CN104877677B - The preparation method of mesoporous silicon oxide/carbon quantum dot nano composite material - Google Patents
The preparation method of mesoporous silicon oxide/carbon quantum dot nano composite material Download PDFInfo
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Abstract
The invention discloses mesoporous silicon oxide/carbon quantum dot nano composite material and preparation method thereof, comprise the steps: the six side ordered mesoporous silica dioxide SBA 15 that the first step uses triblock copolymer P123 to be templated synthesis larger aperture (about 8 nm)；Mesoporous SBA 15 silicon dioxide is impregnated absorption in certain density aqueous citric acid solution by second step, citric acid molecule is filled in the duct of mesoporous SBA 15；3rd step be the SBA 15 by being loaded with citric acid in chamber type electric resistance furnace roasting, i.e. obtain mesoporous silicon oxide/carbon quantum dot nano composite material.The present invention is by carbon quantum dot uniform load to the duct of mesoporous SBA 15, is prepared for a kind of multifunctional nanocomposites with ordered mesopore structure and fluorescence property, and this invention has that preparation technology is simple, reaction condition is gentle and the advantage of environmental protection.
Description
Technical field
The present invention relates to a kind of mesoporous silicon oxide/carbon quantum dot nano composite material, the invention still further relates to is the preparation method of a kind of mesoporous silicon oxide/carbon quantum dot nano composite material.
Background technology
Mesoporous silicon oxide has bigger aperture (more than 2 nm), huge specific surface area and pore volume, and the hole arrangement of high-sequential, aperture size is adjustable in broad range.Additionally, there is abundant silicone hydroxyl on its surface, it is easy to carry out surface modification and modification.Wherein, SBA-15 mesoporous silicon oxide has the cylindrical bore of high-sequential Hexagonal array, and aperture can reach about 8 nm, is conducive to assembling guest molecule and the microreactor as guest molecule reaction in its duct.Compared with tradition mesoporous siliceous MCM-41, SBA-15 heat stability and mechanical performance significantly improve.In recent years, drug molecule is loaded in mesoporous silicon oxide duct, and one of be used for the research just hot subject becoming research of Drug controlled release.But, owing to its surface group is single, again limit its range of application in some field.Therefore, meso-porous titanium dioxide silicon face and duct are carried out modification, cause the great interest of people giving its more performance.
The class ball shaped nano material that carbon quantum dot is a kind of single dispersing, size is less, can emit a brilliant light under light conditions.Compared with other fluorescent materials, carbon quantum dot has the characteristics such as higher, nontoxic, the good water solublity of chemically stable and biocompatibility, in fields such as bio-imaging, biomarker and drug controlled release, there is huge development potentiality and application prospect, increasingly by concern and the attention of research worker, relevant report is the most increasing.Therefore, if being combined with carbon quantum dot by Metaporous silicon dioxide material, a kind of novel multifunctional composite will be obtained, will there is in terms of biomarker, cell imaging and drug controlled release important Research Significance and potential using value.
At present, existing much about the report of fluorescence meso-porous titanium dioxide silicon composite, as by inorganic quantum graftings such as traditional organic fluorescence materials or CdSe in meso-porous titanium dioxide silicon face or duct, but the shortcoming that organic fluorescence materials has fluorescence decay and quencher, and inorganic metal class quantum dot has certain toxicity, greatly limit its range of application, be unfavorable for being applied in biological field.
Summary of the invention
It is an object of the invention to be combined the carbon quantum dot with fluorescence property with mesoporous silicon oxide, obtain a kind of not only there is meso-hole structure but also there is the multifunctional composite of fluorescence property, it is provided that the preparation method of a kind of mesoporous silicon oxide/carbon quantum dot nano composite material.
