CN113930232A - Solid carbon-point zeolite composite material fingerprint developing powder and preparation method thereof - Google Patents
Solid carbon-point zeolite composite material fingerprint developing powder and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 239000010457 zeolite Substances 0.000 title claims abstract description 47
- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 45
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000000843 powder Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000007787 solid Substances 0.000 title claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 44
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 42
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 238000011068 loading method Methods 0.000 claims abstract description 14
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 3
- 230000032683 aging Effects 0.000 claims abstract description 3
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 6
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- 239000002243 precursor Substances 0.000 claims description 2
- RSMUVYRMZCOLBH-UHFFFAOYSA-N metsulfuron methyl Chemical compound COC(=O)C1=CC=CC=C1S(=O)(=O)NC(=O)NC1=NC(C)=NC(OC)=N1 RSMUVYRMZCOLBH-UHFFFAOYSA-N 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 11
- 238000003384 imaging method Methods 0.000 abstract description 4
- 238000005119 centrifugation Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 33
- 239000000243 solution Substances 0.000 description 14
- 229910001868 water Inorganic materials 0.000 description 8
- 239000011259 mixed solution Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 4
- 238000004043 dyeing Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000002189 fluorescence spectrum Methods 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 230000000171 quenching effect Effects 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
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- 238000001179 sorption measurement Methods 0.000 description 2
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
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- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
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- 210000003811 finger Anatomy 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 238000001215 fluorescent labelling Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
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- 231100001231 less toxic Toxicity 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
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- 239000012229 microporous material Substances 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
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- 210000004935 right thumb Anatomy 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/117—Identification of persons
- A61B5/1171—Identification of persons based on the shapes or appearances of their bodies or parts thereof
- A61B5/1172—Identification of persons based on the shapes or appearances of their bodies or parts thereof using fingerprinting
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- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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Abstract
The invention belongs to the technical field of fingerprint identification, and particularly relates to a carbon-point zeolite composite fingerprint developing powder and a preparation method thereof. The fingerprint developing powder is obtained by taking Silicalite-1 zeolite as a carrier to load carbon points and is marked as a carbon point @ Silicalite-1 zeolite composite material; the carbon point loading was 2-10% based on the amount of Silicalite-1 zeolite. The preparation method comprises the steps of mixing tetrapropylammonium hydroxide, a sodium hydroxide solution, ethyl orthosilicate and deionized water according to a certain proportion, adding carbon dot powder after uniformly stirring, aging at room temperature, heating and stirring, and carrying out centrifugation, washing, drying and grinding on a product after reaction to obtain the carbon dot @ Silicalite-1 zeolite composite material. The composite material can be used for fingerprint detection and imaging of developed fingerprints under an ultraviolet lamp.
Description
Technical Field
The invention belongs to the technical field of fingerprint identification, and particularly relates to carbon-point zeolite composite fingerprint developing powder and a preparation method thereof.
Background
Fingerprints have important significance in identity identification, and fingerprint detection becomes an important means for crime scene investigation and evidence analysis. However, the existing fingerprint detection technology has the defects of low sensitivity, low selectivity, high susceptibility to interference and the like. In recent years, carbon dots have been more applied in the field of fingerprint detection due to excellent optical properties, good biocompatibility, and tunable light color, and have higher sensitivity, more prominent background contrast, and better selectivity. Carbon dots have advantages over earlier used group II-VI quantum dots in that they are less toxic, less costly and more biocompatible.
In the existing research, carbon dots are applied to fingerprint detection in a liquid state and a solid state respectively. Chen et al developed a red light carbon dot aqueous solution to detect fingerprints, but the aqueous solution had poor stability and had very limited application to substrates such as glass and plastic. In addition, the aqueous solution takes a long time from spraying to developing, and quick response cannot be realized, so that the solid carbon dots are more advantageous in fingerprint detection. However, the aggregation-induced quenching properties of solid-state carbon dots limit their applications. In the existing research, it is useful to disperse carbon dots with a host matrix to maintain its fluorescent properties, but since the composite material generally has a fixed shape, there are only a few reports of solid composite materials, such as montmorillonite, silica, etc., that can be used for fingerprint detection. There is a strong need for a carbon dot composite powder with good binding ability for fingerprint detection. The carbon dot @ Silicalite-1 zeolite composite material constructed by the invention solves the aggregation-induced quenching characteristic of solid carbon dots, and realizes quick-response fingerprint development.
Disclosure of Invention
The invention aims to provide solid carbon-point zeolite composite fingerprint developing powder and a preparation method thereof.
