CN105907389A - Preparation methods of noble-metal nanocluster development reagents and sweat fingerprint development method - Google Patents
Preparation methods of noble-metal nanocluster development reagents and sweat fingerprint development method Download PDFInfo
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- CN105907389A CN105907389A CN201610283026.0A CN201610283026A CN105907389A CN 105907389 A CN105907389 A CN 105907389A CN 201610283026 A CN201610283026 A CN 201610283026A CN 105907389 A CN105907389 A CN 105907389A
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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
- C09K11/58—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing copper, silver or gold
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/117—Identification of persons
- A61B5/1171—Identification of persons based on the shapes or appearances of their bodies or parts thereof
- A61B5/1172—Identification of persons based on the shapes or appearances of their bodies or parts thereof using fingerprinting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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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
- C09K11/87—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing platina group metals
Abstract
The invention provides preparation methods of four kinds of noble-metal nanocluster development reagents and sweat fingerprint development methods. Noble-metal nanoclusters are one of gold nanoclusters, silver nanoclusters, gold-silver alloy nanoclusters and platinum noble-metal nanoclusters; the noble-metal nanocluster development reagents are prepared through an ultrasound-microwave assisted preparation method. The old sweat fingerprint development methods include six steps of reagent preparation, fingerprint restrain, fingerprint drip development, flooding washing, fingerprint drying and fingerprint observation and fixation. The prepared gold, silver, gold-silver alloy and platinum fluorescent noble-metal nanoclusters are high in fluorescent quantum yield, long in fluorescence duration and low in toxicity; fingerprint development is fast and efficient in operation, 30-days-old fingerprints can be developed clearly, and the effect is superior to that of the development methods of conventional development reagents.
Description
Technical field
The invention belongs to public security Forensic Science finger mark and identify field, be specifically related to a kind of noble-metal nanoclusters and manifest reagent
Preparation and the method manifesting Sweat latent fingerprint.
Background technology
Noble-metal nanoclusters, as a kind of novel luminescent material, refers to be made up of several to dozens of precious metal atoms
Particle diameter in the cluster of about 2nm, there is the advantages such as more stable fluorescence property, high-biocompatibility, hypotoxicity, last decade
Coming, the photoluminescent property of noble-metal nanoclusters is mainly used in fluorescent probe detection metal ion, live cell fluorescent imaging, fluorescence biography
Sensor etc..But the research in science and technology concerning criminal matters field and application rarely have document to report, are still at the initial stage.
Fingerprint has people's thing trace characteristic variant, the most constant, tactile, has " human body identity card " and the U.S. of " king of evidence "
Claim, to disclosing, confirm crime and identifying that criminal has considerable effect.It is distributed on the mastoid process decorative pattern of people's both hands finger finger
Pore, the perspiration of pore secretion often contains oils and fats and other small materials.Therefore the Sweat latent fingerprint composition being retained on object
Comprise the Organic substances such as a small amount of water, a small amount of inorganic matter, protein, oils and fats.
Finger mark appearing technique has gone up the history of a century, and tradition process for show has 502 smoked aobvious method, ninhydrin method, DFO methods
Deng.Along with developing rapidly of nanotechnology, novel nano-material is applied to latent and manifests the concern causing researcher,
Occur in that and utilize metal, up-conversion luminescence, magnetic Nano material to manifest the methods such as finger mark.
Traditional fluorescent material, such as organic dyestuff, fluorescin, has cost of manufacture height, high toxicity, fluorescence duration time
Short and the shortcomings such as outmoded finger mark can not be manifested.At present, noble-metal nanoclusters synthesis to be used traditional heating method and hatches method, as
Ying seminar, under the conditions of hatching 12h, utilizes BSA to be prepared for, for protective agent and stabilizer, the Jenner that fluorescence quantum efficiency is 6%
Rice bunch, but this method time loss length, power consumption compared with big, response speed slow, particle diameter compared with big, to prepare product property low, in real work
In be difficult to be promoted.
The application manifesting aspect at latent of gold nanoclusters: patent 201310364617.7 prepares bovine serum albumin and protects
The red fluorescence gold nanoclusters protected, is applied to the labelling to fingerprint latent on PVDF membrane and adhesive tape substrate and shows
Existing, but this research manifests only for latent on semi-permeable object, and range of application is little.Patent 201210443554.X prepares
The fluorogold nano-cluster of glutathione functionalization, and be applied to Sweat latent fingerprint on silicon chip, glass, blood finger mark manifests, widen
The range of application that finger mark manifests.Above-mentioned two researchs all use tradition incubation heating means, the longest (12h-in preparation process
72h), complex operation, the advantage not possessing green high-efficient, combined coefficient is relatively low, and does not all explore and manifest outmoded effect.
From the foregoing, it will be observed that in existing finger mark appearing technique, conventional fluorescent material also exists cost of manufacture height, high toxicity, fluorescence
Persistent period is short and can not manifest the shortcomings such as outmoded finger mark；Gold nanoclusters also exists time-consuming longer (12h-72h), complex operation,
The problems such as combined coefficient is relatively low.
Summary of the invention
For solving the problems referred to above present in existing finger mark appearing technique, the present invention proposes a kind of noble-metal nanoclusters and manifests
The preparation of reagent and the method manifesting Sweat latent fingerprint.
A kind of noble-metal nanoclusters of the present invention manifests the preparation method of reagent, it is characterised in that described noble-metal nanoclusters
For any one in gold nanoclusters, silver nanoclusters, electrum nano-cluster and platinum noble metals nano-cluster；And described noble metal receives
Rice bunch is manifested reagent and is prepared by ultrasonic-microwave cooperating preparation method.
