CN110408390A - A kind of cerium enhancing wheat bran is carbon source red fluorescence carbon quantum dot preparation method - Google Patents
A kind of cerium enhancing wheat bran is carbon source red fluorescence carbon quantum dot preparation method Download PDFInfo
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- CN110408390A CN110408390A CN201910774035.3A CN201910774035A CN110408390A CN 110408390 A CN110408390 A CN 110408390A CN 201910774035 A CN201910774035 A CN 201910774035A CN 110408390 A CN110408390 A CN 110408390A
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7715—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing cerium
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Abstract
It is carbon source red fluorescence carbon quantum dot preparation method the invention discloses a kind of cerium enhancing wheat bran, it is characterised in that: firstly, preparing cerous nitrate solution；Then, using wheat bran and ammonium chloride as reaction raw materials, DMF is as reaction dissolvent, by wheat bran under room temperature, ammonium chloride, DMF and cerous nitrate solution are transferred in the reaction kettle containing polytetrafluoroethylliner liner after being sufficiently mixed uniformly, and reaction kettle is placed in baking oven, hydro-thermal reaction 10h at 180 ± 5 DEG C of temperature, the solution after reaction obtain the red fluorescence carbon quantum dot of cerium enhancing through centrifugation, filtering, dialysis.The present invention is using natural material wheat bran as carbon source, a step solvent thermal reaction need to only be carried out, materials are convenient, it is easy to operate, the fluorescent carbon quantum dot prepared is doped with two kinds of elements of N and Cl, biocompatibility and optical stability are all fine, and the addition of cerium can make the fluorescence quantum yield of carbon quantum dot reach as high as 46%, and fluorescence property improves 54% or so.
Description
Technical field
It is carbon source red fluorescence carbon quantum dot preparation method the present invention provides a kind of cerium enhancing wheat bran, belongs to nano luminescent
The technical field of material preparation.
Background technique
Carbon quantum dot is by partial size less than the carbonaceous skeleton of 10nm and hydrophilic as a kind of emerging fluorescence carbon nanomaterial
Property good surface functional group constitute, therefore compared with traditional semiconductor-quantum-point, organic dyestuff, there is small toxicity, biology
The advantages such as compatibility is good, fluorescent marker, in terms of present good application prospect.But the carbon prepared at present
Quantum dot is blue-fluorescence mostly, and the carbon quantum dot for obtaining multicolor fluorescence transmitting, which becomes, leads to carbon quantum dot broad prospect of application
The only way which must be passed.In recent years, it finds after study, Heteroatom doping can be improved the charge transport ability of carbon dots, to make carbon
The luminescent color of quantum dot changes.Wherein, N element is to prepare doped chemical common in carbon quantum dot, because of nitrogen
It is adjacent with carbon, it can be used as electron donor and carbon quantum dot be doped.Cl element is that one kind can make absorbing wavelength to length
The mobile hetero atom group in wave direction, therefore the excitation wavelength dependence based on carbon quantum dot, are used for carbon amounts for N element and Cl element
Son point doping can make carbon quantum dot launch wavelength mobile to long wave direction, to change luminescent color.
Rare earth element is because of its special electron structure, and the spectral property incomparable with general element, rare earth
Element, which shines, almost covers the scope of entire solid luminescence.The rare earth element of 4f shell with underfill, spectrum is about
There are 30000 observable spectral lines, they can emit the electromagnetism of the various wavelength from ultraviolet light, visible light to infrared light district
Radiation.The transition characteristic of rare earth element energy level abundant and 4f electronics makes rare earth become huge luminous treasure-house, can therefrom excavate
More novel luminescent materials out.It therefore, can be to the optical property of carbon quantum dot into carbon quantum dot by rare earth doped
It improves a lot.
Wheat bran is the byproduct obtained after wheat processing flour, and source is sufficient, cheap, is commonly used for feed, economic valence
It is worth not high.If considerable economic well-being of workers and staff can be brought to agricultural production, food production for its deep processing.In fact, right in wheat bran
Aminobenzoic acid content is highest in plant, and containing carbon source and nitrogen source required for preparation carbon quantum dot in wheat bran, therefore,
It can use raw material of the wheat bran as preparation carbon quantum dot.
