CN105602567A - Application of tellurium mercury cadmium quantum dot and carbon nanotube nanocomposite to improving light conversion efficiency - Google Patents
Application of tellurium mercury cadmium quantum dot and carbon nanotube nanocomposite to improving light conversion efficiency Download PDFInfo
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Abstract
The invention discloses application of a tellurium mercury cadmium quantum dot and carbon nanotube composite to improving light conversion efficiency. A CdTe quantum dot solution is first prepared; then Hg is add to obtain CdHgTe quantum dots; and finally adhering cadmium mercury telluride quantum dots on the surface of carbon nanotubes as the skeleton. The technical scheme of the invention has simple conditions, low cost and easy operation. The near-infrared tellurium mercury cadmium quantum dot and carbon nanotube composite can greatly improve the conversion efficiency of light, and has a good application prospect.
Description
The present patent application is female case application " a kind of tellurium mercury cadmium quantum dot and carbon nanotube composite materials and preparation method thereof "Divisional application, the application number of female case application is 201310636557X, the applying date of female case application is December 2 in 2013Day.
Technical field
The invention belongs to nano composite material technical field, more particularly, relate to visible near-infrared regulate and control tellurium mercury cadmiumTernary alloy nano crystalline substance and carbon nanotube composite materials and preparation method thereof.
Background technology
The nano composite material that the quantum dot that with gap is adjustable and CNT are compounded to form to the performance of regulation and control photoelectric device (tooSun can battery and photodetector) a kind of new thinking (KhalavkaY, SonnichsenC, Growthofgold be providedTipsontohyperbranchedCdTenanostructures, AdvancedMaterrials, 2008,20:588-591.). ?In recent years, on synthetic quantum dot and carbon nano tube compound material, obtained good progress. Research shows, in carbon nanometerPipe tube-surface is coated one deck quantum dot, due to the dimensional effect of quantum dot, and many advantages such as easy photoexcitation, therefore thisNano composite material is expected to for fiberopticscommunication, the fields such as light emitting diode and photoelectric cell (SunWT, YuY, PanHY,GaoXF,ChenQ,PengLM,CdSquantumdotssensitizedTiO2nanotube-arrayphotoelectrodes,JournaloftheAmericanChemicalSociety,2008,130:1124-1125)。
In quantum dot and composite structure of carbon nano tube, quantum dot plays an effect of catching light activated electronics, will catchThe electronics receiving is transferred to CNT, and CNT can be used as an electron propagation ducts, can promptly electronics be passedBe passed on electrode. But quantum dot used is nearly all to absorb in the quantum dot of having reported and carbon nano tube compound materialScope is at visible region, as CdTe, CdSe (YuKH, LuGH, ChenKH, MaoS, KimHJ, ChenJH,ControllablephotoelectrontransferinCdSenanocrystal–carbonnanotubehybridstructures,Nanoscale, 2012,4:742) etc. These quantum dots are because light abstraction width is at visible region (400-700nm), rightThe absorption efficiency of sunshine is very low. The light conversion efficiency of making photoelectric device after compound with CNT is low, and has reportedCompound method be all mostly in oil phase, very complicated, need high temperature, and raw material is harmful.
Tellurium mercury cadmium (MCT) is a kind of very important II-VI family near-infrared ternary alloy three-partalloy semi-conducting material, can be by controllingThe ratio of Hg/Cd can enable bandwidth between-0.15 to 1.6eV arbitrarily variation (McMillanBG, LilleySJ,BerlouisLEA,CruickshankFR,BrevetPF,OpticalcharacterizationofanodicsulphidefilmsOnHgCdTe (MCT) grownbythepotentialstepmethod, Electrochim.Acta, 2004,49:1339), canGreatly to improve light conversion efficiency. Therefore, by CNT and tellurium mercury cadmium quantum dot the two be assembled into one nano combinedThe application prospect of material is very big. Also do not have at present by CNT and tellurium mercury cadmium quantum dot, the two is assembled into oneThe report of individual nano composite material.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of water miscible tellurium mercury with good dispersion is providedCadmium quantum dot and carbon nanotube composite materials and preparation method thereof, the method condition is simple, with low cost, receives with carbonMitron is skeleton, and surface adhesion tellurium mercury cadmium.
