CN111748336B - Fluorescent fingerprint developing powder and preparation method and application thereof - Google Patents
Fluorescent fingerprint developing powder and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses fluorescent fingerprint developing powder and a preparation method and application thereof. The invention adopts a soft template method to prepare nano mesoporous silica, then combines 0.1 to 0.3 part of sodium dodecyl sulfate on the surface of 5 to 15 parts of nano mesoporous silica by a chemical method, and loads 2 to 4 parts of rhodamine B into nano holes of the nano mesoporous silica by electrostatic adsorption to obtain fluorescent fingerprint developing powder. The fluorescent fingerprint developing powder is used for developing and extracting fingerprints, and has the advantages of clearer, no powder stagnation phenomenon, environmental friendliness, zero damage to guest materials, low cost, simple preparation, easiness in mass production and the like.
Description
Technical Field
The invention belongs to the technical field of fingerprint display, and particularly relates to fluorescent fingerprint display powder and a preparation method and application thereof.
Background
The fingerprint is the first of the material evidence in the global judicial world, and because the fingerprint of a person has the characteristics of stability, diversity and uniqueness, the fingerprint is used for carrying out identity verification, and has a crucial role in the detection of the whole criminal act and the identification of the suspects, and the fingerprint becomes an important evidence for finding evidence and disclosing crimes, thereby playing a role in the detection of criminal cases at present. However, the potential fingerprints are difficult to directly distinguish by naked eyes, and are difficult to extract and display due to technical, technological, flow and other aspects. Meanwhile, with the development of technology, cases of high-tech crimes are increased, and the crime making means also has the characteristics of intelligence and technology, which aggravate the difficulties of fingerprint extraction and appearance. The common fingerprint appearance modes mainly comprise an impermeable object surface appearance in an optical appearance mode, a powder appearance mode, a 502 glue appearance mode and a high-vacuum metal coating mode, an impermeable object surface appearance in an ninhydrin compound mode and a physical developer mode, and a comprehensive appearance suitable for various object surfaces in a fumigation appearance mode and a fat dyeing mode, and meanwhile, the appearance effect is enhanced by novel instrument analysis, however, the conventional fingerprint appearance technology has entered a bottleneck period of development, and is applied to potential fingerprint appearance along with development of nano materials and nano technologies, so that the application range of the nano materials is widened, the new directions of fingerprint extraction and appearance are developed, and the development of the latent fingerprints is promoted to be developed to a high-efficiency, low-cost, nontoxic and nondestructive direction.
Disclosure of Invention
The invention aims to provide fluorescent fingerprint developing powder, a preparation method and application thereof, and aims to solve the problems that the existing commonly used powder such as gold powder, silver powder and magnetic powder has poor developing effect on old fingerprints or the chemical developing method has larger damage on guest materials with fingerprints.
The invention is realized in such a way that the fluorescent fingerprint developing powder comprises the following components in parts by mass: 5 to 15 parts of nano mesoporous silica, 2 to 4 parts of fluorescent powder and 0.1 to 0.3 part of sodium dodecyl sulfate.
Preferably, the fluorescent powder is rhodamine B.
The invention further discloses a preparation method of the fluorescent fingerprint developing powder, which comprises the following steps:
(1) Adding 0.5 g-1.5 g of nano mesoporous silica and 0.01-0.03 g of sodium dodecyl sulfate into 100mL of absolute ethyl alcohol, adding 100mL of buffer solution with pH value of 7.8-8.0, stirring uniformly, then carrying out ultrasonic oscillation for 10-20 min, adding 0.2-0.4 g of fluorescent powder, and carrying out ultrasonic oscillation for 2.5-3.5 h under the heating of 35-45 ℃ to obtain a mixed solution;
(2) Centrifuging the mixed solution for 4-6 min at 1800-2200 r/min, taking the precipitate, redissolving the precipitate in 100mL buffer solution with pH=7.8-8.0 to obtain redissolved solution, centrifuging the redissolved solution for 4-6 min at 1800-2200 r/min, taking the precipitate, and drying to obtain fluorescent fingerprint showing powder.
Preferably, the buffer solution is prepared from 5.59g of dipotassium hydrogen phosphate and 0.41g of potassium dihydrogen phosphate in 1000mL of deionized water.
