CN104477967B - A kind of method preparing Red copper oxide crystallite for reducing agent with carbon quantum dot - Google Patents
A kind of method preparing Red copper oxide crystallite for reducing agent with carbon quantum dot Download PDFInfo
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- CN104477967B CN104477967B CN201410656234.1A CN201410656234A CN104477967B CN 104477967 B CN104477967 B CN 104477967B CN 201410656234 A CN201410656234 A CN 201410656234A CN 104477967 B CN104477967 B CN 104477967B
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- quantum dot
- carbon quantum
- copper oxide
- red copper
- reducing agent
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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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
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The present invention relates to Red copper oxide, it is provided that a kind of Red copper oxide crystallite with carbon quantum dot for reducing agent synthesis with special appearance.Described carbon quantum dot is with grass as raw material, utilizes hydro-thermal method to obtain carbon quantum dot.The synthesis of described Red copper oxide is with carbon quantum dot as reducing agent, with mantoquita for copper source, in the presence of surfactant and NaOH solution, utilizes hydro-thermal method, and through washing, alcohol is washed and is centrifuged and dries the Red copper oxide crystallite obtaining a kind of local special appearance.Red copper oxide prepared by the method is micron-scale and scale topography is evenly distributed, and purity is high.
Description
Technical field
The present invention relates to a kind of method preparing Red copper oxide crystallite for reducing agent with carbon quantum dot；Preparation technology is simple, and raw material environmental protection is cheap and easy to get, and product purity is high.
Technical background
As a kind of important P-type mos material, Red copper oxide is in opto-electronic conversion, and gas sensing, the field such as photocatalysis exists potential value and by the extensive concern of Chinese scholars；In the research in past, find to have between the character of Red copper oxide and its pattern and size important contacting；Such as, find during with Red copper oxide for catalyst photo-catalytic degradation of methyl-orange, expose the cubic cuprous oxide catalysis activity of (100) crystal face significantly lower than the regular octahedron type Red copper oxide exposing (111) crystal face, Cao et al. finds that the photocatalytic activity of cubic Red copper oxide increases (Materials Letters along with the reduction of its particle diameter, 2014
114,88)；Owing to Red copper oxide pattern has important impact to its character, thus control the focus that synthesis has the Red copper oxide research the most both at home and abroad of specific dimensions, pattern；In the past few years, many has the micro Nano material of specific morphology and is successively synthesized, such as: cubic, regular octahedron shape, spherical, nanometer wire, nanotube-shaped etc..
Carbon quantum dot is a kind of novel carbon nanomaterial, it has nontoxic, environmental sound, synthesize low cost and other advantages and be widely used in bio-imaging, photocatalysis, the field such as detection of heavy metal ion, prepared in the experiment of Red copper oxide in the past, the reducing agent generally used is micromolecular compound, such as: ascorbic acid, hydrazine hydrate, polyhydric alcohol etc..Relative to above-mentioned used reducing agent, carbon quantum dot reducing agent used in this experiment has cheap and easy to get, environmental protection, the advantage such as stable.
Up to now, being not yet found to have people and use the carbon quantum dot prepared for raw material with grass to prepare Red copper oxide for reducing agent hydrothermal reduction, Red copper oxide prepared by the method is micron-scale and scale topography is evenly distributed, and purity is high.
Summary of the invention
It is an object of the present invention to provide a kind of with the carbon quantum dot prepared by hydro-thermal grass as reducing agent, the method for Hydrothermal Synthesis Red copper oxide crystallite.
The present invention is realized by following steps:
(1) prepare carbon quantum dot reducing agent: weigh a certain amount of grass and be placed in the reactor that liner is politef, add distilled water, hydro-thermal reaction；It is filtrated to get carbon quantum dot solution.
(2) weigh certain mass mantoquita, add distilled water, NaOH solution, carbon quantum dot solution, surfactant, after magnetic agitation, transfer in water heating kettle, after hydro-thermal reaction；The products in water obtained and alcohol are cleaned, centrifugal, dry, obtain Red copper oxide.
In step 1, grass is Korea lawn grass, bent grass or Herba Stenotaphri helferi；The distilled water of every 10 ~ 30 mL adds the grass of 2 ~ 6 g.
In step 1, hydrothermal temperature is 160 ~ 200oC, the response time is 2 ~ 6 h.
In step 2, mantoquita, NaOH solution, surfactant, the mass volume ratio of carbon quantum dot solution and distilled water is: 255 mL:200 ~ 800, mg:10 ~ 20 mg:8 mL:10 mL；Wherein the concentration of NaOH solution is 1 mol/L.
In step 2, mantoquita is CuCl2•2H2O, Cu (NO3) •3H2O or CuSO4•5H2O。
In step 2, surfactant is Polyethylene Glycol, and its molecular weight is 2000.
In step 2, mixing time is 10 ~ 150 min, and stir speed (S.S.) is 100 ~ 1500 r/min.
In step 2, the temperature of hydro-thermal reaction is 160 ~ 200 DEG C, and the time of hydro-thermal reaction is 6 ~ 10 h.
During washing, water used is distilled water, and alcohol used when alcohol is washed is dehydrated alcohol.
The pattern of Red copper oxide is that the spherical Red copper oxide of classification, spherical alumina be cuprous or flower-shaped Red copper oxide；Utilize X x ray diffractometer x (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM) that product is carried out micromorphology analysis.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of prepared carbon quantum dot, and as can be seen from the figure the carbon quantum dot particle diameter prepared by hydro-thermal grass is at 3-5 nm, good dispersion.