For achieving the above object, the present invention is by the following technical solutions:
The preparation method of mesoporous silicon oxide/carbon quantum dot nano composite material, comprises the steps:
Step one, the preparation of mesoporous silicon oxide SBA-15, first 2-3 g triblock copolymer P123 is joined in the dilute hydrochloric acid of 100ml 2.0 mol/L, after stirring 2-8 h in 30-42 DEG C of water bath with thermostatic control, it is stirred vigorously in process and is added dropwise over 4-6 g tetraethyl orthosilicate, drip off rear 30-42 DEG C of constant temperature and continue stirring 12-24 h, then aging 12-24 h in this mixed solution being transferred to 75-85 DEG C of baking oven, it is cooled to sucking filtration after room temperature, it is washed with deionized to non-foam, room temperature is dried, and is finally gradually heating to 530-550 in air atmosphere
Roasting 5-6 h after DEG C, obtains white powder material；
Step 2, the preparation of mesoporous silicon oxide/carbon quantum dot presoma, 0.1-0.2 prepared by step one
G white powder material joins in the citric acid solution of 10-20 mL 30-60 mg/mL, seals, the most at room temperature magnetic agitation 10-20 after ultrasound wave dispersion 10-20 min
H, at room temperature dries after the mixed liquor after stirring is sequentially passed through sucking filtration, 15-20 mL deionized water drip washing, sucking filtration, and the solid matter obtained after finally filtering transfers to 100-120oThe baking oven of C is dried 1-2 h, obtains mesoporous silicon oxide/carbon quantum dot presoma；
Step 3, carbon quantum dot growth in mesoporous SBA-15 duct, SBA-15/ carbon quantum dot presoma step 3 prepared carries out roasting in tube type resistance furnace, then room temperature is naturally cooled to, i.e. obtaining yellowish-brown powder, roasting time 2.5-3.5h, calcination atmosphere are nitrogen, temperature 300-350 DEG C；
Step 4, the preparation of mesoporous silicon oxide/carbon quantum dot, step 3 yellowish-brown powder after roasting is first washed with deionized filtrate is colourless, is then passed through dehydrated alcohol drip washing, sucking filtration, is finally 55-60 in temperatureoBeing vacuum dried 10-12h under C, obtain mesoporous silicon oxide/carbon quantum dot nano composite material, product is designated as SBA-15/ carbon quantum dot.
In described step 2, citric acid solution used is that citric acid dissolves in deionized water, or dissolves in ethanol, or dissolving is prepared from acetone.
The concentration adding citric acid solution in described step 2 is 0.03-0.06 g/mL.
In described step 2, used by every 0.1 g pressed powder, the volume of deionized water is at least 15 m
L, drip washing number of times is at least twice.
In described step one and step 3, the heating rate before roasting is 10-20 DEG C/min.
The present invention is directed to problem and defect that prior art intermediary hole silicon dioxide, fluorescent material and fluorescence meso-porous titanium dioxide silicon composite exist, initially with dipping absorption method, citric acid is filled into inside and outside mesoporous SBA-15 duct, and the citric acid of SBA-15 outer surface absorption is washed away by controlling wash conditions, thus enable citric acid molecule basic load in SBA-15 duct, then citric acid molecule processes through high-temperature calcination and generates the carbon quantum dot with fluorescence property.The present invention utilizes mesoporous silicon oxide SBA-15 duct to limit threshold effect, carbon quantum dot is filled uniformly with in SBA-15 duct, it is to avoid duct blocking；Use nontoxic, water solublity preferably and the carbon quantum dot of stable luminescent property is luminescent material；Employing preparation technology is simple, and the method for reaction condition gentleness is prepared for mesoporous silicon oxide/carbon quantum dot composite.Although the researchs of existing many relevant fluorescence Metaporous silicon dioxide materials both at home and abroad and application, but in the meso-porous titanium dioxide silicon hole bigger about carbon quantum dot being assembled into aperture and be used for the research of pharmaceutical carrier and still belong to blank.
