CN115584259A - Magnetic up-conversion latent fingerprint developer, preparation method thereof and latent fingerprint analysis method - Google Patents
Magnetic up-conversion latent fingerprint developer, preparation method thereof and latent fingerprint analysis method Download PDFInfo
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- 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
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7772—Halogenides
- C09K11/7773—Halogenides with alkali or alkaline earth metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
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- B01F31/80—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
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Abstract
The invention discloses a preparation method of a magnetic up-conversion latent fingerprint developer, which comprises the following steps: under the mechanical stirring state, simultaneously adding the up-conversion luminescent material and the magnetic material turbid liquid into a first solvent to obtain a first mixed solution; after the first mixed solution is sealed and subjected to ultrasonic treatment, adding a ligand connecting agent and an inorganic alkali solution into the first mixed solution to enable the up-conversion luminescent material to be in coordination connection with the magnetic material to obtain a second mixed solution; sealing, heating and stirring the second mixed solution, and then carrying out ultrasonic treatment, centrifugation and drying treatment to obtain the magnetic up-conversion latent fingerprint developer; wherein the luminous wavelength range of the infrared light irradiating the magnetic up-conversion latent fingerprint developer is 507-568 nm. Compared with other fingerprint powder, the magnetic up-conversion latent fingerprint developer obtained by the preparation method has higher contrast, and not only can develop latent fingerprints without damage, but also can effectively solve the problem of background interference and achieve a good fingerprint display result because the developer has magnetic and fluorescent properties.
Description
Technical Field
At least one embodiment of the present invention relates to a latent fingerprint developer, and more particularly, to a magnetic up-conversion latent fingerprint developer, a method of preparing the same, and a method of latent fingerprint analysis.
Background
Latent fingerprints are marks of patterns of friction ridges left under the action of secreted sweat, oily substances and pressure when a finger touches the surface of an object. Latent fingerprints belong to fingerprint marks and have uniqueness and long-term invariance, and the analysis of the latent fingerprints is very important for criminal crime detection work. The fingerprint powder is a simple and convenient latent fingerprint analysis method, and the commonly used fingerprint powder comprises magnetic powder, fluorescent powder and the like. The magnetic powder is used for analyzing the latent fingerprint, and has the advantages that the magnetic fingerprint brush can be used for analyzing the latent fingerprint, the fingerprint does not need to be in physical contact with the fingerprint brush in the process, irreversible damage to the latent fingerprint in the latent fingerprint analysis process is fundamentally avoided, and the magnetic powder can only analyze gray fingerprint patterns and is difficult to cope with interference of dark color and complex background. On the contrary, phosphor powder analyzes out clear obvious latent fingerprint very easily on dark colour and complicated background, no matter daytime night, can all analyze out visible latent fingerprint, however phosphor powder can only utilize traditional physics fingerprint brush to analyze latent fingerprint, the brush need dip in certain phosphor powder and brush in order to guarantee the abundant contact of phosphor powder and fingerprint on the fingerprint surface, this process inevitable can cause certain physics to destroy latent fingerprint, and the phosphor powder residue appears easily in latent fingerprint groove, thereby reduce fingerprint pattern contrast.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a magnetic up-conversion latent fingerprint developer, and the prepared magnetic up-conversion latent fingerprint developer has characteristics of efficient up-conversion luminescence and magnetism, and can realize efficient identification of latent fingerprints without physical damage to the latent fingerprints.
The invention provides a preparation method of a magnetic up-conversion latent fingerprint developer, which comprises the following steps: simultaneously adding the up-conversion luminescent material and the magnetic material suspension into a first solvent under a mechanical stirring state to obtain a first mixed solution; sealing and ultrasonically treating the first mixed solution, and adding a ligand connecting agent and an inorganic alkali solution into the first mixed solution to coordinate and connect the up-conversion luminescent material and the magnetic material to obtain a second mixed solution; sealing, heating and stirring the second mixed solution, and performing ultrasonic treatment, centrifugation and drying treatment to obtain the magnetic upconversion latent fingerprint developer; wherein the luminous wavelength range of the magnetic up-conversion latent fingerprint developer under the irradiation of infrared light is 507-568 nm.
