CN105236386A - Method for preparing carbon nanoparticles through corncob - Google Patents
Method for preparing carbon nanoparticles through corncob Download PDFInfo
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- CN105236386A CN105236386A CN201510760499.0A CN201510760499A CN105236386A CN 105236386 A CN105236386 A CN 105236386A CN 201510760499 A CN201510760499 A CN 201510760499A CN 105236386 A CN105236386 A CN 105236386A
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Abstract
The invention relates to a method for preparing carbon nanoparticles through corncob. The method includes the steps that the corncob is dried, then calcination is conducted under the protection of inert gases, natural cooling is carried out, samples are taken out, grinding is performed, and powder is obtained; the powder is placed in mixed liquor of concentrated sulfuric acid and concentrated nitric acid, reacting is conducted for 6-48 hours at the temperature of 80-120 DEG C, the temperature drops to an indoor temperature, and a mixed solution is obtained; ultrapure water is poured into the mixed solution, reacting is conducted for 1-60 min, and ultrapure water is added to end the reaction; the reaction solution stands, lower layer sediment is collected, and centrifuging is conducted; afterwards, ultrapure water is added, ultrasound and centrifuging are carried out till supernatant liquid is transparent, lower layer powder is collected for vacuum freeze-drying, and accordingly the carbon nanoparticles are obtained. According to the method, the renewable resource corncob is used as the raw material, and thus has the advantages of being not prone to deterioration and capable of being stably stored for a long time at the indoor temperature. The nanoparticles obtained through the method are uniform in size and have the potential to be applied to various fields such as fluorescent powder and biomarkers.
Description
Technical field
The invention belongs to the preparation method field of carbon nano-particle, particularly a kind of method utilizing corn cob to prepare carbon nano-particle.
Background technology
The definition of carbon nano-particle: at least size is less than the carbon granule of 100 nanometers in a dimension.Because carbon nano-particle has nontoxic, good biocompatibility, the feature such as with low cost, this material is widely used in the fields such as biomarker, metal ion detection, catalyzed degradation.At present, the raw materials of carbon nano-particle is various in style, mainly some carbohydrate (as glucose, chitosan), the small molecules (e.g., Trisodium Citrate and trimeric cyanamide) of carbon containing, plant and plant milk extract (as, Viscotrol C, Watermelon rind, orange juice), petroleum chemicals (e.g., coal and graphite) etc.Along with the exhaustion day by day of the natural resourcess such as oil, renewable resources as an alternative product causes the extensive concern of scientific circles.The people such as India scientist Sahu use orange juice as reaction raw materials, utilize the evengranular carbon nano-particle (SahuS. of water heat transfer, BeheraB, MaitiT.K., etal.Simpleone-stepsynthesisofhighlyluminescentcarbondot sfromorangejuice:applicationasexcellentbio-imagingagents, 2012,48,8835-8837.).The people such as India scientist Muthukumar use Viscotrol C as raw material, utilize combustion method to collect the Viscotrol C cigarette produced that burns and prepare carbon nano-particle (MuthukumarT., PrabhavathiS., ChamundeeswariM., etal.Bio-modifiedcarbonnanoparticlesloadedwithmethotrexa tepossiblecarrierforanticancerdrugdelivery, MaterialsScienceandEngineeringC, 2014,36,14-19.).In addition, the material such as strawberry juice, orange peel is also had by use biological material.Although above-mentioned biological material is all renewable energy source, major part is that itself is edible.Even if waste, as the limits throughput of orange peel itself, and the requirement of raw material to condition of storage is high.Corn cob is as renewable raw materials, and output own is very large and condition of storage is less demanding.The product separation finally obtained is purified easily, and uniform particles; Do not need to use dialysis tubing, the devices such as inorganic filter membrane carry out separating-purifying, and technique is simple.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method utilizing corn cob to prepare carbon nano-particle, the method productive rate is high, be applicable to suitability for industrialized production, the carbon nano-particle particle size uniformity obtained, has the potentiality being applied to the every field such as fluorescent material, biomarker.
