CN114214068B - Preparation method of metal-doped fluorescent biomass carbon quantum dot - Google Patents
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- 239000002028 Biomass Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910052751 metal Inorganic materials 0.000 claims abstract description 34
- 239000002184 metal Substances 0.000 claims abstract description 34
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 13
- 239000012498 ultrapure water Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000004108 freeze drying Methods 0.000 claims abstract description 8
- 230000001050 lubricating effect Effects 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000000502 dialysis Methods 0.000 claims description 7
- 239000000654 additive Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
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- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 4
- 238000007792 addition Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims 2
- 238000009210 therapy by ultrasound Methods 0.000 claims 1
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 239000012043 crude product Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 239000002243 precursor Substances 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- 239000008367 deionised water Substances 0.000 abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 abstract description 4
- 230000005284 excitation Effects 0.000 abstract description 4
- 238000004020 luminiscence type Methods 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
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- 239000012467 final product Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 13
- 239000000243 solution Substances 0.000 description 12
- 239000010949 copper Substances 0.000 description 10
- 238000005461 lubrication Methods 0.000 description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000002189 fluorescence spectrum Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000011656 manganese carbonate Substances 0.000 description 2
- 229940093474 manganese carbonate Drugs 0.000 description 2
- 235000006748 manganese carbonate Nutrition 0.000 description 2
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 2
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 description 2
- 239000012264 purified product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002109 single walled nanotube Substances 0.000 description 2
- BYMUNNMMXKDFEZ-UHFFFAOYSA-K trifluorolanthanum Chemical compound F[La](F)F BYMUNNMMXKDFEZ-UHFFFAOYSA-K 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 239000004246 zinc acetate Substances 0.000 description 2
- 240000002234 Allium sativum Species 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 240000007049 Juglans regia Species 0.000 description 1
- 235000009496 Juglans regia Nutrition 0.000 description 1
- XOJVVFBFDXDTEG-UHFFFAOYSA-N Norphytane Natural products CC(C)CCCC(C)CCCC(C)CCCC(C)C XOJVVFBFDXDTEG-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012984 biological imaging Methods 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 150000001860 citric acid derivatives Chemical class 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001917 fluorescence detection Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 235000004611 garlic Nutrition 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000010329 laser etching Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000003921 particle size analysis Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000013456 study Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 235000020234 walnut Nutrition 0.000 description 1
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- 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
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
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- 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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Abstract
A preparation method of metal doped fluorescent biomass carbon quantum dots relates to the technical field of carbon quantum dot synthesis, citric acid is used as a carbon source, a precursor of required doped metal is introduced, deionized water or ultrapure water is added into a hydrothermal reaction kettle, and hydrothermal reaction is carried out to obtain a crude product of the metal doped carbon quantum dots; filtering, dialyzing, and freeze-drying to obtain the final product. The prepared metal doped fluorescent biomass carbon quantum dot emits bright blue fluorescence under the irradiation of an ultraviolet lamp, and emits light in the range of 100-750 nm under the excitation wavelength of 310nm, wherein the broad peak of 400-575 nm belongs to the characteristic emission wavelength of the carbon quantum dot. The invention has the advantages of high purity of the synthesized product, good product luminescence and stability, high yield and formation of the wear-resistant protective film on the metal-based surface, overcomes the defect that the traditional carbon quantum dot has single lubricating property, ensures that the base material reduces wear to a certain extent, and has good application prospect in the mechanical field.
Description
Technical Field
The invention relates to the technical field of carbon quantum dot synthesis, in particular to a preparation method of metal doped fluorescent biomass carbon quantum dots.
Background
Carbon Quantum Dots (CQDs) have been widely studied as a fluorescent carbon nanomaterial. The fluorescent carbon quantum dot has small particle size, good water solubility, stable optical performance and better biocompatibility, and is widely applied to the fields of medicine, biological imaging, fluorescence detection and the like.