Technical purpose of the present invention is achieved by following technical proposals:
A kind of tellurium mercury cadmium quantum dot and carbon nanotube composite materials and preparation method thereof, taking CNT as skeleton, tableFace is adhering to tellurium mercury cadmium quantum dot, is prepared according to following step:
Step 1, by CdC12·2.5H2O and TGA (TGA) are dissolved in and in deionized water, obtain mixed solution, andUse NaOH adjustment pH value is 11.0～12.0 and passes into inert gas removal oxygen, obtains A solution;
Specifically, by CdC12·2.5H2O and TGA are dissolved in deionized water and obtain mixed solution, use 1MIt is 11.0～12.0 that the NaoH aqueous solution is adjusted to pH value, then gained solution is poured in there-necked flask into logical argon gas under stirring at room temperature(or nitrogen, helium) deoxygenation 20～30min, is designated as A solution.
Step 2 utilizes inert gas to remove oxygen, by KBH in sealed reactor4With Te powder add to fromIn sub-water, obtain mixed solution, i.e. B solution;
Specifically, in the airtight little reaction bulb with pin hole, by KBH4Be dissolved in deionized water and obtain with Te powderTo mixed solution, and utilize argon gas to get rid of oxygen, under magnetic agitation, under 20-25 degrees Celsius of room temperatures, react 30～60min,Obtain lilac transparency liquid, the KHTe aqueous solution of fresh anaerobic, is designated as B solution.
Step 3, under isolated air conditions, is used syringe to take out B solution and is injected in A solution, will mixSolution is heated to 100～130 DEG C, and under magnetic agitation, back flow reaction 2～3h obtains CdTe quantum dot solution;
Specifically, under the condition of isolated air, with syringe taking-up B solution, be injected into fast and contain AIn the there-necked flask of solution, then mixed solution is heated to 100～130 DEG C, under magnetic agitation, back flow reaction 2～3h obtainsTo CdTe quantum dot solution.
Step 4, by Hg (ClO4)2·3H2O and TGA are dissolved in and in deionized water, obtain mixed solution, and useIt is 11.0～12.0 that NaOH is adjusted pH value, is designated as C solution, get C injection of solution and enter CdTe quantum dot solution,At least 12h of back flow reaction under magnetic agitation, preferably 12-24h, can obtain near-infrared CdHgTe quantum dot;
Specifically, by Hg (ClO4)2·3H2O and TGA are dissolved in deionized water and obtain mixed solution, mixedClosing the solution 1MNaoH aqueous solution, to be adjusted to pH value be 11.0～12.0, gets a certain amount of mixed solution injection and enter CdTeQuantum dot solution, back flow reaction 12h under magnetic agitation, can obtain near-infrared CdHgTe quantum dot.
Step 5, is well dispersed in deionized water it by ultrasonic the multi-walled carbon nano-tubes of acidifying, willNaCl, NaOH, polydiene propyl-dimethyl amine hydrochlorate (PDDA) are M (NaCl) in mass ratio:M (NaOH): M (PDDA)=1.16:1.6:2 adds in the aqueous solution that is dispersed with CNT, ultrasonicly makes it abundantMix, by the centrifugal supernatant that removes, precipitation is dissolved in deionized water again to the tellurium that adds step 4 to prepareMercury cadmium quantum dot, ultrasonic centrifugal, remove supernatant, product cleaning is dry, be tellurium mercury cadmium quantum dot and carbon and receiveThe composite of mitron;
Specifically, the multi-walled carbon nano-tubes of described acidifying carries out according to following step: by multi-walled carbon nano-tubes at V(dense H2SO4): V (dense HNO3In the mixed acid of)=3:1, mix, under room temperature, ultrasonic dispersion 30min, then putsIn there-necked flask, at 90 DEG C, stir acidification 8h, be cooled to after room temperature with distilled water diluting, and with aperture G5'sFilter tunnel vacuum filtration, filtrate, again with distilled water diluting vacuum filtration, is repeatedly cleaned to neutral, and product is in 80 DEG CVacuum drying 24h can obtain the MWNTs of acidifying.
Use model TecnaiG2The field transmission electron microscope of F20 characterizes product, as 1-4, accompanying drawingShow, the distribution of sizes homogeneous of prepared CdHgTe quantum dot, size is 4-5nm (shown in Fig. 1), CNTDiameter probably at about 20nm (shown in Fig. 2), CdHgTe quantum dot can well be attached to CNTUpper, between quantum dot, there is not large-area reunion (shown in Fig. 3), can the amount of being clear that from Fig. 4The lattice of son point and the tube wall situation of CNT, also further illustrate quantum dot and well stick to carbon nanometerGuan Shang.