A kind of method utilizing corn cob to prepare carbon nano-particle of the present invention, comprising:
(1) corn cob is dried, put into porcelain boat and send into tube furnace, then calcine under protection of inert gas;
(2), after calcining terminates, naturally cooling, takes out sample, and grinding, obtains powder;
(3) powder obtained in step (2) is put into the mixed solvent of the vitriol oil and concentrated nitric acid, 80 DEG C ~ 120 DEG C reaction 6h ~ 48h, are down to room temperature, obtain mixed solution;
(4) ultrapure water 10ml ~ 100ml is poured in the mixed solution in step (3), reaction 1 ~ 60min, add ultrapure water and terminate reaction;
(5) leaving standstill terminating reacted reaction solution in step (4), getting lower sediment, centrifugal, then add ultrapure water, ultrasonic, centrifugal, transparent to supernatant liquid, take off a layer vacuum powder lyophilize, obtain carbon nano-particle.
In described step (1), porcelain boat is that the resistant to elevated temperatures material such as aluminum oxide or quartz obtains; Reaction tubes in tube furnace is silica glass material or aluminum oxide material.
Corn cob is dried and is referred to that corn cob is put into baking oven and is dried to corn cob weight and no longer changes along with the change of time in described step (1); The temperature of drying is 60 ~ 100 DEG C, and the time is 6 ~ 24h.
In described step (1), rare gas element is nitrogen or argon gas.
In described step (1), the condition of calcining is: heat-up rate is 0.1 ~ 20 DEG C/min, and temperature rises to 500 ~ 2400 DEG C, insulation 0.1 ~ 48h.
Add alcohol during grinding in described step (2), grinding terminates post-drying; Wherein, first roughly grind in agate grinding pot during grinding, put into planetary ball mill subsequently and grind.
In described step (3), the vitriol oil and the molar mass of concentrated nitric acid are than being 10:1 ~ 1:10; The vitriol oil is 1 ~ 1000:1 with the total amount of concentrated nitric acid and the volume mass ratio of powder.
The massfraction of the described vitriol oil is 95% ~ 98%, and the massfraction of concentrated nitric acid is 65% ~ 68%.
When terminating in described step (4) to react, the mass ratio of the acid that ultrapure water and step (3) use is 1 ~ 1000:1.
The time left standstill in described step (5) is 1h ~ 15d.
In described step (5) centrifugal speed be 10000 turns/min ~ 24000 turn/min, centrifugation time is 30min ~ 10h; The ultrasonic time is 10min ~ 6h.
In described step (5) centrifugal and ultrasonic be repeatable operation process, to supernatant liquid is completely transparent.
In described step (5), the vacuum tightness of vacuum lyophilization is less than 20pa, and temperature is-40 DEG C, and the time is 6 ~ 48.
beneficial effect
(1) method of the present invention uses reproducible waste corn cob to be starting material, has and easily deposits and not perishable feature;
(2) method of the present invention is applicable to suitability for industrialized production, and the carbon nano-particle prepared has that productive rate is high, the advantage of particle size uniformity, and is applied to the potentiality of the every field such as fluorescent material, biomarker.
Accompanying drawing explanation
Fig. 1 is the Raman spectrum obtaining the corn cob after calcining in embodiment 1;
Fig. 2 is the transmission electron microscope photo obtaining carbon nano-particle in embodiment 1;
Fig. 3 is the X-ray diffraction spectrum obtaining carbon nano-particle in embodiment 1;
Fig. 4 is the infrared spectra obtaining carbon nano-particle in embodiment 1;
Fig. 5 is the full spectrum of the x-ray photoelectron power spectrum obtaining carbon nano-particle in embodiment 1;
Fig. 6 is the C1s spectrum of the x-ray photoelectron power spectrum obtaining carbon nano-particle in embodiment 1;
Fig. 7 is the fluorescence spectrum obtaining carbon nano-particle in embodiment 1;
Fig. 8 is the up-conversion fluorescence spectrum obtaining carbon nano-particle in embodiment 1;
Fig. 9 be obtain in embodiment 1 carbon nano-particle visible-ultra-violet absorption spectrum;
Figure 10 is the Raman spectrum obtaining carbon nano-particle in embodiment 1.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
Get the baking oven baking 24h that corn cob puts into 60 DEG C.The corn cob of drying rear embrittlement is put into quartz tube furnace, high-temperature calcination under the protection of argon gas atmosphere.(parameter: 5 DEG C/min is warming up to 1000 DEG C, and naturally cooling after being incubated 4 hours at 1000 DEG C.)