The invention also provides a magnetic up-conversion latent fingerprint developer obtained by the preparation method.
The invention also provides a latent fingerprint analysis method using the magnetic up-conversion latent fingerprint developer, which comprises the following steps: attracting the magnetic up-conversion latent fingerprint developer by using a magnetic fingerprint brush, and dripping the magnetic up-conversion latent fingerprint developer on the surface of the substrate deposited with latent fingerprints; after repeated dripping for a plurality of times, removing the magnetic upconversion latent fingerprint developer remained in the groove area of the latent fingerprint, so that the magnetic upconversion latent fingerprint developer is distributed along the extending direction of the ridge of the latent fingerprint; and irradiating the surface of the base material by adopting near-infrared exciting light to enable the magnetic up-conversion latent fingerprint developer to excite green light with the light-emitting wavelength range of 507-568 nm; the image of the latent fingerprint is collected by a CCD image sensor, and is distinguished by utilizing the upconversion luminescence effect of the magnetic upconversion latent fingerprint developer.
According to the preparation method of the magnetic up-conversion latent fingerprint developer provided by the embodiment of the invention, the prepared magnetic up-conversion latent fingerprint developer has the characteristics of efficient up-conversion luminescence and magnetism, can realize efficient identification of latent fingerprints without causing physical damage to the latent fingerprints, and can effectively solve the influence of background interference on latent fingerprint analysis.
According to the magnetic up-conversion latent fingerprint developer provided by the embodiment of the invention, green light with the wavelength range of 507-568 nm can be excited. Because human eyes are sensitive to green light, the quantum efficiency of the CCD image sensor to light with the wavelength range of 500-700 nm is high, and when the prepared magnetically-converted latent fingerprint developing agent is applied to latent fingerprint analysis, a good visual effect and an imaging effect can be realized.
Drawings
Fig. 1 is a flow chart of a method of preparing a magnetic up-conversion latent fingerprint developer according to an embodiment of the present invention;
FIG. 2 is a schematic diagram illustrating an implementation of a latent fingerprint analysis method according to an embodiment of the present invention;
3 (a) -3 (b) are pictorial illustrations of a magnetic fingerprint brush and laser in accordance with an embodiment of the present invention;
4 (a) -4 (b) are luminescence spectra of magnetic up-conversion latent fingerprint developers according to embodiments of the present invention;
FIG. 5 (a) shows Fe 3 O 4 The hysteresis loop of (1); 5 (b) -5 (c) are hysteresis loops of a magnetically up-converted latent fingerprint developer according to an embodiment of the present invention;
FIG. 6 is a diagram of magnetically attracted objects of a magnetically upconverting latent fingerprint developer according to an embodiment of the present invention;
FIG. 7 is a pictorial representation of a magnetic up-conversion latent fingerprint developer performing latent fingerprint analysis on a surface of a metal in accordance with an embodiment of the present invention;
FIG. 8 is a pictorial representation of a magnetic up-conversion latent fingerprint developer performing latent fingerprint analysis on a surface of an impermeable substrate in accordance with an embodiment of the present invention;
FIG. 9 is a pictorial representation of a magnetic up-conversion latent fingerprint developer performing latent fingerprint analysis on a surface of a permeable substrate in accordance with an embodiment of the present invention; and
FIG. 10 is a pictorial representation of a magnetic up-conversion latent fingerprint developer according to an embodiment of the present invention performing latent fingerprint analysis on a surface of a substrate having a dark background.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the accompanying drawings in combination with the embodiments. This invention may, however, be embodied in different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. In the drawings, the size and relative sizes of layers and regions may be exaggerated for clarity, and like reference numerals designate like elements throughout.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The terms "comprises," "comprising," and the like, as used herein, specify the presence of stated features, steps, operations, and/or components, but do not preclude the presence or addition of one or more other features, steps, operations, or components.
