CN104560031A - Rare-earth long afterglow luminescent powder, preparation method of luminescent powder and method applying luminescent powder as hidden fingerprint emergence reagent - Google Patents
Rare-earth long afterglow luminescent powder, preparation method of luminescent powder and method applying luminescent powder as hidden fingerprint emergence reagent Download PDFInfo
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- CN104560031A CN104560031A CN201510054494.6A CN201510054494A CN104560031A CN 104560031 A CN104560031 A CN 104560031A CN 201510054494 A CN201510054494 A CN 201510054494A CN 104560031 A CN104560031 A CN 104560031A
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Abstract
The invention discloses rare-earth long afterglow luminescent powder, a preparation method of the luminescent powder and a method applying the luminescent powder as a hidden fingerprint emergence reagent. The general structural formula of the rare-earth long afterglow luminescent powder is M2MgSi2O7:0.02Eu2+, 0.04Dy3+, wherein M refers to one or two of Sr and Ca; and the particle size of the rare-earth long afterglow luminescent powder is 1-3 microns. The rare-earth long afterglow luminescent powder is prepared by virtue of a high-temperature solid-phase method. The method applying the luminescent powder as the hidden fingerprint emergence reagent comprises the following steps: mixing the rare-earth long afterglow luminescent powder with reduced iron powder, emerging a hidden fingerprint on an object by virtue of the compound, acquiring the fingerprint image by virtue of white light or ultraviolet excitation, or acquiring the self-luminous image. The preparation method is simple, the excited wavelength of the prepared rare-earth long afterglow luminescent powder is wide in range, the emission wavelength peak value of the long afterglow powder can change between 466nm and 533nm by regulating the Sr/Ca ratio, and the field hidden fingerprint emergence is conveniently realized. The rare-earth long afterglow luminescent powder has high fluorescence intensity and long afterglow (self-luminous) characteristics, and the background interference of the object can be effectively eliminated after fingerprint emergence; and moreover, the luminescent powder is non-toxic, nondestructive and environment-friendly.
Description
Technical field:
The invention belongs to Materials science and forensic science field, particularly relate to a kind of rare earth long afterglow luminescent powder and preparation method thereof and apply its method manifesting reagent as latent fingerprint.
Background technology:
In fingerprint displaying, relative to non-luminous powder, fluorescent material is better subject to people's attention because of its susceptibility and selectivity.But when object is luminous and background patterns produces interference, this method often encounters a difficulty, and also annoyings forensic science researchist always.
Rare earth ion doped long after glow luminous material has good light stability, wider excitation spectrum is separated with emmission spectrum with narrower emmission spectrum, excitation spectrum, and the optical signature such as tunable emmission spectrum wavelength, overcome organic fluorescent powder by many defects that photobleaching, emmission spectrum are wider, especially its overlength afterglow characteristic gets more and more people's extensive concerning.In recent years, the successful Application of temporal resolution luminescence technology in biomedical and forensic science is that potential fingerprint displaying on difficult object and complex background object and imaging provide possibility.
Compared with rare earth ion doped aluminate long after glow luminous material, long persistence luminescent silicate material synthesis temperature is low, with low cost, chemical stability and good biocompatibility, and luminous color enriches adjustable, especially resistant to hydrolysis ability is strong, better to the adaptability of environment.In order to expand the range of application of long after glow luminous material, by Sr
2-xca
xmgSi
2o
7︰ 0.02Eu
2+, 0.04Dy
3+(0≤x≤2) luminescent powder is applied to the potential fingerprint displaying on common impermeability object and complex background object, its long afterglow property makes it can absorb and store luminous energy, still can be luminous for a long time after removing light source, for the Time-resolved imaging realizing potential impression of the hand, effectively eliminate (reduction) background interference and have great importance.
Summary of the invention:
Object of the present invention is exactly the deficiency for prior art, and a kind of rare earth long afterglow luminescent powder and preparation method thereof is provided and applies its method manifesting reagent as latent fingerprint, this rare earth long afterglow luminescent powder can solve the fingerprint displaying difficult problem on difficult object and complex background.
