CN106938840A - The preparation method and its product of a kind of carbon quantum dot for TEMP - Google Patents
The preparation method and its product of a kind of carbon quantum dot for TEMP Download PDFInfo
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- CN106938840A CN106938840A CN201710163636.1A CN201710163636A CN106938840A CN 106938840 A CN106938840 A CN 106938840A CN 201710163636 A CN201710163636 A CN 201710163636A CN 106938840 A CN106938840 A CN 106938840A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K11/00—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
Abstract
The invention provides a kind of preparation method of carbon quantum dot for TEMP and its product, pass through the carbon source aqueous solution and phosphorous passivator formation solution I, microwave 1min~5h, microwave intensity is controlled in 20~400Hz, below the 10nm therein particle aqueous solution is obtained by centrifugation, then aqueous solvent is removed by rotary evaporation, obtains the temperature sensitive product carbon quantum dot with fluorescence property.Present invention also offers the product of the preparation method.It is the carbon quantum dot available for TEMP that preparation process of the present invention is simple, take shorter, product.
Description
【Technical field】
The invention belongs to fluorescent nano material technical field, and in particular to a kind of system of carbon quantum dot for TEMP
Preparation Method.
【Background technology】
Temperature is the biological body physiological of influence and biochemical action and the basic thermodynamic variable of process, and its accurate measurement exists
It is significant in terms of biology and medical diagnosis.Up to the present, the means for accurate detection temperature have scanning probe micro-
Mirror, Raman spectrum and the detection technique based on fluorescence.Wherein, the temperature detection technology based on fluorescence nano sensor has height
The advantages of resolution ratio, response quickly, swift and violent hair is obtained in terms of environmental monitoring, food security, bio-sensing in the last few years
Exhibition.At present, conventional fluorescent nano material mainly includes semiconductor-quantum-point, organic fluorescent dye, fluorescent polymer and metal
Cluster etc., but these materials generally have the shortcomings that toxicity, stability is poor, high cost, limit they it is further apply, because
This, it is very necessary to develop new hypotoxicity, stable and low cost temperature sensing material.
Carbon quantum dot is that a kind of particle diameter is less than 10nm, microcosmic intimate torispherical, surface rich in organo-functional group, with fluorescence
The carbon nano-particle of performance.As a kind of Novel Carbon Nanomaterials, carbon quantum dot have toxicity it is low, environment-friendly, by surface
The advantages of functionalization and doping its physical and chemical performance of controllable, can be widely applied to chemical sensitisation, bio-sensing, it is biological into
The numerous areas such as picture, nanosecond medical science, catalysis and photoelectric device.The preparation method of current carbon quantum dot has arc discharge method, laser
Corrode method, electrochemical process, combustion method, pyrolysismethod, template, microwave method etc..Wherein, compared to other several preparation methods,
Microwave method has the advantages that preparation condition is gentle, the reaction time is short, is a kind of relatively new type method, such as publication number in recent years
CN103588193B patent document discloses a kind of method that microwave method prepares high-purity carbon quantum dot, and chitosan solution is passed through
The segmentation microwave method reaction of two steps, then isolated and purified through more than half preparation efficient liquid phases, by the hollow concentration of the solution separated
Dry, obtain high-purity carbon quantum dot；For another example, to disclose a kind of single phosphate auxiliary for publication number CN103482598A patent document
The preparation method of water-soluble row fluorescent carbon quantum dot solid powder is helped, is had with carbohydrate, amino acid, the small molecule containing carboxyl or hydroxyl
Machine thing is added in soluble phosphoric acid salting liquid as precursors, 2~3min of heating using microwave, the dissolving of gained solid powder
In the mixed solution of second alcohol and water, ultrasound after centrifuge, sequentially add strong-base anion-exchange resin and highly acid sun from
Supernatant liquor rotary evaporation is taken after sub-exchange resin, centrifugation, the carbon quantum dot powder purified.But the carbon point of its report is glimmering
Light is main in below 500nm blue light region, hardly results in the fluorescent carbon point of long wavelength.
However, this kind of microwave preparation as disclosed above, all haves the shortcomings that product isolates and purifies difficulty, and prepare
The carbon quantum dot transmitted wave length gone out, functionalization is not ideal enough, and the carbon quantum dot that can be directly used for TEMP is all fresh so far
Have been reported that.
