CN102719248A - Aqueous phase silicon carbide quantum dot and preparation method and application thereof - Google Patents
Aqueous phase silicon carbide quantum dot and preparation method and application thereof Download PDFInfo
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- CN102719248A CN102719248A CN2012102083828A CN201210208382A CN102719248A CN 102719248 A CN102719248 A CN 102719248A CN 2012102083828 A CN2012102083828 A CN 2012102083828A CN 201210208382 A CN201210208382 A CN 201210208382A CN 102719248 A CN102719248 A CN 102719248A
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Abstract
The invention relates to the technical field of biological application of quantum dots, in particular to a non-cytotoxicity aqueous phase silicon carbide quantum dot and a preparation method thereof, and application of the quantum dot as a fluorescent material. The preparation method comprises the following steps: firstly, corroding homogeneous nano beta-SiC particles synthesized by auto-combustion into a mesh structure with corrosive liquid prepared by mixing nitric acid and hydrofluoric acid; secondly, smashing the structure by the cavitation effect of an ultrasonic wave to form silicon carbide nano particles of different sizes; and finally, centrifuging the silicon carbide nano particles at a high speed to obtain quantum dots with controllable sizes, and applying the quantum dots to the fluorescent labeling and imaging of living cells successfully for the first time. The process is simple, the cost is low and the process parameters are easy to control; besides, the prepared quantum dots are non-toxic, excellent in biocompatibility, and obvious in photoluminescence effect, and can be applied to the fluorescent labeling of living cells for a long time.
Description
Technical field
The present invention relates to the biologic applications technical field of quantum dot, be specifically related to a kind of no cytotoxicity water silit quantum dot and preparation method thereof, and this quantum dot is to the application in the active somatic cell fluorescent mark.
Background technology
Follow the development of nano-carbon materials such as C60, CNT and Graphene; Quantum dot is because its remarkable fluorescence property and in the widespread use of biomedical sector; Become the focus of people's research gradually, its compound method mainly is divided into organic synthesis and water-based is synthetic.Therefore the quantum dot of organic synthesis can not directly apply to living things system owing to do not possess wetting ability, must carry out finishing and biological functional processing to it, complicated operating process, and conditional request is higher; The method of the synthetic quantum dot of water is because green, inexpensive more and more comes into one's own, and the research work of relevant this respect makes fast progress.
Up-to-date result of study shows; There are poisonous elements such as Cd, Se in the quantum dot that generally adopts at present; Can reduce greatly though there are some researches show quantum dot toxicity, still can not be ignored to the murder by poisoning enrichment of life entity and to active somatic cell, the physiological influence of the long-time section growth of tissue through the surface parcel.Simultaneously, the toxicant in quantum dot raw material and the preparation process all has detrimentally affect to environment and operator.In addition, to be difficult to effective regulation and control also be the important factor that further develops of this biological nano material of restriction to the quantum dot dimensional structure.Therefore, the quanta point material that utilizes the water method to prepare no cytotoxicity, surface tissue and controllable size has become the common recognition of current biology and material educational circles.
Summary of the invention
In order to overcome the above problems, the invention provides a kind of water silit quantum dot and preparation method thereof, and the first Application that it is successful is in the active somatic cell fluorescent dye.
Silit quantum dot concentration is 0.03-0.06mol/L in the water silit quanta point material of the present invention, and it is closely spherical that quantum dot is, and diameter is 2-5nm.In order to adapt to the application of this material of later stage on active somatic cell, the pH value of this water silit quanta point material is 6.4-6.8.
