CN105482804A - Latent fingerprint detection probe and a preparation method thereof - Google Patents

Latent fingerprint detection probe and a preparation method thereof Download PDF

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CN105482804A
CN105482804A CN201610012292.XA CN201610012292A CN105482804A CN 105482804 A CN105482804 A CN 105482804A CN 201610012292 A CN201610012292 A CN 201610012292A CN 105482804 A CN105482804 A CN 105482804A
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CN105482804B (en
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李鹿
王春刚
苏忠民
李光哲
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Northeastern University China
Northeast Normal University
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
    • C09K11/7784—Chalcogenides
    • C09K11/7787—Oxides

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Abstract

The invention belongs to a latent fingerprint detection probe and a preparation method thereof, and provides a preparation method of a Fe3O4@Gd2O3:Y3+/Er3+ nanometer composite of a mono-dispersed bell-shaped structure and application of the nanometer composite for latent fingerprint development. A high temperature hydrolysis method is adopted, anhydrous FeCl3 is used as a raw material for synthesizing Fe2O3 nano particles, the Fe2O3 nano particles are coated with PAA-NH4 in an isopropanol-water mixing system, GdCl3.6H2O, TCl3.6H2O and an ErCl3.6H2O water solution into the system, stirring, centrifuging and drying are performed, high-temperature calcination is performed, and the Fe3O4@Gd2O3:Y3+/Er3+ nanometer composite of the mono-dispersed bell-shaped structure can be obtained. The obtained composite is good in dispersity, has the magnetic and fluorescence property, and can develop latent fingers on the surfaces of A4 paper, a glass sheet, an experiment tabletop, an apple and leather.