Technology solution of the present invention is as follows:
Rare earth silicate long-afterglow luminescent powder, the general structure of its compound is M
2mgSi
2o
7︰ 0.02Eu
2+, 0.04Dy
3+, M is one or both in Sr, Ca.
The excitation wavelength range of described rare earth long afterglow luminescent powder is 250 ~ 468nm, emission wavelength peak when M is Sr is 466nm, emission wavelength peak when M is Ca is 533nm, M is that Sr, Ca are when coexisting, along with the change of Sr/Ca ratio, the emission wavelength peak of steady persistence powder changes between 466 ~ 533nm.
The luminous time of persistence of described rare earth long afterglow luminescent powder is more than 2 hours.
The preparation method of rare earth long afterglow luminescent powder, it comprises the following steps:
1), MCO is taken according to stoichiometric ratio
3, MgCO
3, SiO
2, Eu
2o
3and Dy
2o
3, then take the solubility promoter H of above-mentioned raw materials total mass 10%
3bO
3or B
2o
3;
2), by step 1) raw material that takes and solubility promoter mixing, in agate mortar, grind half an hour, then proceed in corundum crucible in 1000 DEG C of pre-burnings 1 hour;
3), by the sample of above-mentioned pre-burning again grind half an hour, adopt high temperature solid-state method in gac reducing atmosphere, be heated to 1150 DEG C of sintering and obtain thick product in 3 hours;
4), by thick for above-mentioned long after glow luminous material product grind, then in dispersion agent, carry out ball milling, elimination dispersion agent, be drying to obtain described rare earth long afterglow luminescent powder.
Rare earth long afterglow luminescent powder manifests the method for reagent as latent fingerprint, and it comprises the following steps:
1), adopt 300 ~ 400 mesh sieves to be sieved by reduced iron powder, the ratio being then 1:8 ~ 10 in mass ratio by rare earth long afterglow luminescent powder and the iron powder that obtains of sieving mixes, and obtains mixture;
2), by step 1) mixture that obtains manifests potential impression of the hand on object;
3) impression of the hand, by white light or UV-irradiation manifested, gathers handprint images; Or under gauge without light source irradiation mode, gather luminous handprint images.
Described step 2) in be adopt Magnetic brush brush to show method mixture brush to be shown the potential impression of the hand that object is left over.
Described object comprises impermeability object or semipermeability object.
Described object comprises ceramic tile, plastic sheet, glass, smooth cardboard, copy paper or leather.
Described impression of the hand type is sebum or diving hand print with perspiration.
Described step 3) in be using the UV-light of 365nm or visible ray as excitation light source, irradiate the impression of the hand manifested and gather handprint images after 30 seconds.
Beneficial effect of the present invention is:
1. the rare earth compound M that the present invention's luminous intensity of utilizing high temperature solid-state method to synthesize is high
2mgSi
2o
7︰ 0.02Eu
2+, 0.04Dy
3+, wherein M is one or both in Sr, Ca, and obtains the tiny long afterglow powder of uniform particle sizes in conjunction with Ball milling technology, and granular size is 1 μm ~ 3 μm;
2. preparation method of the present invention is simple, and the rare earth long afterglow luminescent powder of preparation can be used as fingerprint displaying powder, its excitation wavelength range wider (UV-light and visible light source all can excite), and emission wavelength ranges is narrower, is convenient to on-the-spot latent fingerprint and manifests; There is higher fluorescence intensity and steady persistence (luminous) characteristic, after manifesting impression of the hand, can effectively eliminate object background interference;
3. utilize Magnetic brush brush to show method to manifest latent fingerprint, tiny powder can be avoided to be suspended in contaminate environment and harm personnel health in air; Can the common impermeability object of successful presentation and semipermeability object sebum, the diving hand print with perspiration left on the surface;
4. the present invention efficiently solves the interference problem of difficult object and complex background, has expanded rare earth luminous powder and has been applied to the scope that latent fingerprint manifests field, established a kind of efficient, nontoxic, harmless, easy fingerprint displaying technology.
Accompanying drawing illustrates:
Fig. 1 is the XRD figure of rare earth long afterglow luminescent powder of the present invention.