The concrete steps of its preparation are:
A. be that 40% hydrofluoric acid and mass concentration are that 65% nitric acid is mixed with corrosive fluid according to volume ratio 3:1 with mass concentration, and stir;
B. self-propagating combustion synthetic homogeneous nano β-SiC powder is placed the corrosive fluid of steps A configuration, stirring reaction, β-SiC grain diameter is 50-100nm;
C. with the mixture standing and reacting among the step B;
D. with said mixture centrifugal after, extract corrosive fluid out, add high purity water, the SiC particle after utilizing high purity water to corrosion carries out eccentric cleaning;
E. the aqueous solution after the eccentric cleaning is carried out supersound process;
F. the aqueous solution through supersound process is carried out centrifugal treating, get supernatant and be silit Quantum Dot Labeling material, centrifugal speed is 2800-3000rpm.
At first, the present invention is diluted to suitable concentration with commercial concentrated nitric acid and hydrofluoric acid with high purity water, and is configured to corrosive fluid.The contriver because the corrosion process in later stage is an exothermic process, if the proportioning of two kinds of acidic solutions surpasses this ratio, react very violent through experiment showed, that repeatedly hydrofluoric acid and the optimum proportion of salpeter solution after the dilution are 3:1, and experimentation is difficult to be controlled; If be lower than this ratio, react comparatively slow, the quantum dot that finally obtains is less.
The raw material that the present invention adopts is self-propagating combustion synthetic homogeneous nano β-SiC particle (Physical Chemistry Technology Inst., Chinese Academy of Sciences provides); Why select self-propagating combustion synthetic β-SiC particle for use; Be because in its self-propagating combustion reaction process, cool off rapidly, thereby form non-equilibrium crystallization condition, make β-SiC particle surface form more defective (lattice distortion etc.); Active higher; The corrosion intensity of activation is lower, and very easily corrosion forms fenestral fabric in hydrofluoric acid solution, and this structure is the later stage to obtain tiny nearly spherical quantum dot through ultrasonic cavitation to have established condition.In addition, the nitric acid in the corrosive fluid of the present invention has oxidisability, has further strengthened the corrosive nature of corrosive fluid, has reached better corrosive effect.The SiC that this method has been abandoned the chemical synthesis preparation must adopt galvanic corrosion could form the tradition of quantum dot nano-particle.
β-SiC grain diameter is more little, the fenestral fabric of perishable more one-tenth open type, and the quantum dot quantity of acquisition is many more, and promptly quantum yield is high approximately; If particle diameter is too big, then can not be etched into fenestral fabric, the quantum dot of formation is less.In order to obtain quantum dot more and that particle diameter is controlled, β-SiC grain diameter is 50-100nm.
Find in the experimentation,, also produce certain gas as β-when the SiC particle places in the corrosive fluid, can emit big calorimetric; Because β-SiC particle is very little,, can forms bigger bubble and be difficult for breaking attached to the bubble surface; So, just begun β-SiC particle and corrosive fluid elder generation stirring reaction at room temperature, discharge heat when making bubble breaking as early as possible; Guarantee reacting balance, generally react and get final product in 10 minutes that the reaction of this process generation is:
SiC+2HNO
3+2H
2O→2HNO
2+4OH
-+SiC
4+（1）
4OH
-+SiC
4+→SiO
2+CO
2+2H
2 （2）
After question response tends to be steady,, be placed on 60-80 ℃ of reaction in order to guarantee corrosion speed and control reaction preferably faster.The blending ratio of β-SiC particle and corrosive fluid is to add 60g-80g β-SiC particle in every 100ml corrosive fluid.This process reaction chemical equation is:
SiO
2+6HF→H
2SiF
6+2H
2O （3）
In whole corrosion process, hydrofluoric acid makes β-SiC particle surface form close organism reactive groups such as hydroxyl and oxygen base to the dissociation of C-Si key and the oxygenizement of nitric acid, and β-SiC particle is corroded into the perforated grill shape.
Because the whole system in corrosion back is strongly-acid, the pH value can reach about 1.0, and when being applied to the active somatic cell fluorescent mark, it is totally unfavorable for active somatic cell, to grow, and therefore, must fall s.t. to it.