Utilize Keithley (Keithley) 2635 type single channel system digital sourcemeters to carry out the nanometer of CNT/quantum dotThe I-V curved measurement of composite, in figure, 1 is the result of measuring in dark, 2 for adding the result of measuring after illumination,3 for removing the result of again measuring in the dark after illumination, can find out to have added after illumination, and the electric current of material is obviousThere is variation, after illumination removes, can substantially be returned to again original result, as shown in Figure 5. Utilize luckyThe nano composite material of CNT/quantum dot that Shi Li (Keithley) 2635 type single channel system digital sourcemeters are measuredAnd the photoswitch of pure quantum dot, 1 photoswitch that is pure quantum dot in figure, 2 photoswitches that are composite,In Fig. 6, in the time adding illumination, the photoelectric current of pure quantum dot and nano material all increases, remove illumination after photoelectric current allReduce, but the variation of pure quantum dot is not obvious, the nano composite material of CNT/quantum dot is not in the time of illumination andWhen illumination, photoelectric current Strength Changes is very obvious. Illustrate that this material has good photoelectricity corresponding.
The present invention use near-infrared tellurium mercury cadmium quantum dot and CNT compound, the side of preparing quantum dot and compositeMethod is all that condition is simple, with low cost, and easily operation. After near-infrared tellurium mercury cadmium quantum dot and CNT are compoundCan greatly improve light conversion efficiency, have good application prospect.
Brief description of the drawings
Fig. 1 is tellurium mercury cadmium quantum dot transmission electron microscope photo (TEM) prepared by the present invention.
Fig. 2 is the transmission electron microscope photo that does not add the pure nano-carbon tube of quantum dot.
Fig. 3 be in CNT, add CNT/quantum dot nano composite of preparing after CdHgTe quantum dot thoroughlyRadio mirror figure.
Fig. 4 is the high-resolution transmission plot of the nano composite material prepared of the present invention.
Fig. 5 is the I-V curve of the nano composite material of CNT/quantum dot of preparing of the present invention, and in figure, 1 is in darkThe result of measuring, 2 for adding the result of measuring after illumination, and 3 for removing the result of again measuring in the dark after illumination.
Fig. 6 is the nano composite material of CNT/quantum dot and the photoswitch figure (horizontal stroke of pure quantum dot prepared by the present inventionCoordinate is the time, and ordinate is photoelectric current intensity), 1 photoswitch that is pure quantum dot in figure, 2 is compositePhotoswitch.
Detailed description of the invention
Further illustrate technical scheme of the present invention below in conjunction with specific embodiment. First CNT is carried out to acidificationAs follows: by multi-walled carbon nano-tubes at V (dense H2SO4): V (dense HNO3In the mixed acid of)=3:1, mix room temperature 20Ultrasonic dispersion 30min under-25 degrees Celsius, is then placed in there-necked flask and at 90 DEG C, stirs acidification 8h, is cooled to chamberWen Houyong distilled water diluting, and with the filter tunnel vacuum filtration of aperture G5, filtrate is again by distilled water diluting vacuum mistakeFilter, repeatedly cleans to neutral, and product can obtain the MWNTs of acidifying in 80 DEG C of vacuum drying 24h.
Embodiment 1
(1) preparation of cadmium telluride
By 87.5mgCdC12·2.5H2O and 96 μ LTGA are dissolved in 100mL deionized water, mixed solution 1MNaoHBeing adjusted to pH value is 12, then gained solution is poured in there-necked flask, and under stirring at room temperature, logical argon gas deoxygenation 30min, is designated asA solution. In airtight little reaction bulb at another with pin hole, by 50mgKBH4Be dissolved in 27mgTe powderIn 3mL deionized water, room temperature reaction 60min under magnetic agitation, obtains lilac transparency liquid, i.e. fresh anaerobicThe KHTe aqueous solution, be designated as B solution. Under the condition of isolated air, take out the B of 1.5mL with syringeSolution, is injected in the there-necked flask that contains A solution fast. Then mixed solution is heated to 120 DEG C, magnetic force stirsMix lower back flow reaction 3h. Can obtain CdTe quantum dot.
(2) preparation of tellurium mercury cadmium
Take 179.8mgHg (ClO4) 2 and 96 μ LTGA and be dissolved in 100mL deionized water, mixed solution 1MNaoHBeing adjusted to pH value is 12, removes the oxygen in solution, gets 10ml and is injected into fast in CdTe quantum dot solution. ContinueBack flow reaction 12h under magnetic agitation, obtains CdHgTe quantum dot.
