CN105581800B - A kind of fingerprint manifestation method and its application based on upconverting fluorescent material - Google Patents
A kind of fingerprint manifestation method and its application based on upconverting fluorescent material Download PDFInfo
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- CN105581800B CN105581800B CN201410568050.XA CN201410568050A CN105581800B CN 105581800 B CN105581800 B CN 105581800B CN 201410568050 A CN201410568050 A CN 201410568050A CN 105581800 B CN105581800 B CN 105581800B
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Abstract
The present invention provides a kind of fingerprint manifestation methods and applications based on upconverting fluorescent material, the fingerprint manifestation method based on upconverting fluorescent material comprises the following steps that S10) using smoked aobvious agent treat the object shown carry out it is smoked aobvious, to occurring, white is smoked to show fingerprint, wherein, the smoked aobvious agent includes at least cyanoacrylate, or including at least the reagent for generating cyanoacrylate during smoked aobvious；S20) by upconverting fluorescent material brush, apply or be sprayed on the smoked aobvious fingerprint of white, near-infrared laser irradiation shows fingerprint.The present invention provides a kind of fluorescent materials and its preparation method and application.
Description
Technical field
The present invention relates to fingerprinting detection technique field more particularly to a kind of fingerprint manifestation sides based on upconverting fluorescent material
Method and its application.
Background technique
Due to the diversity and complexity for the latent fingerprint object that scene of a crime occurs, it is often necessary to be increased using fluorescent material
Strong fingerprint manifestation.
Fluorescent material is applied to there are mainly two types of the methods of fingerprint manifestation: powder method --- fluorescent material or including phosphor
The reagent that shows of material is adsorbed by physical mechanical or electrostatic interaction with the fingerprint residues object on mastoid process streakline, without fingerprint
The small ditch dug with a plow and fingerprint supporting body of residue will not then adsorb powder；Soak aobvious method --- fluorescent material or including fluorescent material
The reagent that shows pass through remaining protein, amino acid and grease sweat stain in chemical coupling and electrostatic adsorption and fingerprint substance
Deng generation chemical coupling or specific physical absorption, the fluorescent material after making modification is selectively deposited on fingerprint ridge.
But 1) powder method easily damages the residue on fingerprint surface during brush is aobvious, and powder and fingerprint table
The adsorption capacity of face residue is limited；2) aobvious method is soaked there are presentation times longer, the limited problem of adsorption capacity.
Therefore, it is necessary to which providing a kind of can effectively adsorb that fingerprint surface residue, the fingerprint manifestation time is short and can effectively keep away
Exempt from the fingerprint manifestation method and its application of background fluorescence interference.
Summary of the invention
In order to solve the above-mentioned technical problem, it is aobvious that the embodiment of the invention provides a kind of fingerprints based on upconverting fluorescent material
Existing method；The fingerprint manifestation method based on upconverting fluorescent material can effectively adsorb fingerprint surface residue, fingerprint it is aobvious
It is short and effectively background fluorescence can be avoided to interfere between current.
In a first aspect, the present invention provides a kind of fingerprint manifestation method based on upconverting fluorescent material, including following step
It is rapid:
S10) using smoked aobvious agent treat the object shown carry out it is smoked aobvious, to there is the smoked aobvious fingerprint of white, wherein described smoked to show
Agent includes at least cyanoacrylate, or including at least the reagent for generating cyanoacrylate during smoked aobvious；
S20) by upconverting fluorescent material brush, apply or be sprayed on the smoked aobvious fingerprint of white, near-infrared laser irradiation shows finger
Line.
Fingerprint manifestation method provided by the invention based on upconverting fluorescent material combines the excellent of smoked aobvious method and powder method
Gesture, the process employs cyanoacrylate not only have the function of it is preliminary smoked aobvious, there are also protect fingerprint not by it is subsequent brush,
It applies, the effect that spray processing destroys, this method, as coloring agent, is shone strong using upconverting fluorescent material, and uses near-infrared
Excitation, avoids background interference, and the details in fingerprint handled by method provided by the invention is clear, and feature is obvious, and contrast is high,
It is easy to collect evidence.
Preferably, in the step (S10), the object to be shown is solid body.
Preferably, in the step (S10), the object to be shown includes plastic products, glassware, made of metal
Product, woodwork or paper.
Preferably, in the step (S10), the smoked aobvious agent is cyanoacrylate.
