adopt the tube sealing polymerization to prepare body phase material: vinylbenzene to be placed test tube mutually, seal; Reaction system is placed liquid nitrogen, vinylbenzene is solidified mutually; Take out the gas in the reaction system, again closed system; Vinylbenzene melts with water-bath, discharges entrap bubble in the vinylbenzene naturally; Repeat said process 3-5 time, fully remove the gas in the system.70 ℃ of oil baths 24 hours make the vinylbenzene phase-polymerization, then 120 ℃ constant temperature 2-4 hour, make the abundant polymerization of monomer, obtain transparent CdTe nanocrystalline/poly styrene composite material.The quantum yield of nano composite material is as shown in table 1.
Embodiment 31: the synthetic nanocrystalline method of CdTe is as described in the embodiment one 2: synthetic octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride method is as nanocrystalline phase transition and the mass polymerization of 3:CdTe as described in the embodiment one
Get the nanocrystalline colloidal solution 30ml of the CdTe with yellow fluorescence, add 30mg octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride,, take out the chloroform phase with 15ml chloroform extraction 20min; Use anhydrous MgSO
4After the simple drying, use the Rotary Evaporators solvent evaporated, obtain the CdTe/OVDAC composite powder.Take by weighing the 10mgCdTe/OVDAC mixture, be dissolved in 10ml vinylbenzene, ultrasonic dissolution.The initiator A IBN that adds 0.3% weight ratio.Adopt the tube sealing polymerization to prepare body phase material: vinylbenzene to be placed a test tube mutually, seal; Reaction system is placed liquid nitrogen, vinylbenzene is solidified mutually; Take out the gas in the reaction system, again closed system; Vinylbenzene melts with water-bath, discharges entrap bubble in the vinylbenzene naturally; Repeat said process 3-5 time, fully remove the gas in the system.70 ℃ of oil baths 24 hours make the vinylbenzene phase-polymerization, then 120 ℃ constant temperature 2-4 hour, make the abundant polymerization of monomer, obtain transparent CdTe nanocrystalline/poly styrene composite material.
Embodiment 41: the synthetic nanocrystalline method of CdTe is as described in the embodiment one 2: synthetic octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride method is as nanocrystalline phase transition and the mass polymerization of 3:CdTe as described in the embodiment one
Get the nanocrystalline colloidal solution 30ml of the CdTe with fluorescent orange, add 30mg octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride,, take out the vinylbenzene phase with 10ml vinylbenzene extraction 20min; Use anhydrous MgSO
4After the simple drying, add the initiator A IBN of 0.3% weight ratio.Adopt the tube sealing polymerization to prepare body phase material: vinylbenzene to be placed test tube mutually, seal; Reaction system is placed liquid nitrogen, vinylbenzene is solidified mutually; Take out the gas in the reaction system, again closed system; Vinylbenzene melts with water-bath, discharges entrap bubble in the vinylbenzene naturally; Repeat said process 3-5 time, fully remove the gas in the system.70 ℃ of oil baths 24 hours make the vinylbenzene phase-polymerization, then 120 ℃ constant temperature 2-4 hour, make the abundant polymerization of monomer, obtain transparent CdTe nanocrystalline/poly styrene composite material.The quantum yield of nano composite material is as shown in table 1.
Embodiment 51: the synthetic nanocrystalline method of CdTe is as described in the embodiment one 2: synthetic octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride method is as nanocrystalline phase transition and the mass polymerization of 3:CdTe as described in the embodiment one
Get the nanocrystalline colloidal solution 30ml of the CdTe with fluorescent orange, add 30mg octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride,, take out the chloroform phase with 15ml chloroform extraction 20min; Use anhydrous MgSO
4After the simple drying, use the Rotary Evaporators solvent evaporated, obtain the CdTe/OVDAC composite powder.Take by weighing 1g CdTe/OVDAC mixture, be dissolved in 9g vinylbenzene, ultrasonic dissolution.The initiator A IBN that adds 0.3% weight ratio.Adopt the tube sealing polymerization to prepare body phase material: vinylbenzene to be placed a test tube mutually, seal; Reaction system is placed liquid nitrogen, vinylbenzene is solidified mutually; Take out the gas in the reaction system, again closed system; Vinylbenzene melts with water-bath, discharges entrap bubble in the vinylbenzene naturally; Repeat said process 3-5 time, fully remove the gas in the system.70 ℃ of oil baths 24 hours make the vinylbenzene phase-polymerization, then 120 ℃ constant temperature 2-4 hour, make the abundant polymerization of monomer, obtain transparent CdTe nanocrystalline/poly styrene composite material.