Currently, the preparation of carbon quantum dots can be divided into two categories. One is a top-down method, which is mainly to gradually strip macromolecular materials into CQDs (Sun Mojie, zhao Zhihai, chen Gongmei, nie Fujiang) with smaller sizes, the synthesis research of carbon quantum dots progresses and is hopefully [ J ]. Chemical report, 2016,79 (08): 691-698), the main components of which are carbon nanotubes (Xu X, rayR, guY, et al, electric analysis and purification of fluorescent single-walled carbon nanotube fragments [ J ]. Journal of the American Chemical Society,2004,126 (40): 12736-12737 ], graphite, carbon powder and recently raised macromolecules such as garlic, leaves and walnut shells. The top-down method mainly comprises arc discharge, chemical method, laser etching method, chemical oxidation method, etc.
The other is a bottom-up process, which polymerizes into CQDs [ Chen Yue ] by combustion, heating, and microwave means. Synthesis, functionalization and study of fluorescence properties of graphene quantum dots [ D ]. The main raw materials are citrates [ Bottini M, balasubramanian C, dawson M I, et al isolation and characterization of fluorescent nanoparticles from pristine and oxidized electric arc-produced single-walled carbon nanotubes [ J ]. Journal of Physical Chemistry B,2006,110 (2): 831-836 ] carbohydrates, biological small molecules, soot, etc. represented by glucose. The bottom-up method mainly comprises solvothermal/hydrothermal, pyrolysis/combustion, microwaves and the like.
The preparation inevitably has the defects of low purity, poor luminescence, poor stability and the like of the product. Meanwhile, the carbon quantum dots prepared by the prior art have single performance, cannot effectively realize lubricating performance, and cannot be applied to the mechanical field. In view of the above, the metal doped fluorescent biomass carbon quantum dot prepared by the method can solve the problems of product luminescence and stability and has higher lubricating property, so that the prepared material can reduce abrasion to a certain extent and has good application prospect in the mechanical field.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of the metal-doped fluorescent biomass carbon quantum dot, which is simple to operate and environment-friendly.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the metal doped fluorescent biomass carbon quantum dot comprises a one-step hydrothermal synthesis method, wherein citric acid is used as a carbon source, a precursor of the required doped metal is introduced, deionized water or ultrapure water is added into a hydrothermal reaction kettle, and hydrothermal reaction is carried out to obtain a crude product of the metal doped carbon quantum dot; and filtering and dialyzing the crude product to obtain a metal doped carbon quantum dot purified product, and finally freeze-drying to obtain a finished product.
Further, the preparation method of the metal doped fluorescent biomass carbon quantum dot comprises the following steps:
step S1: adding a metal precursor, citric acid, ethanol and deionized water or ultrapure water which are required to be doped into a hydrothermal reaction kettle, covering a cover and screwing;
step S2: heating the hydrothermal reaction kettle in the step S1 to perform hydrothermal reaction, and cooling to room temperature after the reaction is finished to obtain a crude product of the metal-doped carbon quantum dots;
step S3: and (3) filtering and dialyzing the crude product of the metal-doped carbon quantum dots obtained in the step (S2) to obtain a purified product of the metal-doped carbon quantum dots, and finally, freeze-drying to obtain a finished product.
As a preferable technical scheme of the invention, the preparation method of the metal doped fluorescent biomass carbon quantum dot comprises the following steps:
the metal precursor in the step S1 is one or a combination of a plurality of nickel nitrate, copper chloride, manganese carbonate, zinc acetate and lanthanum fluoride. The addition amount of each raw material in the hydrothermal reaction kettle is as follows: 0.001-1 g of metal precursor, 0.05-3 g of citric acid, 10-25 mL of deionized water or ultrapure water and 10-100 mL of ethanol.
In the step S2, a digital display type drying oven heating or an oil bath heating is adopted for carrying out hydrothermal reaction. The hydrothermal reaction temperature is 100-240 ℃, and the reaction time is 2-10 h.
And step S3, filtering the crude product of the metal doped carbon quantum dots through a 0.22 mu m filter membrane, and dialyzing for 12-48 h through a 1000-5000 Da dialysis bag.
