CN101647700A - Method for using fluorescent silicon dioxide to display laten fingerprint - Google Patents

Method for using fluorescent silicon dioxide to display laten fingerprint Download PDF

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CN101647700A
CN101647700A CN200910067470A CN200910067470A CN101647700A CN 101647700 A CN101647700 A CN 101647700A CN 200910067470 A CN200910067470 A CN 200910067470A CN 200910067470 A CN200910067470 A CN 200910067470A CN 101647700 A CN101647700 A CN 101647700A
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silicon dioxide
fluorescent silicon
laten fingerprints
powder
solution
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苏忠民
柴芳
王婷婷
王春刚
马占芳
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Northeast Normal University
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Northeast Normal University
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Abstract

The invention relates to a method for using fluorescent silicon dioxide to display laten fingerprints, belonging to the technical field of detection. In the invention, a fluorescent silicon dioxide monodisperse nanometer rubber ball is prepared by a reverse-phase microemulsion polymerization method, and a classical st ber method is used and improved, a fluorescent silicon dioxide rubber ball doping dyes is synthesized in one step by hydrolyzing TEOS in alkaline condition, and the laten fingerprints with different object surfaces are displayed by the fluorescent silicon dioxide rubber ball. Thenanometer powder of the fluorescent silicon dioxide has high fluorescence intensity and can be used for displaying the laten fingerprints positioned on the surfaces of a glass sheet, a plastic bottle, a pop can, a copper sheet, an aluminium foil and a desk or an experiment table in a brushing way or displaying the laten fingerprints positioned on moist surfaces by an ultraphonic precipitation method, and the displayed laten fingerprints emit orange light under an ultraviolet light source. The invention has easy operation, small using amount, large application range and good effect and can display the laten fingerprints positioned on a plurality of specific objects.