Preferably, in the step (1), the formation method of the nano mesoporous silica includes the following steps:
A. adding 0.45-0.55 g of P123 into 34-36 mL of acetic acid-sodium acetate buffer solution with pH of 4.9-5.1 under the conditions of water bath at 34-36 ℃ and continuous stirring, adding 0.09-0.11 g of SDS after the solution becomes semitransparent, and adding 0.18-0.22 mg of anhydrous Na after the solution becomes colorless and transparent 2 SO 4 After being stirred uniformly, 0.7-0.9 mg TMOS is added, and the mixture is stirred for five minutes, and the solution is kept stand for 24 hours after being changed from colorless and transparent to milky;
B. and (3) carrying out hydrothermal crystallization on the white solution after standing for 24 hours at 98-100 ℃, washing, dewatering and drying the obtained white precipitate, and calcining the dried white precipitate at 545-555 ℃ for 5-6 hours to obtain the white bulk solid nano mesoporous silica.
Preferably, in the step B, the obtained white precipitate is repeatedly washed with ethanol and secondary water, filtered in vacuum to remove water, left at room temperature for 1-2 days to remove water, and then dried at 35 ℃.
The invention further discloses application of the fluorescent fingerprint developing powder in developing and extracting fingerprints.
The invention overcomes the defects of the prior art and provides fluorescent fingerprint developing powder, a preparation method and application thereof, wherein the invention adopts a soft template method to prepare nano mesoporous silica, then combines 0.1 to 0.3 part of sodium dodecyl sulfate on the surface of 5 to 15 parts of nano mesoporous silica by a chemical method, and loads 2 to 4 parts of rhodamine B into nano holes of the nano mesoporous silica by electrostatic adsorption to obtain the fluorescent fingerprint developing powder; the nano mesoporous silica is used as a carrier of other components, is easy to combine with other molecules due to higher chemical activity, has larger specific surface area and larger contact area with fingerprint substances, and can fully react when the fingerprint is displayed; the dodecyl sodium sulfate is a main component for enhancing the binding force between a material and a fingerprint substance, the material is long-chain amphiphilic molecules, nano mesoporous silicon dioxide modified by the dodecyl sodium sulfate has a dodecyl chain with very strong oleophylic and hydrophobic properties on the surface, and when the dodecyl chain encounters grease remained in old fingerprints, the dodecyl chain is tightly and accurately adsorbed, so that the recognition degree is good, and the sensitivity is high; in addition, rhodamine B mainly plays a role in enabling the material to have fluorescence characteristics, and can effectively overcome the defect that fingerprints left on the surface of a complex object of a conventional material are difficult to observe under natural light.
In the invention, the micelle formed by the polymer P123 and the sodium sulfate mixed solution is used as a template to prepare the nano mesoporous silica, and the nano mesoporous silica has the advantages of large specific surface area, uniform aperture, controllable particle size and the like; on the basis, the invention utilizes the characteristic that nano mesoporous silica is easy to be chemically modified, long-chain molecule sodium dodecyl sulfate is combined to the surface of the nano mesoporous silica by a chemical method, the binding force between the nano mesoporous silica and main components in the fingerprint is enhanced, and the fingerprint display efficiency is improved; in addition, the invention combines the fluorescent powder and the nano mesoporous silica by utilizing the characteristic of larger specific surface area of the nano mesoporous silica and through electrostatic adsorption, so that the material has fluorescent characteristic and enhances the effect of showing the handprint left on the surface of the complex object.
Compared with the defects and shortcomings of the prior art, the invention has the following beneficial effects:
(1) The fluorescent fingerprint showing powder can improve the fingerprint showing effect of old fingerprints and complex background objects, has no damage to the object materials, and is low in cost and environment-friendly;
(2) The fluorescent fingerprint showing powder can effectively show old oil sweat mixed fingerprints on a board with a matte finish, and compared with the traditional reagent showing effect, the fluorescent fingerprint showing powder has the advantages that the fingerprint lines showing the powder are clearer, the detail characteristics are obvious, and the powder stagnation phenomenon does not exist on the surface;
(3) Compared with the traditional reagent, the fluorescent fingerprint showing powder has obvious advantages, and the showing effect is less influenced by object background, so that the fluorescent fingerprint showing powder can be theoretically suitable for showing potential fingerprints of any objects;
(4) The fluorescent fingerprint developing powder disclosed by the invention is simple in fingerprint brushing, high in sensitivity, easy to operate, and free from fingerprint line blurring caused by excessive developing powder, and the developing effect and the identification value of potential fingerprints are ensured;
(5) The preparation process of the fluorescent fingerprint developing powder is simple and easy to popularize, and the cost is low and the mass production is easy.