Fig. 2 is the excitation-emission spectrogram of rare earth long afterglow luminescent powder of the present invention.
Fig. 3 is fresh sebum impression of the hand figure (365nm ultraviolet excitation, luminous) on aluminium foil.
Fig. 4 is tile fresh sebum impression of the hand figure (365nm ultraviolet excitation, luminous).
Fig. 5 is fresh sebum impression of the hand figure (365nm ultraviolet excitation, luminous) on glass.
Fig. 6 is the upper fresh sebum impression of the hand figure (365nm ultraviolet excitation, luminous) of paint wood.
Fig. 7 magnetic card is left over the sebum impression of the hand fluorogram (white light excites) of 1 month.
Fig. 8 magnetic card is left over the sebum impression of the hand figure (365nm ultraviolet excitation, luminous) of 1 month.
Fig. 9 is fresh diving hand print with perspiration figure (luminous) on ticker tape.
Figure 10 is fresh diving hand print with perspiration figure (luminous) on leather.
Figure 11 is fresh sebum impression of the hand fluorescence contrast figure on complex background object (left-half is that steady persistence powder manifests, and right half part is that common phosphors manifests, and white light excites).
Fresh sebum impression of the hand comparison diagram (white light excites, luminous) on Figure 12 complex background object.
Embodiment:
Embodiment 1, the invention provides a kind of rare earth long afterglow luminescent powder, and the general structure of its compound is M
2mgSi
2o
7︰ 0.02Eu
2+, 0.04Dy
3+, wherein M is one or both in Sr, Ca, and the particle diameter of this rare earth long afterglow luminescent powder is 1 ~ 3 μm.As shown in Figure 2, when M is Sr, utilize FDAC F-4500 type luminoscope to detect, the excitation wavelength range of this rare earth long afterglow luminescent powder is 250 ~ 450nm, and emission wavelength is 466nm.
The luminous time of persistence of this rare earth long afterglow luminescent powder is more than 2 hours.In the present embodiment, the measuring method of luminous time of persistence is: irradiation luminous material 5 minutes under sunlight, is then placed in darkroom and observes its luminous situation.
The preparation method of above-mentioned rare earth long afterglow luminescent powder, it comprises the following steps:
1), MCO is taken according to stoichiometric ratio
3, MgCO
3, SiO
2, Eu
2o
3and Dy
2o
3, then take the solubility promoter H of above-mentioned raw materials total mass 10%
3bO
3or B
2o
3;
2), by step 1) raw material that takes and solubility promoter mixing, in agate mortar, grind half an hour, then proceed in corundum crucible in 1000 DEG C of pre-burnings 1 hour;
3), by the sample of above-mentioned pre-burning again grind half an hour, adopt high temperature solid-state method in gac reducing atmosphere, be heated to 1150 DEG C of sintering and obtain thick product in 3 hours;
4), thick for above-mentioned long after glow luminous material product is ground, then in dispersion agent dehydrated alcohol, carry out ball milling 15 minutes, stratification removing supernatant, puts into far infrared drying oven by throw out, at 90 DEG C of dry 2h, obtain the powder of particle diameter fine uniform.The XRD analysis utilizing Japanese RIGAKU.D/max-3B powder diffraction instrument to detect, confirms that this product is target product, as shown in Figure 1 (75-1736 is consistent for contrast international standard card).
Apply above-mentioned rare earth long afterglow luminescent powder manifests reagent method as latent fingerprint, it comprises the following steps:
1), adopt 300 mesh sieves to be sieved by commercially available reduced iron powder, then by rare earth long afterglow luminescent powder with sieve the iron powder that obtains in mass ratio for the ratio of 1:8 mixes, obtain mixture;
2), Magnetic brush brush is adopted to show method by step 1) mixture that obtains manifests the latent fingerprint that the impermeability objects such as aluminium foil, ceramic tile, glass, paint wood, magnetic card are left over;
3), irradiate the impression of the hand manifested gather handprint images after 30 seconds by white light or UV-light (365nm), handprint images as shown in Figures 3 to 8.From Fig. 3 to Fig. 8, rare earth long afterglow luminescent powder of the present invention has clearly shown the feature streakline details of potential impression of the hand on the impermeability objects such as aluminium foil, ceramic tile, glass, paint wood, magnetic card.