Description

A kind of laten fingerprints detection probes and preparation method thereof
Technical field
The invention belongs to nano composite material and applied technical field thereof, be specifically related to a kind of single dispersing jingle bell type structure Fe 3o 4gd 2o 3: Y 3+/ Er 3+the preparation method of nano composite material and the application in developing latent finger prints thereof.
Background technology
Fingerprint, the i.e. decorative pattern of human hands skin, the fingerprint on ordinary meaning, refers to that the application of papillary ridges two fingerprint in investigation conclusion on the finger first segment palmar aspect skin of people is long-standing.Because it has special physiological structure and feature architecture, so become a kind of material evidence having much superiority.Fingerprint is unchangeable to be referred to from when fetus forms fingerprint in 6 months, arrive when after death dermal papilla layer rots through birth and stop, finger papillary ridges type, concrete form, the feature summation that the shape of each minutia, quantity, position and mutual relationship are formed is constant all the time.By analysis, comparison latent fingerprint and known individual fingerprint, the conclusion determining or get rid of certain suspect can be made.Early stage fingerprint identification mainly refers to that the visible fingerprint to being retained in crime scene carries out naked eyes identification; Modern forensic science worker then utilizes multiple science and technology to search fingerprint.Be applied to the method that fingerprint on site manifests at present to mainly contain: optics appearance method, physics appearance method and chemical appearance method.The common weakness of these methods is that sensitivity is low, produces interference after the method application wherein had to the sensitivity of DNA tests and result.Compare other method, fluorescent appear method has special advantage, can manifest the laten fingerprints that some differentiate unconspicuous background surface, the photoluminescent techniques used at present simultaneously reasons for its use fluorescence is very large to the interference of the photoluminescence Bio-imprinting identification of routine, and difficulty reaches the requirement of expection.Therefore, Non-toxic, research and development that are easy to operate and highly sensitive live biometric trace appearing technique have become the emphasis of forensic science research and the striving direction of countries in the world criminal technique personnel.
Rare earth up-conversion luminescence nanomaterial is the fluorescent material that a class utilizes near infrared light to excite and short wavelength launches.The shortcoming that when up-conversion luminescence nanomaterial can overcome downconversion fluorescent material imaging, background fluorescence is strong and being paid close attention to widely, it can convert near infrared light to short-wave radiation by multi-photon mechanism, launches ultraviolet or visible ray.Such material is compared other fluorescent material and is had plurality of advantages: chemical stability is good, and luminescence process is hardly by the impact of temperature, humidity, pH etc.; Photochemical stability is good, still has very high optical stability for a long time under high light or excitation light irradiation; Up-conversion luminescent material excitation wavelength is generally near infrared light, and in living things system, most of chaff interference can not be excited, and reduces detection background, makes sensitivity obtain very large raising; Near infrared or the infrared excitation optical wavelength of up-conversion luminescent material are long, and energy is low, so can well penetrate some biological tissues and can not produce injury to it; Emission wavelength is adjustable, and the different rare earth ion that adulterates in building-up process can obtain the emitting fluorescence of different colours.Can find out that up-conversion nano material is the biological labled material that a class is very superior from above advantage.Therefore, we, for adapting to more application conditions and use range, have invented the Fe of a kind of both magnetic and up-conversion fluorescence 3o 4gd 2o 3: Y 3+/ Er 3+nanoparticle, can manifest laten fingerprints as manifesting reagent, and material synthesis method is simple and to manifest process fast.
Summary of the invention
The object of this invention is to provide a kind of single dispersing jingle bell type structure Fe 3o 4gd 2o 3: Y 3+/ Er 3+the preparation method of nano composite material and the application in developing latent finger prints thereof, use single dispersing jingle bell type structure Fe prepared by the method 3o 4gd 2o 3: Y 3 +/ Er 3+nano composite material good dispersity, magnetic are strong, fluorescence intensity is high, can manifest A4 paper, sheet glass, experiment table, apple and leather surface latent fingerprint.Powder adherence shows streakline on the sweat of laten fingerprints, and unnecessary powder can be siphoned away by magnetic brush, can be observed fingerprint lines clearly.Under 980nm LASER Light Source is irradiated, can be observed luminous fingerprint lines.
Single dispersing jingle bell type structure Fe of the present invention 3o 4gd 2o 3: Y 3+/ Er 3+the preparation method of nano composite material comprises the steps:
(1) by a certain amount of liquor ferri trichloridi (2 × 10 -2m) one is joined with in the round-bottomed flask of prolong, 100 oin C oil bath magnetic agitation reaction 70 ~ 80h, carry out centrifugation after react, gained solid again with deionized water wash several, gained solid 50 ~ 75 oc vacuum-drying 8 ~ 10h, obtains dry Fe 3o 2nanoparticle.
(2) by Fe that 4 ~ 6mg step (1) obtains 3o 2ammoniacal liquor (2mol/L) and 10 ~ 15mL deionized water of nanoparticle, 50 ~ 100 μ L polyacrylic acid aqueous solution (0.2g/mL) and 75 ~ 150 μ L join in 100mL round-bottomed flask, ultrasonic disperse 10 ~ 20min.