Drawings
FIG. 1 is a morphology of the internal structure of a single particle nano-mesoporous silica;
FIG. 2 is a surface morphology of a plurality of particulate nano-mesoporous silica;
FIG. 3 is a comparative graph of the effects of a commercially available powder and the present development powder on the development of fingerprints with a residence time of up to 15 days, respectively;
fig. 4 is a tabular summary of the effects of the present invention on the development of fingerprints for different carry-over times compared to commercially available conventional powders.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
(1) Adding 0.50g of P123 into 35mL of acetic acid-sodium acetate buffer solution with pH of=5 under the condition of continuous stirring in a water bath at 35 ℃, adding 0.1g of SDS after the solution becomes semitransparent, adding 0.2mg of anhydrous Na after the solution becomes colorless and transparent 2 SO 4 After stirring uniformly, 0.8mg of TM is addedOS, stirring for five minutes, and continuously standing for 24 hours until the solution turns from colorless transparent to milky white;
(2) And (3) carrying out hydrothermal crystallization on the white solution after standing for 24 hours at 99 ℃, repeatedly washing the obtained white precipitate by using ethanol and secondary water, carrying out vacuum filtration to remove water, standing for 1.5t at room temperature to remove water, drying at 35 ℃, and calcining the dried white precipitate at 550 ℃ for 5.5 hours to obtain the white bulk solid nano mesoporous silica 1.
Example 2
(1) Under the condition of water bath at 34 ℃ and continuous stirring, 0.45g of P123 is added into 34mL of acetic acid-sodium acetate buffer solution with pH of 4.9, after the solution becomes semitransparent, 0.09g of SDS is added, after the solution becomes colorless and transparent, 0.18mg of anhydrous Na is added 2 SO 4 After being stirred uniformly, 0.7mg TMOS is added, and the mixture is stirred for five minutes, and the solution is kept stand for 24 hours after being changed from colorless and transparent to milky;
(2) And (3) carrying out hydrothermal crystallization on the white solution after standing for 24 hours at 98 ℃, repeatedly washing the obtained white precipitate by using ethanol and secondary water, carrying out vacuum filtration to remove water, standing for 1t at room temperature to remove water, drying at 35 ℃, and calcining the dried white precipitate at 545 ℃ for 5 hours to obtain the white bulked solid nano mesoporous silica 2.
Example 3
(1) Under continuous stirring in 36℃water bath, 0.55g of P123 was added to 36mL of acetic acid-sodium acetate buffer solution having pH=5.1, after the solution became translucent, 0.11g of SDS was further added, after the solution became colorless and transparent, 0.22mg of anhydrous Na was further added 2 SO 4 After being stirred uniformly, 0.9mg TMOS is added, and the mixture is stirred for five minutes, and the solution is kept stand for 24 hours after being changed from colorless and transparent to milky;
(2) And (3) carrying out hydrothermal crystallization on the white solution after standing for 24 hours at the temperature of 100 ℃, repeatedly washing the obtained white precipitate with ethanol and secondary water, carrying out vacuum filtration for water removal, standing for 2t at room temperature for water removal, drying at the temperature of 35 ℃, and calcining the dried white precipitate at the temperature of 555 ℃ for 5-6 hours to obtain the white bulk solid nano mesoporous silica 3.
