CN104352242B - Method for displaying latent fingerprints by surface-modified aluminum oxide nano particles - Google Patents
Method for displaying latent fingerprints by surface-modified aluminum oxide nano particles Download PDFInfo
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- CN104352242B CN104352242B CN201410683288.7A CN201410683288A CN104352242B CN 104352242 B CN104352242 B CN 104352242B CN 201410683288 A CN201410683288 A CN 201410683288A CN 104352242 B CN104352242 B CN 104352242B
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- fingerprint
- silane coupler
- water
- aluminum oxide
- visualization reagent
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Classifications
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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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/48—Other medical applications
Abstract
The invention relates to a displaying agent containing surface-modified aluminum oxide nano particles, a of the displaying agent and a method for displaying latent fingerprints by the displaying agent and the kit. The displaying agent disclosed by the invention is prepared by modifying aluminum oxide by a silane coupling agent. Compared with conventional nano particles, the displaying agent has a better surface adsorption effect in a fingerprint displaying process; furthermore, by the adoption of a surface modification group, the displaying agent is higher in specific substance targeted adsorption capacity and is higher in fingerprint displaying sensitivity.
Description
Technical field
The invention belongs to public security Forensic Science field is and in particular to a kind of aluminium sesquioxide nanometer containing surface modification
The visualization reagent of grain and its method for developing latent finger printss.
Background technology
Fingerprint, has each one and respectively refers to the reflection of the unchangeable stability of different specificity, feature and tactile thing trace
Etc. feature, in forensic science, the fingerprint showing is analyzed, identifies, identifies, be asserting crime suspect's identity according to
According to, it is also the examination of investigation department, disclose and confirm the most quick, the most efficient approach of suspect's crime, judicial in the whole world
There is in boundary the title of " first of material evidence ".
Appearing Techniques of Human Fingerprints has multiple process for show, is divided with the principle of finger mark material association reaction according to it, mainly
There are optical check, powder inspection, chemistry exerts a gradual, corrupting influence on inspection, vacuum coating manifests, radiological techniques appearance method etc..Optical check method mainly has
The methods of inspection such as natural light, laser, multiband light, ultraviolet light, due to only need to can discern whether there is finger mark, finger mark by illumination
Type, form etc., are referred to as a kind of method of inspection to the no damage of finger mark material.But the enhancing presentation capability to finger mark for the method
Limited, and instrument and equipment is expensive, cannot popularize；Powder appearance method is only applicable to relative smooth and inviscid all kinds of object table
Face, and time etc. of leaving of the humiture of environment, fingerprint all the method is had a strong impact on using generation；Chemical appearance method,
Mainly there are silver nitrate, 1,2,3-indantrione monohydrate, DFO method etc., sensitivity finger mark being manifested due to such method is high, it is many to manifest reagent type,
Manifest that reagent is firmly combined with finger mark material and process for show is various, thus become domestic and international forensic science worker favor
Process for show, range is wide, frequency is high.But it is manifested reagent and is typically reacted with some inorganic substances in finger mark, and
Such inorganic substances not distinctive material of finger mark and unstable, the finger mark therefore manifesting is not easy to stable, objective reaction fingerprint
Unique characteristics and make the effect manifesting undesirable.
Therefore although current developing latent finger printss technology is gradually improved, but still face many new difficult problems.One side people
Easily left fingerprints bear that the wide variety of object, color be numerous and diverse, object surface is recessed for the various furniture that use, cabinet, vessel etc.
The difference such as convex affects the formation of fingerprint, and these difficult objects require that fingerprint manifestation has higher sensitivity, and traditional is aobvious
Existing method shows slightly unable to do what one wishes；Another aspect powder generally to improve the method in manifesting by way of reducing powder size
Sensitivity.However, powder size is less, the amount that it suspends in atmosphere is bigger, and the time of suspension is longer, to professional and technical personnel
Physical impairment bigger.Simultaneously some poisonous and harmfuls having the fluorescent dye of carcinogenesis, smoked aobvious reagent dissociation reaction to produce
Gas also causes serious harm to the healthy of professional and technical personnel.Therefore, a kind of high sensitivity, the showing of Non-toxic are developed
Field fingerprint manifestation method will become one of emphasis of fingerprint manifestation research.