(3) under magnetic stirring 100 ~ 150mL Virahol is slowly added dropwise in the solution that step (2) obtains, subsequently by 10 ~ 15mgGdCl 36H 2o, 2 ~ 3mgYCl 36H 2o and 0.2 ~ 0.3mgErCl 36H 2o successively joins in solution, and magnetic agitation 2-4h, carries out centrifugation after having reacted, gained solid 50 ~ 75 oc vacuum-drying 8 ~ 12h.
(4) solid that step (3) obtains is placed in tube furnace, 600 ~ 700 ocalcine 2 ~ 3h under C argon shield, obtain jingle bell type structure Fe 3o 4gd 2o 3: Y 3+/ Er 3+nano composite material.
Tool of the present invention has the following advantages:
1. the present invention adopts unique PAA-NH 4masterplate method, by its guiding and stabilization, synthesis jingle bell type structure nano particle, had both shortened the polymolecularity that reactions steps in turn ensure that particle.
2. the single dispersing Fe that obtains of the present invention 3o 4gd 2o 3: Y 3+/ Er 3+nanoparticle is the multifunctional nanoparticle of a kind of both magnetic and up-conversion fluorescence, can be applicable to more many condition and scope, and has no side effect.
3. the single dispersing Fe that obtains of the present invention 3o 4gd 2o 3: Y 3+/ Er 3+nanoparticle, its shell is up-conversion luminescence nanomaterial, and the shortcoming that when can overcome downconversion fluorescent material imaging, background fluorescence is strong, improves display effect greatly.
4. the single dispersing Fe that obtains of the present invention 3o 4gd 2o 3: Y 3+/ Er 3+nano particle diameter is even, good dispersity, can manifest the laten fingerprints of various quality surface (A4 paper, sheet glass, experiment table top, apple and leather surface).
Accompanying drawing explanation
Fig. 1, the Fe prepared for the present invention 3o 4gd 2o 3: Y 3+/ Er 3+the transmission electron microscope picture of nanoparticle;
Fig. 2, for using Fe 3o 4gd 2o 3: Y 3+/ Er 3+material brush manifests the image of glass surface laten fingerprints;
Fig. 3, for using Fe 3o 4gd 2o 3: Y 3+/ Er 3+material brush shows the image of experiment table surface laten fingerprints;
Fig. 4, for using Fe 3o 4gd 2o 3: Y 3+/ Er 3+material brush shows the image of permeability object A4 paper surface laten fingerprints;
Fig. 5, for using Fe 3o 4gd 2o 3: Y 3+/ Er 3+material brush shows the image of apple surface laten fingerprints.
Embodiment
Set forth the present invention further below in conjunction with specific embodiment, embodiment is only not used in for illustration of the present invention and limits the scope of the invention.
Specific embodiment
Embodiment 1:
By 100mL ferric chloride aqueous solutions (2 × 10 -2m) one is joined with in the round-bottomed flask of prolong, 100 omagnetic agitation reaction 70h in C oil bath, with deionized water wash, ultrasonic and centrifugal (7000rpm, 10min), repeatedly super work three times, gained solid 75 oc vacuum-drying 8h, obtains dry Fe 3o 2nanoparticle.The Fe that 5mg has been prepared 3o 2nanoparticle and 10mL deionized water add in 100mL flask, after ultrasonic disperse 10min, successively add the ammoniacal liquor of the 50 μ L0.2g/mLPAA aqueous solution and 75 μ L2mol/L, subsequently by 10mgGdCl 36H 2o, 2mgYCl 36H 2o and 0.2mgErCl 36H 2o successively joins in solution, and magnetic agitation 2h, carries out centrifugation after having reacted, gained solid 75 oc vacuum-drying 8h.The solid obtained is placed in tube furnace, 600 ocalcine 2h under C argon shield, obtain jingle bell type structure Fe 3o 4gd 2o 3: Y 3+/ Er 3+nano composite material.
Embodiment 2:
By 80mL ferric chloride aqueous solutions (2 × 10 -2m) one is joined with in the round-bottomed flask of prolong, 100 omagnetic agitation reaction 80h in C oil bath, with deionized water wash, ultrasonic and centrifugal (9000rpm, 5min), repeatedly super work three times, gained solid 70 oc vacuum-drying 9h, obtains dry Fe 3o 2nanoparticle.The Fe that 4mg has been prepared 3o 2nanoparticle and 10mL deionized water add in 100mL flask, after ultrasonic disperse 10min, successively add the ammoniacal liquor of the 70 μ L0.2g/mLPAA aqueous solution and 70 μ L2mol/L, subsequently by 12mgGdCl 36H 2o, 2.2mgYCl 36H 2o and 0.22mgErCl 36H 2o successively joins in solution, and magnetic agitation 2h, carries out centrifugation after having reacted, gained solid 70 oc vacuum-drying 9h.The solid obtained is placed in tube furnace, 700 ocalcine 2h under C argon shield, obtain jingle bell type structure Fe 3o 4gd 2o 3: Y 3+/ Er 3+nano composite material.
Embodiment 3:
By 100mL ferric chloride aqueous solutions (2 × 10 -2m) one is joined with in the round-bottomed flask of prolong, 100 omagnetic agitation reaction 80h in C oil bath, with deionized water wash, ultrasonic and centrifugal (8000rpm, 8min), repeatedly super work three times, gained solid 60 oc vacuum-drying 10h, obtains dry Fe 3o 2nanoparticle.The Fe that 5mg has been prepared 3o 2nanoparticle and 10mL deionized water add in 100mL flask, after ultrasonic disperse 8min, successively add the ammoniacal liquor of the 100 μ L0.2g/mLPAA aqueous solution and 100 μ L2mol/L, subsequently by 15mgGdCl 36H 2o, 2.5mgYCl 36H 2o and 0.25mgErCl 36H 2o successively joins in solution, and magnetic agitation 2h, carries out centrifugation after having reacted, gained solid 60 oc vacuum-drying 10h.The solid obtained is placed in tube furnace, 700 ocalcine 3h under C argon shield, obtain jingle bell type structure Fe 3o 4gd 2o 3: Y 3+/ Er 3+nano composite material.
The described single dispersing jingle bell type structure Fe prepared 3o 4gd 2o 3: Y 3+/ Er 3+nano composite material is used for fingerprint and shows.During use, magnetic powder is picked up with Magnetic brush, powder is formed " magnetic force powder fringe " under the effect of magnetic force, the various object surfaces of laten fingerprints are gently stenciled with powder fringe tip, comprise A4 paper, sheet glass, experiment table top, apple and leather surface, namely can be observed to manifest fingerprint lines, magnetic fluorescence powder is under 980nm LASER Light Source, show the fingerprint lines of glow green, take pictures with digital camera.