Mesoporous silicon oxide prepared by the present invention/carbon quantum dot nano composite material has a following feature: 1) employing mesoporous SBA-15 is material of main part, one is that its good heat stability is especially suitable for using the method for calcining to prepare carbon quantum dot, two are its bigger aperture and uniform duct is suitable to the load of guest molecule citric acid and is used as to generate the microreactor of carbon quantum dot, thus reach mesoporous silicon oxide and carbon quantum dot on a molecular scale compound.2) due to carbon quantum dot uniformly filling in duct, the composite of gained still has the pore structure of both ends open, is suitable as the release that nano-medicament carrier controls and follows the tracks of medicine.3) preparation technology is simple, and reaction condition is gentle, is suitable for industrialization large-scale production.Expect that this composite is applied in terms of the controllable release and tracking of medicine.
Accompanying drawing explanation
Fig. 1 is the mesoporous SBA-15 SEM photograph not loading carbon quantum dot.
Fig. 2 is the mesoporous SBA-15 SEM photograph being loaded with carbon quantum dot.
Fig. 3 SBA-15 and SBA-15/ carbon quantum dot composite XRD figure spectrum.
Fig. 4 carbon quantum dot, SBA-15/ carbon quantum dot composite and the FT-IR collection of illustrative plates of SBA-15.
Fig. 5 SBA-15 and the N of SBA-15/ carbon quantum dot composite2Adsorption-desorption isothermal.
Fig. 6 SBA-15 and the pore-size distribution of SBA-15/ carbon quantum dot composite.
The fluorescence spectrum of Fig. 7 SBA-15/ carbon quantum dot composite.
Detailed description of the invention
Embodiment 1
The preparation method of mesoporous silicon oxide/carbon quantum dot nano composite material, comprises the steps:
Step one, the preparation of mesoporous silicon oxide SBA-15, first 2-3 g triblock copolymer P123 is joined in the dilute hydrochloric acid of 100 ml 2.0 mol/L, after stirring 2-8 h in 30-42 DEG C of water bath with thermostatic control, it is stirred vigorously in process and is added dropwise over 4-6 g tetraethyl orthosilicate, drip off rear 30-42 DEG C of constant temperature and continue stirring 12-24h, then aging 12-24 h in this mixed solution being transferred to 75-85 DEG C of baking oven, it is cooled to sucking filtration after room temperature, it is washed with deionized to non-foam, room temperature is dried, roasting 5-6 h after being finally gradually heating to 530-550 DEG C in air atmosphere, obtain white powder material；
Step 2, the preparation of mesoporous silicon oxide/carbon quantum dot presoma, 0.1-0.2 g white powder material step one prepared joins 10-20
In the citric acid solution of mL 30-60 mg/mL, seal after ultrasound wave dispersion 10-20 min, the most at room temperature magnetic agitation 10-20 h, the mixed liquor after stirring is sequentially passed through sucking filtration, 15-20
At room temperature drying after mL deionized water drip washing, sucking filtration, the solid matter obtained after finally filtering transfers to 100-120oThe baking oven of C is dried 1-2h, obtains mesoporous silicon oxide/carbon quantum dot presoma；
Step 3, carbon quantum dot growth in mesoporous SBA-15 duct, SBA-15/ carbon quantum dot presoma step 2 prepared carries out roasting in tube type resistance furnace, then room temperature is naturally cooled to, i.e. obtaining yellowish-brown powder, roasting time 2.5-3.5 h, calcination atmosphere are nitrogen, temperature 300-350 DEG C；
Step 4, the preparation of mesoporous silicon oxide/carbon quantum dot, step 3 yellowish-brown powder after roasting is first washed with deionized filtrate is colourless, is then passed through dehydrated alcohol drip washing, sucking filtration, is finally 55-60 in temperature
oBeing vacuum dried 10-12 h under C, obtain mesoporous silicon oxide/carbon quantum dot nano composite material, product is designated as SBA-15/ carbon quantum dot.
In described step 2, citric acid solution used is that citric acid dissolves in deionized water, or dissolves in ethanol, or dissolving is prepared from acetone.
The concentration adding citric acid solution in described step 2 is 0.03-0.06 g/mL.
In described step 2, used by every 0.1 g pressed powder, the volume of deionized water is at least 15 m
L, drip washing number of times is at least twice.
In described step one and step 3, the heating rate before roasting is 10-20 DEG C/min.