Preferably, in the step (S10), the smoked aobvious agent is that the examination of cyanoacrylate is generated during smoked aobvious
Agent.
Preferably, in the step (S10), the smoked aobvious agent is 502 glue.
Under this optimum condition, it is described the object shown treated using smoked aobvious agent carry out smoking aobvious step include:
After being mixed using inorganic base as catalyst and 502 glue, treats the object shown and carry out smoked aobvious processing.
It is further preferred that the inorganic base is at least one in sodium hydroxide, potassium hydroxide, sodium carbonate or potassium carbonate
Kind.
Preferably, in the step (S10), the smoked aobvious processing can operate in fuming box, specifically: by alkali and
502 glue carry out mixing and are placed in fuming box, and then object to be shown is placed at other one in fuming box, smoke aobvious
It 0.5 hour or so or smoked shows to there is the smoked aobvious fingerprint of white.
Preferably, in the step (S10), the smoked aobvious processing can for by appropriate NaOH solution drop on absorbent cotton,
It takes isometric commercialization " 502 " glue drop on absorbent cotton again, the body surface to be shown for having fingerprint is buckled in degreasing at once
It smokes aobvious 0.5 hour or so or smokes on cotton and show to the smoked aobvious fingerprint of appearance white.
Under this optimum condition, it is described using smoked aobvious agent treat the object shown carry out it is smoked it is aobvious after, object table to be shown
There is the smoked aobvious fingerprint of white in face.
Preferably, described to smoke aobvious range not less than the region where fingerprint in the step (S10).
Preferably, in the step (S10), the brush, the range for applying or spraying are not less than the region where fingerprint.
Preferably, in the step (S20), it is described by upconverting fluorescent material brush, apply or be sprayed on the smoked aobvious fingerprint of white
Afterwards；20s~60s is waited, the luminescent material of the excess surface of object to be shown is brushed away；It is irradiated, is shown using near-infrared laser again
Fingerprint.
Preferably, in the step (S20), the wavelength that near-infrared laser irradiation uses is 980nm.
When using near infrared light (such as 980nm) as excitation light source, the upconverting fluorescent material that the present invention uses is excited to issue
Visible fluorescence, and object background does not shine or issues invisible fluorescence, can effectively avoid background interference.In addition, using this property
Matter can observe fingerprint, since in the dark, background color can not for the object that some backcolors become clear in the dark
See, background interference very little, it is easy to see the bright fingerprint in dark background.
In addition, comparing with traditional fluorescent material, traditional fluorescent material is often needed using burst of ultraviolel.However, in purple
Under outer high energy excitation, background where certain latent fingerprints is easy to produce background fluorescence, if background fluorescence covering fluorescent material
Emission peak or the main generation peak used with fluorescence are overlapped, and will lead to can not show potential fingerprint, identify.And this hair
The method of bright offer is used to be excited in near-infrared, and object does not shine or issue invisible fluorescence under the shooting condition, can be to avoid
Background interference.
Preferably, in the step (S20), the upconverting fluorescent material be upper conversion fluorescent nano particle, it is described on
The average grain diameter of conversion fluorescent nano particle is 50nm~2 μm.
It is further preferred that the upconverting fluorescent material is upper conversion fluorescent nano particle in the step (S20),
The average grain diameter of the upper conversion fluorescent nano particle is 1.5 μm.
The cyanoacrylate polymer is the polymer with 1~2 μm of aperture, when the upconverting fluorescent material used
Particle size be less than the polymer aperture when, the upconverting fluorescent material can firmly be dispersed in the hole of polymer
In diameter, to achieve the effect that dyeing enhancing.
As described in the present invention, " latent fingerprint " can be interchanged with " potential fingerprint ", indicate object on wait show, wait know
Other fingerprint.
Preferably, in the step (S20), the upconverting fluorescent material includes NaYF4:Yb3+,Er3+、YF3:Yb3+,
Er3+、NaYF4:Yb3+,Tm3+、YF3:Yb3+,Tm3+、NaYF4:Yb3+,Ho3+And YF3:Yb3+,Ho3+At least one of.
It is further preferred that the upconverting fluorescent material is upper conversion fluorescent nano particle, the up-conversion fluorescence
The average grain diameter of nano particle is 50nm~2 μm.
It is further preferred that the upconverting fluorescent material is upper conversion fluorescent nano particle, the up-conversion fluorescence is received
The average grain diameter of rice grain is 1.5 μm.