Further, described noble-metal nanoclusters is manifested reagent and is prepared by ultrasonic-microwave cooperating preparation method, including,
Prepare the method that gold nanoclusters manifests reagent, comprise the following steps:
(1) solution preparation, is dissolved in gold chloride pure water and is configured to the solution of 0.01 mol/L；Bovine serum albumin is 37 DEG C of conditions
Under be dissolved in pure water and be configured to 50 mg/mL solution；Potassium hydroxide is dissolved in pure water and is configured to 1 mol/L solution；
(2) hybrid reaction, is 1:1 by volume, chlorauric acid solution is added bovine serum albumin solution, is existed by mixed solution
3min is reacted under the effect of magnetic stirring apparatus；
(3) pH value regulation, is added drop-wise to the chlorauric acid solution obtained by step (2) molten with bovine serum albumin by potassium hydroxide solution
In the mixed liquor of liquid, regulation pH is 12；
(4) ultrasonic disperse, is placed in ultrasonic disperse 1h in ultrasonic washing instrument by the mixed solution obtained by step (3)；
(5) microwave radiation, is then placed in the solution obtained by step (4) in microwave oven, microwave radiation 40 ~ 60s, prepares gold
Nano-cluster manifests reagent；
Prepare the method that silver nanoclusters manifests reagent, comprise the following steps:
(1) solution preparation, is dissolved in silver nitrate pure water and is configured to the solution of 0.01 mol/L；Bovine serum albumin is 37 DEG C of conditions
Under be dissolved in pure water and be configured to 50 mg/mL solution；Potassium hydroxide is dissolved in pure water and is configured to 1 mol/L solution；
(2) hybrid reaction, is 1:1 by volume, silver nitrate solution is added bovine serum albumin solution, is existed by mixed solution
3min is reacted under the effect of magnetic stirring apparatus；
(3) pH value regulation, is added drop-wise to the silver nitrate solution obtained by step (2) and bovine serum albumin by potassium hydroxide solution
In the mixed liquor of solution, regulation pH is 12；
(4) ultrasonic disperse, is placed in ultrasonic disperse 1h in ultrasonic washing instrument by the mixed solution obtained by step (3)；
(5) microwave radiation, is then placed in the solution obtained by step (4) in microwave oven, microwave radiation 40 ~ 60s, prepares silver
Nano-cluster manifests reagent；
Prepare the method that gold silver nano-cluster manifests reagent, comprise the following steps:
(1) solution preparation, is dissolved in gold chloride pure water and is configured to the solution of 0.01 mol/L；Silver nitrate is dissolved in pure water and is configured to
The solution of 0.01 mol/L；Bovine serum albumin is dissolved in pure water under the conditions of 37 DEG C and is configured to 50 mg/mL solution；By hydroxide
Potassium is dissolved in pure water and is configured to 1 mol/L solution；
(2) hybrid reaction, is 1:1:2 by volume, and chlorauric acid solution, silver nitrate solution are added bovine serum albumin solution,
Mixed solution is reacted under the effect of magnetic stirring apparatus 3min；
(3) pH value regulation, is added drop-wise to potassium hydroxide solution in the mixed liquor obtained by step (2), and regulation pH is 12；
(4) ultrasonic disperse, is placed in ultrasonic disperse 1h in ultrasonic washing instrument by the mixed solution obtained by step (3)；
(5) microwave radiation, is then placed in the solution obtained by step (4) in microwave oven, microwave radiation 40 ~ 60s, prepares silver
Nano-cluster manifests reagent；
Prepare the method that platinum cluster manifests reagent, comprise the following steps:
(1) solution preparation, is dissolved in chloroplatinic acid pure water and is configured to the solution of 0.01 mol/L；Bovine serum albumin is at 37 DEG C of bars
It is dissolved in pure water under part and is configured to 50 mg/mL solution；Potassium hydroxide is dissolved in pure water and is configured to 1 mol/L solution；
(2) hybrid reaction, is 1:1 by volume, platinum acid chloride solution is added bovine serum albumin solution, is existed by mixed solution
3min is reacted under the effect of magnetic stirring apparatus；
(3) pH value regulation, is added drop-wise to the platinum acid chloride solution obtained by step (2) and bovine serum albumin by potassium hydroxide solution
In the mixed liquor of solution, regulation pH is 12；
(4) ultrasonic disperse, is placed in ultrasonic disperse 1h in ultrasonic washing instrument by the mixed solution obtained by step (3)；
(5) microwave radiation, is then placed in the solution obtained by step (4) in microwave oven, microwave radiation 40 ~ 60s, prepares silver
Nano-cluster manifests reagent.
Present invention additionally comprises and utilize above-mentioned noble-metal nanoclusters to manifest the method that reagent manifests outmoded Sweat latent fingerprint, including with
Lower step:
Prepared by S1, reagent, prepare noble-metal nanoclusters and manifest reagent；
S2, restraining finger mark, after hand washing is dried by volunteer only, on glass, plastics, preservative film, metal object, stamp antiperspirant is latent refers to
Print, it is thus achieved that finger mark sample.
S3, drip aobvious finger mark, by step S1 prepare manifest reagent drip aobvious step S2 prepare Sweat latent fingerprint, react 1-
3h；
S4, wash away loose colour, use ultra-pure water wash away step S3 drip aobvious after Sweat latent fingerprint loose colour；
S5, finger mark are dried, and step S4 washes away the Sweat latent fingerprint after loose colour and dries；
S6, finger mark are observed fixing, under manifesting viewing system, observe the Sweat latent fingerprint image after fixing step S5 is dried；
It is characterized in that, described noble-metal nanoclusters is that gold nanoclusters, silver nanoclusters, electrum nano-cluster and platinum noble metals are received
Rice bunch in any one.