(3) preparation of nano composite material
The multi-walled carbon nano-tubes of 1mg acidifying is fully dissolved in 40ml water, add 1.16gNaCl, 1.6gNaOH,200 μ l polydiene propyl-dimethyl amine hydrochlorates, ultrasonic a period of time is fully mixed it, removes supernatant after centrifugalBeing dissolved in deionized water, add 1.5ml tellurium mercury cadmium quantum dot, ultrasonic a period of time, centrifugal, remove supernatantLiquid, goes to precipitate and washs dry, obtains the composite of tellurium mercury cadmium and CNT
Embodiment 2
(1) preparation of cadmium telluride
By 137.4mgCdC12·2.5H2O and 157 μ LTGA are dissolved in 100mL deionized water, mixed solution 1MNaoHBeing adjusted to pH value is 11.5, then gained solution is poured in there-necked flask into logical argon gas deoxygenation 30min under stirring at room temperature, noteFor A solution. In airtight little reaction bulb at another with pin hole, by 50mgKBH4Molten with 27mgTe powderIn 3mL deionized water, room temperature reaction 60min under magnetic agitation, obtains lilac transparency liquid, i.e. fresh nothingThe KHTe aqueous solution of oxygen, is designated as B solution. Under the condition of isolated air, take out the B of 1.5mL with syringeSolution, is injected in the there-necked flask that contains A solution fast. Then mixed solution is heated to 120 DEG C, magnetic force stirsMix lower back flow reaction 3h. Can obtain CdTe quantum dot.
(2) preparation of tellurium mercury cadmium
Take 179.8mgHg (ClO4) 2 and 96 μ LTGA and be dissolved in 100mL deionized water, mixed solution 1MNaoHBeing adjusted to pH value is 11.5, removes the oxygen in solution, gets 20ml and is injected into fast in CdTe quantum dot solution. ContinueBack flow reaction 20h under continuous magnetic agitation, obtains CdHgTe quantum dot.
(3) preparation of nano composite material
The multi-walled carbon nano-tubes of 1mg acidifying is fully dissolved in 40ml water, add 1.16gNaCl, 1.6gNaOH,200 μ l polydiene propyl-dimethyl amine hydrochlorates, ultrasonic a period of time is fully mixed it, removes supernatant after centrifugalBeing dissolved in deionized water, add 1.5ml tellurium mercury cadmium quantum dot, ultrasonic a period of time, centrifugal, remove supernatantLiquid, goes to precipitate and washs dry, obtains the composite of tellurium mercury cadmium and CNT
Embodiment 3
(1) preparation of cadmium telluride
By 87.5mgCdC12·2.5H2O and 96 μ LTGA are dissolved in 100mL deionized water, mixed solution 1MNaoHBeing adjusted to pH value is 11, then gained solution is poured in there-necked flask, and under stirring at room temperature, logical argon gas deoxygenation 30min, is designated asA solution. In airtight little reaction bulb at another with pin hole, by 50mgKBH4Be dissolved in 27mgTe powderIn 3mL deionized water, room temperature reaction 60min under magnetic agitation, obtains lilac transparency liquid, i.e. fresh anaerobicThe KHTe aqueous solution, be designated as B solution. Under the condition of isolated air, take out the B of 1.5mL with syringeSolution, is injected in the there-necked flask that contains A solution fast. Then mixed solution is heated to 120 DEG C, magnetic force stirsMix lower back flow reaction 3h. Can obtain CdTe quantum dot.
(2) preparation of tellurium mercury cadmium
Take 208mgHg (ClO4) 2 and 114 μ LTGA and be dissolved in 100mL deionized water, mixed solution 1MNaoHBeing adjusted to pH value is 11, removes the oxygen in solution, gets 50ml and is injected into fast in CdTe quantum dot solution. ContinueBack flow reaction 24h under magnetic agitation, obtains CdHgTe quantum dot.
(3) preparation of nano composite material
The multi-walled carbon nano-tubes of 5mg acidifying is fully dissolved in 200ml water, add 5.16gNaCl, 6.6gNaOH,200 μ l polydiene propyl-dimethyl amine hydrochlorates, ultrasonic a period of time is fully mixed it, removes supernatant after centrifugalBeing dissolved in deionized water, add 7.5ml tellurium mercury cadmium quantum dot, ultrasonic a period of time, centrifugal, remove supernatantLiquid, goes to precipitate and washs dry, obtains the composite of tellurium mercury cadmium and CNT
Above the present invention is done to exemplary description, should be noted that in the situation that not departing from core of the present invention,The replacement that is equal to that any simple distortion, amendment or other those skilled in the art can not spend creative work all fallsEnter protection scope of the present invention.