The carbon point zeolite composite fingerprint developing powder provided by the invention is obtained by taking Silicalite-1 zeolite as a carrier to load carbon points, and is marked as carbon point @ Silicalite-1 zeolite composite, wherein the carbon point loading range is 2-10% (the carbon point loading is measured by taking the amount of the Silicalite-1 zeolite as a basis).
In the following, the carbon dots are labeled CDs, tetrapropylammonium hydroxide is labeled TPAOH, sodium hydroxide is labeled NaOH, tetraethoxysilane is labeled TEOs, deionized water is labeled H2O。
The invention provides a preparation method of the carbon point @ Silicalite-1 zeolite composite material fingerprint developing powder, which comprises the following specific steps:
(1) the precursor solutions TPAOH, NaOH solution, TEOs and H2Mixing O, and stirring uniformly at room temperature to obtain Silicalite-1 zeolite; TPAOH, NaOH solution (1 wt%), TEOs and H2The proportion of O is 10-20 g: 0.5-4 g: 15-35 g: 20-60 mL;
(2) adding a certain amount of solid CDs powder, aging at room temperature, heating and stirring for reaction; controlling the addition amount of CDs powder, and based on the amount of Silicalite-1 zeolite, enabling the carbon point loading amount to be 2-10%;
(3) and purifying the product after the reaction, and then drying and grinding to obtain the carbon point @ Silicalite-1 zeolite composite material. The purification is carried out by utilizing any one or a combination of the following modes: centrifuging and filtering with microporous membrane.
In the step (1), stirring at room temperature for 20-24 h;
in the step (2), heating and stirring are carried out, wherein the heating temperature is 60-100 ℃, and the stirring time is 24-72 hours;
in the step (3), the drying is carried out at the temperature of 40-60 ℃ for 20-30 h.
The carbon dot @ Silicalite-1 zeolite composite material prepared by the invention can be used for fingerprint dyeing, and specifically comprises the following components: pressing any finger on different base materials (plastic, glass, tinfoil and aluminum alloy) to leave a latent fingerprint, dipping a little carbon point @ Silicalite-1 zeolite composite material powder on a brush, slightly shaking a brush handle at a position 5-8 cm away from the latent fingerprint part to deposit the powder, then brushing off redundant powder by using a soft brush to develop the fingerprint, and imaging the developed fingerprint under an ultraviolet lamp.
The invention has the following beneficial technical effects:
(1) the solid carbon point @ Silicalite-1 zeolite composite material provided by the invention utilizes a simple and convenient synthesis method, and solves the aggregation induction quenching effect of the solid carbon points by growing the carbon points in situ in the Silicalite-1 zeolite material, and the method has the advantages of simple process and environmental protection;
(2) the carbon dot @ Silicalite-1 zeolite composite material provided by the invention is small in particle size, good in monodispersity and strong in adhesive force, and can be applied to fingerprint detection. Can be applied to more substrates than previously applied aqueous solutions and can enable faster development of latent fingerprints. The carbon dot @ Silicalite-1 zeolite composite material is used for fingerprint fluorescence labeling on various base materials such as plastic, glass, tinfoil, aluminum alloy and the like, the obtained fingerprint has clear lines, emits bright blue light under the irradiation of an ultraviolet lamp, is free of background dyeing, and proves the potential of the carbon dot @ Silicalite-1 zeolite composite material in the field of fingerprint detection.
Drawings
FIG. 1 is a fluorescence emission spectrum of CDs @ Silicalite-1 composites at different CDs loadings.
FIG. 2 is an SEM and HRTEM representation of the composite material CDs @ Silicalite-1.
FIG. 3 is a graph of the nitrogen adsorption isotherms and pore size distributions of the composite CDs @ Silicalite-1 and Silicalite-1 zeolite materials.
FIG. 4 is a fluorescent photograph of the composite material CDs @ Silicalite-1 under sunlight and 365 nm excitation.
FIG. 5 shows the UV-visible absorption spectrum and the fluorescence emission spectrum of the composite material CDs @ Silicalite-1.
FIG. 6 is a graph of fingerprint staining on various substrates using the composite material CDs @ Silicalite-1.
Detailed Description
The technical scheme of the invention is further explained by combining the drawings and the specific embodiments.