Embodiment 61: the synthetic nanocrystalline method of CdTe is as described in the embodiment one 2: synthetic octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride method is as nanocrystalline phase transition and the mass polymerization of 3:CdTe as described in the embodiment one
Get the nanocrystalline colloidal solution 30ml of the CdTe with red fluorescence, add 30mg octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride,, take out the vinylbenzene phase with 10ml vinylbenzene extraction 20min; Use anhydrous MgSO
4After the simple drying, add the initiator A IBN of 0.3% weight ratio.Adopt the tube sealing polymerization to prepare body phase material: vinylbenzene to be placed test tube mutually, seal; Reaction system is placed liquid nitrogen, vinylbenzene is solidified mutually; Take out the gas in the reaction system, again closed system; Vinylbenzene melts with water-bath, discharges entrap bubble in the vinylbenzene naturally; Repeat said process 3-5 time, fully remove the gas in the system.70 ℃ of oil baths 24 hours make the vinylbenzene phase-polymerization, then 120 ℃ constant temperature 2-4 hour, make the abundant polymerization of monomer, obtain transparent CdTe nanocrystalline/poly styrene composite material.The quantum yield of nano composite material is as shown in table 1.
Embodiment 71: the synthetic nanocrystalline method of CdTe is as described in the embodiment one 2: synthetic octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride method is as nanocrystalline phase transition and the mass polymerization of 3:CdTe as described in the embodiment one
Get the nanocrystalline colloidal solution 30ml of the CdTe with red fluorescence, add 30mg octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride,, take out the chloroform phase with 15ml chloroform extraction 20min; Use anhydrous MgSO
4After the simple drying, use the Rotary Evaporators solvent evaporated, obtain the CdTe/OVDAC composite powder.Take by weighing the 10mgCdTe/OVDAC mixture, be dissolved in 10ml vinylbenzene, ultrasonic dissolution.The initiator A IBN that adds 0.3% weight ratio.Adopt the tube sealing polymerization to prepare body phase material: vinylbenzene to be placed a test tube mutually, seal; Reaction system is placed liquid nitrogen, vinylbenzene is solidified mutually; Take out the gas in the reaction system, again closed system; Vinylbenzene melts with water-bath, discharges entrap bubble in the vinylbenzene naturally; Repeat said process 3-5 time, fully remove the gas in the system.70 ℃ of oil baths 24 hours make the vinylbenzene phase-polymerization, then 120 ℃ constant temperature 2-4 hour, make the abundant polymerization of monomer, obtain transparent CdTe nanocrystalline/poly styrene composite material.
Embodiment 81: the synthetic nanocrystalline method of CdTe is as described in the embodiment one 2: synthetic octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride method is as nanocrystalline phase transition and the mass polymerization of 3:CdTe as described in the embodiment one
Get the nanocrystalline colloidal solution 30ml of the CdTe with red fluorescence, add 30mg octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride,, take out the chloroform phase with 15ml chloroform extraction 20min; Use anhydrous MgSO
4After the simple drying, use the Rotary Evaporators solvent evaporated, obtain the CdTe/OVDAC composite powder.Take by weighing the 10mgCdTe/OVDAC mixture, be dissolved in the mixing solutions of 1ml vinylbenzene and 9ml methyl methacrylate ultrasonic dissolution.The initiator A IBN that adds 0.1% weight ratio.Adopt the tube sealing polymerization to prepare body phase material: mix monomer to be placed a test tube mutually, seal; Reaction system is placed liquid nitrogen, mix monomer is solidified mutually; Take out the gas in the reaction system, again closed system; Mix monomer melts with water-bath, discharges entrap bubble in the mix monomer naturally; Repeat said process 3-5 time, fully remove the gas in the system.In 8 hours, temperature of reaction system from 55 ℃ of temperature programmings to 70 ℃, is made the mix monomer phase-polymerization; 80 ℃ of constant temperature is 12 hours then, makes the abundant polymerization of monomer, obtain transparent CdTe nanocrystalline/the copolymerized material of styrene/methacrylic acid methyl esters.