Claims (2)

1. a preparation method for laten fingerprints detection probes, is characterized in that concrete steps are as follows:
By a certain amount of liquor ferri trichloridi 2 × 10 -2m joins one with in the round-bottomed flask of prolong, 100 oin C oil bath magnetic agitation reaction 70 ~ 80h, carry out centrifugation after react, gained solid again with deionized water wash several, gained solid 50 ~ 75 oc vacuum-drying 8 ~ 10h, obtains dry Fe 3o 2nanoparticle;
By the Fe that 4 ~ 6mg step (1) obtains 3o 2ammoniacal liquor 2mol/L and 10 ~ 15mL deionized water of nanoparticle, 50 ~ 100 μ L polyacrylic acid aqueous solution 0.2g/mL and 75 ~ 150 μ L join in 100mL round-bottomed flask, ultrasonic disperse 10 ~ 20min;
Under magnetic stirring 100 ~ 150mL Virahol is slowly added dropwise in the solution that step (2) obtains, subsequently by 10 ~ 15mgGdCl 36H 2o, 2 ~ 3mgYCl 36H 2o and 0.2 ~ 0.3mgErCl 36H 2o successively joins in solution, and magnetic agitation 2-4h, carries out centrifugation after having reacted, gained solid 50 ~ 75 oc vacuum-drying 8 ~ 12h;
The solid that step (3) obtains is placed in tube furnace, 600 ~ 700 ocalcine 2 ~ 3h under C argon shield, obtain Fe 3o 4gd 2o 3: Y 3+/ Er 3+nano composite material.
2. the application of the laten fingerprints detection probes prepared in accordance with the method for claim 1 in the latent fingerprint manifesting paper, sheet glass, experiment table top, apple and leather surface.
CN201610012292.XA 2016-01-11 2016-01-11 A kind of latent fingerprint detection probe and preparation method thereof Expired - Fee Related CN105482804B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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CN115584259B (en) * 2022-09-30 2023-10-10 中国科学技术大学 Magnetic up-conversion latent fingerprint developer, preparation method thereof and latent fingerprint analysis method

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