Further, in described step S1 prepared by reagent, including,
Prepare the method that gold nanoclusters manifests reagent, comprise the following steps:
(1) solution preparation, is dissolved in gold chloride pure water and is configured to the solution of 0.01 mol/L；Bovine serum albumin is at 37 DEG C of bars
It is dissolved in pure water under part and is configured to 50 mg/mL solution；Potassium hydroxide is dissolved in pure water and is configured to 1 mol/L solution；
(2) hybrid reaction, is 1:1 by volume, chlorauric acid solution is added bovine serum albumin solution, is existed by mixed solution
3min is reacted under the effect of magnetic stirring apparatus；
(3) pH value regulation, is added drop-wise to the chlorauric acid solution obtained by step (2) and bovine serum albumin by potassium hydroxide solution
In the mixed liquor of solution, regulation pH is 12；
(4) ultrasonic disperse, is placed in ultrasonic disperse 1h in ultrasonic washing instrument by the mixed solution obtained by step (3)；
(5) microwave radiation, is then placed in the solution obtained by step (4) in microwave oven, microwave radiation 40 ~ 60s, prepares gold
Nano-cluster manifests reagent；
Prepare the method that silver nanoclusters manifests reagent, comprise the following steps:
(1) solution preparation, is dissolved in silver nitrate pure water and is configured to the solution of 0.01 mol/L；Bovine serum albumin is at 37 DEG C of bars
It is dissolved in pure water under part and is configured to 50 mg/mL solution；Potassium hydroxide is dissolved in pure water and is configured to 1 mol/L solution；
(2) hybrid reaction, is 1:1 by volume, silver nitrate solution is added bovine serum albumin solution, is existed by mixed solution
3min is reacted under the effect of magnetic stirring apparatus；
(3) pH value regulation, is added drop-wise to the silver nitrate solution obtained by step (2) and bovine serum albumin by potassium hydroxide solution
In the mixed liquor of solution, regulation pH is 12；
(4) ultrasonic disperse, is placed in ultrasonic disperse 1h in ultrasonic washing instrument by the mixed solution obtained by step (3)；
(5) microwave radiation, is then placed in the solution obtained by step (4) in microwave oven, microwave radiation 40 ~ 60s, prepares silver
Nano-cluster manifests reagent；
Prepare the method that gold silver nano-cluster manifests reagent, comprise the following steps:
(1) solution preparation, is dissolved in gold chloride pure water and is configured to the solution of 0.01 mol/L；Silver nitrate is dissolved in pure water and is configured to
The solution of 0.01 mol/L；Bovine serum albumin is dissolved in pure water under the conditions of 37 DEG C and is configured to 50 mg/mL solution；By hydroxide
Potassium is dissolved in pure water and is configured to 1 mol/L solution；
(2) hybrid reaction, is 1:1:2 by volume, and chlorauric acid solution, silver nitrate solution are added bovine serum albumin solution,
Mixed solution is reacted under the effect of magnetic stirring apparatus 3min；
(3) pH value regulation, is added drop-wise to potassium hydroxide solution in the mixed liquor obtained by step (2), and regulation pH is 12；
(4) ultrasonic disperse, is placed in ultrasonic disperse 1h in ultrasonic washing instrument by the mixed solution obtained by step (3)；
(5) microwave radiation, is then placed in the solution obtained by step (4) in microwave oven, microwave radiation 40 ~ 60s, prepares silver
Nano-cluster manifests reagent；
Prepare the method that platinum cluster manifests reagent, comprise the following steps:
(1) solution preparation, is dissolved in chloroplatinic acid pure water and is configured to the solution of 0.01 mol/L；Bovine serum albumin is at 37 DEG C of bars
It is dissolved in pure water under part and is configured to 50 mg/mL solution；Potassium hydroxide is dissolved in pure water and is configured to 1 mol/L solution；
(2) hybrid reaction, is 1:1 by volume, platinum acid chloride solution is added bovine serum albumin solution, is existed by mixed solution
3min is reacted under the effect of magnetic stirring apparatus；
(3) pH value regulation, is added drop-wise to the platinum acid chloride solution obtained by step (2) and bovine serum albumin by potassium hydroxide solution
In the mixed liquor of solution, regulation pH is 12；
(4) ultrasonic disperse, is placed in ultrasonic disperse 1h in ultrasonic washing instrument by the mixed solution obtained by step (3)；
(5) microwave radiation, is then placed in the solution obtained by step (4) in microwave oven, microwave radiation 40 ~ 60s, prepares silver
Nano-cluster manifests reagent.
Further, described step S2 restrains finger mark, including, it is thus achieved that resting period of finger mark sample be 7 30 days.
Further, described step S3 drips aobvious finger mark, including, receive with the noble metal obtained by glue head dropper aspiration step S1
Rice bunch manifests reagent so that it is drips aobvious clockwise along finger mark mastoid process streakline, and fully reacts 2h with finger mark material.
Further, described step S5 finger mark is dried, including, in baking oven machine vacuum, dry under the conditions of 37 DEG C.
Further, described step S6 finger mark is observed, including, manifest viewing system for utilizing alternative light source, coloured filter
What light microscopic, digital single-lens reflex camera were built manifests viewing system.
The present invention utilizes noble-metal nanoclusters size closer to Fermi's wavelength of metal electron, and it is with protein, aminoacid
In sulfydryl combine, there is the feature of good fluorescent characteristic, and by ultrasonic with microwave cooperating effect, prepare gold, silver, gold silver
Alloy, platinum fluorescence metal nano-cluster manifest reagent, all can manifest outmoded finger mark fast and efficiently.
The present invention has a following Advantageous Effects:
1. the present invention contains the preparation that four kinds of metal nanometre clusters manifest reagent and the method manifesting outmoded finger mark thereof, and this manifests reagent
Quick (about about the 1h) that synthesis is prepared compared to the method for other patent reports；
2. the gold, silver of preparation, electrum, platinum fluorescence noble-metal nanoclusters fluorescence quantum yield height, and fluorescence duration time is long,
There is hypotoxicity；
3. finger mark manifests operation rapidly and efficiently, can clearly manifest the outmoded finger mark of 30 days；
4. the effect that four kinds of noble-metal nanoclusters that prepared by the present invention manifest outmoded finger mark is superior to tradition and manifests manifesting of reagent
Effect；
5. finger mark manifests viewing system and can preferably fix finger mark information, beneficially test sensitivity.
Accompanying drawing explanation
Fig. 1 is gold nanoclusters, silver nanoclusters, electrum nano-cluster and platinum cluster composition principle figure.
Fig. 2 is that hydro-thermal method, ultrasonic method, microwave method and ultrasonic-microwave cooperating method are to gold nanoclusters fluorescence intensity and average particle
Footpath affect schematic diagram.
Fig. 3 is gold nanoclusters, silver nanoclusters, electrum nano-cluster, platinum cluster fluorescence color figure.
Fig. 4 is gold nanoclusters, silver nanoclusters, electrum nano-cluster, platinum cluster ultraviolet spectrogram.
Fig. 5 is gold nanoclusters, silver nanoclusters, electrum nano-cluster, platinum cluster transmission electron microscope picture.
Fig. 6 is gold nanoclusters, silver nanoclusters, electrum nano-cluster, the infrared spectrogram of platinum cluster.
Fig. 7 is that finger mark manifests viewing system and manifests principle schematic.
Fig. 8 is that gold nanoclusters, silver nanoclusters, electrum nano-cluster, platinum cluster manifest outmoded finger mark at glass object
Figure.
Fig. 9 is that the present invention manifests preparation method of reagent thereof flow chart.
Figure 10 is that the present invention manifests outmoded Sweat latent fingerprint method flow diagram.
Detailed description of the invention
Accompanying drawing 1 is gold nanoclusters, silver nanoclusters, electrum nano-cluster, platinum cluster composition principle figure, bovine serum albumin
White containing the aminoacid such as tyrosine, cysteine, molecular structure is complicated.Stable structure can be formed with gold, silver, pt atom.Adopt
It is nano-cluster Stability Analysis of Structures prepared by stabilizer reducing agent with bovine serum albumin.