Nano material is because its particle diameter can show some special effects in nanoscale and is different from ordinary matter material
The special and excellent physicochemical characteristicss of material are it is easy to be combined with inorganic, the organic species of potential quality India and China.Therefore, for overcoming
Drawbacks described above, it is an object of the invention to provide a kind of visualization reagent of the aluminum oxide nanoparticles containing surface modification, aobvious
Color box set and its method for developing latent finger printss.
Content of the invention
It is an object of the invention to the targets identification work(of the dimensional effect mating surface modified group using nano material
Can, with fingerprint in oils, the absorption of amino acidses material is it is achieved that the fingerprint manifestation effect of high sensitivity, Non-toxic.Pass through
The nano-aluminium oxide of preparation surface modification manifests reagent, occurs with the oils of residual, amino acidses material in latent fingerprint
Electrostatic and oriented adsorption effect, deposit and present white at the lines of fingerprint, and being formed can the clearly fingerprint that arrives of naked eye
Image.
Another object of the present invention be solve run into during latent fingerprint manifests such as to bear object background reflective
The problem that the susceptiveness that interference, powder manifest is weak, associativity is poor and range of application limits.
One aspect of the present invention provides a kind of visualization reagent of the alchlor nano-particle containing surface modification, described manifests
The preparation method of agent includes:Aluminum oxide nanoparticles are put in conical flask, add solvent, add silane coupler,
Stirring, water-bath are heated at reflux and are configured to white " milky " visualization reagent.
Described silane coupler is selected from trichlorosilane, KH 570 silane coupler or KH 318 silane coupler
Kind or more than two kinds of combination.Preferably, described silane coupler is KH 570 silane coupler or KH 318 silane is even
Connection agent.
Described solvent is selected from water, methanol, ethanol, preferably distilled water.
Described aluminum oxide nanoparticles are 25 with the w/v (g/ml) of silane coupler:1-1:1, preferably
10:1-1:1, more preferably 5:1-1:1, more specifically 20:1、15:1、7.5:1、6:1、5:2、3:2.
Described aluminum oxide nanoparticles are 1 with the w/v (g/ml) of solvent:100-1:10；Preferably 1:70-
1:30, more preferably 1:60-1:40, more specifically 3:200、1:20、1:40、1:30.
Described aluminum oxide nanoparticles:Solvent:The w/v g/ml/ml of silane coupler is 3-5:100-
200:0.2-2, it is furthermore preferred that aluminum oxide nanoparticles:Water:The w/v g/ml/ml of silane coupler is 3:
150:0.5；Or, aluminum oxide nanoparticles:Water:The w/v g/ml/ml of silane coupler is 3.5:150:1；
Or, aluminum oxide nanoparticles:Water:The w/v g/ml/ml of silane coupler is 4:180:1.5；Or, three oxygen
Change two aluminum nanoparticles:Water:The w/v g/ml/ml of silane coupler is 4.5:180:2；Or, aluminium sesquioxide is received
Rice grain:Water:The w/v g/ml/ml of silane coupler is 5:200:2
Temperature during described water-bath is 20-60 DEG C, can be specifically 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C etc..
The time of described heating is 0.5-4h, preferably 1-2h, more specifically 1h, 1.5h, 2h.
The rotating speed of described stirring is 100-1000 rev/min, preferably 400-800 rev/min, more specifically 400 turns/
Minute, 450 revs/min, 500 revs/min, 600 revs/min, 700 revs/min, 800 revs/min.