It is further preferred that the upconverting fluorescent material is upper conversion fluorescent nano particle, the up-conversion fluorescence
Nano particle is bar shaped column structure.
It is further preferred that the up-conversion phosphor is using the NaYF prepared following preparation method4:Yb3+,Er3+
Up-conversion phosphor includes the following steps:
1) rare earth element chloride LnCl3(Ln=Y, Yb, Er) and NaCl are dissolved according to the concentration of 0.5mol/L respectively
In ionized water, NH4F is dissolved in deionized water according to the concentration of 1mol/L, and polyethyleneimine (PEI) is according to mass fraction 5%
Concentration is dissolved in deionized water；
2) continue to be passed through under conditions of nitrogen into reaction kettle, in the reaction kettle using polytetrafluoroethylene (PTFE) as liner, be added
5mL PEI solution, 15mL ethyl alcohol, 1mL NaCl solution, 0.77mLYCl3Solution, 0.2mL YbCl3Solution, 0.03mL ErCl3
Solution quickly stirs 5min, adds 4mL NH4F obtains reaction solution, continues to stir 15min；
3) reaction kettle is closed, is placed under 200 DEG C of environment and heats for 24 hours, it is cooling after eccentric cleaning 3 times, and by eccentric cleaning
Gained precipitating is dissolved in the upconversion fluorescence nano material NaYF that High Efficiency Luminescence is arrived in 5mL deionized water afterwards4:Yb3+,Er3+。
Preferably, in the step (S20), the surface modification of the upconverting fluorescent material have polyethyleneimine (PEI),
Disodium ethylene diamine tetraacetate, L-cysteine, thioacetic acid, mercaptoethanol, gamma-aminopropyl-triethoxy-silane or polyethylene pyrrole
Pyrrolidone K30 salt.
Fingerprint manifestation method provided by the invention based on upconverting fluorescent material not only overcomes traditional " 502 " smoked aobvious method
Feature is unobvious, it is difficult to the deficiency of observation；It also solves existing for conventional powder method: being easy during brush is aobvious to fingerprint residues object
It damages, the disadvantage that the adsorption capacity of powder and fingerprint residues object is not strong.
Since the fingerprint manifestation method provided by the invention based on upconverting fluorescent material first uses cyanoacrylate
(effective smoked aobvious ingredients of 502 glue) carry out it is smoked aobvious, cyanoacrylate with wait show the fingerprint residues object on object (such as water,
Amino acid etc.) reaction, and one layer of cyanoacrylate polymer, the polymerizable cyanoacrylate ester are formed on fingerprint to be shown
Object is the smoked aobvious middle smoked aobvious fingerprint of white of tradition.However, encountering the object of light color, colorless or clear background, the smoked aobvious fingerprint of white is not
Easily it is observed, therefore, the present invention further uses upconverting fluorescent material to brush, apply or be sprayed on the smoked aobvious fingerprint of white,
It is attached to due to cyanoacrylate polymer on fingerprint to be shown, has the effect of insulation blocking fingerprint, can prevented subsequent
Fingerprint is destroyed when being brushed, applied to upconverting fluorescent material in operation, spraying processing；In addition, the cyanoacrylate polymer
For the polymer with 1~2 μm of aperture, when the particle size of the upconverting fluorescent material used is less than the aperture of the polymer
When, the upconverting fluorescent material can be firmly dispersed in the aperture of polymer, to achieve the effect that dyeing enhancing.
As described in the present invention, the symbol of element " Y, Yb, Er " respectively indicates yttrium, ytterbium, erbium.
Second aspect, it is aobvious that the present invention also provides a kind of fingerprints based on upconverting fluorescent material as described in relation to the first aspect
Existing application of the method in fingerprint detection.
Beneficial effects of the present invention
Fingerprint manifestation method provided by the invention based on upconverting fluorescent material combines the excellent of smoked aobvious method and powder method
Gesture, the process employs cyanoacrylate not only have the function of it is preliminary smoked aobvious, there are also protect fingerprint not by it is subsequent brush,
It applies, the effect that spray processing destroys, this method, as coloring agent, is shone strong using upconverting fluorescent material, and uses near-infrared
Excitation, avoids background interference, and the details in fingerprint handled by method provided by the invention is clear, and feature is obvious, and contrast is high,
It is easy to collect evidence.