【The content of the invention】
It is an object of the invention to provide a kind of preparation method of carbon quantum dot for TEMP and its product, prepare
It is the carbon quantum dot available for TEMP that process is simple, take shorter, product.
The technical scheme is that：
The preparation method of a kind of carbon quantum dot for TEMP, it is characterised in that comprise the steps of：
(1) the carbon source aqueous solution is prepared, addition phosphorus-containing compound is passivator, forms solution I, carbon source is rubbed with phosphorus-containing compound
You are than being 0.05:(0.1~5)；
(2) by the solution I prepared in (1) in microwave 1min~5h, microwave intensity is controlled in 20~400Hz；Microwave can be
Carry out, can also be carried out in the range of 30~50 DEG C at room temperature, the microwave time changes according to temperature and microwave intensity；
(3) product of (2) is taken, below the 10nm therein particle aqueous solution is obtained by centrifugation, is then steamed by rotating
Hair removes aqueous solvent, obtained solid as product.
Further, above-mentioned carbon source is glucose, fructose, sucrose, citric acid, lactic acid, polyvinyl alcohol, polyacrylic acid, poly-
In ketene imine, chitosan, cellulose, lemon juice, orange juice, Fresh Cucumber Juice, mashed garlic, mashed potatoes, watermelon juice, Aqua Folium Camelliae sinensis
It is one or more of.Wherein, preferably fructose, sucrose, citric acid, lactic acid, lemon juice, orange juice, Fresh Cucumber Juice, reason are these materials
Material is easily carbonized, and beneficial to the doping of P atoms.
Further, the concentration of the above-mentioned carbon source aqueous solution is 0.01~10.0g/mL.The advantage of the concentration range is carbon source
Good dispersion, is uniformly heated beneficial to microwave in the solution, forms the carbon point of size uniformity.
Further, above-mentioned phosphorus-containing compound be phosphoric acid, phosphate, diphosphorus trioxide, phosphorus pentoxide, phosphorus pentahalides,
One or more in tricresyl phosphate, triphenyl phosphate, triethyl phosphate, tributyl phosphate, di-n-butyl phosphite.Its
In, it is preferably phosphoric acid, phosphate, triphenyl phosphate, triethyl phosphate, tributyl phosphate, di-n-butyl phosphite.
Further, more than 10nm particle is removed by centrifugal method in above-mentioned steps (2).
A kind of product of the preparation method of the above-mentioned carbon quantum dot for TEMP, it is characterised in that P atoms can be very
Good is entrained in carbon point inside configuration, causes the fluorescent carbon point for generating long wavelength, its fluorescence emission wavelengths scope 500~
800nm。
Further, the maximum emission wavelength of above-mentioned product is 650nm.
Further, the temperature control of above-mentioned product is higher than 1.07% DEG C-1。
Further, the temperature-responsive scope of above-mentioned product is -35~130 DEG C.
The present invention has following beneficial technique effect：
1) preparation method is simple, time-consuming shorter, without additional purification procedures, low cost；2) particle size size
Small, about 3nm has dispersiveness well in water；3) there is strong fluorescent emission, fluorescence emission wavelengths are long, its fluorescence volume
Sub- efficiency is more than 20%, and the fluorescence of carbon quantum dot is quenched with the rise of temperature, with temperature sensitivity；4) it can apply
In the detection of temperature, and the new carbon-based nano temperature sensor built with its solution can be changed between low temperature and high temperature,
With very high repeatability；5) product is as temperature sensing material, with wide response range, high sensitivity and repeatable
Property, it can apply to the change of Poul Dorset Sheep solution and intracellular temperature.
【Brief description of the drawings】
Fig. 1 is the transmission electron microscope photo of the product of embodiment one；
Fig. 2 is the fluorescence spectra and the dispersed photo in water of the product of embodiment one；
Fig. 3 is the fluorescence intensity figure of temperature sensor temperature-rise period from 20 DEG C to 80 DEG C of embodiment one；
Fig. 4 is the reperformance test figure of the temperature sensor of embodiment one.
