CN115584259B - 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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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
- B01F31/80—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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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, the up-conversion luminescent material and the magnetic material suspension are added into the first solvent at the same time to obtain a first mixed solution; sealing and ultrasonic treating the first mixed liquid, and adding a ligand connecting agent and an inorganic alkali solution into the first mixed liquid to coordinate and connect the up-conversion luminescent material and the magnetic material to obtain a second mixed liquid; sealing, heating and stirring the second mixed liquid, and performing ultrasonic treatment, centrifugation and drying treatment to obtain the magnetic up-conversion latent fingerprint developer; wherein, the light-emitting wavelength range of the infrared light irradiation magnetism up-conversion latent fingerprint developer is 507-568 nm. Compared with other fingerprint powders, the magnetic up-conversion latent fingerprint developer obtained by the preparation method has higher contrast, and can not only nondestructively develop latent fingerprints, but also effectively solve the problem of background interference due to the magnetic property and fluorescence property of the developer, so that a good fingerprint display result is achieved.
Description
Technical Field
At least one embodiment of the invention relates to a latent fingerprint developer, in particular to a magnetic up-conversion latent fingerprint developer, a preparation method thereof and a latent fingerprint analysis method.
Background
Latent fingerprints refer to marks of friction ridge patterns left under the action of secreted sweat, oily substances and pressure when a finger contacts the surface of an object. The latent fingerprint belongs to one of fingerprint marks, has uniqueness and long-term invariance, and is very important for criminal crime forensic work. The fingerprint powder is a simple and convenient method for analyzing the latent fingerprints, and the common fingerprint powder comprises magnetic powder, fluorescent powder and the like. The magnetic powder is used for analyzing the latent fingerprints, and has the advantages that the magnetic fingerprint brush can be utilized to conduct the latent fingerprint analysis process, the fingerprints do not need to be in physical contact with the fingerprint brush in the process, irreversible damage to the latent fingerprints in the latent fingerprint analysis process is fundamentally avoided, however, the magnetic powder can only analyze gray fingerprint patterns, and the interference of dark colors and complex backgrounds is difficult to deal with. In contrast, the fluorescent powder can easily analyze clear and obvious latent fingerprints on dark colors and complex backgrounds, and can analyze visible latent fingerprints no matter day and night, however, the fluorescent powder can only analyze the latent fingerprints by using the traditional physical fingerprint hairbrush, the hairbrush needs to be dipped with certain fluorescent powder to brush on the surface of the fingerprints so as to ensure that the fluorescent powder is fully contacted with the fingerprints, the process inevitably causes certain physical damage to the latent fingerprints, and fluorescent powder residues are easy to appear at the grooves of the latent fingerprints, so that the contrast of fingerprint patterns is reduced.
Disclosure of Invention
In view of the above, the invention provides a preparation method of a magnetic up-conversion latent fingerprint developer, and the prepared magnetic up-conversion latent fingerprint developer has high-efficiency up-conversion luminescence characteristic and magnetism, and can realize high-efficiency identification of the latent fingerprint under the condition of not causing physical damage to the latent fingerprint.
The invention provides a preparation method of a magnetic up-conversion latent fingerprint developer, which comprises the following steps: under the mechanical stirring state, the up-conversion luminescent material and the magnetic material suspension are added into the first solvent at the same time to obtain a first mixed solution; sealing and ultrasonic treating the first mixed liquid, and adding a ligand connecting agent and an inorganic alkali solution into the first mixed liquid to coordinate and connect the up-conversion luminescent material and the magnetic material to obtain a second mixed liquid; sealing, heating and stirring the second mixed liquid, and performing ultrasonic treatment, centrifugation and drying treatment to obtain the magnetic up-conversion latent fingerprint developer; wherein, the luminescence 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 utilizing the magnetic fingerprint brush, and dripping the magnetic up-conversion latent fingerprint developer on the surface of the substrate deposited with the latent fingerprint; after repeated dripping for a plurality of times, removing the magnetic up-conversion latent fingerprint developer remained 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 ridges of the latent fingerprint; and irradiating the surface of the substrate with near infrared excitation light to excite the magnetic up-conversion latent fingerprint developer to emit green light with wavelength range of 507-568 nm; the CCD image sensor is used for collecting the image of the latent fingerprint, and the magnetic up-conversion luminescence of the developer is used for resolving the image of the latent fingerprint.
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 characteristic of high-efficiency up-conversion luminescence and magnetism, can realize high-efficiency identification of the latent fingerprint without physical damage to the latent fingerprint, and can effectively solve the influence of background interference on the analysis of the latent fingerprint.