Detailed description of the invention
Fig. 1 is up-conversion fluorescence rare earth material NaYF prepared by embodiment 14:Yb3+,Er3+Stereoscan photograph；
Fig. 2 is that embodiment 2 fingerprint pattern shows result；
Fig. 3 is that comparative example 1 fingerprint pattern shows result；
Fig. 4 is that embodiment 3 fingerprint pattern shows result sample；
Fig. 5 is that embodiment 4 fingerprint pattern shows result；
Fig. 6 is that embodiment 5 fingerprint pattern shows result；
Fig. 7 is that embodiment 6 fingerprint pattern shows result；
Fig. 8 is that embodiment 7 fingerprint pattern shows result；
Fig. 9 is that embodiment 8 fingerprint pattern shows result.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be pointed out that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
The present invention is further explained in the light of specific embodiments.
Embodiment 1
The embodiment of the invention provides a kind of hydro-thermal methods to prepare upconverting fluorescent material NaYF4:Yb3+,Er3+Method, packet
Include following steps:
1, rare earth element chloride LnCl3(Ln=Y, Yb, Er) and NaCl are dissolved according to the concentration of 0.5mol/L respectively
In ionized water, NH4F is dissolved in deionized water according to the concentration of 1mol/L, and polyethyleneimine (PEI) is according to mass fraction 5%
Concentration is dissolved in deionized water；
2, continue to be passed through under conditions of nitrogen into reaction kettle, in the reaction kettle using polytetrafluoroethylene (PTFE) as liner, be added
5mL PEI solution, 15mL ethyl alcohol, 1mL NaCl solution, 0.77mLYCl3Solution, 0.2mLYbCl3Solution, 0.03mL ErCl3It is molten
Liquid quickly stirs 5min, adds 4mL NH4F obtains reaction solution, continues to stir 15min；
3, reaction kettle is closed, is placed under 200 DEG C of environment and heats for 24 hours, it is cooling after eccentric cleaning 3 times, and by eccentric cleaning
Gained precipitating is dissolved in the upconversion fluorescence nano material NaYF that High Efficiency Luminescence is arrived in 5mL deionized water afterwards4:Yb3+,Er3+。
Fig. 1 is rare earth up-conversion luminescent material NaYF used in the present invention4:Yb3+,Er3+Stereoscan photograph, from figure
In can be seen that, average grain diameter be 1.5 μm.
Reagent used in the embodiment of the present invention and purity: polyetherimide (polyethyleneimine, PEI),
YCl36H20 (99.9%), YbCl36H20 (99.9%), ErCl36H20 (99.9%), NaCl (99+%), NH4F(98
+ %).
Embodiment 2
A kind of fingerprint manifestation method based on upconverting fluorescent material, comprising the following steps:
1. pressing one piece of oil on mineral water plastics package surface dives fingerprint (or invisible fingerprints of sweat) as test sample；
2. take the NaOH solution about 0.5mL drop of 1mol/L on absorbent cotton, then take commercial " 502 " the glue drop of about 0.5mL in
Thereon, at once that the plastics package surface back-off for pressing fingerprint is 30 minutes aobvious in smoking on absorbent cotton；
3. picking NaYF prepared by appropriate embodiment 1 with powder brush4:Yb3+,Er3+Powder is gently brushed and is shown on fingerprint in smoked,
Smoked aobvious fingerprint surface excessive powder is brushed away after about 30 seconds；
4. irradiating fingerprint with 980nm near-infrared laser, it is seen that become clear fingerprint under dark background；Then it is carried out with camera
It takes pictures evidence obtaining, time for exposure 2.5s, focal length is certain.
Fig. 2 is the fingerprint pattern that embodiment 2 obtains, and in Fig. 2, B1 is invisible fingerprints of sweat, have under near-infrared irradiation preferably at
Type fingerprint；B2 is the latent fingerprint of oil, has preferably molding fingerprint, details obvious under laser irradiation；B3 is the latent fingerprint of oil, step 2)
After 502 is smoked aobvious, the left side is handled with water wiping, and the right is not handled, and is then carrying out step 3) brush rare earth powder, it is seen that laser irradiation
Under still have molding fingerprint, but left side details is destroyed, and the right is more visible.