Description

Fluorescent silicon dioxide is used for the method for developing latent finger prints using
Technical field
The invention belongs to the detection technique field, be specifically related to fluorescent silicon dioxide and be used for method for manifesting latent fingerprints.
Background technology
Fingerprint identification is one of the most reliable method of carrying out individual identification, and fingerprint plays important evidential function in forensic science and criminal suit process.Yet in all kinds of crime cases, the crime means that the offender adopts is more and more insidious, hidden more.The fingerprint that occurs in the scene of a crime often is potential, and so-called latent fingerprint is meant people's finger, when palm touches object, because sweat mixed with dirt or oils and fats stay the impression that reflects fingers and palms surface skin papillary ridges when being in contact with one another with body surface on object plane.This impression is retained in can not directly examine by eyesight or by light source on the lusterless body surface to be seen, forms latent image as photographic film through exposure, needs could show original image by development treatment, and this class fingerprint is called latent fingerprint (laten fingerprints).The evaluation laten fingerprints is correctly found, extracts, manifested to science, for the investigation of case with punish crime, has important practice effect and immeasurable social value.
Being applied to on-the-spot biological trace method for visualizing at present mainly contains: physics appearance method (luminescence method, powder method etc.), chemical appearance method (ninhydrin method etc.) and physical chemistry appearance method (many metal deposition appearance methods etc.).Methods such as physical method is a physical attribute of utilizing the material room machine to adhere to, selects the stronger material of adhesive force, and is apparent by brushing, as to exert a gradual, corrupting influence on make streakline or body surface painted and show impression of the hand.Wherein photoluminescence method is started from 1976 as the research of developing latent finger prints using.For the organic components in the laten fingerprints, as oils and fats, aminoacid etc., under considerable situation, the process for show that requires to adopt should possess extra high sensitivity.Though there have been a lot of appearing techniques, research and development nontoxic and the on-the-spot biological trace appearing technique of high sensitivity still are the emphasis of forensic science research and countries in the world Forensic Science personnel's striving direction.
Frederick J.Rowell utilizes tetraethoxysilane (or tetramethoxy-silicane) and the reaction of phenyl triethoxysilane mixed hydrolysis, and the common reaction of addings such as dyestuff obtained hydrophobic silica dioxide granule, be used to detect fingerprint and obtained good effect [Brenden J.Theaker, Katherine E.Hudson, Frederick J.Rowell, Forensic Sci.Int.2008,174,26-34].Kwan H.Cheng is with Eu 3+Ion doping silicon dioxide forms complex, utilizes fluorescent appear laten fingerprints [Li Liu, Simerjeet K.Gill, Yanping Gao, Louisa J.Hope-Weeks, Kwan H.Cheng a, Forensic Sci.Int.2008,176,163-172].
The present invention utilize microemulsion method and
Figure G2009100674709D00011
Method has prepared doping ruthenium pyridine (Rubpy) or 1, and the fluorescent silicon dioxide nanometer powder of 10-o-phenanthroline ruthenium dye can be applicable to manifest the laten fingerprints on different objects surface.
Summary of the invention
The purpose of this invention is to provide a kind of method that fluorescent silicon dioxide is little, nano-particle manifests different objects surface laten fingerprints of using.
The present invention utilizes the conversed phase micro emulsion copolymerization method to prepare fluorescent silicon dioxide dispersed nano glueballs.The present invention also adopts classical
Figure G2009100674709D00021
Method is also improved, and utilizes the fluorescent silicon dioxide glueballs of TEOS hydrolysis one-step synthesis dopant dye under alkali condition.And manifest the laten fingerprints on different objects surface with above material.
The preparation of material and using method:
1, the preparation of fluorescent silicon dioxide nanometer powder: microemulsion is made up of following reagent: room temperature, under magnetic agitation, cyclohexane extraction, hexanol, three kinds of solution of triton x-100 mix, add ruthenium pyridine or 1 then, aqueous solution and the ethyl orthosilicate of 10-phenanthroline ruthenium 20mM, mix and stir after 20-30 minute, the adding mass fraction is 25% ammonia, mentioned reagent cyclohexane extraction in the mixed solution, hexanol, triton x-100, ruthenium pyridine or 1,10-phenanthroline ruthenium aqueous solution (20mM), the volume ratio of ethyl orthosilicate and ammonia was followed successively by 7.5: 1.8: 1.77: 0.48: 0.1-0.5: 0.06-0.3, mixed solution reacts after 20-24 hour under magnetic agitation, add isopyknic acetone breakdown of emulsion, the product that obtains is centrifugal, and clean with ethanol, oven dry just obtains xanchromatic fluorescent silicon dioxide nanometer powder, and particle diameter is about 65nm.
2, improve
Figure G2009100674709D00022
The preparation of method fluorescent silicon dioxide nanometer powder:
(1) obtains mixed solution one in ethyl orthosilicate (being tetraethoxysilane TEOS) the adding 15-25ml alcoholic solution with 4-8ml, with ammonia by 10-15ml, 20-30ml ethanol, 1-3ml, the ruthenium pyridine (Rubpy) or 1 of 20mM, the mixed solution two that the ruthenie aqueous solution of 10-o-phenanthroline obtains; During actual fabrication, can change response magnitude according to the volume ratio of above reaction solution.
