CN101565619A - Small-particle yellow rare-earth fluorescent powder and preparation method and purpose of visualizing latent fingerprint thereof - Google Patents

Small-particle yellow rare-earth fluorescent powder and preparation method and purpose of visualizing latent fingerprint thereof Download PDF

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CN101565619A
CN101565619A CNA2009100622780A CN200910062278A CN101565619A CN 101565619 A CN101565619 A CN 101565619A CN A2009100622780 A CNA2009100622780 A CN A2009100622780A CN 200910062278 A CN200910062278 A CN 200910062278A CN 101565619 A CN101565619 A CN 101565619A
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small
fluorescent powder
earth fluorescent
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CN101565619B (en
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袁曦明
李柳
熊晓波
张剑
王娟娟
王峰
谢安
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China University of Geosciences
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China University of Geosciences
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Abstract

The invention discloses small-particle yellow rare-earth fluorescent powder and a preparation method and a purpose of visualizing a latent fingerprint thereof. The general structure formula of the fluorescent powder is Y3-x-yCexGdyA15O12, wherein the x is not less than 0.1 and no larger than 0.4, y is no less than 0.1 and no larger than 0.4 and the particle size is between 1.5 to 3 Mum. The preparation method comprises the steps of weighing up raw materials according to the stoichiometric ratio of the structure formula, grinding and evenly mixing up the raw materials, sintering the raw materials with high-temperature solid-phase method to obtain powder and obtaining the small-particle yellow rare-earth fluorescent powder by adopting an ultrasonic dispersion technology after the powder goes through a mesh with 300 to 400 eyes. The small-particle yellow rare-earth fluorescent powder can be applied to visualizing the latent finger print after being amido-functionalized by gamma-Aminopropyl triethoxy silane and being mixed with reduced iron powder which goes through a mesh according to a certain ratio. The fluorescent powder provided by the invention has even and small particles, high fluorescent intensity, the excitation wave length between 460 to 480nm which is within the range of the light source commonly used in criminal investigation and the emission wave length between 520 to 570nm, is conducive to visualizing the latent finger print on the site and eliminating the disturbance of the object background and is important for establishing a high-efficient, non-toxic, lossless and convenient finger print visualizing method.

Description

Small-particle yellow rare-earth fluorescent powder and preparation method thereof and the purposes that manifests latent fingerprint
Technical field
The present invention relates to a kind of small-particle yellow rare-earth fluorescent powder and preparation method thereof and the purposes that manifests latent fingerprint, belong to material science, also belong to the forensic science field.
Background technology
The fingerprint displaying technology is as the important branch of forensic science, the development of a century on the process, and having developed into a kind of physics, chemistry, biology, optics of collecting is the science of one.Though the fingerprint displaying technology reaches its maturity, but still it is to be solved to exist a series of problem to have.At first, the process for show of the unfavorable fingerprint sample of many objective condition still is left to be desired; Secondly, existingly manifest reagent and still there is potential safety hazard in process for show, as take to brush be suspended in airborne dust when showing method, some has the fluorescence dye of carcinogenesis and with the toxic and harmful of smoked material decomposition reaction generation when showing method, they all cause serious harm to professional and technical personnel healthy.In addition, some has the use of color reagent can destroy the virgin state of material evidence; Some manifests reagent (as DFO etc.) and can't extensively promote in real work because cost is higher; Some incomplete latent fingerprint own still needs to keep the biological activity of finger mark after manifesting, so that carry out deep DNA check etc., these all become the problem that the forensic science staff must face.
At above problem, the optical check method with highly sensitive short grained rare-earth phosphor powder method and safety has obtained further developing.The short grained rare-earth phosphor raw material is easy to get, and easily preparation, wherein rare-earth yellow emitting phosphor powder has optical signatures such as good light stability, fluorescence intensity height, exciting light safety, utilize the short grained rare-earth luminescent material to manifest potential impression of the hand, it is a kind of easy, nontoxic, harmless process for show, can solve the bottleneck of latent fingerprint appearing technique development, and open up the frontier that fluorescent RE powder is used.