The invention provides a preparation method of a magnetic up-conversion latent fingerprint developer and a latent fingerprint analysis method.
Fig. 1 is a flow chart of a method of making a magnetic up-conversion latent fingerprint developer according to an embodiment of the present invention.
According to an exemplary embodiment of the present invention, there is provided a method of preparing a magnetic up-conversion latent fingerprint developer, as shown in fig. 1, including: and S01 to S03.
In step S01, the up-conversion luminescent material and the magnetic material suspension are simultaneously added to the first solvent under the mechanical stirring state, so as to obtain a first mixed solution.
According to the embodiment of the invention, the up-conversion luminescent material is hexagonal-phase nano NaLnF doped with rare earth ions Ln 4 Particles in which the rare earth ions Ln comprise the sensitizer ions Yb 3+ And an activator ion selected from Gd 3+ 、Nd 3+ 、Y 3+ 、Er 3+ 、Tm 3+ 、Ho 3+ One or more of (a). For example, the rare earth ion Ln may be Yb 3+ And Er 3+ (ii) a Wherein, er 3+ As an activator ion of the up-conversion luminescent material, the active material is easily excited by infrared light with the wavelength of 980nm, 915nm or 808 nm; yb (Yb) 3+ As a sensitizer ion of the up-conversion luminescent material, the up-conversion luminescent material is excited to emit light with the wavelength range of 507-568 nm. The first solvent may be n-propanol.
According to the embodiment of the present invention, the magnetic material is dispersed in the second solvent to obtain the magnetic material suspension. The magnetic material is a ferromagnetic material, and may be cubic phase Fe 3 O 4 、γ-Fe 2 O 3 Or other materials having ferromagnetic properties. The second solvent may be an ethanol solution.
It should be noted that, if the particle size of the up-conversion luminescent material is too small, the crystallinity is poor, the number of defects is large, and the luminescent efficiency is low; the particle size of the up-conversion luminescent material is too large, so that the number of effective luminescent units is reduced, and the luminous efficiency is poor; the particle size of the up-conversion luminescent material is 20nm to 400nm to achieve higher luminous efficiency, for example, the particle size of the up-conversion luminescent material may be 20nm, 30nm, 40nm, 50nm, 60nm, 70nm, 80nm, 90nm, 100nm, 150nm, 200nm, 250nm, 300nm, 350nm, 400nm.
It should be noted that, if the particle size of the magnetic material is too small, many defects and poor magnetic properties are caused; the particle size of the magnetic material is too large, making it difficult for the magnetic material to attach to the surface of the upconversion luminescent material particle through a ligand linker. The particle diameter of the magnetic material may be 20nm to 200nm, and may be, for example, 20nm, 30nm, 40nm, 50nm, 60nm, 70nm, 80nm, 90nm, 100nm, 150nm, 200nm, 250nm, 300nm, 350nm, or 400nm.
According to the embodiment of the invention, the mass ratio of the up-conversion luminescent material to the magnetic material is (1-10): 1, for example, may be 1: 1. 2: 1. 3: 1. 3.5: 1. 4:1. 4.5: 1.5: 1. 6: 1. 7: 1. 8: 1. 9: 1. 10:1.
according to an embodiment of the invention, the rotation speed of the mechanical stirring may be 200 to 600r/min, for example 200r/min, 300r/min, 400r/min, 500r/min, 600r/min.
According to the embodiment of the invention, the particle size of the NaLnF is 1-100 nm 4 The preparation process of the up-conversion luminescent material comprises the following steps: in a 50ml reactor, 1mmol of a rare earth ion salt (LnCl) 3 ) Adding into 4mL oleic acid and 16mL octadecene, heating to 160 deg.C to dissolve to obtain yellow solution, cooling to room temperature, adding 10mL methanol (containing 2.5mmol NaOH and 4mmol NH) 4 F) Stirring for 30min, heating to 100 ℃, keeping for 20min, removing methanol, heating to 300 ℃, reacting for 1.5h, and finally using a mixture of cyclohexane and ethanol in a volume ratio of 1:1 washing off residual organic matters on the surface of the sample, and collecting the final NaLnF by centrifugation 4 Up-conversion of the luminescent product.