Example 1
The preparation method of the carbon point @ Silicalite-1 zeolite composite material comprises the following steps:
dissolving 1g of citric acid monohydrate and 3mL of diethylenetriamine in 10mL of deionized water, transferring the uniformly mixed solution into a stainless steel reaction kettle (the effective volume is 25 mL) with a polytetrafluoroethylene lining, and carrying out hydrothermal reaction for 6h at 180 ℃ to obtain a yellowish-brown CDs solution;
TPAOH, NaOH solution (1 wt%), TEOs and H2O is uniformly mixed according to the proportion of 10g to 0.5g to 15g to 20mL, after stirring for 10min, a sample of 0.15g CDs (2 wt%) is added into the solution, and the mixture is stirred for 24h at room temperature until the mixture is uniformly stirred; then transferring the mixed solution into a 250mL flask, and stirring for 24h at 100 ℃; the resultant was centrifuged at 8000rpm for 10min, washed three times with water, then dried at 60 ℃ for 20 h, and ground into a powder.
Example 2
The preparation method of the carbon point @ Silicalite-1 zeolite composite material comprises the following steps
TPAOH, NaOH solution (1 wt%), TEOs and H2O is evenly mixed according to the proportion of 20 g to 4 g to 35g to 60mL and stirredAfter stirring for 10min, adding a 0.75g CDs (10 wt%) sample into the solution, and stirring for 24h at room temperature until the mixture is uniformly stirred; then transferring the mixed solution into a 250mL flask, and stirring for 24h at 100 ℃; the resultant was centrifuged at 8000rpm for 10min, washed three times with water, then dried at 60 ℃ for 20 h, and ground into a powder.
Example 3
The preparation method of the carbon point @ Silicalite-1 zeolite composite material comprises the following steps
TPAOH, NaOH solution (1 wt%), TEOs and H2Mixing O uniformly according to the proportion of 10g to 0.5g to 35g to 60mL, stirring for 10min, adding 0.30g of CDs (4 wt%) sample into the solution, and stirring for 24h at room temperature until the mixture is uniformly stirred; then transferring the mixed solution into a 250mL flask, and stirring for 24h at 100 ℃; the resultant was centrifuged at 8000rpm for 10min, washed three times with water, then dried at 60 ℃ for 20 h, and ground into a powder.
Example 4
The preparation method of the carbon point @ Silicalite-1 zeolite composite material comprises the following steps
TPAOH, NaOH solution (1 wt%), TEOs and H2Mixing O uniformly according to the proportion of 20 g to 4 g to 15g to 20mL, stirring for 10min, adding a 0.60 g CDs (8 wt%) sample into the solution, and stirring for 24h at room temperature until the mixture is uniformly stirred; then transferring the mixed solution into a 250mL flask, and stirring for 24h at 100 ℃; the resultant was centrifuged at 8000rpm for 10min, washed three times with water, then dried at 60 ℃ for 20 h, and ground into a powder.
Example 5
The preparation method of the carbon point @ Silicalite-1 zeolite composite material comprises the following steps
TPAOH, NaOH solution (1 wt%), TEOs and H2Uniformly mixing O according to the proportion of 15g to 2 g to 20 g to 40 mL, stirring for 10min, adding a 0.45 g CDs (6 wt%) sample into the solution, and stirring for 24h at room temperature until the mixture is uniformly stirred; then transferring the mixed solution into a 250mL flask, and stirring for 24h at 100 ℃; the resultant was centrifuged at 8000rpm for 10min, washed three times with water, then dried at 60 ℃ for 20 h, and ground into a powder.
Example 6
The application method of the carbon point @ Silicalite-1 zeolite composite material in fingerprint development comprises the following steps:
and 3, brushing redundant powder by using a soft brush to develop the fingerprint, and imaging the developed fingerprint under an ultraviolet lamp.
The carbon dot @ Silicalite-1 composites prepared in examples 1-5 all had very good fingerprint imaging results when used for fingerprint development, see FIG. 6.
The fluorescence emission spectra at 380 nm of the materials prepared in examples 1-5 are shown in FIG. 1.
With the increase of the loading amount of CDs, the emission wavelength is kept unchanged, and the fluorescence emission intensity is increased and then decreased, which shows that the loading amount of CDs influences the fluorescence property of the CDs @ Silicalite-1 composite material in the preparation process of the composite material. This is because, if the concentration of CDs is too high during the preparation of the composite material, Silicalite-1 cannot be loaded efficiently, and CDs will aggregate, but instead their fluorescence will be quenched.
As can be seen from FIG. 2, the CDs @ Silicalite-1 composite shows a uniform particle size of about 290 nm, and CDs are well dispersed in Silicalite-1.