In the preferred embodiment of the present invention, in the described preparation method of visualization reagent, adopt a specified conditions preparation
The visualization reagent going out gem-pure can show latent fingerprint, and described preparation method includes：By 3-5g aluminium sesquioxide nanometer
Grain is put in conical flask, adds 100-200ml distilled water, adds 0.2-2ml silane coupler, 20- in magnetic stirring apparatuss
60 DEG C of water-baths are heated at reflux 1-2 hour, set 400-800 rev/min of revolution, are configured to white " milky " visualization reagent.
It is more highly preferred to, described preparation method includes：Aluminum oxide nanoparticles:Water:The weight of silane coupler
Volume ratio (g/ml/ml) is 3:150:0.5th, heating-up temperature be 30 DEG C, heat time heating time be 1h, agitator rotating speed be 400 revs/min
Clock；Or, aluminum oxide nanoparticles:Water:The w/v (g/ml/ml) of silane coupler is 3.5:150:1st, heat
Temperature is 40 DEG C, heat time heating time is 1.5h, the rotating speed of agitator is 450 revs/min；Or, aluminum oxide nanoparticles:
Water:The w/v (g/ml/ml) of silane coupler is 4:180:1.5th, heating-up temperature be 40 DEG C, heat time heating time be 2h, stir
The rotating speed mixing device is 500 revs/min；Or, aluminum oxide nanoparticles:Water:W/v (the g/ of silane coupler
Ml/ml it is) 4.5:180:2nd, heating-up temperature be 50 DEG C, heat time heating time be 1.5h, agitator rotating speed be 600 revs/min；Or
Person, aluminum oxide nanoparticles:Water:Silane coupler w/v (g/ml/ml) is 5:200:2nd, heating-up temperature is 60
DEG C, heat time heating time be 2h, agitator rotating speed be 800 revs/min.
Another aspect of the present invention also provides a kind of colour developing box set, and it comprises visualization reagent of the present invention, and cationic yellow
Stain.Cationic yellow stain of the present invention is prepared by following methods：Cationic yellow is dissolved in methanol, makes sun
Ion xanthochromia toner.The consumption of described cationic yellow is 0.2-0.6g, and methanol usage is 80-120ml.Preferably, described first
The consumption of alcohol is 100ml.
Further aspect of the present invention provides a kind of process for show of latent fingerprint, and it comprises the steps of：White by the present invention
Emulsus visualization reagent shakes up into emulsus, makes to rock in the material immersion liquid to be checked be suspected to have fingerprint, or the white " milky " by the present invention
Visualization reagent drops in the material surface to be checked being suspected to have fingerprint, after standing, that is, has fingerprint to show, then washes loose colour off with clear water, natural
It is dried；Draw appropriate cationic yellow stain with suction pipe, be applied to the material surface to be checked being suspected to have fingerprint, be washed with water removal floating color,
Observe under long-wave ultra violet lamp, fingerprint is in bright trace.
KH 570 silane coupler of the present invention refers to γ-(methacryloxypropyl) propyl trimethoxy silicane, point
Minor is C10H20O5Si；Described KH 318 silane coupler refers to n- octyl group trimethoxy silane, and molecular formula is
C11H26O3Si.
The mechanism of aluminum oxide nanoparticles surface modification of the present invention is as follows：Silane coupler hydrolyzes first
Reaction, hydrolysis generates silanol base (- SiOH).And then occur dehydration to form oligomer, this oligomer and aluminium oxide nano
The hydroxyl of particle surface forms hydrogen bond or is condensed into-SiO-M (M is alumina particulate), by heat drying, dehydration occurs
Forming part covalent bond, meanwhile, each intermolecular silanol base of silane is mutually condensed again, and oligomerisation forms cancellated film and covers
Particle surface, ultimately forms the aluminum oxide nanoparticles of silane coupler surface modification.Particularly, of the present invention
KH 570 and KH 318 is due to having middle alkyl group, the aluminium sesquioxide nanometer of the modificationization ultimately forming in molecular structure
Granule has more excellent effect.