Summary of the invention
It is carbon source red fluorescence carbon quantum dot preparation method the invention reside in a kind of cerium enhancing wheat bran is provided.
A kind of cerium enhancing wheat bran is carbon source red fluorescence carbon quantum dot preparation method, which is characterized in that this method have with
Lower processing step:
(1) preparation of cerium oxide solution: powdered cerium oxide, deionized water and dehydrated alcohol are mixed under magnetic stirring apparatus effect
Merging is heated to 45 ± 2 DEG C of stirring and dissolvings, and three mixes according to following mass percent: cerium oxide 5%-9%, deionized water:
58%-62%, dehydrated alcohol: 30%-34%.
(2) the cerium oxide solution prepared in (1) preparation of cerous nitrate solution: is heated with stirring to 80 ± 2 in beaker
DEG C, after nitric acid is slowly dropped into cerium oxide solution, until dissolution；Then it places the beaker in air dry oven 100 ± 2
DEG C drying, and deionized water circulation drying is continuously added into beaker, remove excessive nitric acid in solution；Finally solution is moved
The constant volume into the volumetric flask of 500 mL obtains cerous nitrate solution.
(3) cerium enhancing wheat bran is the preparation of carbon source red fluorescence carbon quantum dot: the cerous nitrate solution and bran that will be prepared in (2)
Skin, ammonium chloride and DMF are mixed according to following mass percent: cerous nitrate: 1.5%-2.0%, wheat bran: 6%-11%, ammonium chloride: 3%-
8%, DMF:80%-85% are transferred in the reaction kettle containing polytetrafluoroethylliner liner after mixing, and reaction kettle covers sealing cover, is placed in
In baking oven, temperature hydro-thermal reaction 10h at 180 ± 20 DEG C, cooled to room temperature after reaction, by solution through centrifugation, filtering,
After the purification steps such as dialysis, obtaining cerium enhancing wheat bran is carbon source red fluorescence carbon quantum dot solution.
The volume ratio of cerium oxide solution and nitric acid of the present invention are as follows: 1:2-5.
The concentration of cerous nitrate solution of the present invention is 0.3M-0.5M.
The revolving speed of centrifugation of the present invention is 10000-12000r/min, centrifugation time 5-10min.
Filter process of the present invention is using 0.22 μm of miillpore filter.
Dialysis procedure of the present invention is the bag filter of 500D, dialysis time 6h using molecular cut off.
The optimum proportioning of the parameter of the present invention is cerium oxide 5g, deionized water: 61mL, dehydrated alcohol: 31mL, nitre
Sour cerium: 1.6mL, wheat bran: 8g, ammonium chloride: 3g, DMF:80mL.
Cerium enhancing wheat bran prepared by the present invention is carbon source red fluorescence carbon quantum dot under the excitation wavelength of wavelength 550nm,
Red fluorescence (625nm) can be successfully issued, fluorescence quantum yield reaches as high as 46%.
The beneficial effects of the present invention are:
The present invention uses wheat bran for carbon source, and organic solvent DMF mixes with rare-earth salt solution that carry out a step molten as reaction dissolvent
Agent thermal response, materials are convenient, environmental protection easy to operate, and the cerium enhancing wheat bran of preparation is the fluorescence of carbon source red fluorescence carbon quantum dot
It can be than being significantly improved before rare earth doped element, and the carbon quantum dot prepared is of uniform size, good biocompatibility, optics is steady
Qualitative height.
Detailed description of the invention
Fig. 1 is the transmission plot that cerium enhancing wheat bran is carbon source red fluorescence carbon quantum dot.
Fig. 2 is the spectrogram that cerium enhancing wheat bran is carbon source red fluorescence carbon quantum dot.
Specific embodiment
Embodiment 1
(1) preparation of cerium oxide solution: by the powdered cerium oxide of 5 g, 60 mL deionized waters and 30 mL dehydrated alcohols in magnetic force
45 DEG C of stirring and dissolvings are mixed and heated under blender effect.
(2) preparation of cerous nitrate solution: 5 mL of cerium oxide solution prepared in (1) is taken to be heated with stirring to 80 in beaker
DEG C, after 10 mL nitric acid are slowly dropped into cerium oxide solution, until dissolution；Then place the beaker in air dry oven
100 DEG C of drying, and deionized water circulation drying is continuously added into beaker, remove excessive nitric acid in solution；It finally will be molten
Liquid moves to constant volume in the volumetric flask of 500 mL, obtains the cerous nitrate solution that concentration is 0.3 M.