As can be seen from FIG. 3, the two isotherms are at p/p0<The 0.1 region shows the same shape and high adsorptivity, which are characteristic of typical microporous materials. At p/p0<0.1 region, CDThe s @ Silicalite-1 composite had a slightly lower adsorption capacity than Silicalite-1 due to the slight decrease in the crystallinity of the micropores resulting from the successful introduction of CDs. The pore content of the composite increased at 3-5 nm mesopores, indicating successful incorporation of CDs.
As can be seen from the graphs of FIGS. 4-5, the CDs @ Silicalite-1 composite material is white powder under sunlight, and can emit bright blue light under 365 nm ultraviolet light; the absorption spectrum is similar to that of typical CDs, with the emission wavelength fixed at 450 nm as the excitation wavelength increases from 350 nm to 400 nm.
As can be seen from FIG. 6, the composite material CDs @ Silicalite-1 is used for fingerprint dyeing on different base materials, the obtained fingerprint lines are clear, bright blue light is emitted under the irradiation of an ultraviolet lamp, background dyeing is avoided, and the capability of the carbon dot @ Silicalite-1 composite material in the field of fingerprint detection is proved.
Claims (6)
1. A carbon point zeolite composite material fingerprint developing powder is characterized in that the carbon point fingerprint developing powder is obtained by taking Silicalite-1 zeolite as a carrier to load carbon points and is marked as a carbon point @ Silicalite-1 zeolite composite material; wherein the carbon point loading is 2-10% based on the amount of Silicalite-1 zeolite.
2. The preparation method of the carbon point zeolite composite fingerprint developing powder as claimed in claim 1, characterized by comprising the following specific steps:
(1) the precursor solutions TPAOH, NaOH solution, TEOs and H2Mixing O, and stirring uniformly at room temperature to obtain Silicalite-1 zeolite; wherein TPAOH, 1wt% NaOH solution, TEOs and H2The proportion of O is 10-20 g: 0.5-4 g: 15-35 g: 20-60 mL;
(2) adding solid CDs powder, aging at room temperature, heating and stirring for reaction; controlling the addition amount of CDs powder, and based on the amount of Silicalite-1 zeolite, enabling the carbon point loading amount to be 2-10%;
(3) purifying the product after reaction, and then drying and grinding to obtain the carbon point @ Silicalite-1 zeolite composite material;
wherein the content of the first and second substances,CDs denotes carbon point, TPAOH denotes tetrapropylammonium hydroxide, NaOH denotes sodium hydroxide, TEOs denotes tetraethylorthosilicate, H2And O represents deionized water.
3. The method according to claim 2, wherein the stirring in step (1) is carried out at room temperature for 20 to 24 hours.
4. The method according to claim 2, wherein the heating and stirring in step (2) are carried out at a temperature of 60 to 100 ℃ for 24 to 72 hours.
5. The preparation method according to claim 2, wherein in the step (3), the drying is carried out at a temperature of 40-60 ℃ for 20-30 h.
6. The method of using the carbon dot zeolite composite fingerprint developing powder as claimed in claim 1, wherein any finger is pressed on the substrate to leave a latent fingerprint, a little carbon dot zeolite composite fingerprint developing powder is smeared with a brush, the brush handle is gently shaken at a position 5-8 cm away from the latent fingerprint part to deposit the powder, then a soft brush is used to brush off the excess powder to develop the fingerprint, and the developed fingerprint is imaged under an ultraviolet lamp.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112940721A (en) * | 2021-03-10 | 2021-06-11 | 深圳大学 | Solid-state luminescent carbon quantum dot with adjustable fluorescence color, and preparation method and application thereof |
| CN114854394A (en) * | 2022-05-25 | 2022-08-05 | 甘肃政法大学 | Preparation of fluorescent carbon dot nano composite material and application of fluorescent carbon dot nano composite material in latent fingerprint display |
| CN115595145A (en) * | 2022-11-07 | 2023-01-13 | 中国刑事警察学院（Cn） | Preparation method and application of nitrogen-zinc doped carbon dot-hydrotalcite nanocomposite |
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| CN109735324A (en) * | 2019-01-30 | 2019-05-10 | 东华大学 | A kind of method that in-situ method prepares mesoporous silicon dioxide modified carbon dots |
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| CN114854394A (en) * | 2022-05-25 | 2022-08-05 | 甘肃政法大学 | Preparation of fluorescent carbon dot nano composite material and application of fluorescent carbon dot nano composite material in latent fingerprint display |
| CN114854394B (en) * | 2022-05-25 | 2023-11-21 | 甘肃政法大学 | Preparation of fluorescent carbon dot nanocomposite and application of fluorescent carbon dot nanocomposite in latent fingerprint display |
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