But do not occur as yet about small-particle yellow rare-earth fluorescent powder Y at present 3-x-yCe xGd yAl 5O 12And preparation method thereof and use it for the bibliographical information that manifests latent fingerprint.
Summary of the invention
The objective of the invention is to remedy the deficiencies in the prior art; a kind of small-particle yellow rare-earth fluorescent powder and preparation method thereof and the purposes that manifests latent fingerprint are provided; this fluorescent powder grain is tiny evenly; particle diameter is 1.5～3 μ m; its excitation wavelength is that 460～480nm is in criminal investigation light source scope commonly used; emission wavelength is 520～570nm; being convenient to on-the-spot latent fingerprint manifests; and this fluorescent material has higher fluorescence intensity; the object background interference can be rejected after manifesting impression of the hand, the impression of the hand of leaving on common permeability object and the impermeability object surface can be successfully manifested.
The technical scheme that realizes the object of the invention is: a kind of small-particle yellow rare-earth fluorescent powder, the general structure of this fluorescent material are Y 3-x-yCe xGd yAl 5O 12, wherein, 0.1≤x≤0.4,0.1≤y≤0.4, particle diameter is 1.5～3 μ m.
The excitation wavelength of described small-particle yellow rare-earth fluorescent powder is 460～480nm, and emission wavelength is 520～570nm.
The preparation method of small-particle yellow rare-earth fluorescent powder of the present invention is:
(1) presses Y 3-x-yCe xGd yAl 5O 12The stoichiometric ratio of middle metallic element, wherein, 0.1≤x≤0.4,0.1≤y≤0.4 takes by weighing Al 2O 3, Y 2O 3, CeO 2And Gd 2O 3, with the Al that weighs up 2O 3, Y 2O 3, CeO 2And Gd 2O 3Fully grind and mix;
(2) sample behind the mixing is put into the high temperature reduction stove, under logical hydrogen or the condition with carbon reducing agent, in 1200～1500 ℃ of sintering 1～5 hour, the powder that sintering is obtained cooled to room temperature with the furnace;
(3) cooled powder is ground, cross 300～400 mesh sieves, obtain the primary election powder;
(4) be after 1～5% salpeter solution soaks removal of impurities with primary election powder mass percent concentration; ultra-sonic dispersion, leave standstill, remove supernatant liquid, washing; repeat this ultra-sonic dispersion-leave standstill-remove supernatant liquid-water-washing step for several times; the dispersion system that obtains behind ultra-sonic dispersion is electric neutrality; leave standstill again and remove supernatant liquid, remaining throw out is drying to obtain small-particle yellow rare-earth fluorescent powder in 90～110 ℃.
Above-mentioned steps is to take by weighing Al in (1) 2O 3, Y 2O 3, CeO 2And Gd 2O 3After, take by weighing BaF again 2Or H 3BO 3Or BaF 2With H 3BO 3Quality by 1: 1～15 is made fusing assistant than blended mixture, and the weight of fusing assistant is Al 2O 3, Y 2O 3, CeO 2And Gd 2O 30.5～3% of gross weight.
Small-particle yellow rare-earth fluorescent powder of the present invention is used to manifest latent fingerprint, and process for show may further comprise the steps:
(1) with small-particle yellow rare-earth fluorescent powder Y 3-x-yCe xGd yAl 5O 12, 0.1≤x≤0.4,0.1≤y≤0.4, the mixing solutions that is scattered in alcohol and water is in the γ-An Bingjisanyiyangjiguiwan hydrolyzed solution of solvent, wherein, the volume ratio of alcohol and water is 1: 8～10, Y 3-x-yCe xGd yAl 5O 12With the mass ratio of γ-An Bingjisanyiyangjiguiwan be 1: 0.03～0.06, vibrating under 70～90 ℃ of water bath condition then reacts fully, washing, drying obtain the Y of amino functional 3-x-yCe xGd yAl 5O 12
(2) reduced iron powder is crossed 300～400 mesh sieves, then with the Y of amino functional 3-x-yCe xGd yAl 5O 12With the iron powder that obtains of sieving be that 1: 8～10 mixed is even by mass ratio;
(3) with the Y of amino functional 3-x-yCe xGd yAl 5O 12Show the latent fingerprint of leaving on the object with the mixture brush of iron powder.