Fig. 2 is the XRD diffraction spectrogram of prepared three kinds of different-shape Red copper oxide crystallite samples, in figure diffraction maximum all with Emission in Cubic Red copper oxide standard card one_to_one corresponding；The spherical Cu of a: classification2O；B: spherical Cu2O；C: flower-shaped Cu2O。
Fig. 3 is the stereoscan photograph of prepared different-shape Red copper oxide crystallite: the spherical Cu of a, b: classification2O；C, d: spherical Cu2O；E, f: flower-shaped Cu2O。
Detailed description of the invention
Embodiment
1
The preparation of carbon quantum dot
The preparation of carbon quantum dot uses hydrothermal synthesis method: weighs the grass of 4 g in the reactor of the politef of 50 mL, then adds 20 mL distilled water, and be placed on 180oThe drying baker of C is incubated 4 h, after taking-up reactor is after naturally cool to room temperature, filters out solid impurity and obtain carbon quantum dot solution.
Embodiment
2
The preparation of the spherical Red copper oxide of classification
By the Cu (NO of 255 mg3) •3H2O is dissolved in 10 mL distilled water, then add 10 mL NaOH solution (1 mol/L), the carbon quantum solution prepared by the Macrogol 2000 of 600 mg and 8 mL is added after dripping, mixed solution 1500 r/min stirs 10 min, it is then transferred in the reactor of 50 mL politef, put in baking oven, 180oReact 8 h under C, take out reactor and naturally cool to room temperature；Gained sample deionized water and dehydrated alcohol are respectively washed 3 times, centrifugal are placed in vacuum drying oven 60oC is dried 8 h.
Embodiment
3
The preparation that spherical alumina is cuprous
CuCl by 255 mg2•2H2O is dissolved in 10 mL distilled water, then add 20 mL NaOH solution (1 mol/L), the carbon quantum solution prepared by the Macrogol 2000 of 800 mg and 8 mL is added after dripping, mixed solution 100 r/min stirs 150 min, it is then transferred in the reactor of 50 mL politef, put in baking oven, 200oReact 6 h under C, take out reactor and naturally cool to room temperature；Gained sample deionized water and dehydrated alcohol are respectively washed 3 times, centrifugal are placed in vacuum drying oven 60oC is dried 8 h.
Embodiment
4
The preparation of flower-shaped Red copper oxide
CuCl by 255 mg2•2H2O is dissolved in 10 mL distilled water, then add 20 mL NaOH solution (1 mol/L), the carbon quantum solution prepared by the Macrogol 2000 of 200 mg and 8 mL is added after dripping, mixed solution 900 r/min stirs 80 min, it is then transferred in the reactor of 50 mL politef, puts into 160oThe baking oven of C reacts 10 h, takes out reactor and naturally cool to room temperature；Gained sample distilled water and dehydrated alcohol are respectively washed 3 times, centrifugal are placed in vacuum drying oven 60oC is dried 8 h.
Claims (4)
1. the method preparing Red copper oxide crystallite for reducing agent with carbon quantum dot, it is characterised in that: weigh certain mass mantoquita, add
Enter distilled water, NaOH solution, carbon quantum dot solution and surfactant, after magnetic agitation, transfer in water heating kettle, hydro-thermal
After reaction；The products in water obtained and alcohol are cleaned, centrifugal, dry, obtain Red copper oxide crystallite, and the temperature of hydro-thermal reaction is
160～200 DEG C, the time of hydro-thermal reaction is 6～10h；
The preparation method of described carbon quantum dot solution is as follows: weighs a certain amount of grass and is placed in the reactor that liner is politef
In, add distilled water, hydro-thermal reaction；It is filtrated to get carbon quantum dot solution；Described grass is Korea lawn grass, bent grass or Herba Stenotaphri helferi；
The distilled water of every 10～30mL adds the grass of 2～6g；Hydrothermal temperature is 160～200 DEG C, and the response time is 2～6h；
Described mantoquita, NaOH solution, surfactant, the mass volume ratio of carbon quantum dot solution and distilled water is: 255mg:
10～20mL:200～800mg:8mL:10mL；Wherein the concentration of NaOH solution is 1mol/L；
Described surfactant is Polyethylene Glycol, and its molecular weight is 2000.
A kind of method preparing Red copper oxide crystallite for reducing agent with carbon quantum dot, it is characterised in that: copper
Salt is CuCl2·2H2O or CuSO4·5H2O。
A kind of method preparing Red copper oxide crystallite for reducing agent with carbon quantum dot, it is characterised in that: stir
The time of mixing is 10～150min, and stir speed (S.S.) is 100～1500r/min.
A kind of method preparing Red copper oxide crystallite for reducing agent with carbon quantum dot, it is characterised in that: water
When washing, water used is distilled water, and alcohol used when alcohol is washed is dehydrated alcohol.
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| CN111524716B (en) * | 2020-01-10 | 2022-04-29 | 厦门理工学院 | Preparation and application of composite electrode material with manila herb as carbon source |
| CN116396749A (en) * | 2023-02-15 | 2023-07-07 | 桂林电子科技大学 | Synthesis of metal selenide quantum dot and carbon dot and preparation method of light-emitting device |
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| CN103100725B (en) * | 2013-02-28 | 2015-03-04 | 江苏大学 | Preparation method of silver/carbon quantum dot composite nanometer materials |
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