The agate grinding pot that corn cob after calcining and alcohol are put into agate ball is roughly ground, puts into planetary ball mill subsequently and grind 2h.Take out the abrasive material after grinding, it is poured in glass beaker together with alcohol.Toast 12 hours under the condition of 60 DEG C, product is carried out except water treatment.
The product after 1g grinding is taken, HNO dense with 30ml with analytical balance
3, the dense H of 90ml
2sO
4be placed in the heating unit of band reflux condensation mode together with reflux 24h under the condition of 95 DEG C.After question response liquid cooling but, be poured in the glass beaker of 5000ml, add 50ml ultrapure water reaction 15min subsequently, finally add 1000ml ultrapure water termination reaction.
Reaction solution is left standstill 7 days, outwells supernatant liquid gently.Take off under layer is deposited in the speed of 12000 turns/min and get precipitation in centrifugal 2 hours.Subsequently with recentrifuge after ultrapure water cleaning, repeat operation ten times, transparent to supernatant liquid, take out vacuum powder lyophilize (vacuum tightness is 15pa, temperature :-45 DEG C, 96h), the brown-black powder obtained is carbon nano-particle.Carry out test subsequently to characterize.
The corn cob of drying rear embrittlement is put into quartz tube furnace, the Raman spectrogram of the black powder obtained after high-temperature calcination under the protection of argon gas atmosphere by Fig. 1.As can be seen from the figure 1347cm
-1corresponding peak is graphite D peak, 1591cm
-1corresponding peak is the G peak of graphite.
Fig. 2 is the transmission electron microscope photo of prepared brownish black nano particle, can find out prepared carbon nano-particle size uniform clearly from figure.
Fig. 3 is the X-ray diffraction spectrum of prepared brownish black nano particle.As can be seen from Fig.: this peak, at 23 ° of places, is the base peak of nano carbon particle.
Fig. 4 is the infrared spectra of prepared brownish black nano particle.As can be seen from Fig.: this material surface contains obvious carbon containing, oxygen containing functional group.
Fig. 5 is the full spectrum of the x-ray photoelectron power spectrum of prepared brownish black nano particle.As can be seen from the figure: this material contains carbon, oxygen element and nitrogen element.
Fig. 6 is the C1s spectrum of the x-ray photoelectron power spectrum of prepared brownish black nano particle.Can find out that this material contains: C-C, C-N, C-O, C=O, O-C=O by analysis.
Fig. 7 is the fluorescence spectrum of prepared brownish black nano particle.As can be seen from the figure: along with the change of excitation spectrum, the crest of emmission spectrum, all at 520nm place, does not have too large change.
Fig. 8 is the up-conversion fluorescence spectrum of prepared brownish black nano particle.As can be seen from the figure: along with the change of excitation spectrum, the crest of emmission spectrum, all at 520nm place, does not have too large change.
Fig. 9 be prepared brownish black nano particle visible-ultra-violet absorption spectrum.As can be seen from the figure: this material has very strong absorption at visible ray and ultraviolet light range.
Figure 10 is the Raman spectrum of prepared brownish black nano particle.As can be seen from the figure: compared with the Raman spectrum of the corn cob after carbonization, there is broadening mainly owing to can diminish and cause by particle diameter in crest.
Embodiment 2
Get the baking oven baking 6h that corn cob puts into 100 DEG C.The corn cob of drying rear embrittlement is put into quartz tube furnace, high-temperature calcination under the protection of nitrogen atmosphere.(parameter: 10 DEG C/min is warming up to 1200 DEG C, and naturally cooling after being incubated 4 hours at 1200 DEG C.)
The agate grinding pot that corn cob after calcining and alcohol are put into agate ball is roughly ground, puts into planetary ball mill subsequently and grind 2h.Take out the abrasive material after grinding, it is poured in glass beaker together with alcohol.Toast 6 hours under the condition of 100 DEG C, product is carried out except water treatment.