Alcohol is ethanol, n-propyl alcohol, Virahol, propyl carbinol or isopropylcarbinol described in the above-mentioned steps (1).
Be that water-bath was vibrated 1～2 hour under 70～90 ℃ of conditions in the above-mentioned steps (1).
Be that water-bath was vibrated 1.5 hours under 80 ℃ of conditions in the above-mentioned steps (1).
In the above-mentioned steps (3) Y with amino functional 3-x-yCe xGd yAl 5O 12Adopt the Magnetic brush brush to show the latent fingerprint of leaving on the apparent object of method brush with the mixture of iron powder.
After brush showed latent fingerprint, observation manifested the impression of the hand sharpness, gathered the finger mark image, can compare evaluation.
The present invention utilizes high temperature solid-state method to obtain small-particle yellow rare-earth fluorescent powder Y in conjunction with the ultrasonic dispersing technology 3-x-yCe xGd yAl 5O 12(0.1≤x≤0.4,0.1≤y≤0.4) has carried out the optimization aftertreatment according to manifesting the latent fingerprint requirement to this powder then.Fluorescent powder grain of the present invention is tiny evenly, and particle diameter is 1.5～3 μ m, its excitation wavelength be 460nm～480nm (blue light) in criminal investigation light source scope commonly used, emission wavelength is 520～570nm, is convenient to on-the-spot latent fingerprint and manifests; Have higher fluorescence intensity, can reject the object background interference after manifesting impression of the hand; Can successfully manifest sweat latent fingerprint and the grease impression of the hand left on common permeability object such as printer paper, true qualities wood, plastics, sheet glass, ceramic tile or pottery and the impermeability object surface; Utilize the Magnetic brush brush to show method and manifest latent fingerprint, can avoid tiny powder to be suspended in contaminate environment and harm personnel health in the air.The present invention has expanded fluorescent RE powder and has been applied in the scope that latent fingerprint manifests the field, has set up a kind of efficient, nontoxic, harmless, easy fingerprint displaying technology.
Description of drawings
Fig. 1 is the preparation of small-particle yellow rare-earth fluorescent powder of the present invention and the schema that manifests latent fingerprint;
Fig. 2 is the XRD figure of embodiment 1,2,3 gained small-particle yellow rare-earth fluorescent powders;
Fig. 3 is the ultraviolet-visible absorption spectroscopy of embodiment 1 small-particle yellow rare-earth fluorescent powder;
Fig. 4 is the excitation spectrum of embodiment 1 small-particle yellow rare-earth fluorescent powder;
Fig. 5 is the emmission spectrum of embodiment 1 small-particle yellow rare-earth fluorescent powder;
Fig. 6 is the SEM figure of embodiment 1 small-particle yellow rare-earth fluorescent powder;
Infrared spectrogram before and after Fig. 7 embodiment 1 small-particle yellow rare-earth fluorescent powder amination;
Fig. 8 leaves over 3 days sweat latent fingerprint figure for small-particle yellow rare-earth fluorescent powder brush of the present invention shows on the sheet glass;
Fig. 9 leaves over 30 days grease impression of the hand figure for small-particle yellow rare-earth fluorescent powder brush of the present invention shows on the sheet glass;
Figure 10 leaves over 1 day sweat latent fingerprint figure for small-particle yellow rare-earth fluorescent powder brush of the present invention shows on the paint wood.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with specific embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1
(1) presses Y 3-x-yCe xGd yAl 5O 12In the stoichiometric ratio of metallic element (x=0.2 wherein, y=0.2), promptly in Y: the ratio of the amount of substance of Ce: Gd: Al is 2.6: 0.2: 0.2: 5 ratio takes by weighing Al 2O 3, Y 2O 3, CeO 2And Gd 2O 3, take by weighing then and be equivalent to Al 2O 3, Y 2O 3, CeO 2And Gd 2O 3The BaF of gross weight 2% 2Make fusing assistant, load weighted reagent is placed in the agate mortar milling time 20～60min it is ground evenly, after it is mixed, in the corundum crucible of packing into;
(2) corundum crucible that reagent will be housed is put into the high temperature reduction stove, under hydrogen reducing atmosphere (or with carbon reducing agent) condition, in 1400 ℃ of sintering 4 hours, treats then to take out after sample cools to room temperature with the furnace;