Embodiment 2
Step one, the preparation of mesoporous silicon oxide SBA-15, the preparation of mesoporous silicon oxide is with nonionic surfactant-triblock copolymer EO20PO70EO20 For template, using typical sol-gel process to prepare, concrete preparation process is: takes 2-3 g triblock copolymer (P123, Ma ≈ 5800) in conical flask, adds the dilute hydrochloric acid 100 of 2.0 mol/L
ML and deionized water 15 mL, 6 h are stirred in 40 DEG C of waters bath with thermostatic control.It is stirred vigorously down and is added dropwise over 4-6 g tetraethyl orthosilicate, drip off rear 40 DEG C of constant temperature and continue stirring 24 h, then this solution is transferred in baking oven aging 24 h at 80 DEG C.Being cooled to sucking filtration after room temperature, be washed with deionized to non-foam, room temperature is dried, and is finally gradually heating to 550 DEG C of roasting 6 h in air atmosphere, obtains white powder SBA-15, heating rate 1oC/min。
Step 2, the preparation of mesoporous silicon oxide/carbon quantum dot presoma, take 0.1 g
The mesoporous SBA-15 of roasting method removed template method P123, in 50m L conical flask, adds in the aqueous citric acid solution of 15 mL 30 mg/mL, and ultrasound wave disperses 15 min, makes the two seal after forming uniform outstanding mixed liquid, magnetic agitation 12 h under room temperature.Then mixed liquor is transferred in cloth funnel, sucking filtration 5min, then with 15 mL deionized water drip washing twice, continue at room temperature to be dried by filter cake after sucking filtration 10 min, be then transferred in baking oven 100oC is dried 2 h.Citric acid solution is to add 0.03g citric acid to be prepared from the deionized water of 100mL.
Step 3, carbon quantum dot growth in mesoporous SBA-15 duct, sample step 2 prepared is placed in ceramic crucible, in tube type resistance furnace 300oC roasting 2.5 hours, calcination atmosphere be nitrogen, heating rate be 10/oC。
Step 4, the preparation of mesoporous silicon oxide/carbon quantum dot, sample prepared by step 3 after roasting is cooled to room temperature, the yellowish-brown powder of preparation is transferred on cloth funnel, sucking filtration also uses a large amount of deionized water wash, until filtrate is colourless, uses 20 m the most again
L dehydrated alcohol drip washing twice, then sucking filtration 10min.Transfer the sample in evaporating dish, 60oC is vacuum dried 12h, and products therefrom is SBA-15/ carbon quantum dot composite.
Embodiment 3
Step one, the preparation of mesoporous silicon oxide SBA-15, the preparation of mesoporous silicon oxide is with nonionic surfactant-triblock copolymer EO20PO70EO20 For template, using typical sol-gel process to prepare, concrete preparation process is: takes 2.5 g triblock copolymers (P123, Ma ≈ 5800) in conical flask, adds the dilute hydrochloric acid 100 of 2.0 mol/L
ML and deionized water 20 mL, 8 h are stirred in 35 DEG C of waters bath with thermostatic control.It is stirred vigorously down and is added dropwise over 5g tetraethyl orthosilicate, drip off rear 40 DEG C of constant temperature and continue stirring 24 h, then this solution is transferred in baking oven aging 20 h at 75 DEG C.Being cooled to sucking filtration after room temperature, be washed with deionized to non-foam, room temperature is dried, and is finally gradually heating to 530 DEG C of roasting 6 h in air atmosphere, obtains white powder SBA-15, heating rate 2oC/min。
Step 2, the preparation of mesoporous silicon oxide/carbon quantum dot presoma, take the mesoporous SBA-15 of 0.2 g roasting method removed template method P123 in 50 m L conical flasks, add in the citric acid ethanol solution of 15 mL 30 mg/mL, ultrasound wave disperses 15 min, the two is made to seal after forming uniform outstanding mixed liquid, magnetic agitation 20 h under room temperature.Then mixed liquor is transferred in cloth funnel, sucking filtration 5min, then with 15 mL deionized water drip washing three times, continue at room temperature to be dried by filter cake after sucking filtration 10 min, be then transferred in baking oven 120oC is dried 1.5 h.Citric acid solution is to add 0.05g citric acid to be prepared from the ethanol of 100mL.