Because β-the SiC particle is suspension in whole system in the corrosion back,, make that having latticed β-SiC particle after the corrosion separates rapidly with corrosive fluid so the present invention adopts centrifugal treating.After the said mixture spinning; Extract the upper strata corrosive fluid out, add high purity water 200-400ml, stirred 5 minutes; Again it is carried out aforesaid operations; Carry out repeatedly 4 to 5 times, make finally to obtain solution system pH value and be adapted to the active somatic cell that adopted, solution system pH value is at 6.4-6.8 generally speaking.
The silicon-carbide particle suspension-s that will fall after the s.t. imports glass cylinder, in the ultrasonic dispersing appearance, aqueous phase solution is carried out supersound process 20 minutes, and ultrasonic dispersing appearance output rating is 1kW, and frequency is 15kHz.This mainly is to utilize the cavatition of the aqueous solution in UW; To have latticed β-SiC particle breaks to become littler nano-scale particle and become quantum dot and falls into the aqueous solution; And the quantum dot surface can form close organism reactive groups such as O base and COO base; Can combine with materials such as protein, ions thus, single stage method of the present invention has realized the synthetic and surface biological functional modification of quantum dot, has improved preparation efficiency.
Nanoparticle for different size; Adopt centrifugal treating then to cut out through chromatography; Can obtain size mono-dispersed nano particle, so the present invention adopts high speed centrifugation to make different-grain diameter quantum dot size distribution in the supernatant different sites, thereby reach the quantum dot controllable size.Centrifugal speed has determined the cf-size, and rotating speed is too little, and the corrosive powder granule is suspended in solution, and the quantum dot particle dia that obtains is bigger; Rotating speed is too big; The quantum dot number of particles that is suspended in supernatant very little, concentration is lower, centrifugal rotational speed of the present invention adopts 2800-3000rpm more suitable; Silit quantum dot concentration is 0.03-0.06mol/L in the solution system that finally obtains; Be pistac under the visible light, it is closely spherical that quantum dot is, and diameter is 2-5nm.In order to adapt to the application of later stage on active somatic cell, the pH value of water silit quanta point material is 6.4-6.8.
Because the water silit quanta point material no cytotoxicity that the present invention makes; And exciton bohr (Bohr) radius much smaller than the silicon carbide body material; So fluorescent effect is obvious, thus the contriver with this material as fluorescence labeling material, directly it is added in nutrient solution or the substratum of active somatic cell and can realize fluorescent mark; Can form images for a long time, be convenient for people under fluorescent microscope, observe the pattern of active somatic cell.Active somatic cell of the present invention is plant or mikrobe active somatic cell.
In sum, the present invention has the following advantages:
1) the silit quantum dot no cytotoxicity of this water method preparation, and surface has close organism reactive groups such as oxygen base, carboxyl, can not influence active somatic cell growth physiological function, can realize long time-histories fluorescent mark imaging to it.
2) preparation technology is simple, and what abandoned available technology adopting is electrochemical etching method, and adopts direct corroding method, and processing parameter is easy to control, and is with low cost, but single stage method realizes the synthetic and surface biological functional modification of quantum dot.
3) through after ultra-sonic dispersion and the high speed centrifugation processing; Can realize the effective regulation and control to the quantum dot size, the quanta point material of preparing is much smaller than exciton bohr (Bohr) radius of silicon carbide body material, and its pl-effect is remarkable; The emission light intensity is stronger, and fluorescent effect is more obvious.
Description of drawings
Fig. 1 is a latticed microtexture pattern after spreading synthetic β-SiC particle erosion, and this pattern has been established condition for next step obtains tiny nearly spherical quantum dot through ultrasonic cavitation.
Fig. 2 is the TEM photo of color and microtexture under the water silit quanta point material visible light, and quantum dot is closely spherical, the about 2nm of (110) spacing, and this quantum dot can have stronger pl-effect.