(2) under the room temperature, two solution mix rapidly under electronic stirring fast, react after 4-8 hour, and the product that obtains is centrifugal, and clean with secondary water, and oven dry just obtains yellow silicon dioxide microsphere powder.The big I of silicon dioxide microsphere particle diameter is by TEOS in the solution, ammonia, and the difference of the ratio of water is regulated, and the grain size that obtains can be at the 10-100 micrometer range.
3, process for show:
During use, dip in powder, stencil the various surfaces of laten fingerprints gently with hairbrush, comprise sheet glass, plastic bottle, pop can, copper sheet, aluminium foil, desk or laboratory table surface, promptly can be observed the yellow fingerprint lines that manifests, send orange-colored light under ultraviolet source, taking pictures with digital camera gets final product.
Object surface for humidity, the powder of a certain amount of (mass volume ratio W/V is 0.5-3%) is put into water, add small amount of ethanol, ultrasonic 2-3 minute, the sample that will be printed on laten fingerprints is put into dispersion liquid and is soaked, and takes out after 5-20 minute and dries, and can see the clear showing finger print image, send orange-colored light under ultraviolet source, taking pictures with digital camera gets final product.
The present invention has following advantage:
1, method is simple, quick, easy to operate, can be apparent in the laten fingerprints of different objects surface (sheet glass, plastic bottle, pop can, copper sheet, aluminium foil, paper, desk or laboratory table).
2, not by instrument (bore hole observation) can discern and manifest laten fingerprints; All obtain manifests fingerprint and can directly take pictures under natural light and fetch data, and powder is luminous under ultraviolet source, can be used for the manifesting of laten fingerprints on the surface of particular substrate.
3, the present invention easily prepares and preserves; Cost is low, and consumption is few during use.
4, the present invention does not contain poisonous composition, and is safe in utilization, and the operator is had no side effect.
Description of drawings
Accompanying drawing 1, for show the image of glass surface laten fingerprints with fluorescent silicon dioxide nanometer powder (powder 1) brush;
Accompanying drawing 2, for show the image of plastic bottle surface laten fingerprints with fluorescent silicon dioxide nanometer powder (powder 1) brush;
Accompanying drawing 3, for show the image of glass surface laten fingerprints with fluorescent silicon dioxide microsphere powder (powder 2) brush;
The specific embodiment
Embodiment 1:
The preparation of fluorescent silicon dioxide nanometer powder: microemulsion is made up of following reagent: room temperature, under magnetic agitation, cyclohexane extraction 7.5ml, hexanol 1.8ml, three kinds of solution of triton x-100 1.8ml mix, and add 1 of 0.5ml 20mM then, 10-phenanthroline ruthenium aqueous solution, ethyl orthosilicate 0.1ml mixes and stirs after 20 minutes, and the adding mass fraction is 25% ammonia 70 μ l, mixed solution is under stirring rapidly, react after 24 hours, add isopyknic acetone breakdown of emulsion, the product that obtains is centrifugal, and clean with ethanol, oven dry just obtains xanchromatic fluorescent silicon dioxide nanometer powder (powder 1), and particle diameter is about 65 nanometers.
Process for show:
During use, dip in powder with hairbrush, stencil the various surfaces of laten fingerprints gently, comprise sheet glass, plastic bottle, pop can, copper sheet, aluminium foil, desk or laboratory table surface, promptly can be observed the yellow fingerprint lines that manifests, send orange-colored light under ultraviolet source, taking pictures with digital camera gets final product (accompanying drawing 1,2).
Object surface for humidity, the powder of a certain amount of (mass volume ratio W/V is 0.5-3%) is put into water, add small amount of ethanol, ultrasonic 3 minutes, the sample that will be printed on laten fingerprints is put into dispersion liquid and is soaked, and takes out after 20 minutes and dries, and can see the clear showing finger print image, send orange-colored light under ultraviolet source, taking pictures with digital camera gets final product.
Embodiment 2:
The preparation of fluorescent silicon dioxide nanometer powder:
(1) ammonia of (mixed solution one) and 12ml in the ethyl orthosilicate adding 20ml alcoholic solution of preparation 4ml, 25ml ethanol, with 1 of 1ml 20mM, the mixed liquor of the ruthenie aqueous solution of 10-o-phenanthroline (mixed solution two);
(2) under the room temperature, two solution mix rapidly under electronic stirring fast, react after 8 hours, and the product that obtains is centrifugal, and clean with secondary water, and oven dry just obtains yellow silicon dioxide microsphere powder (powder 2).
Process for show:
During use, dip in powder with hairbrush, stencil the various surfaces of laten fingerprints gently, comprise sheet glass, plastic bottle, pop can, copper sheet, aluminium foil, desk or laboratory table surface, promptly can be observed the yellow fingerprint lines that manifests, send orange-colored light under ultraviolet source, taking pictures with digital camera gets final product (accompanying drawing 3).
Object surface for humidity, the powder of a certain amount of (mass volume ratio W/V is 0.5-3%) is put into water, add small amount of ethanol, ultrasonic 2 minutes, the sample that will be printed on laten fingerprints is put into dispersion liquid and is soaked, and takes out after 10 minutes and dries, and can see the clear showing finger print image, send orange-colored light under ultraviolet source, taking pictures with digital camera gets final product.