According to the embodiment of the invention, the NaLnF with the particle size of 80-400 nm 4 The preparation process of the up-conversion luminescent material comprises the following steps: in the reactor, 1mmoL of rare earth ion trifluoroacetate (Ln (CF) is proportioned 3 COO) 3 ) And sodium trifluoroacetate are added into 6mL of oleic acid, heated, stirred and dissolved, 12mL of octadecene is added as an organic solvent, the mixture is heated to 330 ℃ after being vacuumized, the reaction is carried out for 40 to 90min, and finally cyclohexane and ethanol are used according to the volume ratio of 1:1 to wash off residual organic matter on the surface of the sample, and collecting the final NaLnF by centrifugation 4 Up-conversion of the luminescent product.
In step S02, after the first mixed solution is sealed and subjected to ultrasonic treatment, a ligand linker and an inorganic alkali solution are added to the first mixed solution, so that the up-conversion luminescent material is coordinately linked with the magnetic material, and a second mixed solution is obtained.
According to an embodiment of the present invention, the ligand linker is a ligand that can be used to connect the convertible luminescent material and the magnetic material, and may be, for example, ethyl orthosilicate. The inorganic alkali solution is suitable for improving coordination environment, and the inorganic alkali solution can be one or more of sodium hydroxide and potassium hydroxide.
According to embodiments of the present invention, the mass ratio of the up-conversion luminescent material to the ligand linker may be, but is not limited to, (1 to 4): 1; for example, it may be 1: 1. 1.5: 1. 2: 1. 3: 1. 4:1.
according to the embodiment of the invention, the mass ratio of the conversion luminescent material to the inorganic base solution is (2800 to 4000): 1, for example, may be 2800: 1. 2900: 1. 3000: 1. 3100: 1. 3200: 1. 3300: 1. 3400: 1. 3500: 1. 3600: 1. 3700: 1. 3800: 1. 3900: 1. 4000:1.
according to the embodiment of the invention, the time period of the sealing and ultrasonic treatment of the first mixed liquid is 0.5-1 h, for example, 0.5h, 0.6h, 0.7h, 0.8h, 0.9h and 1h.
And S03, sealing, heating and stirring the second mixed solution, and then carrying out ultrasonic treatment, centrifugation and drying treatment to obtain the magnetic up-conversion latent fingerprint developer.
According to the embodiment of the present invention, the heating temperature for sealing, heating and stirring the second mixed solution is 60 to 80 ℃, for example, 60 ℃, 65 ℃, 70 ℃, 75 ℃ and 80 ℃. The heating and stirring time is 15 to 21 hours, and for example, 15 hours, 16 hours, 17 hours, 18 hours, 19 hours, 20 hours and 21 hours.
According to an embodiment of the present invention, the rotation speed of the above-mentioned centrifugation process is 8000rpm/min.
According to the embodiment of the invention, the size of the prepared magnetic upconversion latent fingerprint developer is detected by a transmission electron microscope, and the size of the prepared magnetic upconversion latent fingerprint developer can be 50nm.
According to the embodiment of the invention, the steady-state-transient fluorescence spectrometer can be used for monitoring the intensity change of the converted luminescence on the developer prepared by the method.
The invention also provides a magnetic up-conversion latent fingerprint developer obtained by the preparation method; wherein the luminous wavelength range of the magnetic up-conversion latent fingerprint developer under the irradiation of infrared light is 507-568 nm.
Human eyes are sensitive to green light, and a CCD image sensor (Charge coupled Device) in a camera has high quantum efficiency for light having a wavelength range of 500 to 700 nm. By Yb 3+ The magnetic upconversion latent fingerprint developer is used as sensitizer ions of an upconversion luminescent material to enable the upconversion luminescent material to excite green light with the wavelength range of 507-568 nm, and when the prepared magnetic upconversion latent fingerprint developer is applied to latent fingerprint analysis, good visual effect and imaging effect can be achieved.