Fig. 3 is 2 days and 4 days fluorescent mark imaging gray-scale map that water silit quanta point material is applied to aureobasidium pullulans (Aureobasidium pulluans948) active somatic cell;
Fig. 4 is optics and the fluorescent mark imaging gray-scale map after water silit quanta point material is applied to Arabidopis thaliana root active somatic cell.
Embodiment
Embodiment 1-5 water silit of the present invention quanta point material and preparation method thereof; The application of water silit quanta point material in the active somatic cell fluorescent mark that embodiment 6-7 makes for the present invention.Used self-propagating combustion synthetic homogeneous nano β-SiC particle is provided by Physical Chemistry Technology Inst., Chinese Academy of Sciences.Embodiment 1
A kind of water silit quanta point material, its pH value is 6.4, and silit quantum dot concentration is 0.03mol/L, and it is closely spherical that quantum dot is, and diameter is 5nm.
Its concrete preparation process is:
A. be that 40% hydrofluoric acid and mass concentration are that 65% nitric acid is mixed with corrosive fluid according to volume ratio 3:1 with mass concentration, and stir;
B. self-propagating combustion synthetic homogeneous nano β-SiC powder is placed the corrosive fluid of steps A configuration; Stirred 10 minutes; Wherein, β-SiC grain diameter is 70nm, and the blending ratio of β-SiC particle and corrosive fluid is to add 80g β-SiC particle in every 100ml corrosive fluid;
C. the mixture among the step B was corroded 1 hour in 75 ℃;
D. with said mixture behind the 600rpm low-speed centrifugal, extract corrosive fluid out, add high purity water 200ml, stir 5min, again it is carried out aforesaid operations after the spinning, eccentric cleaning to solution system pH value is 6.4 repeatedly.
E. the aqueous solution after the eccentric cleaning is carried out supersound process, ultrasonic power is 1kW, and frequency is 15kHz, ultrasonic time 20min;
F. the aqueous solution through supersound process is handled in the 2800rpm high speed centrifugation, got supernatant and be silit Quantum Dot Labeling material.
A kind of water silit quanta point material, its pH value is 6.5, and silit quantum dot concentration is 0.06mol/L, and it is closely spherical that quantum dot is, and diameter is 2nm.
Its concrete preparation process is:
A. be that 40% hydrofluoric acid and mass concentration are that 65% nitric acid is mixed with corrosive fluid according to volume ratio 3:1 with mass concentration, and stir;
B. self-propagating combustion synthetic homogeneous nano β-SiC powder is placed the corrosive fluid of steps A configuration; Stirred 10 minutes; Wherein, β-SiC grain diameter is 50nm, and the blending ratio of β-SiC particle and corrosive fluid is to add 70g β-SiC particle in every 100ml corrosive fluid;
C. the mixture among the step B was corroded 1 hour in 65 ℃;
D. with said mixture behind the 800rpm low-speed centrifugal, extract corrosive fluid out, add high purity water 300ml, stir 5min, again it is carried out aforesaid operations after the spinning, eccentric cleaning to solution system pH value is 6.5 repeatedly.
E. the aqueous solution after the eccentric cleaning is carried out supersound process, ultrasonic power is 1kW, and frequency is 15kHz, ultrasonic time 20min;
F. the aqueous solution through supersound process is handled in the 3000rpm high speed centrifugation, got supernatant and be silit Quantum Dot Labeling material.
Embodiment 3
A kind of water silit quanta point material, its pH value is 6.6, and silit quantum dot concentration is 0.04mol/L, and it is closely spherical that quantum dot is, and diameter is 3nm.
Its concrete preparation process is:
A. be that 40% hydrofluoric acid and mass concentration are that 65% nitric acid is mixed with corrosive fluid according to volume ratio 3:1 with mass concentration, and stir;
B. self-propagating combustion synthetic homogeneous nano β-SiC powder is placed the corrosive fluid of steps A configuration; Stirred 10 minutes; Wherein, β-SiC grain diameter is 100nm, and the blending ratio of β-SiC particle and corrosive fluid is to add 60g β-SiC particle in every 100ml corrosive fluid;
C. the mixture among the step B was corroded 1 hour in 70 ℃;
D. with said mixture behind the 500rpm low-speed centrifugal, extract corrosive fluid out, add high purity water 400ml, stir 5min, again it is carried out aforesaid operations after the spinning, eccentric cleaning to solution system pH value is 6.6 repeatedly.