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 CCD image sensor has high quantum efficiency to light with the wavelength range of 500-700 nm, and when the prepared magnetically transformed latent fingerprint developer is applied to latent fingerprint analysis, good visual effect and 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 invention;
FIG. 2 is a schematic diagram illustrating a latent fingerprint analysis method according to an embodiment of the invention;
FIGS. 3 (a) -3 (b) are physical diagrams of a magnetic fingerprint brush and a laser according to embodiments of the present invention;
FIGS. 4 (a) -4 (b) are luminescence spectra of magnetic up-conversion latent fingerprint developers according to embodiments of the present invention;
FIG. 5 (a) is Fe 3 O 4 Hysteresis loop of (2); FIGS. 5 (b) -5 (c) are hysteresis loops of a magnetic up-conversion latent fingerprint developer according to embodiments of the present invention;
FIG. 6 is a magnetic attraction object diagram of a magnetic up-conversion latent fingerprint developer according to an embodiment of the invention;
FIG. 7 is a physical diagram of a magnetic up-conversion latent fingerprint developer for latent fingerprint analysis on a metal surface according to an embodiment of the invention;
FIG. 8 is a physical diagram of a magnetic up-conversion latent fingerprint developer performing latent fingerprint analysis on a surface of an impermeable substrate according to an embodiment of the invention;
FIG. 9 is a physical diagram of a magnetic up-conversion latent fingerprint developer performing latent fingerprint analysis on a surface of a permeable substrate according to an embodiment of the present invention; and
fig. 10 is a physical diagram of a magnetic up-conversion latent fingerprint developer according to an embodiment of the invention for latent fingerprint analysis on a surface of a substrate having a dark background.
Detailed Description
The present invention will be further described in detail below with reference to specific embodiments and with reference to the accompanying drawings, in order to make the objects, technical solutions and advantages of the present invention more apparent. 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 of layers and regions, as well as the relative sizes, may be exaggerated for the same 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/or 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, which are simple and easy to operate, the prepared developer has stable property, strong up-conversion luminescence, and simultaneously has magnetism, and the latent fingerprint analysis can be simply, quickly and clearly carried out through the combined action of a magnetic fingerprint brush and near infrared excitation light.
Fig. 1 is a flowchart of a method of preparing 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 for preparing a magnetic up-conversion latent fingerprint developer, as shown in fig. 1, including: steps S01 to S03.
In step S01, the up-conversion luminescent material and the magnetic material suspension are simultaneously added into the first solvent under the mechanical stirring state to obtain a first mixed solution.
According to an embodiment of the invention, the up-conversion luminescent material is hexagonal phase nano NaLnF doped with rare earth ions Ln 4 Particles, wherein the rare earth ions Ln comprise 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 the following. For example, the rare earth ion Ln can be Yb 3+ And Er 3+ The method comprises the steps of carrying out a first treatment on the surface of the Wherein Er is as follows 3+ As activator ion of up-conversion luminescent material, it is easy to be excited by infrared light with wavelength of 980nm, 915nm or 808nmSending out; yb 3+ As sensitizer ions of the up-conversion luminescent material, the up-conversion luminescent material is excited to emit light with a wavelength ranging from 507 to 568nm. The first solvent may be n-propanol.
According to an embodiment of the present invention, a magnetic material is dispersed in a second solvent to obtain a magnetic material suspension. The magnetic material is a material with ferromagnetism, for example, can be cubic phase Fe 3 O 4 、γ-Fe 2 O 3 Or other material having ferromagnetic properties. The second solvent may be an ethanol solution.
It should be noted that, too small particle size of the up-conversion luminescent material may result in poor crystallinity and many defects, resulting in low luminous efficiency; the particle size of the up-conversion luminescent material is too large, and the effective luminescent units are reduced, so that 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, too small particle size of the magnetic material may cause many defects and poor magnetic properties; the excessively large particle size of the magnetic material may make it difficult for the magnetic material to be connected to the surface of the up-conversion luminescent material particles through the ligand-connecting agent. The particle size of the magnetic material may be 20nm to 200nm, for example, 20nm, 30nm, 40nm, 50nm, 60nm, 70nm, 80nm, 90nm, 100nm, 150nm, 200nm, 250nm, 300nm, 350nm, 400nm.