(3) powder that sintering is obtained grinds, and crosses 300 mesh sieves, obtains the primary election powder;
Ask removal of impurities when being one section of 3% nitric acid dousing with primary election powder mass percent concentration (4), (ultra-sonic dispersion is uniformly dispersed powder and gets final product ultra-sonic dispersion 5min then, be generally 5～15min), remove supernatant liquid behind the standing demix, add distilled water again and carry out stirring and washing, ultra-sonic dispersion 5min, leave standstill and treat the solution layering, remove supernatant liquid, so repeat for several times, the dispersion system behind ultra-sonic dispersion is electric neutrality, the elimination supernatant liquid, remaining throw out is put into far infrared drying oven, and dry 3h under 90 ℃ obtains product.Through XRD analysis (contrast international standard card 70-1677 unanimity), confirm that this product is target product Y 2.6Ce 0.2Gd 0.2Al 5O 12, see curve 1 among Fig. 2.The ultraviolet-visible absorption spectroscopy of this yellow rare-earth fluorescent powder, excitation spectrum, emmission spectrum and SEM figure are respectively shown in Fig. 3,4,5 and 6.
(5) get Y 2.6Ce 0.2Gd 0.2Al 5O 12Sample, the mixing solutions (wherein the volume ratio of second alcohol and water is 1: 9) that is scattered in the second alcohol and water is in γ-An Bingjisanyiyangjiguiwan (the being silane coupling agent KH550) hydrolyzed solution of solvent, makes Y 3-x-yCe xGd yAl 5O 12The mass ratio of sample and γ-An Bingjisanyiyangjiguiwan is 1: 0.03, and vibrate under 70 ℃ of water bath condition then reacted fully in 1～2 hour, and washing, drying obtain the Y of amino functional again 2.6Ce 0.2Gd 0.2Al 5O 12, the dress sample is standby;
Infrared spectrogram before and after this fluorescent material amination as shown in Figure 7, wherein curve A is the infrared spectra of sample before the amination, curve B is the infrared spectra of sample after the amination.
(6) commercially available reduced iron powder is crossed 300 mesh sieves, then with the Y of amino functional 2.6Ce 0.2Gd 0.2Al 5O 12With the iron powder that obtains of sieving be that 1: 8 mixed is even by mass ratio;
(7) brush the latent fingerprint of leaving on apparent printer paper, paint wood, plastics, sheet glass and the ceramic tile respectively with step (6) gained mixture;
(8) gather the light source observation with alert light I type material evidence and manifest the impression of the hand sharpness, the NUANCE420 multispectral analysis system acquisition finger mark image with U.S. CIS company can contrast evaluation.
Embodiment 2
(1) presses Y 3-x-yCe xGd yAl 5O 12In the stoichiometric ratio of metallic element (x=0.1 wherein, y=0.1), promptly in Y: the ratio of the amount of substance of Ce: Gd: Al is 2.8: 0.1: 0.1: 5 ratio takes by weighing Al 2O 3, Y 2O 3, CeO 2And Gd 2O 3, take by weighing then and be equivalent to Al 2O 3, Y 2O 3, CeO 2And Gd 2O 3The H of gross weight 0.5% 3BO 3Make fusing assistant, load weighted reagent is placed in the agate mortar milling time 20～60min it is ground evenly, after it is mixed, in the corundum crucible of packing into;
(2) corundum crucible that reagent will be housed is put into the high temperature reduction stove, under hydrogen reducing atmosphere (or with carbon reducing agent) condition, in 1500 ℃ of sintering 2 hours, treats then to take out after sample cools to room temperature with the furnace;
(3) powder that sintering is obtained grinds, and crosses 360 mesh sieves, obtains the primary election powder;
(4) with primary election powder mass percent concentration be nitric acid dousing for some time removal of impurities of 1%, ultra-sonic dispersion 10min removes supernatant liquid behind the standing demix then, add distilled water again and carry out stirring and washing, ultra-sonic dispersion 10min leaves standstill and treats the solution layering, removes supernatant liquid, so repeat for several times, dispersion system behind ultra-sonic dispersion is electric neutrality, and the elimination supernatant liquid is put into far infrared drying oven with remaining throw out, dry 2h under 100 ℃ obtains product.By the method identical product is carried out XRD analysis (contrast international standard card 70-1677 unanimity), confirm that this product is target product Y with embodiment 1 2.8Ce 0.1Gd 0.1Al 5O 12, see curve 2 among Fig. 2.