It is an advantage of the current invention that：Aluminum oxide nanoparticles after surface modification of the present invention, in fingerprint manifestation
During, compare traditional nano-particle and not only there is stronger surface adsorption effect, and had due to surface-modifying groups
There is stronger predetermined substance targeting absorbability, there is higher fingerprint manifestation sensitivity.Meanwhile, the method is manifested using solution
Mode, it is to avoid the generation of nano-particle airborne dust, entirely manifests that process is pollution-free, nonhazardouss.Therefore, of the present invention manifest
Agent not only can manifest difficult, the complicated fingerprint that offender is retained on various carriers effectively additionally it is possible to overcome existing
Manifest reagent, presentation device expensive and cannot popularize and process for show has the difficult problems such as potential safety hazard.
Brief description
Fig. 1 is to manifest result using embodiment 1 method to fingerprint latent on whiteware experimental material.
Fig. 2 is to manifest result using embodiment 1 method to fingerprint latent on glass check material.
Fig. 3 is to manifest result using embodiment 1 method to fingerprint latent on aluminium foil experimental material.
Fig. 4 is to manifest result using embodiment 1 method to fingerprint latent on green plastic experimental material.
Fig. 5 is to manifest result using embodiment 1 method to fingerprint latent on red lacquer painting can experimental material.
Fig. 6 is to manifest result using embodiment 1 method to fingerprint latent on green lacquer painting can experimental material.
Fig. 7 is to manifest comparing result to different silane couplers to fingerprint latent on experimental material using embodiment 2 method,
It is respectively matched group from left to right, use the test group that KH-318 is silane coupler, use KH-570 to be silane coupler
Test group, using trichlorosilane be silane coupler test group.
Specific embodiment
Embodiment 1
(1) preparation of the aluminum oxide nanoparticles visualization reagent of KH 570 modification
3g aluminum oxide nanoparticles are put in conical flask；Add 200ml distilled water；Add 0.5ml KH
570；In magnetic stirring apparatuss, 30 DEG C of water-baths are heated at reflux 1.5 hours, set 500 revs/min of revolution, are configured to visualization reagent.
(2) preparation method of cationic yellow stain
Take 0.4g cationic yellow, add 100ml methanol, make cationic yellow stain.
(3) the colour developing box set of visualization reagent and cationic yellow stain composition is used for manifesting of the latent fingerprint of 6 kinds of materials to be checked
Visualization reagent prepared by (1) shakes up into emulsus；The material to be checked of fingerprint will be suspected to have respectively：White ceramic tile, glass, aluminum
Paper tinsel, green plastic piece, red lacquer painting can surface, green lacquer painting can surface are immersed in developer and are constantly rocked, that is, have fingerprint
Show；
Wash loose colour off with clear water, spontaneously dry；Draw, with suction pipe, the cationic yellow stain that appropriate (2) prepare, apply
In fingerprint surface, be washed with water removal floating color, observe under long-wave ultra violet lamp, fingerprint is in bright yellow green, concrete outcome referring to
Accompanying drawing 1-6.
Embodiment 2
Different silane couplers manifest contrast test to latent fingerprint
Test group：
(1) 2.5g aluminum oxide nanoparticles are put in conical flask；Add 200ml distilled water；Add 0.5ml tri-
One of chlorosilane, KH 570 or KH-318 silane coupler；In magnetic stirring apparatuss, to be heated at reflux 1.5 little for 30 DEG C of water-baths
When, set 700 revs/min of revolution, be configured to visualization reagent.
(2) take 0.4g cationic yellow, add 100ml methanol, make cationic yellow stain.
(3) visualization reagent preparing (1) shakes up into emulsus；Respectively by the material immersion to be checked being suspected to have fingerprint of identical material
Constantly rock in developer, that is, have fingerprint to show；Wash loose colour off with clear water, spontaneously dry；Draw appropriate (2) with suction pipe to be prepared into
The cationic yellow stain arriving, is applied to fingerprint surface, is washed with water removal floating color, observes under long-wave ultra violet lamp.