Fig. 2 is that hydro-thermal method, ultrasonic method, microwave method and ultrasonic-microwave cooperating method are to gold nanoclusters fluorescence intensity and average particle
Footpath affect schematic diagram.Obviously, the nanocluster fluorescence intensity that prepared by ultrasonic-microwave cooperating heating is substantially better than with size
Other preparation methoies；Nanocluster size prepared by microwave method is less, and this makes solution thermally equivalent relevant with microwave heating；Ultrasonic method
The particle diameter of preparation is more bigger than microwave method, but fluorescence property is excellent；Nano-cluster performance prepared by traditional heating method is worst.Super
Ultrasonic method is combined by sound-microwave cooperating heating with microwave method each advantage, has fully demonstrated the feature of efficient green.It is efficient
Gonosome can not only make particle diameter reduce now, and dispersion effect and fluorescence property strengthen, moreover it is possible to make the response time be substantially reduced, instead
Efficiency is answered to improve；Its green gonosome present BSA biological activity in building-up process does not changes, whole course of reaction safety,
Response time reduces to make to consume energy and reduces, and the amount of reagent simultaneously making preparation same amount nano-cluster need reduces.
Fig. 3 is gold nanoclusters, silver nanoclusters, electrum nano-cluster, (abcd is followed successively by gold to platinum cluster fluorescence color figure
Nano-cluster, silver nanoclusters, electrum nano-cluster, platinum cluster).It can be seen that gold nanoclusters irradiates at alternative light source
Under send fluorescent red-orange；Silver nanoclusters sends fluorescent orange under alternative light source irradiates；Electrum nano-cluster is at many ripples
Duan Guangyuan sends yellow fluorescence under irradiating；Platinum cluster sends blue-green fluorescent under alternative light source irradiates.Noble metal nano
Bunch fluorescence intensity strong.
Fig. 4 is gold nanoclusters, silver nanoclusters, electrum nano-cluster, (abcd is followed successively by gold to platinum cluster ultraviolet spectrogram
Nano-cluster, silver nanoclusters, electrum nano-cluster, platinum cluster).As we know from the figure under about 280 nm ultraviolet radiates, expensive
Metal nanometre cluster all has a stronger ultraviolet absorption peak, and the tryptophan in bovine serum albumin and tyrosine residue uv absorption
Peak also is located at about 280 nm.Bovine serum albumin is wrapped in outside precious metal atom and plays protection Stabilization, therefore nano-cluster
Ultraviolet spectra character close with bovine serum albumin, this explanation is ultrasonic-microwave heating coordination technique prepares nano-cluster and do not destroy
The biological activity of bovine serum albumin.
Fig. 5 is gold nanoclusters, silver nanoclusters, electrum nano-cluster, platinum cluster transmission electron microscope picture.(abcd is followed successively by
Gold nanoclusters, silver nanoclusters, electrum nano-cluster, platinum cluster).Find that nano-cluster dispersing uniformity is good as we know from the figure,
Its average particle size little about 3-5nm. this compared with the Conventional nano particle that particle diameter is 13.3 nm that Du Juan in 2013 reports, chi
Very little much smaller than nanoparticle.Therefore nano-cluster is bigger compared to nanoparticle energy level discontinuity, the ability of electronics generation transition
The strongest, the fluorescence of generation is higher.
Fig. 6 is gold nanoclusters, silver nanoclusters, electrum nano-cluster, (abcd is followed successively by the infrared spectrogram of platinum cluster
Gold nanoclusters, silver nanoclusters, electrum nano-cluster, platinum cluster).It can be seen that the characteristic absorption peak of these three solution
There is not significant change, but the sulfydryl characteristic absorption peak that nano-cluster is located at about 2300 cm-1 disappears, and illustrates to pass through Ultrasonic Heating
Reaction bovine serum albumin molecule the most successfully modifies the surface to nano-cluster.And the characteristic absorption peak of bovine serum albumin self
Do not change significantly after before the reaction, illustrate that the conformation of protein is without substantially changing.
Fig. 7 is that finger mark manifests viewing system and manifests principle schematic.Utilize alternative light source, colour light filter mirror, number
Slr camera is independently built and is manifested viewing system and carry out Sweat latent fingerprint observing fixing.As we know from the figure under dark condition, will
Alternative light source irradiates the Sweat latent fingerprint that stamp is manifested by gold nanoclusters powder, and the fluorescent red-orange that finger mark produces is through coloured filter
Finger mark mastoid process streakline and minutia thereof, by digital single-lens reflex camera record, are fixed up by light microscopic.Do not reflect its of finger mark feature
His veiling glare cannot pass through colour light filter mirror thus can not be by cameras record.It is good that finger mark manifests effect, can examine see the one-level of finger mark, two
Even three grades features of level.
Fig. 8 is that gold nanoclusters, silver nanoclusters, electrum nano-cluster, platinum cluster manifest outmoded finger mark at glass object
Figure.From in figure, noble-metal nanoclusters manifests the effective of outmoded finger mark, is better than traditional powder and shows reagent.Wherein platinum nanometer
Bunch manifest best results, finger mark mastoid process streakline is smooth, and the minutia such as spillikin, point highlights.Electrum nano-cluster, Yin Na
The effect that manifests of rice bunch is taken second place, and it is slightly worse that gold nanoclusters manifests effect.
Embodiment 1
A kind of noble-metal nanoclusters of the present invention manifests the preparation method of reagent, comprises the following steps: be dissolved in pure by the gold chloride of 1%
Water is configured to the solution of 0.01 mol/L；Bovine serum albumin is dissolved under the conditions of 37 DEG C pure water, and to be configured to 50 mg/mL molten
Liquid；Potassium hydroxide is dissolved in pure water and is configured to 1 mol/L solution；By chlorauric acid solution good for above-mentioned configuration, bovine serum albumin
Solution 1:1 by volume mixes, and is placed under magnetic stirring apparatus reaction 3min；Slowly potassium hydroxide solution is added drop-wise to transfusion needle
In the mixed liquor of chlorauric acid solution described in this step and bovine serum albumin solution, regulation pH is 12, now used 0.01
The chlorauric acid solution of mol/L, the bovine serum albumin solution of 50 mg/mL, the potassium hydroxide solution volume ratio of 1 mol/L are 10:
10:1；The mixed solution that pH is 12 is first placed in ultrasonic 1h in ultrasonic washing instrument；It is placed in again in household microwave oven, sets height
(800W) microwave radiation 50s under the conditions of fire, prepared gold nanoclusters manifests reagent.