【Embodiment】
Below in conjunction with specific embodiment, the present invention is described further.
Embodiment provided below is simultaneously not used to the scope that the limitation present invention is covered, described step nor with
To limit its execution sequence.Those skilled in the art do conspicuously improved with reference to existing common knowledge to the present invention, also fall
Enter within the protection domain of application claims.
Embodiment one
In 10mL concentration in 0.1g/L D/W, to add 0.6mmol phosphoric acid, regulation microwave frequency is
100Hz, microwave 1h, obtains the bright yellow solution of transparent clarification at room temperature；Reaction solution obtains below 10nm therein by centrifugation
The particle aqueous solution, then pass through rotary evaporation remove aqueous solvent, obtained solid as product, its transmission electron microscope photo as scheme
Shown in 1.Product is dispersed in water again, the temperature sensor that carbon quantum dot concentration is 10mg/ml is formed, passes through RF-
5301PC XRFs test its photoluminescent property, as a result as shown in Fig. 2 a length of 285nm of its maximum absorption wave, maximum excitation ripple
A length of 370nm, maximum emission wavelength is 520nm.The TEMP for taking the 0.5mL above-mentioned fluorescent carbon quantum dot aqueous solution to be formed
Device, gold nanoclusters probe is tested from 20 DEG C to the fluorescence intensity change of 85 DEG C of temperature-rise periods using RF-5301PC XRFs,
Sensitivity to temperature detects, as a result as shown in figure 3, show average ramp rate about 1.3%/DEG C.Fig. 4 is to this
The stability of temperature sensor is tested, and is carried out retest to product with 85 DEG C at 15 DEG C, is as a result shown, this temperature is passed
Sensor can be changed between low temperature and high temperature, can be 8 times with Reusability.
Embodiment two
0.35g fructose is added in 2.5mL water, stirring to form clear solution to being completely dissolved, then add 0.5mL's
Phosphoric acid, regulation microwave frequency is 100Hz, and microwave 1h, obtains the bright yellow solution of transparent clarification at room temperature；Reaction solution passes through centrifugation
Below the 10nm therein particle aqueous solution is obtained, aqueous solvent, obtained solid as product are then removed by rotary evaporation
As carbon quantum dot.It is dispersed in water again, the temperature sensor that carbon quantum dot concentration is 20mg/ml is formed.
Embodiment three
0.5g fructose and 0.2g sucrose is added in 10mL water, stirring to form clear solution to being completely dissolved, Ran Houjia
Enter 0.5mL triethyl phosphate, regulation microwave frequency is 100Hz, and microwave 30min, obtains the glassy yellow of transparent clarification at room temperature
Solution；Reaction solution obtains below the 10nm therein particle aqueous solution by centrifugation, then removes aqueous solvent by rotary evaporation,
Obtained solid is product as carbon quantum dot.It is dispersed in water again, it is 10mg/ml's to form carbon quantum dot concentration
Temperature sensor.
Claims (9)
1. the preparation method of a kind of carbon quantum dot for TEMP, it is characterised in that comprise the steps of：
(1) the carbon source aqueous solution is prepared, addition phosphorus-containing compound is passivator, forms solution I, the carbon source is rubbed with phosphorus-containing compound
You are than being 0.05:(0.1~5)；
(2) by the solution I prepared in (1) in microwave 1min~5h, microwave intensity is controlled in 20~400Hz；
(3) product of (2) is taken, below the 10nm therein particle aqueous solution is obtained by centrifugation, is then gone by rotary evaporation
Except aqueous solvent, obtained solid as product.
2. the preparation method of the carbon quantum dot according to claim 1 for TEMP, it is characterised in that the carbon source
For glucose, fructose, sucrose, citric acid, lactic acid, polyvinyl alcohol, polyacrylic acid, polyvinyl, chitosan, cellulose,
One or more in lemon juice, orange juice, Fresh Cucumber Juice, mashed garlic, mashed potatoes, watermelon juice, Aqua Folium Camelliae sinensis.
3. the preparation method of the carbon quantum dot according to claim 1 for TEMP, it is characterised in that the carbon source
The concentration of the aqueous solution is 0.01~10.0g/mL.