The product after 1g grinding is taken, HNO dense with 60ml with analytical balance
3, the dense H of 60ml
2sO
4be placed in the heating unit of band reflux condensation mode together with reflux 24h under the condition of 100 DEG C.After question response liquid cooling but, be poured in the glass beaker of 5000ml, add 40ml ultrapure water reaction 15min subsequently, finally add 1000ml ultrapure water termination reaction.
Reaction solution is left standstill seven days, outwells supernatant liquid gently.Take off under layer is deposited in the speed of 12000 turns/min and get precipitation in centrifugal 2 hours.Subsequently with recentrifuge after ultrapure water cleaning, repeat operation ten times, transparent to supernatant liquid, take out vacuum powder lyophilize (vacuum tightness is 10pa, temperature :-45 DEG C, 60h), to obtain final product.
Embodiment 3
Get the baking oven baking 24h that corn cob puts into 80 DEG C.The corn cob of drying rear embrittlement is put into quartz tube furnace, high-temperature calcination under the protection of argon gas atmosphere.(parameter: 8 DEG C/min is warming up to 1300 DEG C, and naturally cooling after being incubated 4 hours at 1300 DEG C.)
The agate grinding pot that corn cob after calcining and alcohol are put into agate ball is roughly ground, puts into planetary ball mill subsequently and grind 4h.Take out the abrasive material after grinding, it is poured in glass beaker together with alcohol.Toast 12 hours under the condition of 80 DEG C, product is carried out except water treatment.
The product after 1g grinding is taken, HNO dense with 60ml with analytical balance
3, the dense H of 90ml
2sO
4be placed in the heating unit of band reflux condensation mode together with reflux 48h under the condition of 95 DEG C.After question response liquid cooling but, be poured in the glass beaker of 5000ml, add 50ml ultrapure water reaction 15min subsequently, finally add 1000ml ultrapure water termination reaction.
Reaction solution is left standstill seven days, outwells supernatant liquid gently.Take off under layer is deposited in the speed of 11000 turns/min and get precipitation in centrifugal 2 hours.Subsequently with recentrifuge after ultrapure water cleaning, repeat operation ten times, transparent to supernatant liquid, take out vacuum powder lyophilize (vacuum tightness is 18pa, temperature :-45 DEG C, 48h), to obtain final product.
Claims (10)
1. utilize corn cob to prepare a method for carbon nano-particle, comprising:
(1) corn cob is dried, put into porcelain boat and send into tube furnace, then calcine under protection of inert gas;
(2), after calcining terminates, naturally cooling, takes out, and grinding, obtains powder;
(3) powder obtained in step (2) is put into the mixed solvent of the vitriol oil and concentrated nitric acid, 80 DEG C ~ 120 DEG C reaction 6h ~ 48h, are down to room temperature, obtain mixed solution;
(4) ultrapure water 10ml ~ 100ml is poured in the mixed solution in step (3), reaction 1 ~ 60min, add ultrapure water and terminate reaction;
(5) leaving standstill terminating reacted reaction solution in step (4), getting lower sediment, centrifugal, then add ultrapure water, ultrasonic, centrifugal, transparent to supernatant liquid, take off a layer vacuum powder lyophilize, obtain carbon nano-particle.
2. a kind of method utilizing corn cob to prepare carbon nano-particle according to claim 1, is characterized in that, in described step (1), porcelain boat is that aluminum oxide or quartz are obtained; Reaction tubes in tube furnace is silica glass material or aluminum oxide material.
3. a kind of method utilizing corn cob to prepare carbon nano-particle according to claim 1, is characterized in that, in described step (1), rare gas element is nitrogen or argon gas.
4. a kind of method utilizing corn cob to prepare carbon nano-particle according to claim 1, it is characterized in that, in described step (1), the condition of calcining is: heat-up rate is 0.1 ~ 20 DEG C/min, and temperature rises to 500 ~ 2400 DEG C, insulation 0.1 ~ 48h.
5. a kind of method utilizing corn cob to prepare carbon nano-particle according to claim 1, is characterized in that, in described step (2), the time of grinding is 2 ~ 4h.
