CN105154075A - Preparation method of graphite-phase carbon nitride solid fluorescent powder and application thereof in light fingerprint extraction - Google Patents
Preparation method of graphite-phase carbon nitride solid fluorescent powder and application thereof in light fingerprint extraction Download PDFInfo
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- CN105154075A CN105154075A CN201510584357.3A CN201510584357A CN105154075A CN 105154075 A CN105154075 A CN 105154075A CN 201510584357 A CN201510584357 A CN 201510584357A CN 105154075 A CN105154075 A CN 105154075A
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- carbon nitride
- phase carbon
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Abstract
The invention provides a preparation method of graphite-phase carbon nitride solid fluorescent powder and application thereof in quickly developing latent fingerprints on different object surfaces. The graphite-phase carbon nitride solid fluorescent powder can be used for fluorescence labeling, and can be used in the fields of crime scene criminal detection and the like. The invention aims to quickly develop latent fingerprints on different individual and different object surfaces by utilizing the characteristic of photoluminescence of the nano graphite-phase carbon nitride. The high-fluorescence-responsivity graphite-phase carbon nitride solid fluorescent powder is prepared by using melamine as an N-containing precursor and using sodium chloride and potassium chloride as assistants. The application process in fingerprints comprises the following steps: lightly dipping a fingerprint brush into a small amount of graphite-phase carbon nitride solid fluorescent powder, lightly brushing the suspected fingerprint region, removing the excess powder, putting under a 365nm ultraviolet lamp, and observing the special blue light which is conveniently photographed and stored by a digital camera. Due to the specific adsorptivity of the nano material, the affinity between the nano powder and fingerprint ridges is high. The graphite-phase carbon nitride solid fluorescent powder can be used for successfully extracting fingerprints on different individual and different object surfaces.
Description
Technical field
The invention belongs to nano material preparation technology and as the Application Areas of fluorescent optical sensor at analysis and detection technology.Be specifically related to a kind of preparation method of graphite phase carbon nitride solid fluorescence powder and the application in shallow fingerprint extraction thereof.
Background technology
Nano luminescent material is widely used in fluorescent mark field due to the optical signature of its uniqueness and nanometer size effect.In recent years, its laten fingerprints that manifests fast being used for detecting site as fluorescent optical sensor obtains and develops fast.The nano luminescent material for fingerprint manifestation reported at present mostly is the elementary composition semiconductor-quantum-point of rare earth ion doped luminescent material and II-VI race.
Sydney, AUS University of Science and Technology
claudeRouxrare earth ion doped up-conversion luminescent material is used for manifesting fingerprint reported first in 2011.Under dark room conditions, be adsorbed with the fingerprint region of up-conversion with near infrared light, can observe fingerprint profile clearly.Because up-conversion luminescence has unique luminescence mechanism, the interference of other background fluorescences can be got rid of, therefore have the susceptibility of its uniqueness.But rare earth ion is poisonous to organism, there is potential harm to criminal detective, limit it and further apply.Semiconductor quantum is that another kind reports the more fluorescent material for fingerprint manifestation, and its size is generally used for manifesting fast of fingerprint by wide coverage between the semiconductor-quantum-point such as 1-10nm, CdTe, CdSe, CdS.But the general more complicated of semiconductor-quantum-point synthesis path, and not easily synthesize in a large number, and Te, Cd belong to heavy metal ion, are confirmed environmentally hazardous substances, are unfavorable for extensively promoting its application.Based on above reason, find the emphasis that a kind of synthetic method is simple, safety non-toxic, fluorescence intensity are high fluorescent probe just becomes research field.
G-C
3n
4as a kind of nano material of nonmetal high fluorescence response, in fluorescent optical sensor, there is huge application prospect.Its synthesis is by the high-temperature hot condensation containing the presoma of N such as cyanamide, Dyhard RU 100, trimeric cyanamide.Often quantum yield is lower for the product of direct pyrocondensation, and fluorescence intensity is more weak.Be suitable for larger scope for strengthening its fluorescence intensity to make it, the present invention is based on trimeric cyanamide as containing N presoma, use sodium-chlor and Repone K process trimeric cyanamide before calcination, utilize the high temperature of villaumite to distil, original position peels off g-C
3n
4, the g-C of high fluorescent can be obtained
3n
4.Because its surface is containing-NH
2isoreactivity group, easily to be adsorbed by chemical coupling or specific physical by the material such as grease and amino acid of chemical reaction and electrostatic interaction and fingerprint region and makes g-C
3n
4be adsorbed on fingerprint ridge.
Summary of the invention
In sum, for the deficiencies in the prior art, the present invention is based on trimeric cyanamide for containing N presoma, assisting the graphite phase carbon nitride solid fluorescence powder having prepared high fluorescence response with sodium-chlor and Repone K, and successfully utilizing it to manifest the fingerprint on Different Individual and different object surface.