Compared with the prior art, the invention has the beneficial effects that:
1. the particle size of the metal doped fluorescent biomass carbon quantum dot prepared by the method is 1.55-3.23 nm, the particle size distribution is uniform and centralized, bright blue fluorescence is emitted under the irradiation of an ultraviolet lamp, and the metal doped fluorescent biomass carbon quantum dot emits light in the range of 100-750 nm under the excitation wavelength of 310nm, wherein the broad peak of 400-575 nm belongs to the characteristic emission wavelength of the carbon quantum dot.
2. The invention has the advantages of high purity of the synthesized product, good product luminescence and stability, high yield and formation of the wear-resistant protective film on the metal-based surface, overcomes the defect that the traditional carbon quantum dot has single lubricating property, ensures that the base material reduces wear to a certain extent, and has good application prospect in the mechanical field.
3. The metal doped carbon quantum dots prepared by the method take different metal compounds as metal sources, volatile components in the metal doped carbon quantum dots are removed by a high-temperature carbonization method, and then the metal doped carbon quantum dots are further processed by filtration and dialysis, so that the different metal doped carbon quantum dots are obtained, the full utilization of biomass resources can be realized, and the process is safe and environment-friendly.
4. Experiments prove that the prepared biomass carbon has fluorescence with different intensities under different excitation wavelengths. The invention not only can realize biomass resource utilization, but also has important theoretical significance and application value in the application field of fluorescent materials.
Drawings
Fig. 1 is a TEM image of La doped carbon quantum dots prepared in example 1.
Fig. 2 is a graph of particle size analysis of La-doped carbon quantum dots prepared in example 1.
FIG. 3 is a graph of fluorescence emission spectrum (inserted as bright blue fluorescence under irradiation of ultraviolet lamp) of La-doped carbon quantum dots prepared in example 1.
Fig. 4 is a graph of the change in coefficient of friction of metal-based carbon quantum dots (Cu doped) as a water-based lubrication additive.
Detailed Description
Example 1
Preparation of La doped carbon quantum dot
80mL of ethanol and 15mL of ultrapure water are measured, 0.089g of citric acid and 0.0045g of lanthanum fluoride are weighed and mixed uniformly by ultrasonic, then the solution is transferred into a polytetrafluoroethylene lining hydrothermal reaction kettle, the constant temperature heating is carried out for 10 hours at 160 ℃, the reaction is naturally cooled to the temperature after the completion, the obtained solution is filtered through a 0.22 mu m filter membrane, dialyzed for 48 hours through a 1000-5000 Da dialysis bag, and finally the finished product is obtained through freeze drying.
The particle size of the prepared carbon quantum dots is more than 1.55-3.23 nm, the average diameter is about 2.48nm, and the particle size distribution is uniform and concentrated as can be observed through figures 1 and 2.
As shown in fig. 3, the lanthanum-doped carbon quantum dot solution prepared in this example emits bright blue fluorescence under irradiation of an ultraviolet lamp. Under the excitation wavelength of 310nm, emission exists in the range of 100-750 nm, wherein the broad peak of 400-575 nm belongs to the characteristic emission wavelength of the carbon quantum dots.
Example 2
Preparation of Mn-doped carbon quantum dots
700mL of ethanol and 10mL of ultrapure water are measured, 2g of citric acid and 0.0025g of manganese carbonate are weighed and mixed uniformly by ultrasonic, then the solution is transferred into a polytetrafluoroethylene lining hydrothermal reaction kettle, the temperature is kept constant at 180 ℃ for 6 hours, the reaction is naturally cooled to the temperature, the obtained solution is filtered through a 0.22 mu m filter membrane, dialyzed for 30 hours through a 1000-5000 Da dialysis bag, and finally the finished product is obtained through freeze drying.
The microstructure and fluorescence emission spectrum of the Mn-doped carbon quantum dot prepared in the embodiment are basically consistent with those of the La-doped carbon quantum dot prepared in the embodiment 1.