Embodiment 2
A kind of noble-metal nanoclusters of the present invention manifests the preparation method of reagent, comprises the following steps: be dissolved in pure by the silver nitrate of 1%
Water is configured to the solution of 0.01 mol/L；Bovine serum albumin is dissolved in pure water under the conditions of 37 DEG C and is configured to solution；By hydrogen-oxygen
Change potassium is dissolved in pure water and is configured to 1 mol/L solution；By silver nitrate solution good for above-mentioned configuration, bovine serum albumin solution by volume
Mix than 1:1, be placed under magnetic stirring apparatus reaction 3min；Slowly potassium hydroxide solution is added drop-wise to described in this step with transfusion needle
Silver nitrate solution is with the mixed liquor of bovine serum albumin solution, and regulation pH is 12, the nitric acid of 0.01 mol/L now used
Silver solution, the bovine serum albumin solution of 50 mg/mL, the potassium hydroxide solution volume ratio of 1 mol/L are 10:10:1；By pH it is
The mixed solution of 12 is first placed in ultrasonic 1h in ultrasonic washing instrument；It is placed in again in household microwave oven, under the conditions of setting high fire
(800W) microwave radiation 60s, prepared silver nanoclusters manifests reagent.
Embodiment 3
A kind of noble-metal nanoclusters of the present invention manifests the preparation method of reagent, comprises the following steps: be dissolved in pure by the gold chloride of 1%
Water is configured to the solution of 0.01 mol/L；The silver nitrate of 1% is dissolved in pure water and is configured to the solution of 0.01 mol/L；By Ox blood serum
Albumin is dissolved in pure water under the conditions of 37 DEG C and is configured to solution；Potassium hydroxide is dissolved in pure water and is configured to 1 mol/L solution；By upper
State configured chlorauric acid solution, silver nitrate solution, bovine serum albumin solution 1:1:2 by volume mixing, be placed in magnetic force and stir
Mix reaction 3min under device；Slowly being added drop-wise to by potassium hydroxide solution in above-mentioned mixed liquor with transfusion needle, regulation pH is 12, now institute
The chlorauric acid solution of 0.01 mol/L, the silver nitrate solution of 0.01 mol/L, the bovine serum albumin solution of 50 mg/mL,
The potassium hydroxide solution volume ratio of 1 mol/L is 5:5:10:1；The mixed solution that pH is 12 is first placed in ultrasonic washing instrument
Ultrasonic 1h；It is placed in again in household microwave oven, (800W) microwave radiation 40s under the conditions of setting high fire, prepares gold silver nano-cluster and manifest
Reagent.
Embodiment 4
A kind of noble-metal nanoclusters of the present invention manifests the preparation method of reagent, comprises the following steps: chloroplatinic acid is dissolved in pure water and joins
It is set to the solution of 0.01 mol/L；Bovine serum albumin is dissolved in pure water under the conditions of 37 DEG C and is configured to solution；By potassium hydroxide
It is dissolved in pure water and is configured to 1 mol/L solution；By platinum acid chloride solution good for above-mentioned configuration, bovine serum albumin solution by volume 1:
1 mixing, is placed under magnetic stirring apparatus reaction 3min；Slowly potassium hydroxide solution is added drop-wise to chlorine platinum described in this step with transfusion needle
Acid solution is with the mixed liquor of bovine serum albumin solution, and regulation pH is 12, and the chloroplatinic acid of 0.01 mol/L now used is molten
Liquid, the bovine serum albumin solution of 50 mg/mL, the potassium hydroxide solution volume ratio of 1 mol/L are 10:10:1；It is 12 by pH
Mixed solution is first placed in ultrasonic 1h in ultrasonic washing instrument；Being placed in household microwave oven, under the conditions of setting high fire, (800W) is micro-again
Wave radiation 45s, prepared platinum cluster manifests reagent.
Embodiment 5
A kind of method utilizing noble-metal nanoclusters to manifest outmoded Sweat latent fingerprint, comprises the following steps:
S1, the gold chloride of 1% is dissolved in pure water it is configured to the solution of 0.01 mol/L；By bovine serum albumin under the conditions of 37 DEG C
It is dissolved in pure water and is configured to 50 mg/mL solution；Potassium hydroxide is dissolved in pure water and is configured to 1 mol/L solution；Above-mentioned configuration is good
Chlorauric acid solution, bovine serum albumin solution 1:1 by volume mixes, and is placed under magnetic stirring apparatus reaction 3min；Use transfusion needle
Slowly potassium hydroxide solution is added drop-wise in the mixed liquor of chlorauric acid solution described in this step and bovine serum albumin solution, regulation
PH is 12, the chlorauric acid solution of 0.01 mol/L now used, the bovine serum albumin solution of 50 mg/mL, 1 mol/L
Potassium hydroxide solution volume ratio is 10:10:1；The mixed solution that pH is 12 is first placed in ultrasonic 1h in ultrasonic washing instrument；Again
Being placed in household microwave oven, (800W) microwave radiation 50s under the conditions of setting high fire, prepared gold nanoclusters manifests reagent；
After hand washing is dried by S2, volunteer only, stamp Sweat latent fingerprint on glass, it is thus achieved that finger mark sample, between finger mark sample is put
Away from moderate, for imitating the outmoded Sweat latent fingerprint left on criminal-scene, this experiment finger mark sample leaves in dry under field conditions (factors)
In clean pallet, the resting period is 30d；
S3, manifest reagent with the gold nanoclusters obtained by glue head dropper aspiration step S1 so that it is clockwise along finger mark mastoid process streakline
Drip aobvious, and fully react 1h with finger mark material；
S4, wash away with ultra-pure water step S3 drip aobvious after Sweat latent fingerprint loose colour；
S5, step S4 is washed away the Sweat latent fingerprint after loose colour in baking oven machine vacuum, dry 0.5h under the conditions of 37 DEG C；
S6, utilize alternative light source, colour light filter mirror, digital single-lens reflex camera independently to build to manifest viewing system and refer to fluorescence antiperspirant is latent
Print carries out observing fixes, and under dark condition, alternative light source irradiates the Sweat latent fingerprint manifested by gold nanoclusters, and finger mark produces
Fluorescence through colour light filter mirror by digital single-lens reflex camera record, finger mark mastoid process streakline and minutia thereof are fixed up.