Fig. 2 is a schematic diagram illustrating an implementation of a method for analyzing latent fingerprints in a magnetic up-conversion latent fingerprint developer according to an embodiment of the present invention. 3 (a) -3 (b) are pictorial diagrams of a magnetic fingerprint brush and a laser in accordance with an embodiment of the present invention.
The present invention also provides a latent fingerprint analysis method using the above-mentioned magnetically up-converting latent fingerprint developer, as shown in fig. 2 and fig. 3 (a) to 3 (b), including:
attracting the magnetic up-conversion latent fingerprint developer by using a magnetic fingerprint brush, and dripping the magnetic up-conversion latent fingerprint developer on the surface of the substrate deposited with latent fingerprints; after repeated dripping for a plurality of times, removing the magnetic upconversion latent fingerprint developer remained in the groove area of the latent fingerprint, so that the magnetic upconversion latent fingerprint developer is distributed along the extending direction of the ridge of the latent fingerprint; irradiating the surface of the base material by near-infrared excitation light emitted by a laser to excite the magnetic upconversion latent fingerprint developer to emit green light with the light-emitting wavelength range of 507-568 nm; the images of the latent fingerprints are collected by a CCD image sensor, and are distinguished by the up-conversion luminescence effect of the magnetic up-conversion latent fingerprint developer.
It should be noted that, the magnetic up-conversion latent fingerprint developer is dropped on the surface of the substrate deposited with latent fingerprints, the developer can be adsorbed on the latent fingerprints formed by the oily substances on the surface of the substrate, and the part of the surface of the substrate not covered with the oily substances can not be adsorbed with the developer and can be attracted by the magnetic fingerprint brush, so that the developer remaining in the groove area of the latent fingerprints can be removed, and the magnetic up-conversion latent fingerprint developer is distributed along the extending direction of the ridges of the latent fingerprints.
According to embodiments of the present invention, the substrate may be an impermeable substrate comprising one or more of glass, acrylic, plastic, ceramic, and metal; the substrate may be a permeable substrate comprising one or more of rubber, paper, wood; the base material can also be base materials with dark color complex backgrounds, such as playing cards, voucher formed with two-dimensional codes and the like.
According to embodiments of the present invention, the wavelength of the near infrared excitation light may be one or more of 980nm, 915nm, 808 nm.
According to the embodiment of the invention, the fingerprint texture cannot be damaged based on the physical adsorption effect of the magnetically up-converted latent fingerprint developer powder, the biological information of the fingerprint can be stored to the maximum extent, meanwhile, the developer powder which is not adsorbed in the groove area of the fingerprint can be removed by using the fingerprint brush, and the clear and high-resolution latent fingerprint development can be easily obtained.
According to the embodiment of the invention, the up-conversion luminescence has the advantages of high contrast, high resolution, excellent stability, narrow emission band, long luminescence life and the like, and meanwhile, the corresponding near-infrared excitation light has strong secrecy in practical use and is not interfered by environmental fluorescence, so that the latent fingerprint analysis method provided by the embodiment of the invention can efficiently identify the latent fingerprint, and is particularly suitable for identifying the latent fingerprint on a substrate with large background interference and deep color.
According to the magnetic up-conversion latent fingerprint developer provided by the embodiment of the invention, the magnetic up-conversion latent fingerprint developer has the characteristic of high-efficiency up-conversion luminescence and magnetism, can realize high-efficiency identification of latent fingerprints without causing physical damage to the latent fingerprints, and can effectively solve the influence of background interference on latent fingerprint analysis.
The magnetic up-conversion latent fingerprint developer provided by the embodiment of the invention can excite green light with the wavelength range of 507-568 nm. Because human eyes are sensitive to green light, the quantum efficiency of the CCD image sensor to light with the wavelength range of 500-700 nm is high, and when the prepared magnetically up-converted latent fingerprint developer is applied to latent fingerprint analysis, a good visual effect and an imaging effect can be realized.