Example 3
Preparation of Zn doped carbon quantum dot
50mL of ethanol and 22mL of ultrapure water are measured, 1.5g of citric acid and 0.005g of zinc acetate are weighed and mixed uniformly by ultrasonic, then the solution is transferred into a polytetrafluoroethylene lining hydrothermal reaction kettle, the temperature is kept constant at 200 ℃ and heated for 5 hours, the solution is naturally cooled to the temperature after the reaction is finished, the obtained solution is filtered through a 0.22 mu m filter membrane, dialyzed for 36 hours through a 1000-5000 Da dialysis bag, and finally the finished product is obtained through freeze drying.
The microscopic morphology and fluorescence emission spectrum of the Zn doped carbon quantum dot prepared in the embodiment are basically consistent with those of the La doped carbon quantum dot prepared in the embodiment 1.
Example 4
Preparation of Cu-doped carbon quantum dots
100mL of ethanol and 10mL of ultrapure water are measured, 0.1g of citric acid and 0.001g of copper chloride are weighed and mixed uniformly by ultrasonic, then the solution is transferred into a polytetrafluoroethylene lining hydrothermal reaction kettle, the temperature is kept constant at 220 ℃ and heated for 3 hours, the solution is naturally cooled to the temperature after the reaction is finished, the obtained solution is filtered through a 0.22 mu m filter membrane, dialyzed for 42 hours through a 1000-5000 Da dialysis bag, and finally the finished product is obtained through freeze drying.
The microscopic morphology and fluorescence emission spectrum of the Cu-doped carbon quantum dot prepared in the embodiment are basically consistent with those of the La-doped carbon quantum dot prepared in the embodiment 1.
The coefficient of friction during the run was recorded by a umt-2 friction tester (load 10N, friction time 0.5 h). The results are shown in fig. 4, and the test data in fig. 4 correspond to:
pure ultrapure water lubrication (H) 2 O), ultra-Pure water lubrication on copper film (Pure water 0.5h, 1h, 2 h), metal-based carbon quantum dots (Cu doping) added in an amount of 0.5wt% as a water-based lubrication additive lubrication on copper film (0.5 wt% cu@cqd 0.5, 1h, 2 h), metal-based carbon quantum dots (Cu doping) added in an amount of 0.5wt% as a water-based lubrication additive direct lubrication (0.5 wt% cu@cqd). Wherein, the copper film is formed by immersing the steel plate in 0.5wt% of metal-based carbon quantum dot (Cu doped) aqueous solution for 0.5h, 1h and 2h respectively.
As can be seen from fig. 4, the value of the friction coefficient of the ultra-pure water lubrication is the largest, and the values of the friction coefficients of the ultra-pure water and the metal-based carbon quantum dot solution lubrication on the copper film are reduced. The metal-based carbon quantum dots (Cu doped) with the additive amount of 0.5wt% have the best lubricating effect and the lowest friction coefficient on the copper film soaked for 1h as the water-based lubricating additive.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (1)
1. The application of the metal doped fluorescent biomass carbon quantum dot as the water-based lubricating additive is characterized in that the preparation method of the metal doped fluorescent biomass carbon quantum dot comprises the following steps:
weighing 100mL of ethanol and 10mL of ultrapure water, weighing 0.1g of citric acid, 0.001g of copper chloride, carrying out ultrasonic treatment to uniformly mix the citric acid and the copper chloride, transferring the solution into a polytetrafluoroethylene lining hydrothermal reaction kettle, heating the solution at a constant temperature of 220 ℃ for 3 hours, naturally cooling the solution to room temperature after the reaction is finished, filtering the solution through a 0.22 mu m filter membrane, dialyzing the solution for 42 hours through a 1000-5000 Da dialysis bag, and finally obtaining a finished Cu-doped carbon quantum dot through freeze drying;
the addition amount of the metal doped fluorescent biomass carbon quantum dots is 0.5wt%.
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