Step 3, carbon quantum dot growth in mesoporous SBA-15 duct, sample step 2 prepared is placed in ceramic crucible, in tube type resistance furnace 350oC roasting 3 hours, calcination atmosphere be nitrogen, heating rate be 20/oC.Then the sample after roasting being cooled to room temperature, transfer on cloth funnel by the yellowish-brown powder of preparation, sucking filtration also uses a large amount of deionized water wash, until filtrate is colourless, uses 20 m the most again
L dehydrated alcohol drip washing twice, then sucking filtration 10 min.
Step 4, the preparation of mesoporous silicon oxide/carbon quantum dot, sample prepared by step 3 after roasting is cooled to room temperature, the yellowish-brown powder of preparation is transferred on cloth funnel, sucking filtration also uses a large amount of deionized water wash, until filtrate is colourless, uses 20 m the most again
L dehydrated alcohol drip washing twice, then sucking filtration 10min.Transfer the sample in evaporating dish, 55oC is vacuum dried 10h, and products therefrom is SBA-15/ carbon quantum dot composite.
Embodiment 4
Step one, the preparation of mesoporous silicon oxide SBA-15, the preparation of mesoporous silicon oxide is with nonionic surfactant-triblock copolymer EO20PO70EO20 For template, using typical sol-gel process to prepare, concrete preparation process is: takes 2.2 g triblock copolymers (P123, Ma ≈ 5800) in conical flask, adds dilute hydrochloric acid 100 mL of 2.0 mol/L
With deionized water 20 mL, 3 h are stirred in 40 DEG C of waters bath with thermostatic control.It is stirred vigorously down and is added dropwise over 5.5g tetraethyl orthosilicate, drip off rear 30 DEG C of constant temperature and continue stirring 24 h, then this solution is transferred in baking oven aging 12h at 80 DEG C.Being cooled to sucking filtration after room temperature, be washed with deionized to non-foam, room temperature is dried, and is finally gradually heating to 550 DEG C of roasting 5h in air atmosphere, obtains white powder SBA-15, heating rate 10oC/min。
Step 2, the preparation of mesoporous silicon oxide/carbon quantum dot presoma, take the mesoporous SBA-15 of 0.1g roasting method removed template method P123 in 50m L conical flask, add in the citric acid acetone soln of 20 mL 30 mg/mL, ultrasound wave disperses 20 min, the two is made to seal after forming uniform outstanding mixed liquid, magnetic agitation 10 h under room temperature.Then mixed liquor is transferred in cloth funnel, sucking filtration 5 min, then with 15 mL deionized water drip washing four times, continue at room temperature to be dried by filter cake after sucking filtration 10 min, be then transferred in baking oven 115oC is dried 1.5 h.Citric acid solution is to add 0.04g citric acid to be prepared from the acetone of 100mL.
Step 3, carbon quantum dot growth in mesoporous SBA-15 duct, sample step 2 prepared is placed in ceramic crucible, in tube type resistance furnace 310oC roasting 3 hours, calcination atmosphere be nitrogen, heating rate be 20/oC.Then the sample after roasting being cooled to room temperature, transfer on cloth funnel by the yellowish-brown powder of preparation, sucking filtration also uses a large amount of deionized water wash, until filtrate is colourless, uses 20 m the most again
L dehydrated alcohol drip washing twice, then sucking filtration 10 min.
Step 4, the preparation of mesoporous silicon oxide/carbon quantum dot, sample prepared by step 3 after roasting is cooled to room temperature, the yellowish-brown powder of preparation is transferred on cloth funnel, sucking filtration also uses a large amount of deionized water wash, until filtrate is colourless, uses 20 m the most again
L dehydrated alcohol drip washing twice, then sucking filtration 10min.Transfer the sample in evaporating dish, 60oC is vacuum dried 11h, and products therefrom is SBA-15/ carbon quantum dot composite.