Matched group：
(1) 2.5g aluminum oxide nanoparticles are put in conical flask, add 200ml distilled water, be configured to visualization reagent.
(2) take 0.4g cationic yellow, add 100ml methanol, make cationic yellow stain.
(3) visualization reagent preparing (1) shakes up into emulsus；By the material to be checked being suspected to have fingerprint with test group identical material
Constantly rock in immersion developer, that is, have fingerprint to show；Wash loose colour off with clear water, spontaneously dry；Draw appropriate (2) system with suction pipe
The standby cationic yellow stain obtaining, is applied to fingerprint surface, is washed with water removal floating color, observes under long-wave ultra violet lamp.
Result of the test：
As Fig. 7 shows, from left to right respectively matched group, using KH-318 be silane coupler test group, use KH-
570 is the test group of silane coupler for the test group of silane coupler, using trichlorosilane.
Graded to manifesting result using perusal：
"+", represents the rank of fingerprint clear, "+" to represent fingerprint clear degree higher more.
Embodiment 3-10
Using the similar visualization reagent of identical step preparation, wherein process conditions carry out suitable change, cation xanthochromia
The preparation method of toner is with embodiment 1, and carries out manifesting latent fingerprint, concrete situation using identical process for show in embodiment 1
And effect please see table：
Embodiment 11-18
Using the similar visualization reagent of step preparation same as Example 1, wherein process conditions carry out suitable change, sun
The preparation method of ion xanthochromia toner is with embodiment 1, and carries out manifesting latent fingerprint using identical process for show in embodiment 1,
Concrete situation and effect please see table：
Claims (8)
1. a kind of visualization reagent containing surface modification alchlor nano-particle it is characterised in that：Its preparation method includes as follows
Step：Aluminum oxide nanoparticles are put in conical flask, adds solvent, add silane coupler, stirring, water-bath backflow
Heating is configured to white " milky " visualization reagent；
Described silane coupler is selected from KH 570 silane coupler or KH 318 silane coupler；
Aluminum oxide nanoparticles in described preparation method:Solvent:The w/v g/ml/ml of silane coupler is 3-
5:100-200:0.2-2, heating-up temperature is 20-60 DEG C, and heat time heating time is 1-2h, and in whipping process, agitator speed is 400-
800 revs/min.
2. a kind of visualization reagent according to claim 1 it is characterised in that：Described solvent is water, ethanol or methanol.
3. a kind of visualization reagent according to claim 2 it is characterised in that：Described solvent is distilled water.
4. a kind of visualization reagent according to claim 1 it is characterised in that：Its preparation method includes：3-5g tri- is aoxidized two
Aluminum nanoparticles are put in conical flask, add 100-200ml distilled water, add 0.2-2ml silane coupler, in magnetic agitation
In device, 20-60 DEG C of water-bath is heated at reflux 1-2 hour, sets 400-800 rev/min of agitator speed and is stirred, is configured to white
Color emulsus visualization reagent.
5. a kind of visualization reagent according to claim 4 is it is characterised in that aluminium sesquioxide nanometer in its preparation method
Grain:Water:The w/v g/ml/ml of silane coupler is 3:150:0.5, heating-up temperature is 30 DEG C, and heat time heating time is 1h, stirs
The rotating speed mixing device is 400 revs/min；
Or, aluminum oxide nanoparticles:Water:The w/v g/ml/ml of silane coupler is 3.5:150:1st, heat
Temperature is 40 DEG C, heat time heating time is 1.5h, the rotating speed of agitator is 450 revs/min；
Or, aluminum oxide nanoparticles:Water:The w/v g/ml/ml of silane coupler is 4:180:1.5th, heat
Temperature is 40 DEG C, heat time heating time is 2h, the rotating speed of agitator is 500 revs/min；
Or, aluminum oxide nanoparticles:Water:The w/v g/ml/ml of silane coupler is 4.5:180:2nd, heat
Temperature is 50 DEG C, heat time heating time is 1.5h, the rotating speed of agitator is 600 revs/min；
Or, aluminum oxide nanoparticles:Water:The w/v g/ml/ml of silane coupler is 5:200:2nd, heat temperature
Spend for 60 DEG C, heat time heating time be 2h, agitator rotating speed be 800 revs/min.