6. a kind of method utilizing corn cob to prepare carbon nano-particle according to claim 1, is characterized in that, in described step (3), the vitriol oil and the molar mass of concentrated nitric acid are than being 10:1 ~ 1:10; The vitriol oil is 1 ~ 1000:1 with the total amount of concentrated nitric acid and the volume mass ratio of powder.
7. a kind of method utilizing corn cob to prepare carbon nano-particle according to claim 1, is characterized in that, the mass ratio of the acid used in ultrapure water and step (3) when terminating reaction in described step (4) is 1 ~ 1000:1.
8. a kind of method utilizing corn cob to prepare carbon nano-particle according to claim 1, is characterized in that, the time left standstill in described step (5) is 1h ~ 15d.
9. a kind of method utilizing corn cob to prepare carbon nano-particle according to claim 1, is characterized in that, in described step (5) centrifugal speed be 10000 turns/min ~ 24000 turn/min, centrifugation time is 30min ~ 10h; The ultrasonic time is 10min ~ 6h.
10. a kind of method utilizing corn cob to prepare carbon nano-particle according to claim 1, is characterized in that, in described step (5), the vacuum tightness of vacuum lyophilization is less than 20pa, and temperature is-40 DEG C, and the time is 6 ~ 48h.
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Cited By (5)
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CN106745645A (en) * | 2016-12-20 | 2017-05-31 | 山西省环境科学研究院 | The preparation method and applications of nano zero-valence iron composite material |
CN109054825A (en) * | 2018-08-24 | 2018-12-21 | 华南理工大学 | A kind of fluorescent carbon quantum dot and its high efficiency preparation method |
CN111196932A (en) * | 2020-01-17 | 2020-05-26 | 中山大学 | Method for preparing nano biochar |
CN113353916A (en) * | 2020-03-05 | 2021-09-07 | 宁夏大学 | Salix purpurea carbonized nanoparticle, Salix purpurea carbonized nanoparticle reinforced composite material, and preparation method and application thereof |
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CN104555978A (en) * | 2013-10-17 | 2015-04-29 | 中国科学院理化技术研究所 | Preparation method of photoluminescent carbon dots |
CN104650864A (en) * | 2015-03-04 | 2015-05-27 | 东华大学 | Method for preparing biomass based carbon quantum dots |
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CN102180459A (en) * | 2011-03-02 | 2011-09-14 | 中北大学 | Method for preparing carbon quantum dots |
CN104555978A (en) * | 2013-10-17 | 2015-04-29 | 中国科学院理化技术研究所 | Preparation method of photoluminescent carbon dots |
CN104650864A (en) * | 2015-03-04 | 2015-05-27 | 东华大学 | Method for preparing biomass based carbon quantum dots |
Cited By (8)
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CN106745645A (en) * | 2016-12-20 | 2017-05-31 | 山西省环境科学研究院 | The preparation method and applications of nano zero-valence iron composite material |
CN106745645B (en) * | 2016-12-20 | 2020-09-22 | 山西省环境科学研究院 | Preparation method and application of nano zero-valent iron composite material |
CN109054825A (en) * | 2018-08-24 | 2018-12-21 | 华南理工大学 | A kind of fluorescent carbon quantum dot and its high efficiency preparation method |
CN109054825B (en) * | 2018-08-24 | 2020-09-22 | 华南理工大学 | Fluorescent carbon quantum dot and efficient preparation method thereof |
CN111196932A (en) * | 2020-01-17 | 2020-05-26 | 中山大学 | Method for preparing nano biochar |
CN113353916A (en) * | 2020-03-05 | 2021-09-07 | 宁夏大学 | Salix purpurea carbonized nanoparticle, Salix purpurea carbonized nanoparticle reinforced composite material, and preparation method and application thereof |
CN114014301A (en) * | 2021-11-17 | 2022-02-08 | 北京师范大学 | Synthetic method of fluorescent carbon nano onion |
CN114014301B (en) * | 2021-11-17 | 2023-03-03 | 北京师范大学 | Synthetic method of fluorescent carbon nano onion |
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