Embodiment 6
A kind of method utilizing noble-metal nanoclusters to manifest outmoded Sweat latent fingerprint, comprises the following steps:
S1, the silver nitrate of 1% is dissolved in pure water it is configured to the solution of 0.01 mol/L；By bovine serum albumin under the conditions of 37 DEG C
It is dissolved in pure water and is configured to solution；Potassium hydroxide solution pure water is configured to 1 mol/L solution；The silver nitrate that above-mentioned configuration is good is molten
Liquid, bovine serum albumin solution 1:1 by volume mixes, and is placed under magnetic stirring apparatus reaction 3min；With transfusion needle slowly by hydrogen
Potassium oxide is dissolved in the mixed liquor being added drop-wise to silver nitrate solution described in this step and bovine serum albumin solution, and regulation pH is 12,
The silver nitrate solution of 0.01 mol/L used by now, the bovine serum albumin solution of 50 mg/mL, the potassium hydroxide of 1 mol/L
Liquor capacity is than for 10:10:1；The mixed solution that pH is 12 is first placed in ultrasonic 1h in ultrasonic washing instrument；It is placed in domestic again
In microwave oven, (800W) microwave radiation 60s under the conditions of setting high fire, prepared silver nanoclusters manifests reagent；
After hand washing is dried by S2, volunteer only, stamp Sweat latent fingerprint on plastics, it is thus achieved that finger mark sample, between finger mark sample is put
Away from moderate, for imitating the outmoded Sweat latent fingerprint left on criminal-scene, this experiment finger mark sample leaves in dry under field conditions (factors)
In clean pallet, the resting period is 30d；
S3, manifest reagent with the silver nanoclusters obtained by glue head dropper aspiration step S1 so that it is clockwise along finger mark mastoid process streakline
Drip aobvious, and fully react 2h with finger mark material；
S4, wash away with ultra-pure water step S3 drip aobvious after Sweat latent fingerprint loose colour；
S5, step S4 is washed away the Sweat latent fingerprint after loose colour in baking oven machine vacuum, dry 10min under the conditions of 37 DEG C；
S6, utilize alternative light source, colour light filter mirror, digital single-lens reflex camera independently to build to manifest viewing system and refer to fluorescence antiperspirant is latent
Print carries out observing fixes, and under dark condition, alternative light source irradiates the Sweat latent fingerprint manifested by silver nanoclusters, and finger mark produces
Fluorescence through colour light filter mirror by digital single-lens reflex camera record, finger mark mastoid process streakline and minutia thereof are fixed up.
Embodiment 7
A kind of method utilizing noble-metal nanoclusters to manifest outmoded Sweat latent fingerprint, comprises the following steps:
S1, the gold chloride of 1% is dissolved in pure water it is configured to the solution of 0.01 mol/L；The silver nitrate of 1% is dissolved in pure water be configured to
The solution of 0.01 mol/L；Bovine serum albumin is dissolved in pure water under the conditions of 37 DEG C and is configured to solution；Potassium hydroxide is dissolved in
Pure water is configured to 1 mol/L solution；Chlorauric acid solution good for above-mentioned configuration, silver nitrate solution, bovine serum albumin solution are pressed
Volume ratio 1:1:2 mixes, and is placed under magnetic stirring apparatus reaction 3min；Slowly potassium hydroxide solution is added drop-wise to above-mentioned with transfusion needle
In mixed liquor, regulation pH is 12, the chlorauric acid solution of 0.01 mol/L now used, the silver nitrate solution of 0.01 mol/L,
The bovine serum albumin solution of 50 mg/mL, the potassium hydroxide solution volume ratio of 1 mol/L are 5:5:10:1；By pH be 12 mixed
Close solution and be first placed in ultrasonic 1h in ultrasonic washing instrument；It is placed in again in household microwave oven, (800W) microwave under the conditions of setting high fire
Radiation 40s, prepares gold silver nano-cluster and manifests reagent；
After hand washing is dried by S2, volunteer only, stamp Sweat latent fingerprint on preservative film, it is thus achieved that finger mark sample, finger mark sample is put
Spacing is moderate, and for imitating the outmoded Sweat latent fingerprint left on criminal-scene, this experiment finger mark sample leaves under field conditions (factors)
In clean pallet, the resting period is 30d；
S3, manifest reagent with the gold silver nano-cluster obtained by glue head dropper aspiration step S1 so that it is along finger mark mastoid process streakline up time
Pin drips aobvious, and fully reacts 3h with finger mark material；
S4, wash away with ultra-pure water step S3 drip aobvious after Sweat latent fingerprint loose colour；
S5, step S4 is washed away the Sweat latent fingerprint after loose colour in baking oven machine vacuum, dry 10min under the conditions of 37 DEG C；
S6, utilize alternative light source, colour light filter mirror, digital single-lens reflex camera independently to build to manifest viewing system and refer to fluorescence antiperspirant is latent
Print carries out observing fixes, and under dark condition, alternative light source irradiates the Sweat latent fingerprint manifested by gold silver nano-cluster, and finger mark produces
Finger mark mastoid process streakline and minutia thereof by digital single-lens reflex camera record, are fixed up by raw fluorescence through colour light filter mirror.
Embodiment 8 one kinds utilizes the method that noble-metal nanoclusters manifests outmoded Sweat latent fingerprint, comprises the following steps:
S1, chloroplatinic acid is dissolved in pure water it is configured to the solution of 0.01 mol/L；Bovine serum albumin is dissolved under the conditions of 37 DEG C
Pure water is configured to solution；Potassium hydroxide is dissolved in pure water and is configured to 1 mol/L solution；By platinum acid chloride solution good for above-mentioned configuration,
Bovine serum albumin solution 1:1 by volume mixes, and is placed under magnetic stirring apparatus reaction 3min；With transfusion needle slowly by hydroxide
Potassium solution is added drop-wise in the mixed liquor of platinum acid chloride solution described in this step and bovine serum albumin solution, and regulation pH is 12, now
The used platinum acid chloride solution of 0.01 mol/L, the bovine serum albumin solution of 50 mg/mL, the potassium hydroxide solution of 1 mol/L
Volume ratio is 10:10:1；The mixed solution that pH is 12 is first placed in ultrasonic 1h in ultrasonic washing instrument；It is placed in domestic microwave again
In stove, (800W) microwave radiation 45s under the conditions of setting high fire, prepared platinum cluster manifests reagent；
After hand washing is dried by S2, volunteer only, stamp Sweat latent fingerprint on metal, it is thus achieved that finger mark sample, between finger mark sample is put
Away from moderate, for imitating the outmoded Sweat latent fingerprint left on criminal-scene, this experiment finger mark sample leaves in dry under field conditions (factors)
In clean pallet, the resting period is 30d；
S3, manifest reagent with the platinum cluster obtained by glue head dropper aspiration step S1 so that it is clockwise along finger mark mastoid process streakline
Drip aobvious, and fully react 2.5h with finger mark material；
S4, wash away with ultra-pure water step S3 drip aobvious after Sweat latent fingerprint loose colour；
S5, step S4 is washed away the Sweat latent fingerprint after loose colour in baking oven machine vacuum, dry 20min under the conditions of 37 DEG C；
S6, utilize alternative light source, colour light filter mirror, digital single-lens reflex camera independently to build to manifest viewing system and refer to fluorescence antiperspirant is latent
Print carries out observing fixes, and under dark condition, alternative light source irradiates the Sweat latent fingerprint manifested by platinum cluster, and finger mark produces
Fluorescence through colour light filter mirror by digital single-lens reflex camera record, finger mark mastoid process streakline and minutia thereof are fixed up.