Comparative example 1
To embody creativeness of the invention, the present invention is also provided with the comparative example of embodiment 2, comparative example and reality
The difference for applying example 1 is that comparative example does not use " 502 " glue smoked aobvious, directly shows upconverting fluorescent material with powder method brush, right
Include: than the step of embodiment
1. pressing one piece of oil on mineral water plastics package surface dives fingerprint (or invisible fingerprints of sweat) as test sample；
2. picking NaYF prepared by appropriate embodiment 1 with powder brush4:Yb3+,Er3+Powder is gently brushed and is shown on fingerprint in smoked,
Smoked aobvious fingerprint surface excessive powder is brushed away after about 30 seconds；
3. irradiating fingerprint with 980nm near-infrared laser；Then evidence obtaining of taking pictures is carried out to it with camera, time for exposure 2.5s,
Focal length is certain.
Fig. 3 is the fingerprint pattern of comparative example 1, and the two is under the irradiation of same power 980nm near-infrared laser, by Canon
650D slr camera takes pictures to obtain, and the time for exposure is 2.5s, and focal length of taking pictures is certain.
In Fig. 3, A1 invisible fingerprints of sweat, without molding fingerprint under near-infrared excitation；A2 oil is dived fingerprint, has molding under near-infrared irradiation
Fingerprint, but part details lacks；A3 oil is dived fingerprint, has molding fingerprint under laser irradiation, but intermediate region details is fuzzy
In Fig. 2, since after smoked aobvious, 502 polymer of latent fingerprint Surface Creation have 1~2 μm of aperture, greater than making
NaYF4:Yb3+,Er3+The particle size of powder, allows aperture to fix NaYF4:Yb3+,Er3+Crystal, to reach dye
The effect of color enhancing.By comparing with Fig. 3 it is found that the fingerprint pattern handled through the method for the present invention, is easy to collect evidence, details is clear
Clear, luminous intensity is high, and contrast is high, has certain protective role to fingerprint.
Embodiment 3
A kind of fingerprint manifestation method based on upconverting fluorescent material, comprising the following steps:
1. pressing one piece of oil on mineral water plastics package surface dives fingerprint as test sample；
2. taking the NaOH solution 0.5mL drop of 1mol/L on absorbent cotton, then by commercial " 502 " the glue drop of 0.5mL in it
On, it is at once that the plastics package surface back-off for pressing fingerprint is 30 minutes aobvious in smoking on absorbent cotton；
3. picking the NaYF of the preparation of embodiment 1 with powder brush4:Yb3+,Er3+Powder is gently brushed and is shown on fingerprint in smoked, after 30s
Brush away the powder of smoked aobvious fingerprint excess surface；
4. using 980nm near infrared light fingerprint, evidence obtaining of taking pictures, time for exposure 2.5s are then carried out to it with camera.
Embodiment 4
A kind of fingerprint manifestation method based on upconverting fluorescent material, comprising the following steps:
1. pressing one piece of oil in aluminium foil surface dives fingerprint as test sample；
2. take the NaOH solution 0.5mL drop of 1mol/L on absorbent cotton, then thereon by commercial " 502 " the glue drop of 0.5mL,
It is at once that the aluminium foil surface back-off for pressing fingerprint is 30 minutes aobvious in smoking on absorbent cotton；
3. picking the NaYF of the preparation of embodiment 1 with powder brush4:Yb3+,Er3+Powder is gently brushed and is shown on fingerprint in smoked, after 30s
Brush away the powder of smoked aobvious fingerprint excess surface；
4. using 980nm near infrared light fingerprint, evidence obtaining of taking pictures, time for exposure 2.5s are then carried out to it with camera.
Embodiment 5
A kind of fingerprint manifestation method based on upconverting fluorescent material, comprising the following steps:
1. pressing the latent fingerprint of one piece of oil as test sample thickening frosting；
2. take the NaOH solution 0.5mL drop of 1mol/L on absorbent cotton, then thereon by commercial " 502 " the glue drop of 0.5mL,
It is at once that the thickening frosting back-off for pressing fingerprint is 30 minutes aobvious in smoking on absorbent cotton；
3. picking the NaYF of the preparation of embodiment 1 with powder brush4:Yb3+,Er3+Powder is gently brushed and is shown on fingerprint in smoked, after 30s
Brush away the powder of smoked aobvious fingerprint excess surface；
4. using 980nm near infrared light fingerprint, evidence obtaining of taking pictures, time for exposure 2.5s are then carried out to it with camera.