(3) cerium enhancing wheat bran is the preparation of carbon source red fluorescence carbon quantum dot: the cerous nitrate solution and bran that will be prepared in (2)
Skin, ammonium chloride and DMF are mixed according to following mass percent: cerous nitrate: 1.6 mL, wheat bran: 8 g, ammonium chloride: 3 g, DMF:
80mL is transferred in the reaction kettle containing polytetrafluoroethylliner liner after mixing, and reaction kettle covers sealing cover, is placed in baking oven, temperature
Degree hydro-thermal reaction 10h, cooled to room temperature after reaction, by solution through purification steps such as centrifugation, filtering, dialysis at 180 DEG C
Afterwards, obtaining cerium enhancing wheat bran is carbon source red fluorescence carbon quantum dot solution.
Embodiment 2
(1) preparation of cerium oxide solution: by the powdered cerium oxide of 5 g, 61 mL deionized waters and 31 mL dehydrated alcohols in magnetic force
45 DEG C of stirring and dissolvings are mixed and heated under blender effect.
(2) preparation of cerous nitrate solution: 5 mL of cerium oxide solution prepared in (1) is taken to be heated with stirring to 80 in beaker
DEG C, after 12 mL nitric acid are slowly dropped into cerium oxide solution, until dissolution；Then place the beaker in air dry oven
100 DEG C of drying, and deionized water circulation drying is continuously added into beaker, remove excessive nitric acid in solution；It finally will be molten
Liquid moves to constant volume in the volumetric flask of 500 mL, obtains the cerous nitrate solution that concentration is 0.35 M.
(3) cerium enhancing wheat bran is the preparation of carbon source red fluorescence carbon quantum dot: the cerous nitrate solution and bran that will be prepared in (2)
Skin, ammonium chloride and DMF are mixed according to following mass percent: cerous nitrate: 1.7 mL, wheat bran: 9 g, ammonium chloride: 4 g, DMF:
81mL is transferred in the reaction kettle containing polytetrafluoroethylliner liner after mixing, and reaction kettle covers sealing cover, is placed in baking oven, temperature
Degree hydro-thermal reaction 10h, cooled to room temperature after reaction, by solution through purification steps such as centrifugation, filtering, dialysis at 180 DEG C
Afterwards, obtaining cerium enhancing wheat bran is carbon source red fluorescence carbon quantum dot solution.
Embodiment 3
(1) preparation of cerium oxide solution: by the powdered cerium oxide of 6 g, 62 mL deionized waters and 32 mL dehydrated alcohols in magnetic force
45 DEG C of stirring and dissolvings are mixed and heated under blender effect.
(2) preparation of cerous nitrate solution: 5 mL of cerium oxide solution prepared in (1) is taken to be heated with stirring to 80 in beaker
DEG C, after 15 mL nitric acid are slowly dropped into cerium oxide solution, until dissolution；Then place the beaker in air dry oven
100 DEG C of drying, and deionized water circulation drying is continuously added into beaker, remove excessive nitric acid in solution；It finally will be molten
Liquid moves to constant volume in the volumetric flask of 500 mL, obtains the cerous nitrate solution that concentration is 0.4 M.
(3) cerium enhancing wheat bran is the preparation of carbon source red fluorescence carbon quantum dot: the cerous nitrate solution and bran that will be prepared in (2)
Skin, ammonium chloride and DMF are mixed according to following mass percent: cerous nitrate: 1.8 mL, wheat bran: 10 g, ammonium chloride: 5 g, DMF:
83mL is transferred in the reaction kettle containing polytetrafluoroethylliner liner after mixing, and reaction kettle covers sealing cover, is placed in baking oven, temperature
Degree hydro-thermal reaction 10h, cooled to room temperature after reaction, by solution through purification steps such as centrifugation, filtering, dialysis at 180 DEG C
Afterwards, obtaining cerium enhancing wheat bran is carbon source red fluorescence carbon quantum dot solution.