According to an embodiment of the present invention, the mass ratio of the up-conversion luminescent material to the magnetic material is (1 to 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 can be 200-600 r/min, for example, 200r/min, 300r/min, 400r/min, 500r/min and 600r/min.
According to an embodiment of the present invention, naLnF having a particle size of 1 to 100nm 4 Up-conversionThe preparation process of the luminescent material comprises the following steps: in a 50ml reactor, 1mmol of rare earth ion salt (LnCl 3 ) Adding into 4mL oleic acid and 16mL octadecene, heating to 160deg.C to dissolve to yellow solution, cooling to room temperature, adding 10mL methanol (containing 2.5mmol NaOH and 4mmol NH) 4 F) Stirring for 30min, heating to 100 ℃, maintaining for 20min, removing methanol, heating to 300 ℃ finally, reacting for 1.5h, and finally using cyclohexane and ethanol in a volume ratio of 1:1, washing the residual organic matters on the surface of the sample by using the mixed solvent, and collecting the final NaLnF by centrifugation 4 Up-converting the luminescent product.
According to an embodiment of the present invention, naLnF having a particle size of 80 to 400nm 4 The preparation process of the up-conversion luminescent material comprises the following steps: in the reactor, 1mmoL of rare earth ion trifluoroacetate salt (Ln (CF) 3 COO) 3 ) And sodium trifluoroacetate is added into 6mL of oleic acid, heated, stirred and dissolved, 12mL of octadecene is added as an organic solvent, the mixture is vacuumized and heated to 330 ℃ for reaction for 40-90 min, and finally cyclohexane and ethanol are used in a volume ratio of 1:1, washing the residual organic matters on the surface of the sample by using the mixed solvent, and collecting the final NaLnF by centrifugation 4 Up-converting the luminescent product.
In step S02, after sealing and ultrasonic treatment of the first mixed solution, a ligand-linking agent and an inorganic alkali solution are added into the first mixed solution, so that the up-conversion luminescent material and the magnetic material are coordinately connected to obtain a second mixed solution.
According to an embodiment of the present invention, the ligand-linking agent is a ligand that can be used to link the up-conversion luminescent material and the magnetic material, and may be, for example, ethyl orthosilicate. The inorganic alkali solution is suitable for improving coordination environment, and can be one or more of sodium hydroxide and potassium hydroxide.
According to an embodiment of the present invention, the mass ratio of the up-conversion luminescent material to the ligand-linking agent may be, but is not limited to, (1 to 4): 1, a step of; for example, it may be 1: 1. 1.5: 1. 2: 1. 3: 1. 4:1.
according to an embodiment of the present invention, the mass ratio of the conversion luminescent material to the inorganic alkaline solution is (2800 to 4000): 1, for example, 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 first mixed liquid is sealed and subjected to ultrasonic treatment for 0.5-1 h, for example, 0.5h, 0.6h, 0.7h, 0.8h, 0.9h and 1h.
And in the step S03, the second mixed liquid is sealed, heated and stirred, and then subjected to ultrasonic treatment, centrifugation and drying treatment to obtain the magnetic up-conversion latent fingerprint developer.
According to an embodiment of the present invention, the second mixed liquid is sealed, heated and stirred at a heating temperature of 60 to 80 ℃, for example, 60 ℃, 65 ℃, 70 ℃, 75 ℃ and 80 ℃. The heating and stirring time is 15-21 h, for example, 15h, 16h, 17h, 18h, 19h, 20h and 21h.
According to an embodiment of the present invention, the rotational speed of the above-mentioned centrifugation process is 8000rpm/min.
According to the embodiment of the invention, the size of the prepared magnetic up-conversion latent fingerprint developer is detected by adopting a transmission electron microscope, and the size of the prepared magnetic up-conversion latent fingerprint developer can be 50nm.
According to the embodiment of the invention, a steady-state transient fluorescence spectrometer can be adopted to monitor the intensity change of the up-conversion luminescence of the prepared developer.
The invention also provides a magnetic up-conversion latent fingerprint developer obtained by the preparation method; wherein, the luminescence wavelength range of the magnetic up-conversion latent fingerprint developer under the irradiation of infrared light is 507-568 nm.
The human eye is sensitive to green light, and the CCD image sensor (Charge coupled Device) in the photographing camera has high quantum efficiency for light with a wavelength range of 500-700 nm. Yb is adopted 3+ As sensitizer ions of the up-conversion luminescent material, the up-conversion luminescent material is excited to emit green light with the wavelength range of 507-568 nm, and when the prepared magnetic up-conversion latent fingerprint developer is applied to latent fingerprint analysis, good visual effect and imaging effect can be realized.