Embodiment 6
A kind of fingerprint manifestation method based on upconverting fluorescent material, comprising the following steps:
1. pressing one piece of oil on adhesive tape surface dives fingerprint as test sample；
2. take the NaOH solution 0.5mL drop of 1mol/L on absorbent cotton, then thereon by commercial " 502 " the glue drop of 0.5mL,
It is at once that the adhesive tape surface back-off for pressing fingerprint is 30 minutes aobvious in smoking on absorbent cotton；
3. picking the NaYF of the preparation of embodiment 1 with powder brush4:Yb3+,Er3+Powder is gently brushed and is shown on fingerprint in smoked, after 30s
Brush away the powder of smoked aobvious fingerprint excess surface；
4. using 980nm near infrared light fingerprint, evidence obtaining of taking pictures, time for exposure 2.5s are then carried out to it with camera.
Embodiment 7
A kind of fingerprint manifestation method based on upconverting fluorescent material, comprising the following steps:
1. pressing one piece of oil on plated film hardboard paper surface dives fingerprint as test sample；
2. taking the NaOH solution about 0.5mL drop of 1mol/L on absorbent cotton, then by commercial " 502 " the glue drop of 0.5mL in it
On, it is at once that the plated film hardboard paper surface back-off for pressing fingerprint is 30 minutes aobvious in smoking on absorbent cotton；
3. picking the NaYF of the preparation of embodiment 1 with powder brush4:Yb3+,Er3+Powder is gently brushed and is shown on fingerprint in smoked, after 30s
Brush away the powder of smoked aobvious fingerprint excess surface；
4. using 980nm near infrared light fingerprint, evidence obtaining of taking pictures, time for exposure 2.5s are then carried out to it with camera.
Fig. 4~Fig. 8 is the fingerprint pattern that embodiment 3~7 obtains respectively, and the left figure of Fig. 4-Fig. 8 is to clap under indoor light
The fingerprint pattern taken the photograph, the right figure of Fig. 4~Fig. 8 are under the irradiation of same power 980nm near-infrared laser, by Canon 650D single-lens reflex camera phase
The pattern that machine is taken pictures, time for exposure are 2.5s, and focal length of taking pictures is certain.
Fig. 4~Fig. 8 is shown by the fingerprint to different object surfaces, it can be seen that on different object surfaces
The brilliant green fingerprint under dark background is clearly shown, luminous intensity is high, and details is clear, and contrast is high, effectively reduces
Background interference further demonstrates the versatility of process for show of the present invention.
Embodiment 8
A kind of fingerprint manifestation method based on upconverting fluorescent material, comprising the following steps:
1. pressing one piece of oil in paper surface dives fingerprint as test sample；
2. take the NaOH solution 0.5mL drop of 1mol/L on absorbent cotton, then thereon by commercial " 502 " the glue drop of 0.5mL,
It is at once that the paper surface back-off for pressing fingerprint is 30 minutes aobvious in smoking on absorbent cotton；
3. picking the NaYF of the preparation of embodiment 1 with powder brush4:Yb3+,Er3+Powder is gently brushed and is shown on fingerprint in smoked, after 30s
Brush away the powder of smoked aobvious fingerprint excess surface；
4. using 980nm near infrared light fingerprint, evidence obtaining of taking pictures then is carried out to it with camera, time for exposure 2.5s is clapped
It is certain according to focal length.
Fig. 9 is the fingerprint pattern that embodiment 8 obtains, and is to take pictures to obtain by Canon's 650D slr camera.Wherein, left, in,
Right figure is obtained pattern of the blank sheet of paper object of carrying fingerprint under daylight, ultraviolet lamp, 980nm near infrared light respectively.
It can be seen that from the middle figure of Fig. 9, blank sheet of paper generates strong background fluorescence, seriously under the ultraviolet lamp excitation of high-energy
The detection of interference fingerprint.In Fig. 9 right figure, when the near infrared light using low energy is as excitation light source, object blank sheet of paper is not issued
Visible fluorescence, simply and effectively can avoid background fluorescence from interfering, and clearly show the finger for being marked with up-conversion luminescent material
Line pattern, contrast is high, and the details of fingerprint is clear, has further effectively proved the versatility of process for show of the present invention.
For those skilled in the art, without departing from the principle of the present invention, it can also do
Several improvements and modifications out, these modifications and embellishments are also considered to be within the scope of the present invention.