4. the preparation method of the carbon quantum dot according to claim 1 for TEMP, it is characterised in that described phosphorous
Compound is phosphoric acid, phosphate, diphosphorus trioxide, phosphorus pentoxide, phosphorus pentahalides, tricresyl phosphate, triphenyl phosphate, phosphorus
One or more in triethylenetetraminehexaacetic acid ester, tributyl phosphate, di-n-butyl phosphite.
5. the preparation method of the carbon quantum dot according to claim 1 for TEMP, it is characterised in that the step
(2) more than 10nm particle is removed by centrifugal method in.
6. a kind of product of the preparation method of the carbon quantum dot as claimed in claim 1 for TEMP, it is characterised in that
The fluorescence emission wavelengths scope of the product is in 500~800nm.
7. the product of the preparation method of the carbon quantum dot according to claim 6 for TEMP, it is characterised in that institute
The maximum emission wavelength for stating product is 650nm.
8. the product of the preparation method of the carbon quantum dot according to claim 6 for TEMP, it is characterised in that institute
The temperature control for stating product is higher than 1.07% DEG C-1。
9. the product of the preparation method of the carbon quantum dot according to claim 6 for TEMP, it is characterised in that institute
The temperature-responsive scope for stating product is -35~130 DEG C.
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| CN201710163636.1A CN106938840A (en) | 2017-03-20 | 2017-03-20 | The preparation method and its product of a kind of carbon quantum dot for TEMP |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107312535A (en) * | 2017-07-26 | 2017-11-03 | 广西师范学院 | Excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration |
| CN107555417A (en) * | 2017-08-29 | 2018-01-09 | 湖南农业大学 | Commercialization beverage prepares the method for fluorescent carbon point and its fluorescent carbon point of preparation |
| CN108192602A (en) * | 2018-01-22 | 2018-06-22 | 吉林大学 | It is a kind of with room temperature phosphorimetry property without metal-containing polymer carbon dots, preparation method and applications |
| CN108410457A (en) * | 2018-04-25 | 2018-08-17 | 山西大学 | A kind of Multifunction fluorescent carbon quantum dot and its preparation method and application |
| CN109052368A (en) * | 2018-10-30 | 2018-12-21 | 郑州大学 | A method of carbon quantum dot film being prepared using hydrothermal technique using garlic as raw material |
| CN109385273A (en) * | 2017-08-09 | 2019-02-26 | 中国科学院宁波材料技术与工程研究所 | Extra long life room temperature phosphorimetry material, preparation method and application |
| CN109399606A (en) * | 2018-12-21 | 2019-03-01 | 北京工业大学 | A kind of preparation method of efficient photothermal conversion carbon dots base foam |
| CN109990915A (en) * | 2017-12-29 | 2019-07-09 | Tcl集团股份有限公司 | Temperature sensor |
| CN110951487A (en) * | 2019-12-26 | 2020-04-03 | 宁波大学 | Preparation method of diphenyl azide phosphate modified graphene quantum dots |
| CN111620320A (en) * | 2020-06-19 | 2020-09-04 | 苏州星烁纳米科技有限公司 | Phosphorescent carbon quantum dot and preparation method thereof |
| CN112299405A (en) * | 2020-11-19 | 2021-02-02 | 福州大学 | Preparation method of low-temperature easily-graphitized three-dimensional biomass porous carbon with high specific surface area |
| CN114015440A (en) * | 2021-12-10 | 2022-02-08 | 兰州大学 | Fluorescent carbon dot for temperature sensing and preparation method thereof |
| CN115427349A (en) * | 2020-05-21 | 2022-12-02 | 株式会社吴羽 | Composition and method for producing the same |
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| CN103482598A (en) * | 2013-08-30 | 2014-01-01 | 吉林大学 | Preparation method for monophosphate-adjuvant water-soluble fluorescent carbon quantum dot solid powder |
| CN103588193A (en) * | 2013-11-28 | 2014-02-19 | 张岐 | Method for preparing high purity carbon quantum dots by using microwave method |