6. a kind of colour developing box set it is characterised in that：Described box set comprises the arbitrary described visualization reagent of claim 1-5, Yi Jiyang
Ion xanthochromia toner, the preparation method of described cationic yellow stain includes：Cationic yellow is dissolved in methanol, make sun from
Sub- xanthochromia toner, the consumption of described cationic yellow is 0.2-0.6g, and methanol usage is 80-120ml.
7. a kind of process for show of latent fingerprint is it is characterised in that comprise the steps of：
Arbitrary for claim 1-5 described visualization reagent is shaken up into emulsus；Make to be suspected to have the material immersion emulsus colour developing to be checked of fingerprint
Rock in agent, or emulsus visualization reagent is dropped in the material surface to be checked being suspected to have fingerprint, after standing, that is, have fingerprint to show；Use clear water
Wash loose colour off, spontaneously dry, draw cationic yellow stain with suction pipe, be applied to fingerprint surface, be washed with water removal floating color, in long wave
Observe under uviol lamp, fingerprint is in bright color mark；The preparation method of described cationic yellow stain includes：Cationic yellow is molten
In methanol, make cationic yellow stain, the consumption of described cationic yellow is 0.2-0.6g, and methanol usage is 80-120ml.
8. the process for show of the latent fingerprint described in claim 7 is it is characterised in that the described material to be checked being suspected to have fingerprint is gold
Genus, one of pottery, glass, plastics.
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| CN201410683288.7A CN104352242B (en) | 2014-11-24 | 2014-11-24 | Method for displaying latent fingerprints by surface-modified aluminum oxide nano particles |
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| CN201410683288.7A CN104352242B (en) | 2014-11-24 | 2014-11-24 | Method for displaying latent fingerprints by surface-modified aluminum oxide nano particles |
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| CN104352242B true CN104352242B (en) | 2017-02-08 |
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| CN101381368A (en) * | 2008-10-22 | 2009-03-11 | 江苏警官学院 | Ethylenediamine schiff base type sweat fingerprint fluorescent reagent, synthesis and use thereof |
| CN101565619A (en) * | 2009-05-27 | 2009-10-28 | 中国地质大学（武汉） | Small-particle yellow rare-earth fluorescent powder and preparation method and purpose of visualizing latent fingerprint thereof |
| CN103431867A (en) * | 2013-08-20 | 2013-12-11 | 北京科技大学 | Method for displaying latent fingerprints on fluorogold nano-cluster protected by protein |
| CN103908260A (en) * | 2014-01-16 | 2014-07-09 | 中国刑事警察学院 | Latent fingerprint displaying method |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101268946A (en) * | 2008-04-30 | 2008-09-24 | 东北师范大学 | Method for latency fingerprint appearance of surface functionalization nano-gold particle |
| CN101308061A (en) * | 2008-07-09 | 2008-11-19 | 北京理工大学 | Rapid latent fingerprint presentation reagent preparation method |
| CN101381368A (en) * | 2008-10-22 | 2009-03-11 | 江苏警官学院 | Ethylenediamine schiff base type sweat fingerprint fluorescent reagent, synthesis and use thereof |
| CN101565619A (en) * | 2009-05-27 | 2009-10-28 | 中国地质大学（武汉） | Small-particle yellow rare-earth fluorescent powder and preparation method and purpose of visualizing latent fingerprint thereof |
| CN103431867A (en) * | 2013-08-20 | 2013-12-11 | 北京科技大学 | Method for displaying latent fingerprints on fluorogold nano-cluster protected by protein |
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