Example 4
(1) 5.59g of dipotassium hydrogen phosphate and 0.41g of potassium dihydrogen phosphate were dissolved in 1000mL of deionized water to prepare a buffer solution having pH=7.9;
(2) Adding 1.0g of nano mesoporous silica 1 and 0.02g of sodium dodecyl sulfate prepared in the embodiment 1 into 100mL of absolute ethyl alcohol, adding 100mL of buffer solution with PH=7.9, stirring uniformly, performing ultrasonic oscillation for 15min, adding 0.3g of fluorescent powder, and performing ultrasonic oscillation for 3h under heating at 40 ℃ to obtain a mixed solution;
(3) Centrifuging the mixed solution at 2000r/min for 5min, taking the precipitate, redissolving the precipitate in 100mL of buffer solution with pH=7.9 to obtain redissolved solution, centrifuging the redissolved solution at 2000r/min for 5min, taking the obtained precipitate, and drying to obtain fluorescent fingerprint developing powder 1.
Example 5
(1) 5.59g of dipotassium phosphate and 0.41g of potassium dihydrogen phosphate were dissolved in 1000mL of deionized water to prepare a buffer solution having pH=7.8;
(2) Adding 0.5g of nano mesoporous silica 2 prepared in example 2 and 0.01g of sodium dodecyl sulfate into 100mL of absolute ethyl alcohol, adding 100mL of buffer solution with PH=7.8, stirring uniformly, then carrying out ultrasonic oscillation for 10min, adding 0.2g of fluorescent powder, and carrying out ultrasonic oscillation for 2.5h under heating at 35 ℃ to obtain a mixed solution;
(3) Centrifuging the mixed solution for 4min at 1800r/min, taking the precipitate, redissolving the precipitate in 100mL of buffer solution with pH=7.8 to obtain redissolved solution, centrifuging the redissolved solution for 4min at 1800r/min, taking the obtained precipitate, and drying to obtain fluorescent fingerprint developing powder 2.
Example 6
(1) 5.59g of dipotassium hydrogen phosphate and 0.41g of potassium dihydrogen phosphate were dissolved in 1000mL of deionized water to prepare a buffer solution having pH=8.0;
(2) Adding 1.5g of nano mesoporous silica 3 prepared in example 3 and 0.03g of sodium dodecyl sulfate into 100mL of absolute ethyl alcohol, adding 100mL of buffer solution with PH=8.0, stirring uniformly, then carrying out ultrasonic oscillation for 20min, adding 0.4g of fluorescent powder, and carrying out ultrasonic oscillation for 3.5h under the heating of 45 ℃ to obtain a mixed solution;
(3) Centrifuging the mixed solution at 2200r/min for 6min, taking the precipitate, redissolving the precipitate in 100mL of buffer solution with pH=8.0 to obtain redissolved solution, centrifuging the redissolved solution at 2200r/min for 6min, taking the obtained precipitate, and drying to obtain fluorescent fingerprint developing powder 3.
Comparative examples
This comparative example is substantially the same as example 4 above, except that in step (2), commercially available nano silica is selected instead of nano mesoporous silica 1, and finally fluorescent fingerprint developing powder X is obtained.
Effect examples
1. The nano mesoporous silica 1 prepared in the example 1 is selected for observation, and the results are shown in fig. 1-2, and as can be seen from fig. 1, the nano mesoporous silica synthesized by the invention has a hexagonal porous structure, the pore size is 8nm, and the pore size is uniform; as can be seen from FIG. 2, the nano mesoporous silica synthesized by the method is of a polyhedral structure similar to a hexagonal prism, the particle dispersion degree is good, the morphology uniformity is high, and the particle size is about 400 nm.
The comparison of the nano mesoporous silica 1 of the invention with the nano silica commonly used in the market can find that the nano mesoporous silica prepared by the invention has special nano aperture and particle morphology, and is specifically expressed as follows:
(1) The nano mesoporous silica has an obvious hexagonal hole structure, the pore diameter can be adjusted between 6 and 20nm through the change of the proportion of the synthetic raw materials, and the commercially available common nano silica material does not have the structure;
(2) The single particles of the nano mesoporous silica are about 400nm, the particle sizes are uniform, and the particles are polyhedrons similar to hexagonal prisms; the common nano silicon dioxide material particles sold in the market are 2 mu m to 50nm, the particle size distribution of the particles is wider, and the particle morphology is irregular;
(3) The nano mesoporous silica surface of the invention has more OH, which is beneficial to the subsequent chemical modification of SDS; the surface chemical groups of the common nano silicon dioxide materials are complex, which is not beneficial to the chemical modification.