E. the aqueous solution after the eccentric cleaning is carried out supersound process, ultrasonic power is 1kW, and frequency is 15kHz, ultrasonic time 20min;
F. the aqueous solution through supersound process is handled in the 2900rpm high speed centrifugation, got supernatant and be silit Quantum Dot Labeling material.
Embodiment 4
A kind of water silit quanta point material, its pH value is 6.7, and silit quantum dot concentration is 0.05mol/L, and it is closely spherical that quantum dot is, and diameter is 4nm.
Its concrete preparation process is:
A. be that 40% hydrofluoric acid and mass concentration are that 65% nitric acid is mixed with corrosive fluid according to volume ratio 3:1 with mass concentration, and stir;
B. self-propagating combustion synthetic homogeneous nano β-SiC powder is placed the corrosive fluid of steps A configuration; Stirred 10 minutes; Wherein, β-SiC grain diameter is 60nm, and the blending ratio of β-SiC particle and corrosive fluid is to add 65g β-SiC particle in every 100ml corrosive fluid;
C. the mixture among the step B was corroded 1 hour in 60 ℃;
D. with said mixture behind the 700rpm low-speed centrifugal, extract corrosive fluid out, add high purity water 220ml, stir 5min, again it is carried out aforesaid operations after the spinning, eccentric cleaning to solution system pH value is 6.7 repeatedly.
E. the aqueous solution after the eccentric cleaning is carried out supersound process, ultrasonic power is 1kW, and frequency is 15kHz, ultrasonic time 20min;
F. the aqueous solution through supersound process is handled in the 2800rpm high speed centrifugation, got supernatant and be silit Quantum Dot Labeling material.
Embodiment 5
A kind of water silit quanta point material, its pH value is 6.8, and silit quantum dot concentration is 0.03mol/L, and it is closely spherical that quantum dot is, and diameter is 2nm.
Its concrete preparation process is:
A. be that 40% hydrofluoric acid and mass concentration are that 65% nitric acid is mixed with corrosive fluid according to volume ratio 3:1 with mass concentration, and stir;
B. self-propagating combustion synthetic homogeneous nano β-SiC powder is placed the corrosive fluid of steps A configuration; Stirred 10 minutes; Wherein, β-SiC grain diameter is 80nm, and the blending ratio of β-SiC particle and corrosive fluid is to add 75g β-SiC particle in every 100ml corrosive fluid;
C. the mixture among the step B was corroded 1 hour in 80 ℃;
D. with said mixture behind the 650rpm low-speed centrifugal, extract corrosive fluid out, add high purity water 330ml, stir 5min, again it is carried out aforesaid operations after the spinning, eccentric cleaning to solution system pH value is 6.8 repeatedly.
E. the aqueous solution after the eccentric cleaning is carried out supersound process, ultrasonic power is 1kW, and frequency is 15kHz, ultrasonic time 20min;
F. the aqueous solution through supersound process is handled in the 3000rpm high speed centrifugation, got supernatant and be silit Quantum Dot Labeling material.
Embodiment 6
1, aureobasidium pullulans (Aureobasidium pulluans 948) culture condition
Slant medium (W/V): peptone 2%, yeast extract paste 1%, glucose 2%, agar 2%, 6.0121 ℃ of sterilizations of pH 20min.