The preparation method of the magnetic up-conversion latent fingerprint developer provided by the embodiment of the invention has the advantages of simple operation, short period, small synthesis difficulty, easy regulation and control and the like, has low process requirement and high success rate, and has advantages in future large-scale and industrialization aspects.
The following schematically illustrates the preparation process of the magnetic up-conversion latent fingerprint developer. It should be noted that the illustrated embodiments are only examples of the present invention, and should not limit the scope of the present invention.
It should be noted that all the raw materials used in the present invention are not particularly limited in their sources and are commercially available; meanwhile, the purity of the product is not particularly limited, and the product is analytically pure. There is also no particular limitation on the reaction or detection apparatus or device used.
Example 1
In a reactor, 1mmoL of rare earth ion trifluoroacetate (0.78 mmoL Gd (CF) is proportioned 3 COO) 3 ，0.2mmoL Yb(CF 3 COO) 3 ，0.02mmoL Er(CF 3 COO) 3 ) And 1.46mL of trifluoroacetic acid are added into 6.4mL of oleic acid, heated, stirred and dissolved, 12.8mL of octadecene is added as an organic solvent, after 20min of vacuum pumping, the mixture is heated to 300 ℃ and reacts for 1h, and finally a mixed solvent of cyclohexane and ethanol in a volume ratio of 1 4 The Yb and Er up-conversion luminescent material is characterized by a transmission electron microscope, and the particle size of the prepared up-conversion luminescent material is 60nm.
A500 mL round bottom flask was charged with 72mL n-propanol, stirred using a mechanical stir plate with a Teflon stir bar, while adding 72mg NaGdF 4 And 20mL of 1mg/mL Fe 3 O 4 (the grain diameter is 50 nm) ethanol suspension, wherein the mass ratio of the up-conversion luminescent material to the magnetic material is 4:1. ultrasonic dispersing for 30min under sealed condition, and adding 360. Mu.L of 2M NaOH solution and 60. Mu.L of TEOS. Using a mechanical stirring table with a sealing plug, stirring was carried out in a 70 ℃ oil bath for 18h in a sealed state. Transferring the product to a 50mL centrifuge tube after the reaction is finished, adding pure water and absolute ethyl alcohol for centrifugation (8000 r/min,3 min), repeatedly centrifuging and washing for three times, and finally performing vacuum drying treatment to obtain NaGdF 4 :Yb,Er-Fe 3 O 4 A composite nanomaterial.
The prepared magnetic up-conversion latent fingerprint developer is used for testing the luminous intensity through a steady-state-transient luminous spectrometer. The detection conditions of the luminescence spectrum are as follows: JY Fluorolog-3-Tou,980nm exciting light, power is 192.4mW cm -2 The scanning range is 300-750 nm.
Fig. 4 (a) -4 (b) are luminescence spectra of the magnetic up-conversion latent fingerprint developer according to the embodiment of the present invention.
Referring to fig. 4 (a), the prepared magnetic up-conversion latent fingerprint developer can emit green visible light under the irradiation of 980nm excitation light. When NaGdF 4 Yb, er and Fe 3 O 4 When the mass ratio of (2) to (3.5) is 1, the luminous intensity is weak; when NaGdF 4 Yb, er and Fe 3 O 4 The mass ratio of (1) to (4.0). Referring to fig. 4 (b), the sealing, heating and stirring periods of the second mixed solution were set to 15h, 18h, and 21h, respectively, and magnetic up-conversion latent fingerprint developers having a large luminous intensity were prepared.
FIG. 5 (a) shows Fe 3 O 4 The hysteresis loop of (1); FIG. 5 (b) shows that when the time period of heating and stirring is set to 18h, the prepared magnetic upconversion latent fingerprint developer NaGdF 4 :Yb,Er-Fe 3 O 4 A hysteresis loop of (1); FIG. 5 (c) shows NaGdF 4 Yb, er and Fe 3 O 4 When the mass ratio of (1) is 4.0 4 :Yb,Er-Fe 3 O 4 A hysteresis loop of (c).