The present invention, by ultrasonic and microwave cooperating effect, prepares gold, silver, electrum, platinum fluorescence metal nano-cluster manifest
Reagent, all can manifest outmoded finger mark fast and efficiently.The method is simple for process；The gold, silver of preparation, electrum, platinum are glimmering
Light noble-metal nanoclusters fluorescence quantum yield is high, and fluorescence duration time is long, has hypotoxicity；Can clearly manifest 30 days outmoded
Finger mark；Independently build and manifest viewing system and can preferably fix finger mark information, beneficially test sensitivity.
Above example is only in order to illustrate technical scheme and unrestricted, although with reference to preferred embodiment to this
Bright it is described in detail, it will be understood by those within the art that, technical scheme can be modified
Or equivalent, without deviating from objective and the scope of technical solution of the present invention, it all should contain the claim in the present invention
In the middle of scope.
Claims (8)
1. a noble-metal nanoclusters manifests the preparation method of reagent, it is characterised in that described noble-metal nanoclusters is gold nano
Bunch, any one in silver nanoclusters, electrum nano-cluster and platinum noble metals nano-cluster；And described noble-metal nanoclusters manifests
Reagent is prepared by ultrasonic-microwave cooperating preparation method.
The most according to claim 1, noble-metal nanoclusters manifests the preparation method of reagent, it is characterised in that described noble metal is received
Rice bunch manifests the preparation method of reagent, including,
Prepare the method that gold nanoclusters manifests reagent, comprise the following steps:
(1) solution preparation, is dissolved in gold chloride pure water and is configured to the solution of 0.01mol/L；Bovine serum albumin is 37 DEG C of conditions
Under be dissolved in pure water and be configured to 50mg/mL solution；Potassium hydroxide is dissolved in pure water and is configured to 1 mol/L solution；
(2) hybrid reaction, is 1:1 by volume, chlorauric acid solution is added bovine serum albumin solution, is existed by mixed solution
3min is reacted under the effect of magnetic stirring apparatus；
(3) pH value regulation, is added drop-wise to the chlorauric acid solution obtained by step (2) molten with bovine serum albumin by potassium hydroxide solution
In the mixed liquor of liquid, regulation pH is 12；
(4) ultrasonic disperse, is placed in ultrasonic disperse 1h in ultrasonic washing instrument by the mixed solution obtained by step (3)；
(5) microwave radiation, is then placed in the solution obtained by step (4) in microwave oven, microwave radiation 40 ~ 60s, prepares gold
Nano-cluster manifests reagent；
Prepare the method that silver nanoclusters manifests reagent, comprise the following steps:
(1) solution preparation, is dissolved in silver nitrate pure water and is configured to the solution of 0.01mol/L；Bovine serum albumin is 37 DEG C of conditions
Under be dissolved in pure water and be configured to 50mg/mL solution；Potassium hydroxide is dissolved in pure water and is configured to 1 mol/L solution；
(2) hybrid reaction, is 1:1 by volume, silver nitrate solution is added bovine serum albumin solution, is existed by mixed solution
3min is reacted under the effect of magnetic stirring apparatus；
(3) pH value regulation, is added drop-wise to the silver nitrate solution obtained by step (2) and bovine serum albumin by potassium hydroxide solution
In the mixed liquor of solution, regulation pH is 12；
(4) ultrasonic disperse, is placed in ultrasonic disperse 1h in ultrasonic washing instrument by the mixed solution obtained by step (3)；
(5) microwave radiation, is then placed in the solution obtained by step (4) in microwave oven, microwave radiation 40 ~ 60s, prepares silver
Nano-cluster manifests reagent；
Prepare the method that gold silver nano-cluster manifests reagent, comprise the following steps:
(1) solution preparation, is dissolved in gold chloride pure water and is configured to the solution of 0.01mol/L；Silver nitrate is dissolved in pure water and is configured to
The solution of 0.01mol/L；Bovine serum albumin is dissolved in pure water under the conditions of 37 DEG C and is configured to 50mg/mL solution；By potassium hydroxide
It is dissolved in pure water and is configured to 1 mol/L solution；
(2) hybrid reaction, is 1:1:2 by volume, and chlorauric acid solution, silver nitrate solution are added bovine serum albumin solution,
Mixed solution is reacted under the effect of magnetic stirring apparatus 3min；
(3) pH value regulation, is added drop-wise to potassium hydroxide solution in the mixed liquor obtained by step (2), and regulation pH is 12；
(4) ultrasonic disperse, is placed in ultrasonic disperse 1h in ultrasonic washing instrument by the mixed solution obtained by step (3)；
(5) microwave radiation, is then placed in the solution obtained by step (4) in microwave oven, microwave radiation 40 ~ 60s, prepares silver
Nano-cluster manifests reagent；
Prepare the method that platinum cluster manifests reagent, comprise the following steps:
(1) solution preparation, is dissolved in chloroplatinic acid pure water and is configured to the solution of 0.01mol/L；Bovine serum albumin is at 37 DEG C of bars
It is dissolved in pure water under part and is configured to 50mg/mL solution；Potassium hydroxide is dissolved in pure water and is configured to 1 mol/L solution；
(2) hybrid reaction, is 1:1 by volume, platinum acid chloride solution is added bovine serum albumin solution, is existed by mixed solution
3min is reacted under the effect of magnetic stirring apparatus；
(3) pH value regulation, is added drop-wise to the platinum acid chloride solution obtained by step (2) and bovine serum albumin by potassium hydroxide solution
In the mixed liquor of solution, regulation pH is 12；
(4) ultrasonic disperse, is placed in ultrasonic disperse 1h in ultrasonic washing instrument by the mixed solution obtained by step (3)；
(5) microwave radiation, is then placed in the solution obtained by step (4) in microwave oven, microwave radiation 40 ~ 60s, prepares silver
Nano-cluster manifests reagent.