Seed liquor substratum (W/V): 2% glucose, 2% yeast extract paste, 0.5%K
2HPO
4, 0.1%NaCl, 0.02%MgSO
47H
2O, 0.06% (NH
4)
2SO
4, initial 6.5,8 pounds of sterilizations of pH (121 ℃) 20min;
Fermention medium: 4% glucose, 2% yeast extract paste, 0.5%K
2HPO
4, 0.1%NaCl, 0.02%MgSO
47H
2O, 0.06% (NH
4)
2SO
4, initial 6.5,8 pounds of sterilizations of pH (121 ℃) 20min; Be made into 60ml solution, in solution, add the water silit quanta point material that 5ml embodiment 1 makes.
2, experimental technique
The slant strains of preservation in the biochemical incubator scraped get two and encircle to and carry out activation in the seed culture medium for preparing, 28 ℃, 200r/min cultivated 2 days.Again with the activatory bacterial classification with 7% inoculum size with the seed liquor bacterial classification inoculation to fermention medium, cultivate after 2-4 days, under fluorescent microscope, observe the active somatic cell pattern.
Can know through embodiment 6 and Fig. 3: 1, the SiC fluorescent material no cytotoxicity of this patent preparation; Growth does not have influence for active somatic cell; Can show the pattern (during beginning be granular, spherical, long-time growth after then become silk palpus shape) of weak point stalk mould in different time sections that sprout; 2, the Aureobasidium pullulans mycetocyte can fluoresce for a long time, explains that the SiC fluorescent material is difficult for by cancellation; 3, in nutrient solution, add the SiC fluorescent material and can realize fluorescent dye, method is simple and effective.
Embodiment 7
Arabidopis thaliana (Arobidopsis thaliana L.) (environmental for Columbia) seed is dispersed on the GM minimum medium after through sterilization, wherein adds the water silit quanta point material that the embodiment 3 of volume ratio 40% makes.Place for 4 ℃ and move to growth room's cultivation after 4 days, temperature is 20-22 ℃, and illumination condition is illumination in 16 hours, 8 hours dark, and growth of seedling is used to observe root section observation of cell structure and pattern under fluorescent microscope after 10 days.
Can know through embodiment 7 and Fig. 4:
1, the SiC fluorescent material no cytotoxicity of this patent preparation; Growth does not have influence for active somatic cell; Can demonstrate the pattern of Arabidopis thaliana root, and root different sites fluorescence power difference to some extent, eugonic position (root teat position) fluorescence is stronger; 2, the Arabidopis thaliana root cell can fluoresce for a long time, explains that the SiC fluorescent material is difficult for by cancellation; 3, in nutrient solution, add the SiC fluorescent material and can realize fluorescent dye, method is simple and effective.
Claims (9)
1. water silit quanta point material, it is characterized in that: silit quantum dot concentration is 0.03-0.06mol/L, and it is closely spherical that quantum dot is, and diameter is 2-5nm.
2. water silit quanta point material according to claim 1 is characterized in that: the pH value of water silit quanta point material is 6.4-6.8.
3. prepare the method for water silit quanta point material according to claim 1 or claim 2, it is characterized in that: its concrete steps are:
A. be that 40% hydrofluoric acid and mass concentration are that 65% nitric acid is mixed with corrosive fluid according to volume ratio 3:1 with mass concentration, and stir;
B. self-propagating combustion synthetic homogeneous nano β-SiC powder is placed the corrosive fluid of steps A configuration, stirring reaction, β-SiC grain diameter is 50-100nm
C. with the mixture standing and reacting among the step B;
D. with said mixture centrifugal after, extract corrosive fluid out, add high purity water, the SiC particle after utilizing high purity water to corrosion carries out eccentric cleaning;
E. the aqueous solution after the eccentric cleaning is carried out supersound process;
F. the aqueous solution through supersound process is carried out centrifugal treating, get supernatant and be silit Quantum Dot Labeling material, centrifugal speed is 2800-3000rpm.
4. the preparation method of water silit quanta point material according to claim 3 is characterized in that: the blending ratio of β among the step B-SiC particle and corrosive fluid is to add 60g-80g β-SiC particle in every 100ml corrosive fluid.