A preparation method for graphite phase carbon nitride solid fluorescence powder, with weight part, comprises following concrete steps as follows:
A, the trimeric cyanamide taking 8-10 part, 10-12 part sodium-chlor and 12-14 part Repone K are in mortar, and abundant ground and mixed is evenly for subsequent use;
B, the batch mixing prepared by step a proceed in crucible, are placed in retort furnace, in air atmosphere high-temperature calcination 1h, and calcining temperature is 670 DEG C;
C, then at room temperature to cool, the block product after calcining is pulverized and is dispersed in the dilute hydrochloric acid of 0.3mol/l, then centrifugal segregation supernatant liquor; Then repetitive scrubbing repeatedly, the product after washing is placed in 60 DEG C of baking ovens oven dry and is graphite phase carbon nitride solid fluorescence powder.
In addition, the invention provides the application of a kind of graphite phase carbon nitride solid fluorescence powder in laten fingerprints extracts.
beneficial effect:
1. synthetic method is simple, is easy to a large amount of synthesis, can manifests the latent fingerprint on Different Individual and different object surface.
2. nanometer powder is combined comparatively tight with fingerprint ridge, and with other regions in conjunction with poor, manifest result comparatively accurate.
3. namely directly do not observe fingerprint effect by bore hole by any instrument, fingerprint design sketch can be recorded clearly by common digital camera, be convenient to comparison and preserve.
4. synthesis material is less expensive, and product safety non-toxic, any harm can not be brought to operator.
Accompanying drawing explanation
Fig. 1 is the in kind photo of graphite phase carbon nitride solid fluorescence powder before and after 365nm ultra violet lamp prepared by the present invention.
Fig. 2 is the XRD figure of graphite phase carbon nitride solid fluorescence powder prepared by the present invention.
Fig. 3 is the fluorescence spectrum figure of graphite phase carbon nitride solid fluorescence powder prepared by the present invention.
Fig. 4 is the fingerprint design sketch that graphite phase carbon nitride solid fluorescence powder prepared by the present invention manifests Different Individual.
Fig. 5 is the fingerprint design sketch that graphite phase carbon nitride solid fluorescence powder prepared by the present invention manifests different object surface, and wherein a, b, c, d correspond to the fingerprint of mouse, cigarette case, pop can, glass surface respectively.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated:
embodiment 1
A preparation method for graphite phase carbon nitride solid fluorescence powder, comprises the steps:
A, the trimeric cyanamide taking 8g, 10g sodium-chlor and 12g Repone K are in mortar, and abundant ground and mixed is evenly for subsequent use;
B, the batch mixing prepared by step a proceed in crucible, are placed in retort furnace, in air atmosphere high-temperature calcination 1h, and calcining temperature is 670 DEG C;
C, be then cooled to room temperature, the block product after calcining is pulverized and is dispersed in the dilute hydrochloric acid of 0.3mol/l, then centrifugal segregation supernatant liquor; Then repetitive scrubbing repeatedly, the product after washing is placed in 60 DEG C of baking ovens oven dry and is graphite phase carbon nitride solid fluorescence powder.
Graphite phase carbon nitride solid fluorescence powder is used for the presentation application example of Different Individual fingerprint:
Get 4 pieces of slide glasss to rinse well, dry under state of nature.Choose the volunteer that four, laboratory is different, with suds by abundant for hand washes clean, after drying under state of nature, press slide glass gently with finger, can fingerprint be left.
Dip a small amount of graphite phase carbon nitride solid fluorescence powder powder gently with import squirrel hair fingerprint brush, brush aobvious fingerprint gently along fingerprint ridge, blow away the unnecessary graphite phase carbon nitride solid fluorescence powder be not combined with fingerprint ridge with rubber suction bulb.
Slide glass being placed in wavelength is observe under the ultraviolet lamp of 365nm, can see fingerprint ridge clearly, to take pictures preservation with digital camera.
embodiment 2:
A preparation method for graphite phase carbon nitride solid fluorescence powder, comprises the steps:
A, the trimeric cyanamide taking 9g, 11g sodium-chlor and 13g Repone K are in mortar, and abundant ground and mixed is evenly for subsequent use.
B, the batch mixing prepared by step a proceed in crucible, are placed in retort furnace, in air atmosphere high-temperature calcination 1h, and calcining temperature is 670 DEG C.
C, be then cooled to room temperature, the block product after calcining is pulverized and is dispersed in the dilute hydrochloric acid of 0.3mol/l, then centrifugal segregation supernatant liquor; Then repetitive scrubbing repeatedly, the product after washing is placed in 60 DEG C of baking ovens oven dry and is graphite phase carbon nitride solid fluorescence powder.