Embodiment 4
(1) preparation of cerium oxide solution: by the powdered cerium oxide of 7 g, 62 mL deionized waters and 32 mL dehydrated alcohols in magnetic force
45 DEG C of stirring and dissolvings are mixed and heated under blender effect.
(2) preparation of cerous nitrate solution: 6 mL of cerium oxide solution prepared in (1) is taken to be heated with stirring to 80 in beaker
DEG C, after 15 mL nitric acid are slowly dropped into cerium oxide solution, until dissolution；Then place the beaker in air dry oven
100 DEG C of drying, and deionized water circulation drying is continuously added into beaker, remove excessive nitric acid in solution；It finally will be molten
Liquid moves to constant volume in the volumetric flask of 500 mL, obtains the cerous nitrate solution that concentration is 0.5 M.
(3) cerium enhancing wheat bran is the preparation of carbon source red fluorescence carbon quantum dot: the cerous nitrate solution and bran that will be prepared in (2)
Skin, ammonium chloride and DMF are mixed according to following mass percent: cerous nitrate: 2.0 mL, wheat bran: 11 g, ammonium chloride: 8 g, DMF:
85mL is transferred in the reaction kettle containing polytetrafluoroethylliner liner after mixing, and reaction kettle covers sealing cover, is placed in baking oven, temperature
Degree hydro-thermal reaction 10h, cooled to room temperature after reaction, by solution through purification steps such as centrifugation, filtering, dialysis at 180 DEG C
Afterwards, obtaining cerium enhancing wheat bran is carbon source red fluorescence carbon quantum dot solution.
Embodiment 5
Fluorescence quantum yield is one of the important parameter for showing a substance fluorescent characteristic.Cerium enhancing wheat bran is carbon source in the present invention
The measurement of the fluorescence quantum yield of red fluorescence carbon quantum dot uses reference method, using quinine sulfate as marker, by sulphur
Sour quinine (its quantum yield is 54%) is dissolved in the H of 0.1 mol/L2SO4 In solution.It is divided first using UV, visible light
Photometer tests the absorbance value A of test substance and quinine sulfate under some selected wavelength, uses identical excitation wavelength
The fluorescence spectrum for testing test substance and marker quinine sulfate under same concentration respectively obtains fluorescence by integral and integrates face
Product.The fluorescence quantum yield that sample is measured by relative method, can be calculated by following formula:
WhereinThe fluorescence quantum yield of standard and sample is respectively represented,For
Standard and sample excitation wavelength absorbance (0.01 < A < 0.05 reabsorbs effect to reduce),
Indicate the integral area of the emission spectrum of standard and sample under identical testing conditions.Enhance bran by measuring the cerium prepared
Skin is carbon source red fluorescence carbon quantum dot under the excitation wavelength of wavelength 550nm, can successfully be issued red fluorescence (625nm), glimmering
Quantum yield is up to 46%.
Claims (8)
1. a kind of cerium enhancing wheat bran is carbon source red fluorescence carbon quantum dot preparation method, which is characterized in that this method has following
Processing step:
(1) preparation of cerium oxide solution: powdered cerium oxide, deionized water and dehydrated alcohol are mixed under magnetic stirring apparatus effect
Merging is heated to 45 ± 2 DEG C of stirring and dissolvings, and three mixes according to following mass percent: cerium oxide 5%-9%, deionized water:
58%-62%, dehydrated alcohol: 30%-34%；
(2) preparation of cerous nitrate solution: being heated with stirring to 80 ± 2 DEG C for the cerium oxide solution prepared in (1) in beaker, after
Nitric acid is slowly dropped into cerium oxide solution, until dissolution；Then it places the beaker in air dry oven and is dried at 100 ± 2 DEG C
It is dry, and deionized water circulation drying is continuously added into beaker, remove excessive nitric acid in solution；Solution is finally moved to 500
Constant volume in the volumetric flask of mL obtains cerous nitrate solution；
(3) cerium enhancing wheat bran is the preparation of carbon source red fluorescence carbon quantum dot: the cerous nitrate solution that will be prepared in (2) and wheat bran,
Ammonium chloride and DMF are mixed according to following mass percent: cerous nitrate: 1.5%-2.0%, wheat bran: 6%-11%, ammonium chloride: 3%-8%,
DMF:80%-85% is transferred in the reaction kettle containing polytetrafluoroethylliner liner after mixing, and reaction kettle covers sealing cover, is placed in baking
In case, temperature hydro-thermal reaction 10h at 180 ± 20 DEG C, cooled to room temperature after reaction, by solution through centrifugation, filtering, thoroughly
After the purification steps such as analysis, obtaining cerium enhancing wheat bran is carbon source red fluorescence carbon quantum dot solution.