5. the preparation method of water silit quanta point material according to claim 3 is characterized in that: temperature of reaction is 60 ℃-80 ℃ among the step C, and the reaction times is 1 hour.
6. the preparation method of water silit quanta point material according to claim 3 is characterized in that: centrifugal speed is 500-800rpm among the step D.
7. the preparation method of water silit quanta point material according to claim 3 is characterized in that: among the step D after the eccentric cleaning solution system pH value be 6.4-6.8.
8. the preparation method of water silit quanta point material according to claim 3 is characterized in that: ultrasonic power is 1kW in the step e, and frequency is 15kHz, and ultrasonic time is 20min.
9. claim 1 or 2 described water silit quanta point materials are used for the purposes of fluorescence labeling material.
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| CN103194224A (en) * | 2013-04-10 | 2013-07-10 | 中国人民解放军国防科学技术大学 | Silicon carbide quantum dot and preparation method thereof |
| CN103232845A (en) * | 2013-05-08 | 2013-08-07 | 安徽工业大学 | Preparation and application for silicon quantum dots |
| CN104028291A (en) * | 2014-06-12 | 2014-09-10 | 大连理工大学 | Nitrogen-doped fluorescent carbon-dot and carbon-dot graphene composite as well as production method and application thereof |
| CN104353251A (en) * | 2014-11-07 | 2015-02-18 | 山西大学 | Carbon nano fluorescent bubble liquid |
| CN104028291B (en) * | 2014-06-12 | 2016-11-30 | 大连理工大学 | N doping fluorescent carbon point and carbon point graphene complex and preparation method thereof and application |
| CN109772397A (en) * | 2019-03-11 | 2019-05-21 | 扬州大学 | Liquid laser ablation prepares oxide-Silicon carbide quantum dot composite nanostructure visible light catalytic material method |
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2012
- 2012-06-21 CN CN201210208382.8A patent/CN102719248B/en not_active Expired - Fee Related
Non-Patent Citations (1)
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| 范吉阳等: "3C-SiC纳米颗粒量子限制效应的实验证据", 《研究快讯》 * |
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| CN103194224A (en) * | 2013-04-10 | 2013-07-10 | 中国人民解放军国防科学技术大学 | Silicon carbide quantum dot and preparation method thereof |
| CN103232845A (en) * | 2013-05-08 | 2013-08-07 | 安徽工业大学 | Preparation and application for silicon quantum dots |
| CN103232845B (en) * | 2013-05-08 | 2014-08-27 | 安徽工业大学 | Preparation and application for silicon quantum dots |
| CN104028291A (en) * | 2014-06-12 | 2014-09-10 | 大连理工大学 | Nitrogen-doped fluorescent carbon-dot and carbon-dot graphene composite as well as production method and application thereof |
| CN104028291B (en) * | 2014-06-12 | 2016-11-30 | 大连理工大学 | N doping fluorescent carbon point and carbon point graphene complex and preparation method thereof and application |
| CN104353251A (en) * | 2014-11-07 | 2015-02-18 | 山西大学 | Carbon nano fluorescent bubble liquid |
| CN104353251B (en) * | 2014-11-07 | 2016-06-01 | 山西大学 | A kind of carbon nano fluorescent bubble liquid |
| CN109772397A (en) * | 2019-03-11 | 2019-05-21 | 扬州大学 | Liquid laser ablation prepares oxide-Silicon carbide quantum dot composite nanostructure visible light catalytic material method |
| CN113936906A (en) * | 2021-09-30 | 2022-01-14 | 安徽瑞德磁电科技有限公司 | Sphericizing preparation method of broken iron-silicon-aluminum magnetic powder particles |
| CN113936906B (en) * | 2021-09-30 | 2023-08-11 | 安徽瑞德磁电科技有限公司 | Sphericizing preparation method of broken sendust magnetic powder particles |
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