(5) get Y 2.8Ce 0.1Gd 0.1Al 5O 12Sample, the mixing solutions (wherein the volume ratio of n-propyl alcohol and water is 1: 8) that is scattered in n-propyl alcohol and water is in γ-An Bingjisanyiyangjiguiwan (the being silane coupling agent KH550) hydrolyzed solution of solvent, makes Y 3-x-yCe xGd yAl 5O 12The mass ratio of sample and γ-An Bingjisanyiyangjiguiwan is 1: 0.05, and vibration reacted fully in 1.5 hours under 80 ℃ of water bath condition then, and washing, drying again obtain the Y of amino functional 2.8Ce 0.1Gd 0.1Al 5O 12, the dress sample is standby;
(6) commercially available reduced iron powder is crossed 300 mesh sieves, then with the Y of amino functional 2.8Ce 0.1Gd 0.1Al 5O 12With the iron powder that obtains of sieving be that 1: 9 mixed is even by mass ratio;
(7) show the latent fingerprint of leaving on printer paper, paint wood, plastics, sheet glass, the ceramic tile with step (6) gained mixture brush;
(8) gather the light source observation with alert light I type material evidence and manifest the impression of the hand sharpness, the NUANCE420 multispectral analysis system acquisition finger mark image with U.S. CIS company can contrast evaluation.
Embodiment 3
(1) presses Y 3-x-yCe xGd yAl 5O 12In the stoichiometric ratio of metallic element (x=0.4 wherein, y=0.4), promptly in Y: the ratio of the amount of substance of Ce: Gd: Al is 2.2: 0.4: 0.4: 5 ratio takes by weighing Al 2O 3, Y 2O 3, CeO 2And Gd 2O 3, take by weighing then and be equivalent to Al 2O 3, Y 2O 3, CeO 2And Gd 2O 3The BaF of gross weight 3% 2With H 3BO 3Mixture (BaF wherein 2With H 3BO 3Mass ratio is 1: 1～15) make fusing assistant, load weighted reagent is placed on grinds 20～60min in the agate mortar it is ground evenly, after it is mixed, in the corundum crucible of packing into;
(2) corundum crucible that reagent will be housed is put into the high temperature reduction stove, under hydrogen reducing atmosphere (or with carbon reducing agent) condition, in 1200 ℃ of sintering 5 hours, treats then to take out after sample cools to room temperature with the furnace;
(3) powder that sintering is obtained grinds, and crosses 360 mesh sieves, obtains the primary election powder;
(4) with primary election powder mass percent concentration be nitric acid dousing for some time removal of impurities of 5%, ultra-sonic dispersion 15min removes supernatant liquid behind the standing demix then, add distilled water again and carry out stirring and washing, ultra-sonic dispersion 15min leaves standstill and treats the solution layering, removes supernatant liquid, so repeat for several times, dispersion system behind ultra-sonic dispersion is electric neutrality, and the elimination supernatant liquid is put into far infrared drying oven with remaining throw out, dry 2h under 110 ℃ obtains product.By the method identical product is carried out XRD analysis (contrast international standard card 70-1677 unanimity), confirm that this product is target product Y with embodiment 1 2.2Ce 0.4Gd 0.4Al 5O 12, see curve 3 among Fig. 2.