2. Comparison of the fingerprint development Effect of commercially available conventional powder and the developed powder of the present invention
Selecting the fluorescent fingerprint developing powder 1, the existing gold powder, silver powder and magnetic powder prepared in the embodiment 4 for fingerprint developing experimental comparison; wherein the gold powder is golden fingerprint powder, the product number is No.2003, and the gold powder is purchased from Beijing Bulan police equipment liability company; silver powder is silver fingerprint powder, the product number is No.2007, and the silver powder is purchased from Beijing Bulan police equipment liability company; the magnetic powder is black magnetic powder, the product number is No.2013, and the magnetic powder is purchased from Beijing Bulan police equipment liability company. The specific operation process is that a gray mouse brush is used for brushing sweat fingerprints; dipping a proper amount of powder by using a brush, then lightly lifting the brush to a position suspected to leave a fingerprint, and lightly sweeping the surface of the object by using the part with the powder at the front end of the brush in a clockwise direction so that the powder can be uniformly dispersed on the surface of the object; after the outline of the hand print appears, lightly sweeping the hand print along the line direction of the hand print by using a brush; and (3) observing under natural light or proper illumination conditions, and fixing the sample display result by using a macro camera.
The experimental results are shown in FIGS. 3 to 4. As can be seen from fig. 3, the gold powder, silver powder and magnetic powder commonly used in the market at present have poor appearance effect on fingerprints of 15 days, obvious adhesion occurs on fingerprint lines, the detail loss of the lines is more, the number of characteristic points is insufficient, and the fingerprint comparison and identification standard cannot be met; the development effect of the development powder is obviously superior to that of the common powder on the market, the lines are clear and not deformed, the line details are obvious, sweat pore structures in the hand printing lines can be observed locally and amplified, the number of characteristic points is more, and the hand printing comparison and identification standard is reached.
In fig. 4, "+" represents that a hand print contour may be revealed; "++" indicates that lines can be revealed but are not clear; "+++". Representative may be the hand-print lines are shown to be present, the lines are clearer, but the detail features are not obvious; "+++" "representative of the hand print lines are clear and the hand print lines are clear, the detail characteristics are obvious; "+++" -represents the hand print lines are clear and the hand print lines are clear, the detailed characteristics are obvious and the method has the advantages that, tiny sweat pore structures can be seen in the ridge lines. As can be seen from fig. 4, the effect of commercially available conventional powder on the impression of the hand is inversely proportional to the impression leave-on time, the longer the impression leave-on time, the worse the effect is; the development powder has good development effect on fingerprints, high stability and no influence on the development effect of fingerprints within 15 days after the fingerprints are left.
3. Fluorescent fingerprint development powder X prepared in comparative example and fingerprint development effect of the development powder of the present invention
The difference between the developing powder 1 and the developing powder X of the invention is that:
(1) The invention shows that the powder 1 has uniform particle shape, when the fingerprints are shown, the fingerprint lines are more complete and clear, and obvious break points can not appear; the powder X particles are not uniform in morphology, and obvious break points exist on the fingerprint lines when fingerprints are displayed;
(2) The specific surface area of the developing powder 1 is larger than that of the developing powder X, and the developing powder 1 has a hexagonal hole-shaped structure, so that the fluorescent substance loading capacity is stronger, the fluorescent efficiency is far higher than that of the developing powder X, and the fluorescent effect is better when the fingerprint is developed.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (4)
1. A method for preparing fluorescent fingerprint developing powder, which is characterized by comprising the following steps:
(1) Adding 0.5 g-1.5 g of nano mesoporous silica and 0.01-0.03 g of sodium dodecyl sulfate into 100mL of absolute ethyl alcohol, adding 100mL of buffer solution with pH value of 7.8-8.0, stirring uniformly, then carrying out ultrasonic oscillation for 10-20 min, adding 0.2-0.4 g of fluorescent powder, and carrying out ultrasonic oscillation for 2.5-3.5 h under the heating of 35-45 ℃ to obtain a mixed solution;
in the step (1), the generation mode of the nano mesoporous silica comprises the following steps:
A. adding 0.4 to 34-36 mL acetic acid-sodium acetate buffer solution with pH=4.9-5.1 in 34-36 ℃ water bath and continuous stirring condition5 to 0.55g of P123, after the solution turns into semitransparent state, 0.09 to 0.11g of SDS is added, after the solution turns into colorless transparent state, 0.18 to 0.22mg of anhydrous Na is added 2 SO 4 After being stirred uniformly, 0.7-0.9 mg TMOS is added, and the mixture is stirred for five minutes, and the solution is kept stand for 24 hours after being changed from colorless and transparent to milky;
B. carrying out hydrothermal crystallization on the white solution after standing for 24 hours at 98-100 ℃, washing, dewatering and drying the obtained white precipitate, and calcining the dried white precipitate at 545-555 ℃ for 5-6 hours to obtain white bulk solid nano mesoporous silica;
(2) Centrifuging the mixed solution for 4-6 min at 1800-2200 r/min, taking the precipitate, redissolving the precipitate in 100mL buffer solution with pH=7.8-8.0 to obtain redissolved solution, centrifuging the redissolved solution for 4-6 min at 1800-2200 r/min, taking the precipitate, and drying to obtain fluorescent fingerprint showing powder.