Graphite phase carbon nitride solid fluorescence powder is used for the presentation application example of different object fingerprint surface:
Choose mouse, cigarette case, pop can, glass four kinds of objects as fingerprint supporting body, with the cotton balls being moistened with ethanol gently wiping dry, with suds by abundant for hand washes clean, after drying under state of nature, press object surface gently with finger, can fingerprint be left.
Dip a small amount of graphite phase carbon nitride solid fluorescence powder powder gently with import squirrel hair fingerprint brush, brush aobvious fingerprint gently along fingerprint ridge, blow away the unnecessary graphite phase carbon nitride solid fluorescence powder powder be not combined with fingerprint ridge with rubber suction bulb.
Different objects being placed in respectively wavelength is observe under the ultraviolet lamp of 365nm, can see fingerprint ridge clearly, to take pictures preservation with digital camera.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (2)
1. a preparation method for graphite phase carbon nitride solid fluorescence powder, is characterized in that, comprises the steps: with parts by weight
A, the trimeric cyanamide taking 8-10 part, 10-12 part sodium-chlor and 12-14 part Repone K are in mortar, and abundant ground and mixed is evenly for subsequent use;
B, the batch mixing prepared by step a proceed in crucible, are placed in retort furnace, in air atmosphere high-temperature calcination 1h, and calcining temperature is 670 DEG C;
C, then at room temperature to cool, the block product after calcining is pulverized and is dispersed in the dilute hydrochloric acid of 0.3mol/l, then centrifugal segregation supernatant liquor; Then repetitive scrubbing repeatedly, the product after washing is placed in 60 DEG C of baking ovens oven dry and is graphite phase carbon nitride solid fluorescence powder.
2. the application of a graphite phase carbon nitride solid fluorescence powder according to claim 1 in shallow fingerprint extraction.
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Cited By (5)
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| CN106744743A (en) * | 2016-12-05 | 2017-05-31 | 北京工业大学 | A kind of one-step synthesis water solubility g C3N4The preparation method of material |
| CN107576640A (en) * | 2017-08-31 | 2018-01-12 | 扬州大学 | Nitridation carbon quantum dot is used for the method for quickly showing the latent fingerprint in smooth object surface |
| CN107746710A (en) * | 2017-09-06 | 2018-03-02 | 郑州大学 | One kind nitridation carbon quantum dot and its preparation method and application |
| CN110745794A (en) * | 2019-09-24 | 2020-02-04 | 东北大学 | Preparation method of rare earth metal ion doped graphite phase carbon nitride |
| CN111317483A (en) * | 2018-12-17 | 2020-06-23 | 深圳先进技术研究院 | AIE composite material for latent fingerprint display, preparation method thereof and method for displaying latent fingerprints |
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| CN102502540A (en) * | 2011-11-24 | 2012-06-20 | 重庆工商大学 | C3N4 preparation method |
| CN102992282A (en) * | 2012-11-08 | 2013-03-27 | 南京大学 | Mesoporous C3N4 photocatalytic material prepared by using molten salt method and application thereof in photocatalysis field |
| CN103086332A (en) * | 2013-01-30 | 2013-05-08 | 华南理工大学 | Carbon nitride compound fluorescent powder and preparation method thereof |
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| CN102502540A (en) * | 2011-11-24 | 2012-06-20 | 重庆工商大学 | C3N4 preparation method |
| CN102992282A (en) * | 2012-11-08 | 2013-03-27 | 南京大学 | Mesoporous C3N4 photocatalytic material prepared by using molten salt method and application thereof in photocatalysis field |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106744743A (en) * | 2016-12-05 | 2017-05-31 | 北京工业大学 | A kind of one-step synthesis water solubility g C3N4The preparation method of material |
| CN107576640A (en) * | 2017-08-31 | 2018-01-12 | 扬州大学 | Nitridation carbon quantum dot is used for the method for quickly showing the latent fingerprint in smooth object surface |
| CN107746710A (en) * | 2017-09-06 | 2018-03-02 | 郑州大学 | One kind nitridation carbon quantum dot and its preparation method and application |
| CN107746710B (en) * | 2017-09-06 | 2020-09-04 | 郑州大学 | Carbon nitride quantum dot and preparation method and application thereof |
| CN111317483A (en) * | 2018-12-17 | 2020-06-23 | 深圳先进技术研究院 | AIE composite material for latent fingerprint display, preparation method thereof and method for displaying latent fingerprints |
| CN110745794A (en) * | 2019-09-24 | 2020-02-04 | 东北大学 | Preparation method of rare earth metal ion doped graphite phase carbon nitride |
| CN110745794B (en) * | 2019-09-24 | 2022-06-03 | 东北大学 | Preparation method of rare earth metal ion doped graphite phase carbon nitride |
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