(5) get Y 2.2Ce 0.4Gd 0.4Al 5O 12Sample, the mixing solutions (wherein the volume ratio of propyl carbinol and water is 1: 10) that is scattered in propyl carbinol and water is in γ-An Bingjisanyiyangjiguiwan (the being silane coupling agent KH550) hydrolyzed solution of solvent, makes Y 3-x-yCe xGd yAl 5O 12The mass ratio of sample and γ-An Bingjisanyiyangjiguiwan is 1: 0.06, and vibrate under 90 ℃ of water bath condition then reacted fully in 1～2 hour, and washing, drying obtain the Y of amino functional again 2.2Ce 0.4Gd 0.4Al 5O 12, the dress sample is standby;
(6) commercially available reduced iron powder is crossed 400 mesh sieves, then with the Y of amino functional 2.2Ce 0.4Gd 0.4Al 5O 12With the iron powder that obtains of sieving be that 1: 9 mixed is even by mass ratio;
(7) adopt the Magnetic brush brush to show method and show the latent fingerprint of leaving on printer paper, paint wood, plastics, sheet glass, the ceramic tile with step (6) gained mixture brush;
(8) gather the light source observation with alert light I type material evidence and manifest the impression of the hand sharpness, the NUANCE420 multispectral analysis system acquisition finger mark image with U.S. CIS company can contrast evaluation.
Fig. 8,9 and 10 is respectively small-particle yellow rare-earth fluorescent powder of the present invention brush and shows on the grease impression of the hand figure that leaves over 30 days on the sweat latent fingerprint figure that leaves over 3 days on the sheet glass, the sheet glass and the paint wood and leave over 1 day sweat latent fingerprint figure.

Claims (10)

1. small-particle yellow rare-earth fluorescent powder, it is characterized in that: the general structure of this fluorescent material is Y 3-x-yCe xGd yAl 5O 12, wherein, 0.1≤x≤0.4,0.1≤y≤0.4, particle diameter is 1.5～3 μ m.
2. small-particle yellow rare-earth fluorescent powder according to claim 1 is characterized in that: the excitation wavelength of this fluorescent material is 460～480nm, and emission wavelength is 520～570nm.
3. the preparation method of the described small-particle yellow rare-earth fluorescent powder of claim 1 is characterized in that may further comprise the steps:
(1) presses Y 3-x-yCe xGd yAl 5O 12The stoichiometric ratio of middle metallic element, wherein, 0.1≤x≤0.4,0.1≤y≤0.4 takes by weighing Al 2O 3, Y 2O 3, CeO 2And Gd 2O 3, with the Al that weighs up 2O 3, Y 2O 3, CeO 2And Gd 2O 3Fully grind and mix;
(2) sample behind the mixing is put into the high temperature reduction stove, under logical hydrogen or the condition with carbon reducing agent, in 1200～1500 ℃ of sintering 1～5 hour, the powder that sintering is obtained cooled to room temperature with the furnace;
(3) cooled powder is ground, cross 300～400 mesh sieves, obtain the primary election powder;
(4) be after 1～5% salpeter solution soaks removal of impurities with primary election powder mass percent concentration; ultra-sonic dispersion, leave standstill, remove supernatant liquid, washing; repeat this ultra-sonic dispersion-leave standstill-remove supernatant liquid-water-washing step for several times; the dispersion system that obtains behind ultra-sonic dispersion is electric neutrality; leave standstill again and remove supernatant liquid, remaining throw out is drying to obtain small-particle yellow rare-earth fluorescent powder in 90～110 ℃.
4. the preparation method of small-particle yellow rare-earth fluorescent powder according to claim 3, it is characterized in that: step is to take by weighing Al in (1) 2O 3, Y 2O 3, CeO 2And Gd 2O 3After, take by weighing BaF again 2Or H 3BO 3Or BaF 2With H 3BO 3Quality by 1: 1～15 is made fusing assistant than blended mixture, and the weight of fusing assistant is Al 2O 3, Y 2O 3, CeO 2And Gd 2O 30.5～3% of gross weight.
5. small-particle yellow rare-earth fluorescent powder as claimed in claim 1 is used to manifest the purposes of latent fingerprint.