2. The method of preparing a fluorescent hand print visualization powder of claim 1, wherein the buffer solution is prepared from 5.59g of dipotassium hydrogen phosphate and 0.41g of potassium dihydrogen phosphate in 1000mL of deionized water.
3. The method for preparing fluorescent fingerprint development powder according to claim 1, wherein in the step B, the obtained white precipitate is repeatedly washed with ethanol and secondary water, vacuum filtered to remove water, left at room temperature for 1 to 2 days to remove water, and dried at 35 ℃.
4. A fluorescent fingerprint development powder obtained by the production process according to any one of claims 1 to 3.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1328094A (en) * | 2001-06-26 | 2001-12-26 | 中山大学 | Nm-class composite mesoporous organic/Si-base fluorescent pigment and its preparing process |
| CN103908260A (en) * | 2014-01-16 | 2014-07-09 | 中国刑事警察学院 | Latent fingerprint displaying method |
| CN104382600A (en) * | 2014-11-24 | 2015-03-04 | 中国刑事警察学院 | Two-step latent fingerprint manifesting method based on nano-particles |
| CN104386700A (en) * | 2014-11-05 | 2015-03-04 | 江苏省检验检疫科学技术研究院 | Method for preparing mesoporous silicon dioxide microspheres |
| CN105199710A (en) * | 2015-08-25 | 2015-12-30 | 武汉理工大学 | Fluorescent mesoporous silica composite nanoparticles and preparing method thereof |
| CN106634980A (en) * | 2016-11-23 | 2017-05-10 | 沈阳大学 | Method for preparing and applying latent fingerprint development luminescent nanopowder |
-
2020
- 2020-07-08 CN CN202010651125.6A patent/CN111748336B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1328094A (en) * | 2001-06-26 | 2001-12-26 | 中山大学 | Nm-class composite mesoporous organic/Si-base fluorescent pigment and its preparing process |
| CN103908260A (en) * | 2014-01-16 | 2014-07-09 | 中国刑事警察学院 | Latent fingerprint displaying method |
| CN104386700A (en) * | 2014-11-05 | 2015-03-04 | 江苏省检验检疫科学技术研究院 | Method for preparing mesoporous silicon dioxide microspheres |
| CN104382600A (en) * | 2014-11-24 | 2015-03-04 | 中国刑事警察学院 | Two-step latent fingerprint manifesting method based on nano-particles |
| CN105199710A (en) * | 2015-08-25 | 2015-12-30 | 武汉理工大学 | Fluorescent mesoporous silica composite nanoparticles and preparing method thereof |
| CN106634980A (en) * | 2016-11-23 | 2017-05-10 | 沈阳大学 | Method for preparing and applying latent fingerprint development luminescent nanopowder |
Non-Patent Citations (2)
| Title |
|---|
| Fluorescent Nanomaterials for the Development of Latent Fingerprints in Forensic Sciences;Meng Wang等;《Adv. Funct. Mater.》;20170228;第27卷;1606243 * |
| Systematic study of dye loaded small mesoporous silica nanoparticles for detecting latent fingerprints on various substrates;Meiqin Zhang等;《J Porous Mater》;20160629;第24卷;13-30 * |
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