Referring to FIGS. 5 (a) -5 (c), the hysteresis loop is plotted by a hysteresis loop meter, in comparison to Fe 3 O 4 The saturation magnetization of the prepared magnetic up-conversion latent fingerprint developer is reduced to a certain extent, but still has the same value as that of Fe 3 O 4 The saturation magnetization of (a) is maintained at the same order of magnitude level.
FIG. 6 is a diagram of magnetically attracted objects of a magnetically upconverting latent fingerprint developer according to an embodiment of the invention. Referring to fig. 6, the magnetic up-conversion latent fingerprint developer prepared has magnetism.
The latent fingerprint analysis process by using the magnetic up-conversion latent fingerprint developer comprises the following steps: the latent fingerprint is first deposited by pressing a fingertip against a smooth metal substrate. Sucking approximately 20mg NaGdF with a magnetic fingerprint brush 4 :Yb,Er-Fe 3 O 4 And (3) moving the latent fingerprint developer to the upper part of the fingerprint, closing the fingerprint brush magnet, enabling the developer to fall off, covering the surface of the fingerprint, opening the magnet rod again, enabling the developer not attached to the surface of the fingerprint to be attracted again, repeating the attraction and falling process, and then blowing gently to remove the redundant powder between the fingerprint grooves. And (3) irradiating the fingerprint image fixed by the latent fingerprint developer by using a 980nm infrared lamp to enable the developer to emit green light so as to analyze the latent fingerprint.
FIG. 7 is a pictorial representation of a magnetic up-conversion latent fingerprint developer performing latent fingerprint analysis on a surface of a metal in accordance with an embodiment of the present invention. Referring to fig. 7, the prepared magnetic up-conversion latent fingerprint developing agent can realize the analysis of the latent fingerprint deposited on the metal surface.
Example 2
The specific process is the same as that of example 1, and the rare earth ion Er doped in the latent fingerprint developing agent of example 1 3+ Change to Tm 3+ Preparing to obtain NaGdF 4 :Yb,Tm-Fe 3 O 4 And irradiating the fingerprint image fixed by the latent fingerprint developer by using a 980nm infrared lamp to emit blue light so as to analyze the latent fingerprint.
Example 3
The specific process is the same as that of the example 1, and the doped rare earth ion Nd is added into the latent fingerprint developing agent of the example 1 3+ To prepare NaGdF 4 :Nd,Yb,Er-Fe 3 O 4 Use ofThe fingerprint image fixed by the latent fingerprint developer is irradiated by an infrared lamp with wavelength of 808nm to emit green light so as to analyze the latent fingerprint.
Examples 4 to 7
The specific process is the same as that of example 1, and the smooth metal substrate is replaced by non-permeable substrates such as glass, acrylic, plastic, ceramic and the like.
FIG. 8 is a pictorial representation of a magnetic up-conversion latent fingerprint developer according to an embodiment of the present invention performing latent fingerprint analysis on a surface of an impermeable substrate. Referring to fig. 8, the prepared magnetic up-conversion latent fingerprint developing agent can realize analysis of latent fingerprints deposited on the surface of an impermeable substrate.
Examples 8 to 10
The procedure was the same as in example 1, except that the smooth metal substrate was replaced with a permeable substrate such as rubber, paper, or wood.
FIG. 9 is a pictorial representation of a magnetic up-conversion latent fingerprint developer according to an embodiment of the present invention performing latent fingerprint analysis on a surface of a permeable substrate. Referring to fig. 9, the prepared magnetic up-conversion latent fingerprint developing agent can realize analysis of latent fingerprints deposited on the surface of a permeable substrate.
Examples 11 to 12
The specific process is the same as that of the embodiment 1, and the smooth metal substrate is respectively replaced by the substrate with dark color complex background, such as playing cards, gift certificates with two-dimensional codes and the like.