Claims (3)

1, fluorescent silicon dioxide is used for the method for developing latent finger prints using, it is characterized in that concrete steps are as follows:
Dip in the fluorescent silicon dioxide powder with hairbrush, stencil the various objects surface of laten fingerprints gently, comprise sheet glass, plastic bottle, pop can, copper sheet, aluminium foil, desk or laboratory table surface, promptly observe the yellow fingerprint lines that manifests, send orange-colored light under ultraviolet source, taking pictures with digital camera gets final product;
Object surface for humidity, with the mass volume ratio is the ratio of 0.5-3%, the fluorescent silicon dioxide powder is put into water and alcohol mixed solution, ultrasonic 2-3 minute, the sample that will be printed on laten fingerprints is put into dispersion liquid and is soaked, and takes out after 5-20 minute and dries, and can see the clear showing finger print image, send orange-colored light under ultraviolet source, taking pictures with digital camera gets final product.
2, the preparation method of fluorescent silicon dioxide nanometer powder is characterized in that concrete steps are as follows:
Room temperature, under magnetic agitation, cyclohexane extraction, hexanol, three kinds of solution of triton x-100 mix, add ruthenium pyridine or 1 then, aqueous solution and the ethyl orthosilicate of 10-phenanthroline ruthenium 20mM, mix and stir after 20-30 minute, the adding mass fraction is 25% ammonia, the mentioned reagent cyclohexane extraction, hexanol, triton x-100, ruthenium pyridine or 1,10-phenanthroline ruthenium aqueous solution (20mM), the volume ratio of ethyl orthosilicate and ammonia was followed successively by 7.5: 1.8: 1.77: 0.48: 0.1-0.5: 0.06-0.3, mixed solution reacts after 20-24 hour under magnetic agitation, adds isopyknic acetone breakdown of emulsion, and the product that obtains is centrifugal, and clean with ethanol, oven dry just obtains xanchromatic fluorescent silicon dioxide nanometer powder, and particle diameter is about 65nm.
3, the preparation method of fluorescent silicon dioxide nanometer powder is characterized in that concrete steps are as follows:
At first preparing two kinds of mixed solutions, is that tetraethoxysilane TEOS adds in the 15-25ml alcoholic solution and mixes and obtains mixed solution (1) with the ethyl orthosilicate of 4-8ml; Ammonia with 10-15ml, 20-30ml ethanol and 1-3ml, the ruthenium pyridine or 1 of 20mM/L, the ruthenie aqueous solution three of 10-o-phenanthroline is mixed into mixed solution (2), then (1) and (2) two mixed solutions are mixed rapidly under electronic stirring fast, react after 4-8 hour, the product that obtains is centrifugal, and with ethanol and the cleaning of secondary water, dry, just obtain yellow silicon dioxide microsphere powder, volume ratio according to above reaction solution changes response magnitude, and the size of silicon dioxide microsphere particle diameter is by TEOS in the solution, ammonia, the difference of the ratio of water is regulated, and the grain size that obtains is at the 10-100 micrometer range.
CN200910067470A 2009-08-28 2009-08-28 Method for using fluorescent silicon dioxide to display laten fingerprint Pending CN101647700A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102988058A (en) * 2011-09-16 2013-03-27 国家纳米科学中心 Color silica nano-particle used for displaying latent fingerprints and preparation method thereof
CN104337522A (en) * 2014-11-24 2015-02-11 中国刑事警察学院 Method for displaying latent fingerprints by adopting fluorescent dye-modified nano particles
CN104382600A (en) * 2014-11-24 2015-03-04 中国刑事警察学院 Two-step latent fingerprint manifesting method based on nano-particles
CN106634980A (en) * 2016-11-23 2017-05-10 沈阳大学 Method for preparing and applying latent fingerprint development luminescent nanopowder
CN107163931A (en) * 2017-05-16 2017-09-15 北京科技大学 Application process of the fluorescence conjugated oligomer silica composite nanoparticle in latent print development
CN107177355A (en) * 2017-05-16 2017-09-19 北京科技大学 The conjugate oligomeric thing of superelevation fluorescence quantum yield and the preparation method of silica fluorescent composite nanoparticle
CN108315011A (en) * 2016-11-15 2018-07-24 香港科技大学 Fingerprint imaging composition and its application

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102988058A (en) * 2011-09-16 2013-03-27 国家纳米科学中心 Color silica nano-particle used for displaying latent fingerprints and preparation method thereof
CN102988058B (en) * 2011-09-16 2015-05-13 国家纳米科学中心 Color silica nano-particle used for displaying latent fingerprints and preparation method thereof
CN104337522A (en) * 2014-11-24 2015-02-11 中国刑事警察学院 Method for displaying latent fingerprints by adopting fluorescent dye-modified nano particles
CN104382600A (en) * 2014-11-24 2015-03-04 中国刑事警察学院 Two-step latent fingerprint manifesting method based on nano-particles
CN104382600B (en) * 2014-11-24 2017-01-11 中国刑事警察学院 Two-step latent fingerprint manifesting method based on nano-particles
CN104337522B (en) * 2014-11-24 2017-01-11 中国刑事警察学院 Method for displaying latent fingerprints by adopting fluorescent dye-modified nano particles
CN108315011A (en) * 2016-11-15 2018-07-24 香港科技大学 Fingerprint imaging composition and its application
CN106634980A (en) * 2016-11-23 2017-05-10 沈阳大学 Method for preparing and applying latent fingerprint development luminescent nanopowder
CN107163931A (en) * 2017-05-16 2017-09-15 北京科技大学 Application process of the fluorescence conjugated oligomer silica composite nanoparticle in latent print development
CN107177355A (en) * 2017-05-16 2017-09-19 北京科技大学 The conjugate oligomeric thing of superelevation fluorescence quantum yield and the preparation method of silica fluorescent composite nanoparticle
CN107177355B (en) * 2017-05-16 2020-04-10 北京科技大学 Preparation method of conjugated oligomer and silicon dioxide fluorescent composite nanoparticles with ultrahigh fluorescence quantum yield
CN107163931B (en) * 2017-05-16 2020-05-08 北京科技大学 Application method of fluorescent conjugated oligomer silicon dioxide composite nanoparticles in latent fingerprint development

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Inventor after: Yang Guochun

Inventor after: Su Zhongmin

Inventor after: Chai Fang

Inventor after: Wang Tingting

Inventor after: Wang Chungang

Inventor after: Ma Zhanfang

Inventor before: Su Zhongmin

Inventor before: Chai Fang

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Inventor before: Wang Chungang

Inventor before: Ma Zhanfang

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Open date: 20100217