3. noble-metal nanoclusters manifests the method that reagent manifests outmoded Sweat latent fingerprint, comprises the following steps: use right to want
The noble-metal nanoclusters asking preparation method described in 1 or 2 to prepare manifests reagent and manifests outmoded Sweat latent fingerprint, comprises the following steps,
Prepared by S1, reagent, prepare noble-metal nanoclusters and manifest reagent；
S2, restraining finger mark, after hand washing is dried by volunteer only, on glass, plastics, preservative film, metal object, stamp antiperspirant is latent refers to
Print, it is thus achieved that finger mark sample；
S3, drip aobvious finger mark, by step S1 prepare manifest reagent drip aobvious step S2 prepare Sweat latent fingerprint, react 1-3h；
S4, wash away loose colour, use ultra-pure water wash away step S3 drip aobvious after Sweat latent fingerprint loose colour；
S5, finger mark are dried, and step S4 washes away the Sweat latent fingerprint after loose colour and dries；
S6, finger mark are observed fixing, under manifesting viewing system, observe the Sweat latent fingerprint image after fixing step S5 is dried；
It is characterized in that, described noble-metal nanoclusters is that gold nanoclusters, silver nanoclusters, electrum nano-cluster and platinum noble metals are received
Rice bunch in any one.
The method manifesting outmoded Sweat latent fingerprint the most according to claim 3, it is characterised in that your gold is described step S1 prepare
Belong to nano-cluster and manifest reagent, including,
Prepare the method that gold nanoclusters manifests reagent, comprise the following steps:
(1) solution preparation, is dissolved in gold chloride pure water and is configured to the solution of 0.01 mol/L；Bovine serum albumin is at 37 DEG C of bars
It is dissolved in pure water under part and is configured to 50 mg/mL solution；Potassium hydroxide is dissolved in pure water and is configured to 1 mol/L solution；
(2) hybrid reaction, is 1:1 by volume, chlorauric acid solution is added bovine serum albumin solution, is existed by mixed solution
3min is reacted under the effect of magnetic stirring apparatus；
(3) pH value regulation, is added drop-wise to the chlorauric acid solution obtained by step (2) and bovine serum albumin by potassium hydroxide solution
In the mixed liquor of solution, regulation pH is 12；
(4) ultrasonic disperse, is placed in ultrasonic disperse 1h in ultrasonic washing instrument by the mixed solution obtained by step (3)；
(5) microwave radiation, is then placed in the solution obtained by step (4) in microwave oven, microwave radiation 40 ~ 60s, prepares gold
Nano-cluster manifests reagent；
Prepare the method that silver nanoclusters manifests reagent, comprise the following steps:
(1) solution preparation, is dissolved in silver nitrate pure water and is configured to the solution of 0.01 mol/L；Bovine serum albumin is at 37 DEG C of bars
It is dissolved in pure water under part and is configured to 50 mg/mL solution；Potassium hydroxide is dissolved in pure water and is configured to 1 mol/L solution；
(2) hybrid reaction, is 1:1 by volume, silver nitrate solution is added bovine serum albumin solution, is existed by mixed solution
3min is reacted under the effect of magnetic stirring apparatus；
(3) pH value regulation, is added drop-wise to the silver nitrate solution obtained by step (2) and bovine serum albumin by potassium hydroxide solution
In the mixed liquor of solution, regulation pH is 12；
(4) ultrasonic disperse, is placed in ultrasonic disperse 1h in ultrasonic washing instrument by the mixed solution obtained by step (3)；
(5) microwave radiation, is then placed in the solution obtained by step (4) in microwave oven, microwave radiation 40 ~ 60s, prepares silver
Nano-cluster manifests reagent；
Prepare the method that gold silver nano-cluster manifests reagent, comprise the following steps:
(1) solution preparation, is dissolved in gold chloride pure water and is configured to the solution of 0.01 mol/L；Silver nitrate is dissolved in pure water and is configured to
The solution of 0.01 mol/L；Bovine serum albumin is dissolved in pure water under the conditions of 37 DEG C and is configured to 50 mg/mL solution；By hydroxide
Potassium is dissolved in pure water and is configured to 1 mol/L solution；
(2) hybrid reaction, is 1:1:2 by volume, and chlorauric acid solution, silver nitrate solution are added bovine serum albumin solution,
Mixed solution is reacted under the effect of magnetic stirring apparatus 3min；
(3) pH value regulation, is added drop-wise to potassium hydroxide solution in the mixed liquor obtained by step (2), and regulation pH is 12；
(4) ultrasonic disperse, is placed in ultrasonic disperse 1h in ultrasonic washing instrument by the mixed solution obtained by step (3)；
(5) microwave radiation, is then placed in the solution obtained by step (4) in microwave oven, microwave radiation 40 ~ 60s, prepares silver
Nano-cluster manifests reagent；
Prepare the method that platinum cluster manifests reagent, comprise the following steps:
(1) solution preparation, is dissolved in chloroplatinic acid pure water and is configured to the solution of 0.01 mol/L；Bovine serum albumin is at 37 DEG C of bars
It is dissolved in pure water under part and is configured to 50 mg/mL solution；Potassium hydroxide is dissolved in pure water and is configured to 1 mol/L solution；
(2) hybrid reaction, is 1:1 by volume, platinum acid chloride solution is added bovine serum albumin solution, is existed by mixed solution
3min is reacted under the effect of magnetic stirring apparatus；
(3) pH value regulation, is added drop-wise to the platinum acid chloride solution obtained by step (2) and bovine serum albumin by potassium hydroxide solution
In the mixed liquor of solution, regulation pH is 12；
(4) ultrasonic disperse, is placed in ultrasonic disperse 1h in ultrasonic washing instrument by the mixed solution obtained by step (3)；
(5) microwave radiation, is then placed in the solution obtained by step (4) in microwave oven, microwave radiation 40 ~ 60s, prepares silver
Nano-cluster manifests reagent.
5. according to the method manifesting outmoded Sweat latent fingerprint described in claim 3 or 4, it is characterised in that described step S2 is restrained
Finger mark, including, it is thus achieved that resting period of finger mark sample be 7 30 days.
6. according to the method manifesting outmoded Sweat latent fingerprint described in claim 3 or 4, it is characterised in that described step S3 is dripped aobvious
Finger mark, including, manifest reagent with the noble-metal nanoclusters obtained by glue head dropper aspiration step S1 so that it is along finger mark mastoid process streakline
Drip aobvious clockwise, and fully react 2h with finger mark material.
7. according to the method manifesting outmoded Sweat latent fingerprint described in claim 3 or 4, it is characterised in that described step S5 finger mark
Dry, including, in baking oven machine vacuum, dry under the conditions of 37 DEG C.
8. according to the method manifesting outmoded Sweat latent fingerprint described in claim 3 or 4, it is characterised in that described step S6 finger mark
Observe, including, manifesting viewing system is to utilize what alternative light source, colour light filter mirror, digital single-lens reflex camera built to manifest observation
System.
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