Embodiment 2
The rare earth long afterglow luminescent powder that Application Example 1 prepares manifests the method for reagent as latent fingerprint, and it comprises the following steps:
1), adopt 100 mesh sieves to be sieved by commercially available reduced iron powder, the rare earth long afterglow luminescent powder then embodiment 1 prepared with sieve the iron powder that obtains in mass ratio for the ratio of 1:10 mixes, obtain mixture;
2), Magnetic brush brush is adopted to show method by step 1) the mixture brush that obtains shows the fresh diving hand print with perspiration that the semipermeability such as ticker tape, leather object is left over;
3), irradiate by white light or UV-light (365nm) impression of the hand manifested and gather handprint images after 30 seconds.M
2mgSi
2o
7︰ 0.02Eu
2+, 0.04Dy
3+on the semipermeability object that (when M is Sr) steady persistence powder manifests, latent fingerprint imaging picture as shown in Figure 9, Figure 10.From Fig. 9, Figure 10, rare earth long afterglow luminescent powder of the present invention has clearly shown potential impression of the hand feature streakline details on the semipermeability such as ticker tape, leather object.
Embodiment 3
The rare earth long afterglow luminescent powder that Application Example 1 prepares manifests the method for reagent as latent fingerprint, and it comprises the following steps:
1), adopt 100 mesh sieves to be sieved by commercially available reduced iron powder, the rare earth long afterglow luminescent powder then embodiment 1 prepared with sieve the iron powder that obtains in mass ratio for the ratio of 1:9 mixes, obtain mixture;
2), Magnetic brush brush is adopted to show method by step 1) the mixture brush that obtains shows fresh sebum impression of the hand on complex background object;
3) impression of the hand, by white light manifested, gathers the handprint images under two kinds of different modes respectively: first is under light source activation pattern, gathers impression of the hand fluoroscopic image; Second is removing under light source mode, gathering luminous handprint images in dark room conditions.M
2mgSi
2o
7︰ 0.02Eu
2+, 0.04Dy
3+on the complex background object that (when M is for Sr) steady persistence powder and common phosphors manifest, fresh sebum impression of the hand imaging picture is as shown in Figure 11, Figure 12, Figure 11, Figure 12 are one piece of complete finger mark and cut into two portions, left-half is the image that steady persistence powder manifests, and right half part is the image that common phosphors manifests.From Figure 11, Figure 12, rare earth long afterglow luminescent powder of the present invention no matter luminous intensity, still manifests (imaging) effect and is all better than common phosphors, also achieve the imaging of temporal resolution impression of the hand simultaneously, effectively eliminate or reduce background interference.
Other rare earth silicate steady persistence powder Sr
2-xca
xmgSi
2o
7︰ 0.02Eu
2+, 0.04Dy
3+the preparation of (0≤x≤2) and manifest impression of the hand method and Sr
2mgSi
2o
7︰ 0.02Eu
2+, 0.04Dy
3+similar, no longer describe in detail in this specification sheets.
Claims (10)
1. rare earth silicate long-afterglow luminescent powder, is characterized in that: the general structure of its compound is M
2mgSi
2o
7︰ 0.02Eu
2+, 0.04Dy
3+, M is one or both in Sr, Ca.
2. rare earth silicate long-afterglow luminescent powder according to claim 1, it is characterized in that: the excitation wavelength range of described rare earth long afterglow luminescent powder is 250 ~ 468nm, emission wavelength peak when M is Sr is 466nm, emission wavelength peak when M is Ca is 533nm, M is that Sr, Ca are when coexisting, along with the change of Sr/Ca ratio, the emission wavelength peak of steady persistence powder changes between 466 ~ 533nm.
3. rare earth silicate long-afterglow luminescent powder according to claim 1, is characterized in that: the luminous time of persistence of described rare earth long afterglow luminescent powder is more than 2 hours.