Fig. 2 is a schematic diagram of an implementation process of a magnetic up-conversion latent fingerprint developer latent fingerprint analysis method according to an embodiment of the invention. Fig. 3 (a) -3 (b) are physical diagrams of a magnetic fingerprint brush and a laser according to an embodiment of the present invention.
The present invention also provides a method for analyzing latent fingerprints using the magnetic up-conversion latent fingerprint developer, as shown in fig. 2 and fig. 3 (a) to 3 (b), comprising:
attracting the magnetic up-conversion latent fingerprint developer by utilizing the magnetic fingerprint brush, and dripping the magnetic up-conversion latent fingerprint developer on the surface of the substrate deposited with the latent fingerprint; after repeated dripping for a plurality of times, removing the magnetic up-conversion latent fingerprint developer remained 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 ridges of the latent fingerprint; and irradiating the surface of the substrate with near infrared excitation light emitted by a laser, so that the magnetic up-conversion latent fingerprint developer excites green light with the wavelength range of light emission of 507-568 nm; the CCD image sensor is used for collecting the image of the latent fingerprint, and the magnetic up-conversion luminescence of the developer is used for resolving the image of the latent fingerprint.
The developer for magnetic up-conversion latent fingerprints is dripped on the surface of the substrate on which the latent fingerprints are deposited, the developer is adsorbed on the latent fingerprints formed by oily substances on the surface of the substrate, the part of the surface of the substrate, which is not covered with the oily substances, does not adsorb the developer and can be attracted by the magnetic fingerprint brush, and further, the developer remained in the groove areas of the latent fingerprints can be removed, so that the developer for magnetic up-conversion latent fingerprints 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 a base material with dark complex background such as playing cards, and vouchers formed with two-dimension codes.
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 physical adsorption effect of the developer powder based on magnetic up-conversion latent fingerprints does not damage the fingerprint texture, the biological information of the fingerprints can be stored to the greatest extent, meanwhile, the developer powder which is left in the groove areas of the fingerprints and is not adsorbed can be removed by utilizing 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 privacy in actual 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 the latent fingerprint under the condition of not causing physical damage to the latent fingerprint, and can effectively solve the influence of background interference on the analysis of the latent fingerprint.
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 CCD image sensor has high quantum efficiency to light with the wavelength range of 500-700 nm, and when the prepared magnetically transformed latent fingerprint developer is applied to latent fingerprint analysis, good visual effect and 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, easiness in regulation and control and the like, has low process requirements and high success rate, and has advantages in future scale and industrialization.
The following schematically illustrates the preparation process of the magnetic up-conversion latent fingerprint developer. It should be noted that the examples are only specific embodiments of the present invention and are not intended to 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 is not particularly limited, and the present invention adopts analytical purity. The reaction or detection apparatus or device used is also not particularly limited.
Example 1
In the reactor, 1mmoL of rare earth ion trifluoroacetate salt (0.78 mmoL Gd (CF) 3 COO) 3 ，0.2mmoL Yb(CF 3 COO) 3 ，0.02mmoL Er(CF 3 COO) 3 ) Adding 1.46mL of trifluoroacetic acid into 6.4mL of oleic acid, heating, stirring and dissolving, adding 12.8mL of octadecene as an organic solvent, vacuumizing for 20min, heating to 300 ℃, reacting for 1h, finally washing off residual organic matters on the surface of a sample by using a mixed solvent of cyclohexane and ethanol in a volume ratio of 1:1, and collecting NaGdF through centrifugation 4 The up-conversion luminescent material of Yb and Er is characterized by a transmission electron microscope, and the particle size of the prepared up-conversion luminescent material is 60nm.
Into a 500mL round bottom flask was added 72mL of n-propanol and stirred using a mechanical stirring table with a polytetrafluoroethylene stirring bar while adding 72mg of NaGdF 4 And 20mL of 1mg/mL Fe 3 O 4 (particle diameter is 50 nm) ethanol suspension, at this time, the charging mass ratio of up-conversion luminescent material to magnetic material is 4:1. sealed and sonicated for 30min, 360 μl 2M NaOH solution and 60 μl TEOS were added. A mechanical stirring table with a sealing plug is used, and oil bath stirring is carried out for 18h at 70 ℃ under the sealing state. Transferring the product to 50mL centrifuge tube after the reaction, adding pure water and absolute ethanol for centrifuging (8000 r/min,3 min), repeatedly centrifuging and washing for three times, and vacuum drying to obtain NaGdF 4 :Yb,Er-Fe 3 O 4 Composite nanomaterial.