Claims (5)
1. tellurium mercury cadmium quantum dot and carbon nanotube composite materials are in the application improving in light conversion efficiency, and its feature existsIn, tellurium mercury cadmium quantum dot and carbon nanotube composite materials are taking CNT as skeleton, and surface adhesion tellurium mercury cadmium quantumPoint, is prepared according to following step:
Step 1, by CdC12·2.5H2O and TGA are dissolved in and in deionized water, obtain mixed solution, and use hydrogen-oxygenChange sodium adjustment pH value is 11.0～12.0 and passes into inert gas removal oxygen, obtains A solution;
Step 2 utilizes inert gas to remove oxygen, by KBH in sealed reactor4With Te powder add to fromIn sub-water, obtain mixed solution, i.e. B solution;
Step 3, under isolated air conditions, is used syringe to take out B solution and is injected in A solution, will mixSolution is heated to 100～130 DEG C, and under magnetic agitation, back flow reaction 2～3h obtains CdTe quantum dot solution;
Step 4, by Hg (ClO4)2·3H2O and TGA are dissolved in and in deionized water, obtain mixed solution, and useIt is 11.0～12.0 that NaOH is adjusted pH value, is designated as C solution, get C injection of solution and enter CdTe quantum dot solution,At least 12h of back flow reaction under magnetic agitation, can obtain near-infrared CdHgTe quantum dot;
Step 5, is well dispersed in deionized water it by ultrasonic the multi-walled carbon nano-tubes of acidifying, willNaCl, NaOH, polydiene propyl-dimethyl amine hydrochlorate are M (NaCl) in mass ratio:M (NaOH): M (PDDA)=1.16:1.6:2 adds in the aqueous solution that is dispersed with CNT, ultrasonicly makes it abundantMix, by the centrifugal supernatant that removes, precipitation is dissolved in deionized water again to the tellurium that adds step 4 to prepareMercury cadmium quantum dot, ultrasonic centrifugal, remove supernatant, product cleaning is dry, be tellurium mercury cadmium quantum dot and carbon and receiveThe composite of mitron.
2. tellurium mercury cadmium quantum dot according to claim 1 and carbon nanotube composite materials are improving light conversion efficiencyIn application, it is characterized in that, in described step 1, inert gas select argon gas, nitrogen or helium, deoxygenation20～30min。
3. tellurium mercury cadmium quantum dot according to claim 1 and carbon nanotube composite materials are improving light conversion effectApplication in rate, is characterized in that, in described step 2, inert gas is selected argon gas, nitrogen or helium, willKBH4Be dissolved in and in deionized water, obtain mixed solution with Te powder, reaction under 20-25 degrees Celsius of room temperatures under magnetic agitation30～60min, obtains lilac transparency liquid, and the KHTe aqueous solution of fresh anaerobic, is designated as B solution.
4. tellurium mercury cadmium quantum dot according to claim 1 and carbon nanotube composite materials are improving light conversion effectApplication in rate, is characterized in that, in described step 4, and preferably 12-24h of back flow reaction under magnetic agitation.
5. tellurium mercury cadmium quantum dot according to claim 1 and carbon nanotube composite materials are improving light conversion effectApplication in rate, is characterized in that, in described step 5, the multi-walled carbon nano-tubes of described acidifying is according to followingStep is carried out: by multi-walled carbon nano-tubes at volume ratio V (dense H2SO4): V (dense HNO3In the mixed acid of)=3:1, mixEvenly, ultrasonic dispersion 30min under room temperature, is then placed in there-necked flask and at 90 DEG C, stirs acidification 8h, is cooled toAfter room temperature, with distilled water diluting, and with the filter tunnel vacuum filtration of aperture G5, filtrate is again by distilled water diluting vacuumFilter, repeatedly clean to neutral, product can obtain the MWNTs of acidifying in 80 DEG C of vacuum drying 24h.
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| CN114217012B (en) * | 2021-11-10 | 2023-09-12 | 中国科学院上海技术物理研究所 | In-situ modification method in mercury system quantum dot traditional heat injection flow |
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| CN102557002B (en) * | 2011-11-29 | 2013-10-16 | 上海师范大学 | Carbon nanotube/ternary chalcogenide semiconductor nano composite material and preparation method thereof |
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| CN108743973A (en) * | 2018-05-25 | 2018-11-06 | 宁夏医科大学 | Stratiform magnetic fluorescence multifunctional nano carries powder |
| CN108822854A (en) * | 2018-06-06 | 2018-11-16 | 澳洋集团有限公司 | A kind of preparation method of semiconductor selenide-carbon nano tube compound material |
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| CN105419803A (en) | 2016-03-23 |
| CN105419803B (en) | 2017-08-08 |
| CN104673316A (en) | 2015-06-03 |
| CN104673316B (en) | 2016-08-17 |
| CN105602567B (en) | 2017-08-08 |
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