2. cerium enhancing wheat bran is carbon source red fluorescence carbon quantum dot preparation method according to claim 1, which is characterized in that
The volume ratio of the cerium oxide solution and nitric acid is 1:2-5.
3. cerium enhancing wheat bran is carbon source red fluorescence carbon quantum dot preparation method according to claim 1, which is characterized in that
The concentration of the cerous nitrate solution is 0.3M-0.5M.
4. cerium enhancing wheat bran is carbon source red fluorescence carbon quantum dot preparation method according to claim 1, which is characterized in that
The revolving speed of step (3) centrifugation is 10000-12000r/min, centrifugation time 5-10min.
5. cerium enhancing wheat bran is carbon source red fluorescence carbon quantum dot preparation method according to claim 1, which is characterized in that
Step (3) filter process is using 0.22 μm of miillpore filter.
6. cerium enhancing wheat bran is carbon source red fluorescence carbon quantum dot preparation method according to claim 1, which is characterized in that
The dialysis procedure is the bag filter of 500D, dialysis time 6h using molecular cut off.
7. cerium enhancing wheat bran is carbon source red fluorescence carbon quantum dot preparation method according to claim 1, which is characterized in that
The optimum proportioning of the parameter be cerium oxide 5g, deionized water: 61mL, dehydrated alcohol: 31mL, cerous nitrate: 1.6mL, wheat bran:
8g, ammonium chloride: 3g, DMF:80mL.
8. the cerium enhancing wheat bran of any one of -7 method preparations is carbon source red fluorescence carbon quantum dot, feature according to claim 1
It is, the cerium enhancing wheat bran of preparation is carbon source red fluorescence carbon quantum dot under the excitation wavelength of wavelength 550nm, can successfully be issued
Red fluorescence 625nm, fluorescence quantum yield reach as high as 46%.
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| CN113096885A (en) * | 2021-04-07 | 2021-07-09 | 宁波龙圣新材料科技有限公司 | Preparation method of low-resistance high-transparency conductive film |
| CN114088668A (en) * | 2021-10-12 | 2022-02-25 | 江苏大学 | Preparation method and application of ratio type fluorescent paper-based sensor |
| CN115651647A (en) * | 2022-11-16 | 2023-01-31 | 河北美星化工有限公司 | Rare earth doped carbon quantum dot material and preparation method and application thereof |
| CN116179198A (en) * | 2023-02-27 | 2023-05-30 | 河北大学 | Method for preparing solid rare earth doped fluorescent carbon dots by one-step hydrothermal method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113096885A (en) * | 2021-04-07 | 2021-07-09 | 宁波龙圣新材料科技有限公司 | Preparation method of low-resistance high-transparency conductive film |
| CN113096885B (en) * | 2021-04-07 | 2022-09-09 | 佳雅(威海)新材料科技有限公司 | Preparation method of low-resistance high-transparency conductive film |
| CN114088668A (en) * | 2021-10-12 | 2022-02-25 | 江苏大学 | Preparation method and application of ratio type fluorescent paper-based sensor |
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| CN115651647A (en) * | 2022-11-16 | 2023-01-31 | 河北美星化工有限公司 | Rare earth doped carbon quantum dot material and preparation method and application thereof |
| CN115651647B (en) * | 2022-11-16 | 2023-08-15 | 河北美星化工有限公司 | Rare earth doped carbon quantum dot material and preparation method and application thereof |
| CN116179198A (en) * | 2023-02-27 | 2023-05-30 | 河北大学 | Method for preparing solid rare earth doped fluorescent carbon dots by one-step hydrothermal method |
| CN116179198B (en) * | 2023-02-27 | 2023-12-05 | 河北大学 | Method for preparing solid rare earth doped fluorescent carbon dots by one-step hydrothermal method |
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