| CN103721736A (en) * | 2013-12-27 | 2014-04-16 | 北京大学 | Iron nitride/nitrogen-doped graphene aerogel as well as preparation method and application thereof |
| CN104263364A (en) * | 2014-08-25 | 2015-01-07 | 中国科学院长春光学精密机械与物理研究所 | Bio-based carbon nano dot fluorescent powder, preparation method and applications thereof |
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| CN103482598A (en) * | 2013-08-30 | 2014-01-01 | 吉林大学 | Preparation method for monophosphate-adjuvant water-soluble fluorescent carbon quantum dot solid powder |
| CN103588193A (en) * | 2013-11-28 | 2014-02-19 | 张岐 | Method for preparing high purity carbon quantum dots by using microwave method |
| CN103721736A (en) * | 2013-12-27 | 2014-04-16 | 北京大学 | Iron nitride/nitrogen-doped graphene aerogel as well as preparation method and application thereof |
| CN104263364A (en) * | 2014-08-25 | 2015-01-07 | 中国科学院长春光学精密机械与物理研究所 | Bio-based carbon nano dot fluorescent powder, preparation method and applications thereof |
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107312535A (en) * | 2017-07-26 | 2017-11-03 | 广西师范学院 | Excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration |
| CN107312535B (en) * | 2017-07-26 | 2019-05-17 | 广西师范学院 | Excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration |
| CN109385273B (en) * | 2017-08-09 | 2021-10-12 | 中国科学院宁波材料技术与工程研究所 | Ultra-long-life room temperature phosphorescent material, and preparation method and application thereof |
| CN109385273A (en) * | 2017-08-09 | 2019-02-26 | 中国科学院宁波材料技术与工程研究所 | Extra long life room temperature phosphorimetry material, preparation method and application |
| CN107555417A (en) * | 2017-08-29 | 2018-01-09 | 湖南农业大学 | Commercialization beverage prepares the method for fluorescent carbon point and its fluorescent carbon point of preparation |
| CN109990915A (en) * | 2017-12-29 | 2019-07-09 | Tcl集团股份有限公司 | Temperature sensor |
| CN108192602A (en) * | 2018-01-22 | 2018-06-22 | 吉林大学 | It is a kind of with room temperature phosphorimetry property without metal-containing polymer carbon dots, preparation method and applications |
| CN108192602B (en) * | 2018-01-22 | 2020-09-01 | 吉林大学 | Metal-free polymer carbon dot with room-temperature phosphorescence property, and preparation method and application thereof |
| CN108410457B (en) * | 2018-04-25 | 2020-11-10 | 山西大学 | Multifunctional fluorescent carbon quantum dot and preparation method and application thereof |
| CN108410457A (en) * | 2018-04-25 | 2018-08-17 | 山西大学 | A kind of Multifunction fluorescent carbon quantum dot and its preparation method and application |
| CN109052368A (en) * | 2018-10-30 | 2018-12-21 | 郑州大学 | A method of carbon quantum dot film being prepared using hydrothermal technique using garlic as raw material |
| CN109399606A (en) * | 2018-12-21 | 2019-03-01 | 北京工业大学 | A kind of preparation method of efficient photothermal conversion carbon dots base foam |
| CN110951487A (en) * | 2019-12-26 | 2020-04-03 | 宁波大学 | Preparation method of diphenyl azide phosphate modified graphene quantum dots |
| CN110951487B (en) * | 2019-12-26 | 2022-12-20 | 宁波大学 | Preparation method of diphenyl azide phosphate modified graphene quantum dots |
| CN115427349A (en) * | 2020-05-21 | 2022-12-02 | 株式会社吴羽 | Composition and method for producing the same |
| US11898077B2 (en) | 2020-05-21 | 2024-02-13 | Kureha Corporation | Composition and method for producing same |
| CN111620320A (en) * | 2020-06-19 | 2020-09-04 | 苏州星烁纳米科技有限公司 | Phosphorescent carbon quantum dot and preparation method thereof |
| CN112299405A (en) * | 2020-11-19 | 2021-02-02 | 福州大学 | Preparation method of low-temperature easily-graphitized three-dimensional biomass porous carbon with high specific surface area |
| CN114015440A (en) * | 2021-12-10 | 2022-02-08 | 兰州大学 | Fluorescent carbon dot for temperature sensing and preparation method thereof |
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