FIG. 10 is a pictorial representation of a magnetic up-conversion latent fingerprint developer according to an embodiment of the invention performing latent fingerprint analysis on a surface of a substrate having a dark background. Referring to fig. 10, the prepared magnetic up-conversion latent fingerprint developer can realize the analysis of latent fingerprints deposited on the surface of a substrate having a dark complex background.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a magnetic up-conversion latent fingerprint developer is characterized by comprising the following steps:
under the mechanical stirring state, simultaneously adding the up-conversion luminescent material and the magnetic material turbid liquid into a first solvent to obtain a first mixed solution;
after the first mixed solution is sealed and subjected to ultrasonic treatment, adding a ligand connecting agent and an inorganic alkali solution into the first mixed solution to enable the up-conversion luminescent material to be in coordination connection with the magnetic material, so as to obtain a second mixed solution; and
sealing, heating and stirring the second mixed solution, and then carrying out ultrasonic treatment, centrifugation and drying treatment to obtain a magnetic up-conversion latent fingerprint developer;
wherein the luminous wavelength range of the magnetic up-conversion latent fingerprint developer under the irradiation of infrared light is 507-568 nm.
2. The method of claim 1, wherein the upconversion luminescent material is NaLnF doped with rare earth ion Ln 4 The nano-material is prepared from a nano-material,
the rare earth ions Ln comprise Yb 3+ And is selected from Gd 3+ 、Nd 3+ 、Y 3+ 、Er 3+ 、Tm 3+ 、Ho 3+ One or more of;
the up-conversion luminescent material is granular, and the grain diameter of the granules is 20 nm-400 nm.
3. The production method according to claim 1, wherein a magnetic material is dispersed in a second solvent to obtain the magnetic material suspension;
the magnetic material is a ferromagnetic material;
preferably, the magnetic material comprises cubic phase Fe 3 O 4 ；
The magnetic material is granular, and the grain diameter of the granules is 20 nm-200 nm.
4. The method according to claim 1, wherein the ligand linker is tetraethoxysilane or other material suitable for coordinately linking the up-conversion luminescent material and the magnetic material;
the inorganic alkali solution comprises one or more of sodium hydroxide and potassium hydroxide.
5. The preparation method according to claim 1, wherein the first mixed solution is sealed and subjected to ultrasonic treatment for 0.5 to 1 hour;
and sealing the second mixed solution, heating and stirring at the heating temperature of 60-80 ℃, wherein the heating and stirring time is 15-21 h.
6. The method according to claim 1, wherein the mass ratio of the up-conversion luminescent material to the magnetic material is (1 to 10): 1;
the mass ratio of the up-conversion luminescent material to the ligand linker is (1 to 4): 1;
the mass ratio of the up-conversion luminescent material to the inorganic alkali solution is (2800 to 4000): 1.
7. a magnetic up-conversion latent fingerprint developer obtained by the production method according to any one of claims 1 to 6.
8. A latent fingerprint analysis method using the magnetically up-converting latent fingerprint developer according to claim 7, comprising:
attracting the magnetic up-conversion latent fingerprint developer by using a magnetic fingerprint brush, and dripping the magnetic up-conversion latent fingerprint developer on the surface of the substrate deposited with latent fingerprints;
repeatedly dripping for multiple times, and removing the magnetic up-conversion latent fingerprint developer remaining in the groove area of the latent fingerprint so that the magnetic up-conversion latent fingerprint developer is distributed along the extending direction of the ridge of the latent fingerprint; and
irradiating the surface of the base material by adopting near-infrared excitation light to enable the magnetic up-conversion latent fingerprint developer to excite green light with the light-emitting wavelength range of 507-568 nm;
and collecting the image of the latent fingerprint by using a CCD image sensor, and distinguishing the image of the latent fingerprint by using the up-conversion luminescence effect of the magnetic up-conversion latent fingerprint developer.
9. The latent fingerprint analysis method of claim 8,
the substrate is a non-permeable substrate comprising one or more of glass, acrylic, plastic, ceramic, and metal;
the substrate is a permeable substrate, and the permeable substrate comprises one or more of rubber, paper and wood;
the substrate is a substrate with a dark background.
10. The latent fingerprint analysis method of claim 8,
the wavelength of the near infrared exciting light comprises one or more of 980nm, 915nm and 808 nm.
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