4. the preparation method of rare earth long afterglow luminescent powder, is characterized in that: it comprises the following steps:
1), MCO is taken according to stoichiometric ratio
3, MgCO
3, SiO
2, Eu
2o
3and Dy
2o
3, then take the solubility promoter H of above-mentioned raw materials total mass 10%
3bO
3or B
2o
3;
2), by step 1) raw material that takes and solubility promoter mixing, in agate mortar, grind half an hour, then proceed in corundum crucible in 1000 DEG C of pre-burnings 1 hour;
3), by the sample of above-mentioned pre-burning again grind half an hour, adopt high temperature solid-state method in gac reducing atmosphere, be heated to 1150 DEG C of sintering and obtain thick product in 3 hours;
4), by thick for above-mentioned long after glow luminous material product grind, then in dispersion agent, carry out ball milling, elimination dispersion agent, be drying to obtain described rare earth long afterglow luminescent powder.
5. rare earth long afterglow luminescent powder according to claim 1 manifests the method for reagent as latent fingerprint, it is characterized in that: it comprises the following steps:
1), adopt 300 ~ 400 mesh sieves to be sieved by reduced iron powder, the ratio being then 1:8 ~ 10 in mass ratio by rare earth long afterglow luminescent powder and the iron powder that obtains of sieving mixes, and obtains mixture;
2), by step 1) mixture that obtains manifests potential impression of the hand on object;
3) impression of the hand, by white light or UV-irradiation manifested, gathers handprint images; Or under gauge without light source irradiation mode, gather luminous handprint images.
6. rare earth long afterglow luminescent powder according to claim 5 manifests the method for reagent as latent fingerprint, it is characterized in that: described step 2) in be adopt Magnetic brush brush to show method mixture brush to be shown the potential impression of the hand that object is left over.
7. rare earth long afterglow luminescent powder according to claim 5 manifests the method for reagent as latent fingerprint, it is characterized in that: described object comprises impermeability object or semipermeability object.
8. the rare earth long afterglow luminescent powder according to claim 5 or 6 or 7 manifests the method for reagent as latent fingerprint, it is characterized in that: described object comprises ceramic tile, plastic sheet, glass, smooth cardboard, copy paper or leather.
9. the rare earth long afterglow luminescent powder according to claim 5 or 6 manifests the method for reagent as latent fingerprint, it is characterized in that: described impression of the hand type is sebum or diving hand print with perspiration.
10. rare earth long afterglow luminescent powder according to claim 5 manifests the method for reagent as latent fingerprint, it is characterized in that: described step 3) in be using the UV-light of 365nm or visible ray as excitation light source, irradiate the impression of the hand manifested and gather handprint images after 30 seconds.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106367059A (en) * | 2016-08-01 | 2017-02-01 | 李安格 | Preparation method for fluorescence development powder |
| CN114032090A (en) * | 2021-12-03 | 2022-02-11 | 广东电网有限责任公司 | Yellow-green afterglow material and preparation method thereof |
| CN111190004B (en) * | 2020-01-10 | 2023-11-10 | 上海泰辉生物科技有限公司 | Instant detection system of immunochromatography test strip |
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2015
- 2015-02-03 CN CN201510054494.6A patent/CN104560031A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102746845A (en) * | 2012-07-20 | 2012-10-24 | 中国地质大学（武汉） | Rare earth long-persistence luminescent powder, preparation method and application thereof |
Non-Patent Citations (2)
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| LI LIU 等: "The effectiveness of strong afterglow phosphor powder in the detection", 《FORENSIC SCIENCE INTERNATIONAL》, vol. 183, 20 October 2008 (2008-10-20) * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106367059A (en) * | 2016-08-01 | 2017-02-01 | 李安格 | Preparation method for fluorescence development powder |
| CN111190004B (en) * | 2020-01-10 | 2023-11-10 | 上海泰辉生物科技有限公司 | Instant detection system of immunochromatography test strip |
| CN114032090A (en) * | 2021-12-03 | 2022-02-11 | 广东电网有限责任公司 | Yellow-green afterglow material and preparation method thereof |
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Application publication date: 20150429 |