6. small-particle yellow rare-earth fluorescent powder according to claim 5 is used to manifest the purposes of latent fingerprint, it is characterized in that the concrete steps that described small-particle yellow rare-earth fluorescent powder is used to manifest latent fingerprint are:
(1) with small-particle yellow rare-earth fluorescent powder Y 3-x-yCe xGd yAl 5O 12, 0.1≤x≤0.4,0.1≤y≤0.4, the mixing solutions that is scattered in alcohol and water is in the γ-An Bingjisanyiyangjiguiwan hydrolyzed solution of solvent, wherein, the volume ratio of alcohol and water is 1: 8～10, Y 3-x-yCe xGd yAl 5O 12With the mass ratio of γ-An Bingjisanyiyangjiguiwan be 1: 0.03～0.06, vibrating under 70～90 ℃ of water bath condition then reacts fully, washing, drying obtain the Y of amino functional 3-x-yCe xGd yAl 5O 12
(2) reduced iron powder is crossed 300～400 mesh sieves, then with the Y of amino functional 3-x-yCe xGd yAl 5O 12With the iron powder that obtains of sieving be that 1: 8～10 mixed is even by mass ratio;
(3) Y of usefulness amino functional 3-x-yCe xGd yAl 5O 12Show the latent fingerprint of leaving on the object with the mixture brush of iron powder.
7. small-particle yellow rare-earth fluorescent powder according to claim 6 is used to manifest the purposes of latent fingerprint, it is characterized in that: alcohol described in the step (1) is ethanol, n-propyl alcohol, Virahol, propyl carbinol or isopropylcarbinol.
8. small-particle yellow rare-earth fluorescent powder according to claim 6 is used to manifest the purposes of latent fingerprint, it is characterized in that: be that water-bath was vibrated 1～2 hour under 70～90 ℃ of conditions in the step (1).
9. small-particle yellow rare-earth fluorescent powder according to claim 8 is used to manifest the purposes of latent fingerprint, it is characterized in that: be that water-bath was vibrated 1.5 hours under 80 ℃ of conditions in the step (1).
10. small-particle yellow rare-earth fluorescent powder according to claim 6 is used to manifest the purposes of latent fingerprint, it is characterized in that: be the Y with amino functional in the step (3) 3-x-yCe xGd yAl 5O 12Adopt the Magnetic brush brush to show the latent fingerprint of leaving on the apparent object of method brush with the mixture of iron powder.
CN200910062278A 2009-05-27 2009-05-27 Small-particle yellow rare-earth fluorescent powder and preparation method and purpose of visualizing latent fingerprint thereof Expired - Fee Related CN101565619B (en)

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CN102703074A (en) * 2012-03-12 2012-10-03 芜湖旭普荧光材料科技有限公司 Preparation method of yellow fluorescent powder
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
CN102746845B (en) * 2012-07-20 2014-07-09 中国地质大学（武汉） Rare earth long-persistence luminescent powder, preparation method and application thereof
CN103815915A (en) * 2014-03-25 2014-05-28 黄大明 Method and device for fingerprint brush to dip in fingerprint powder
CN104382600B (en) * 2014-11-24 2017-01-11 中国刑事警察学院 Two-step latent fingerprint manifesting method based on nano-particles
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
CN104352242A (en) * 2014-11-24 2015-02-18 中国刑事警察学院 Method for displaying latent fingerprints by surface-modified aluminum oxide nano particles
CN104352242B (en) * 2014-11-24 2017-02-08 中国刑事警察学院 Method for displaying latent fingerprints by surface-modified aluminum oxide nano particles
CN106367059A (en) * 2016-08-01 2017-02-01 李安格 Preparation method for fluorescence development powder
CN113841978A (en) * 2021-10-26 2021-12-28 中国地质大学（北京） Method for preparing yellow chalcedony by optimizing and processing gray white chalcedony
CN113841978B (en) * 2021-10-26 2023-09-05 中国地质大学（北京） Method for preparing yellow and chalcedony by optimizing off-white chalcedony
CN114479829A (en) * 2021-12-15 2022-05-13 重庆盾银科技有限公司 Photosensitive visualization reagent and preparation method thereof
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