Embodiment 5-16
Implementing step such as embodiment 2, concrete technology parameter is as shown in table 1:
Laboratory test results
The sample used in the middle of this experiment test is that embodiment 2 prepares, the model of XRD figure spectrum test employing instrument is: D8 FOCUS(Germany Bruker), excitation and emission spectra figure employing INSTRUMENT MODEL is: FLS920P(Edinburgh, Britain), Fourier transform infrared spectroscopy employing INSTRUMENT MODEL is: (U.S.'s thermoelectricity), N2Adsorption/desorption isotherms test uses Merck & Co., Inc of INSTRUMENT MODEL: the ASAP 2020 HD88(U.S.), the INSTRUMENT MODEL that electron scanning micrograph uses is: FEI Co. of the Quanta 200(U.S.).
SEM tests: from sample drawing 1 with the photo of Fig. 2 it can be seen that SBA-15/ carbon quantum dot composite has the pattern similar to SBA-15, the club shaped structure of the most about 3-5 micron.Meanwhile, do not observe the existence of SBA-15 outer surface carbon quantum dot, show that carbon quantum dot is mainly distributed in the duct of SBA-15.
XRD tests: in Fig. 3, a is the diffracting spectrum of SBA-15, b is the diffracting spectrum after carbon quantum dot load SBA-15, can be seen that from the collection of illustrative plates of sample drawing 3, in the duct of the SBA-15 of carbon quantum dot load, afterproduct still has orderly hexagonal mesoporous structure, does not destroys the order mesoporous pore structure of SBA-15 during illustrating to synthesize carbon quantum dot in SBA-15 duct.
FT-IR tests: in Fig. 4, a, b, c are respectively carbon quantum dot, SBA-15/ carbon quantum dot composite, the FT-IR collection of illustrative plates of SBA-15.Figure 4, it is seen that SBA-15/ carbon quantum dot composite is in addition to the typical absorption peak of SBA-15, also 2927cm-1,801
The characteristic absorption peak of carbon quantum dot occurs at cm-1, shows that carbon quantum dot the most successfully loads in SBA-15 duct.
N2Adsorption-desorption isothermal is tested: in Fig. 5, a, b are respectively the N2 adsorption-desorption isothermal of SBA-15 and SBA-15/ carbon quantum dot composite.From the point of view of the low temperature N2 adsorption-desorption isothermal of sample, the adsorption isotherm of SBA-15 and SBA-15/ carbon quantum dot composite is the adsorption isotherm (IV type isothermal line) of typical mesoporous material, shows that SBA-15/ carbon quantum dot composite is typical mesoporous material.In addition, be it can also be seen that by Fig. 5, the suction of SBA-15/ carbon quantum dot composite, desorption curve hysteresis loop are typical H1 type hysteresis loop, show that carbon quantum dot is filled into SBA-15 duct composite and still has the pore structure of both ends open, carbon quantum dot the duct of unplugged SBA-15.From Fig. 6 (pore-size distribution of a, respectively SBA-15 and SBA-15/ carbon quantum dot composite).From the absorption graph of pore diameter distribution of sample it can be seen that the aperture of SBA-15/ carbon quantum dot composite and SBA-15 project are than about decreasing 0.7
Nm, shows that carbon quantum dot has been filled in the duct of SBA-15 really.The data of table 2 are further characterized by carbon quantum dot and successfully load in mesoporous silicon oxide SBA-15 duct.
Fluorescent emission and excitation spectrum test: Fig. 7 is fluorescent emission and the excitation spectrum of SBA-15/ carbon quantum dot composite, can be seen that, with 260nm ultraviolet as excitation wavelength, SBA-15/ carbon quantum dot composite has strong emission peak at 510 nm, shows that this composite has preferable luminescent properties.