And the prepared magnetic up-conversion latent fingerprint developer is subjected to luminescence intensity test through a steady-state transient luminescence spectrometer. The detection conditions of the luminescence spectrum are as follows: JY Fluorolog-3-Tou,980nm excitation light with power of 192.4mW cm -2 The scanning range is 300-750 nm.
Fig. 4 (a) to 4 (b) are luminescence spectra of the magnetic up-conversion latent fingerprint developer according to the embodiment of the 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) is 3.5:1, the luminous intensity is weaker; when NaGdF 4 Yb, er and Fe 3 O 4 When the mass ratio of (2) is 4.0:1 or 4.5:1, the luminous intensity is stronger. Referring to fig. 4 (b), the second mixed liquid is sealed, heated and stirred for 15h, 18h and 21h respectively, so as to prepare the magnetic up-conversion latent fingerprint developer with high luminous intensity.
FIG. 5 (a) is Fe 3 O 4 Hysteresis loop of (2); FIG. 5 (b) shows a magnetic up-conversion latent fingerprint developer NaGdF prepared when the heating and stirring time period is set to 18 hours 4 :Yb,Er-Fe 3 O 4 Hysteresis loop of (2); FIG. 5 (c) is NaGdF 4 Yb, er and Fe 3 O 4 When the mass ratio of the magnetic up-conversion latent fingerprint developer NaGdF is 4.0:1, the prepared magnetic up-conversion latent fingerprint developer NaGdF 4 :Yb,Er-Fe 3 O 4 Is provided.
Referring to FIGS. 5 (a) to 5 (c), a hysteresis loop is drawn by a hysteresis loop meter, compared with Fe 3 O 4 The saturation magnetization of the prepared magnetic up-conversion latent fingerprint developer is reduced to a certain extent, but still is matched with Fe 3 O 4 The saturation magnetization of (2) is maintained at the same level.
Fig. 6 is a magnetic attraction object diagram of a magnetic up-conversion latent fingerprint developer according to an embodiment of the invention. Referring to fig. 6, the prepared magnetic up-conversion latent fingerprint developer has magnetism.
The process of performing latent fingerprint analysis using the magnetic up-conversion latent fingerprint developer described above includes: the latent fingerprint is first deposited by pressing a fingertip against a smooth metal substrate. About 20mg NaGdF was extracted with a magnetic fingerprint brush 4 :Yb,Er-Fe 3 O 4 Latent fingerprint developer, moving to above the fingerprint, closing the fingerprint brush magnetAnd the developer falls off to cover the surface of the fingerprint, the magnet rod is opened again, the developer which is not attached to the surface of the fingerprint is attracted again, the attraction and falling-off process is repeated, and then the excessive powder between the fingerprint grooves is removed by gentle blowing. The latent fingerprint developer is irradiated with a 980nm infrared lamp to fix the fingerprint image, so that the developer emits green light to analyze the latent fingerprint.
Fig. 7 is a physical diagram of a magnetic up-conversion latent fingerprint developer according to an embodiment of the invention for latent fingerprint analysis on a metal surface. Referring to fig. 7, the prepared magnetic up-conversion latent fingerprint developer can realize analysis of latent fingerprints deposited on a metal surface.
Example 2
The specific process is the same as that of example 1, the rare earth ion Er doped in the latent fingerprint developer of example 1 3+ Change to Tm 3+ Preparing NaGdF 4 :Yb,Tm-Fe 3 O 4 The fingerprint image fixed by the latent fingerprint developer is irradiated by using a 980nm infrared lamp, and blue light is emitted to analyze the latent fingerprint.
Example 3
The specific process is the same as that of example 1, and doped rare earth ion Nd is added into the latent fingerprint developer of example 1 3+ Preparing NaGdF 4 :Nd,Yb,Er-Fe 3 O 4 The fingerprint image fixed by the latent fingerprint developer is irradiated by using an infrared lamp of 808nm, and green light is emitted to analyze the latent fingerprint.
Examples 4 to 7
The specific procedure was the same as in example 1, and the smooth metal substrate was replaced with an impermeable substrate such as glass, acryl, plastic, ceramic, etc.
Fig. 8 is a physical diagram of a magnetic up-conversion latent fingerprint developer according to an embodiment of the invention performing latent fingerprint analysis on a surface of an impermeable substrate. Referring to fig. 8, the prepared magnetic up-conversion latent fingerprint developer can realize analysis of latent fingerprints deposited on the surface of an impermeable substrate.