Claims (5)
1. a kind of fingerprint manifestation method based on upconverting fluorescent material, which is characterized in that steps are as follows:
S10) using smoked aobvious agent, and using inorganic base as catalyst, treated after being mixed the object shown carry out it is smoked show, until
There is the smoked aobvious fingerprint of white, wherein the smoked aobvious agent includes at least cyanoacrylate, or produces including at least during smoked aobvious
The reagent of raw cyanoacrylate；The inorganic base is at least one in sodium hydroxide, potassium hydroxide, sodium carbonate or potassium carbonate
Kind；
S20) by upconverting fluorescent material brush, apply or be sprayed on the smoked aobvious fingerprint of white, near-infrared laser irradiation shows fingerprint；Institute
Stating upconverting fluorescent material is upper conversion fluorescent nano particle, and the average grain diameter of the upper conversion fluorescent nano particle is 1.5 μm,
The upper conversion fluorescent nano particle is bar shaped column structure；
Wherein, the upconverting fluorescent material includes NaYF4:Yb3+,Er3, the upconverting fluorescent material NaYF4:Yb3+,Er3's
Preparation method includes the following steps:
1) rare earth element chloride LnCl3(Ln=Y, Yb, Er) and NaCl are dissolved in deionized water according to the concentration of 0.5mol/L respectively
In, NH4F is dissolved in deionized water according to the concentration of 1mol/L, and polyethyleneimine (PEI) is molten according to the concentration of mass fraction 5%
In deionized water；
2) continue to be passed through under conditions of nitrogen into reaction kettle, in the reaction kettle using polytetrafluoroethylene (PTFE) as liner, 5mL is added
PEI solution, 15mL ethyl alcohol, 1mL NaCl solution, 0.77mLYCl3Solution, 0.2mL YbCl3Solution, 0.03mL ErCl3Solution,
Quickly stirring 5min, adds 4mL NH4F obtains reaction solution, continues to stir 15min；
3) reaction kettle is closed, is placed under 200 DEG C of environment and heats for 24 hours, it is cooling after eccentric cleaning 3 times, and by institute after eccentric cleaning
The upconversion fluorescence nano material NaYF for being dissolved in and arriving High Efficiency Luminescence in 5mL deionized water must be precipitated4:Yb3+,Er3+。
2. the fingerprint manifestation method based on upconverting fluorescent material as described in claim 1, which is characterized in that the step
(S10) in, the smoked aobvious agent is 502 glue.
3. the fingerprint manifestation method based on upconverting fluorescent material as described in claim 1, which is characterized in that the step
(S20) in, it is described by upconverting fluorescent material brush, apply or be sprayed on the smoked aobvious fingerprint of white after；20s~60s is waited, is brushed away to aobvious
The luminescent material of the excess surface of existing object；It is irradiated again using near-infrared laser, shows fingerprint.
4. the fingerprint manifestation method based on upconverting fluorescent material as described in claim 1, which is characterized in that the upper conversion
The surface modification of fluorescent material has polyethyleneimine (PEI), disodium ethylene diamine tetraacetate, L-cysteine, thioacetic acid, sulfydryl
Ethyl alcohol, gamma-aminopropyl-triethoxy-silane or PVP K30 salt.
5. a kind of fingerprint manifestation method answering in fingerprint detection based on upconverting fluorescent material as described in claim 1
With.
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| CN106108914B (en) * | 2016-06-22 | 2018-11-27 | 中国科学院上海有机化学研究所 | A kind of agent of modification finger print fumigation display and preparation method based on cyanoacrylate |
| CN106957644B (en) * | 2017-03-13 | 2019-03-19 | 武汉大学 | A kind of fingerprint detection probe based on long-persistence nano material and preparation method thereof and the application in latent fingerprint detection |
| CN107049332A (en) * | 2017-04-12 | 2017-08-18 | 苏州大学 | Application and fingerprint manifestation method of the conjugated polymer fluorescent material in fingerprint manifestation |
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| CN109001169B (en) * | 2018-06-22 | 2020-10-27 | 浙江大学 | Latent fingerprint display and chemical residue detection method based on up-conversion nanoparticles |
| CN110710980A (en) * | 2019-10-09 | 2020-01-21 | 苏州大学 | Latent fingerprint showing cotton piece and application |
| CN111673709B (en) * | 2020-06-30 | 2022-07-08 | 天津大学 | Fingerprint identification robot device based on up-conversion long afterglow material and control method |
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