Claims (5)
1. the preparation method of mesoporous silicon oxide/carbon quantum dot nano composite material, it is characterised in that comprise the steps:
Step one, the preparation of mesoporous silicon oxide SBA-15, first 2-3g triblock copolymer P123 is joined in the dilute hydrochloric acid of 100 ml 2.0 mol/L, 2-8 h is stirred in 30-42 DEG C of water bath with thermostatic control, whipping process adds 4-6 g tetraethyl orthosilicate, after addition, 30-42 DEG C of constant temperature continues stirring 12-24h, then aging 12-24h in this mixed solution being transferred to 75-85 DEG C of baking oven, it is cooled to sucking filtration after room temperature, it is washed with deionized to non-foam, room temperature is dried, roasting 5-6 h after being finally gradually heating to 530-550 DEG C in air atmosphere, obtain white powder material；
Step 2, the preparation of mesoporous silicon oxide/carbon quantum dot presoma, 0.1-0.2g white powder material step one prepared joins 10-20 mL
In the citric acid solution of 30-60 mg/mL, ultrasound wave dispersion 10-20
Sealing after min, the most at room temperature magnetic agitation 10-20 h, at room temperature dry after the mixed liquor after stirring is sequentially passed through sucking filtration, deionized water drip washing, sucking filtration, the solid matter obtained after finally filtering transfers to 100-120oThe baking oven of C is dried 1-2h, obtains SBA-15/ carbon quantum dot presoma；
Step 3, carbon quantum dot growth in mesoporous SBA-15 duct, SBA-15/ carbon quantum dot presoma step 2 prepared carries out roasting in tube type resistance furnace, then room temperature is naturally cooled to, i.e. obtaining yellowish-brown powder, roasting time 2.5-3.5h, calcination atmosphere are nitrogen, temperature 300-350 DEG C；
Step 4, the preparation of mesoporous silicon oxide/carbon quantum dot composite, step 3 yellowish-brown powder after roasting is first washed with deionized filtrate is colourless, is then passed through dehydrated alcohol drip washing, sucking filtration, is finally 55-60 in temperatureoIt is vacuum dried 10-12 h under C, obtains mesoporous silicon oxide/carbon quantum dot nano composite material.
The preparation method of mesoporous silicon oxide the most according to claim 1/carbon quantum dot nano composite material, it is characterized in that: in described step 2, citric acid solution used is that citric acid dissolves in deionized water, or dissolve in ethanol, or dissolving is prepared from acetone.
The preparation method of mesoporous silicon oxide the most according to claim 2/carbon quantum dot nano composite material, it is characterised in that: in described step 2, the concentration of citric acid is 0.03-0.06g/mL.
4. according to the preparation method of the mesoporous silicon oxide described in claim 1 or 3/carbon quantum dot nano composite material, it is characterised in that: in described step 2, used by every 0.1g pressed powder, the volume of deionized water is at least 15 m L, and drip washing number of times is at least twice.
The preparation method of mesoporous silicon oxide the most according to claim 1/carbon quantum dot nano composite material, it is characterised in that: in described step one and step 3, heating rate during roasting is 10-20 DEG C/min.
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| CN115322774B (en) * | 2022-06-20 | 2023-12-05 | 爱科美材料科技(南通)有限公司 | Wen Luguang-resistant fluorescent powder and preparation method thereof |
| CN116440940B (en) * | 2023-06-14 | 2023-08-15 | 北京兴德通医药科技股份有限公司 | Carbon quantum dot catalyst, preparation method thereof and prepared carbon quantum dot |
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| CN102994080B (en) * | 2012-12-07 | 2014-07-09 | 上海大学 | Method for preparing fluoresent carbon nanoparticles |
| CN103484111B (en) * | 2013-09-13 | 2016-06-08 | 中国科学院宁波材料技术与工程研究所 | Mesoporous silicon fluorescent material and preparation method |
| CN103466600B (en) * | 2013-09-26 | 2015-04-22 | 沈阳大学 | Preparation method of environment-friendly low-toxic fluorescent carbon nano particle liquor |
| CN103771391B (en) * | 2014-01-21 | 2016-04-13 | 中国计量学院 | A kind of preparation method with the water-soluble carbon nano-particles of photoluminescent property |
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