Examples 8 to 10
The specific procedure was the same as in example 1, except that the smooth metal substrate was replaced with a permeable substrate such as rubber, paper, wood, etc.
Fig. 9 is a physical diagram of a magnetic up-conversion latent fingerprint developer according to an embodiment of the invention performing latent fingerprint analysis on the surface of a permeable substrate. Referring to fig. 9, the prepared magnetic up-conversion latent fingerprint developer 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 smooth metal substrates are respectively replaced by substrates with dark complex backgrounds such as playing cards, gold coupons with two-dimensional codes and the like.
Fig. 10 is a physical diagram of a magnetic up-conversion latent fingerprint developer according to an embodiment of the invention for 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 analysis of latent fingerprints deposited on the surface of a substrate with dark complex background.
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the invention, and is not meant to limit the invention thereto, but to limit the invention thereto, and any modifications, equivalents, improvements and equivalents thereof may be made without departing from the spirit and principles of the invention.
Claims (10)
1. The preparation method of the magnetic up-conversion latent fingerprint developer is characterized by comprising the following steps of:
under the mechanical stirring state, the up-conversion luminescent material and the magnetic material suspension are added into the first solvent at the same time to obtain a first mixed solution;
sealing and ultrasonic treating the first mixed liquid, and adding a ligand connecting agent and an inorganic alkali solution into the first mixed liquid to coordinate and connect the up-conversion luminescent material and the magnetic material to obtain a second mixed liquid; and
sealing, heating and stirring the second mixed liquid, and performing ultrasonic treatment, centrifugation and drying treatment to obtain a magnetic up-conversion latent fingerprint developer;
wherein the up-conversion luminescent material is NaLnF doped with rare earth ions Ln 4 The nanometer material is prepared from the nanometer 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 following;
the up-conversion luminescent material is granular, and the grain diameter of the grains is 20 nm-400 nm;
the magnetic material is granular, and the grain diameter of the granular is 20 nm-200 nm;
the ligand connecting agent is ethyl orthosilicate;
the luminescence wavelength range of the magnetic up-conversion latent fingerprint developer under the irradiation of infrared light is 507-618 nm.
2. The 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 material with ferromagnetism.
3. The method of claim 2, wherein the magnetic material comprises cubic phase Fe 3 O 4 。
4. The method according to claim 1, wherein,
the inorganic alkaline solution comprises one or more of sodium hydroxide and potassium hydroxide.
5. The method according to claim 1, wherein the first mixed liquid is sealed and subjected to ultrasonic treatment for a period of 0.5 to 1 hour;
and sealing the second mixed liquid, and heating and stirring at a heating temperature of 60-80 ℃ for 15-21 h.
6. The method of claim 1, wherein the mass ratio of the up-conversion luminescent material to the magnetic material is 1-10:1;
the mass ratio of the up-conversion luminescent material to the ligand connecting agent is 1-4:1;
the mass ratio of the up-conversion luminescent material to the inorganic alkaline solution is 2800-4000:1.
7. A magnetic up-conversion latent fingerprint developer obtained by the production method according to any one of claims 1 to 6.
8. A method of latent fingerprint analysis using the magnetic up-conversion latent fingerprint developer of claim 7, comprising:
attracting the magnetic up-conversion latent fingerprint developer by utilizing a magnetic fingerprint brush, and dripping the magnetic up-conversion latent fingerprint developer on the surface of the substrate on which the latent fingerprint is deposited;
after repeated dripping for a plurality of times, removing the magnetic up-conversion latent fingerprint developer remained 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 ridges of the latent fingerprint; and
adopting near infrared excitation light to irradiate the surface of the substrate, so that the magnetic up-conversion latent fingerprint developer excites green light with the wavelength range of light emission of 507-618 nm;
and acquiring the image of the latent fingerprint by using a CCD image sensor, and resolving the image of the latent fingerprint by using the up-conversion luminescence function of the magnetic up-conversion latent fingerprint developer.
9. The method of latent fingerprint analysis according to claim 8, wherein,
the substrate is an impermeable substrate comprising one or more of glass, acrylic, plastic, ceramic and metal;
alternatively, the substrate is a permeable substrate comprising one or more of rubber, paper, wood.
10. The method of latent fingerprint analysis according to claim 8, wherein,
the wavelength of the near infrared excitation light comprises one or more of 980nm, 915nm and 808 nm.
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