Embodiment 91: the synthetic nanocrystalline method of CdTe is as described in the embodiment one 2: synthetic octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride method is as nanocrystalline phase transition and the mass polymerization of 3:CdTe as described in the embodiment one
Get the nanocrystalline colloidal solution 30ml of the CdTe with fluorescent orange, add 30mg octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride,, take out the chloroform phase with 15ml chloroform extraction 20min; Use anhydrous MgSO
4After the simple drying, use the Rotary Evaporators solvent evaporated, obtain the CdTe/OVDAC composite powder.Take by weighing the 10mgCdTe/OVDAC mixture, be dissolved in the mixing solutions of 5ml vinylbenzene and 5ml butyl methacrylate ultrasonic dissolution.The initiator A IBN that adds 0.2% weight ratio.Adopt the tube sealing polymerization to prepare body phase material: mix monomer to be placed a test tube mutually, seal; Reaction system is placed liquid nitrogen, mix monomer is solidified mutually; Take out the gas in the reaction system, again closed system; Mix monomer melts with water-bath, discharges entrap bubble in the mix monomer naturally; Repeat said process 3-5 time, fully remove the gas in the system.In 8 hours, temperature of reaction system from 55 ℃ of temperature programmings to 70 ℃, is made the mix monomer phase-polymerization; 80 ℃ of constant temperature is 12 hours then, makes the abundant polymerization of monomer, obtain transparent CdTe nanocrystalline/the copolymerized material of styrene/methacrylic acid butyl ester.
Claims (6)
1, a kind of preparation method who contains the CdTe nano crystal transparent polymer body phase material comprises synthetic, nanocrystalline phase transition and three steps of mass polymerization that prepare water-soluble CdTe semiconductor nano, polymerisable surfactant, it is characterized in that:
(1) the nanocrystalline synthesis material of CdTe is cadmium salt, ionic tellurium source, mercaptan carboxylic acid, at cadmium salt and mercaptan carboxylic acid's the aqueous solution, is transferred to neutrality or weakly alkaline with NaOH and HCl, at N
2Will be under the gas shiled by Te powder and NaBH
4The NaHTe of prepared in reaction joins in cadmium salt and mercaptan carboxylic acid's the aqueous solution, and the concentration of cadmium salt is 3.0 * 10
-2N-1.0 * 10
-3N, cadmium salt, ionic tellurium source, mercaptan carboxylic acid's ratio is 1: 0.5: 2, colloidal solution refluxed 0.5 hour to 2 days down at 100 ℃, got the nanocrystalline water-sol of glow color from the green glow to ruddiness;
(2) polymerisable surfactant is to have quaternary ammonium salt head, the alkyl chain of 18 above length of carbon, the cats product of at least one styrene group, is prepared by ordinary method by satisfactory alkylammonium and the compound that contains styrene group;
(3) organic solvent of nanocrystalline phase transition: water is 1: 2-3, the ratio of the polymerisable surfactant and the CdTe water-sol is the 1-5 mg/ml, phase transition and monomer carry out bulk polymerization, the nanocrystalline add-on of CdTe is no more than the 20wt% of reaction system total amount, used initiator amount was the 0.1wt%-0.3wt% of reaction system total amount, at 55-130 ℃ of following polymerization 20-30 hour.
2, the preparation method who contains the CdTe nano crystal transparent polymer body phase material as claimed in claim 1 is characterized in that: cadmium salt can be CdCl
2Or Cd (ClO
4)
2Ionic tellurium source can be H
2Te or NaHTe; The mercaptan carboxylic acid can be Thiovanic acid, thiohydracrylic acid or Gelucystine.
3, the preparation method who contains the CdTe nano crystal transparent polymer body phase material as claimed in claim 1, it is characterized in that: polymerisable surfactant is an octadecyl dimethyl Bian Ji vinylbenzene ammonium chloride, by N, N-dimethyl stearyl ammonium and 4-Bian Ji chloro-styrene prepared in reaction.
4, the preparation method who contains the CdTe nano crystal transparent polymer body phase material as claimed in claim 1 is characterized in that: described organic solvent is toluene, chloroform or vinylbenzene.
5, the preparation method who contains the CdTe nano crystal transparent polymer body phase material as claimed in claim 1 is characterized in that: used monomer of bulk polymerization stage can be vinylbenzene, can also be styrene monomer and the monomeric mixture of methyl acrylic ester.
6, the preparation method who contains the CdTe nano crystal transparent polymer body phase material as claimed in claim 1 is characterized in that: nanocrystalline phase transition promptly can be direct extraction, also can be to obtain earlier dissolving behind the powder again.
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| CN109422989B (en) * | 2017-08-30 | 2021-07-09 | 天津大学 | Polymethyl methacrylate-vinyl benzyl dimethyl dodecyl ammonium chloride-barium titanate composite material and preparation method thereof |
| WO2021017904A1 (en) * | 2019-07-31 | 2021-02-04 | Auiset Biotechnology Co. Ltd. | Fabrication of fluorescent nanoparticles and their conjugates for in vitro and in vivo diagnostics |
| CN115232267A (en) * | 2022-07-27 | 2022-10-25 | 吉林大学 | Polymer/nanocrystal hybrid light guide plate and preparation method thereof |
| CN115232267B (en) * | 2022-07-27 | 2023-12-08 | 吉林大学 | Polymer/nanocrystalline hybrid light guide plate and preparation method thereof |
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