CN106865615A - A kind of preparation of copper/chromium composite black nanometer powder and its finger mark process for show - Google Patents
A kind of preparation of copper/chromium composite black nanometer powder and its finger mark process for show Download PDFInfo
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- CN106865615A CN106865615A CN201710078917.7A CN201710078917A CN106865615A CN 106865615 A CN106865615 A CN 106865615A CN 201710078917 A CN201710078917 A CN 201710078917A CN 106865615 A CN106865615 A CN 106865615A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G37/00—Compounds of chromium
- C01G37/14—Chromates; Bichromates
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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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- 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
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/68—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals containing chromium, molybdenum or tungsten
- C09K11/681—Chalcogenides
Abstract
The present invention proposes preparation and its finger mark process for show of a kind of copper/chromium composite black nanometer powder.The preparation method is comprised the following steps:S1, prepare copper chromium salt solution;S2, prepare citric acid solution;S3, prepare copper chrome lemon hydrochlorate;S4, prepare gel;S5 prepares precursor powder;S6, Muffle furnace calcining.Finger mark process for show of the invention includes directly brushing aobvious method, and aobvious method and the aobvious method of suspension spray are trembled in dusting.The present invention has following Advantageous Effects:It is good to the fingerprint displaying effect in old impression of the hand and permeability object;Product possesses environmental protection feature, harmless to operator;Preparation method is simple and easy to apply, it is easy to popularization and application.
Description
Technical field
The present invention relates to public security criminal technique finger mark identification field, more particularly to a kind of copper/chromium composite black nanometer powder
Preparation and its finger mark process for show.
Background technology
Impression of the hand is human contact's object and in the reflecting image of contact surface surface structure left by body surface;And finger
Line has people variant, the characteristics of being basically unchanged throughout one's life.Therefore, it can directly assert individual according to impression of the hand.In solving criminal cases and
Impression of the hand can be played and provide the important function that evidence was solved a case and tried to investigation clue, offer in trial.As can be seen here, latent fingerprint
Appearing technique is the precondition and guarantee for being disclosed and being confirmed crime using impression of the hand.At present, powder method and small-particle suspension method are because of behaviour
Make simple, preparation simple, impression of the hand most efficient method is manifested as scene.Then, powder conventional at present, such as bronze, magnetic
Powder etc. is larger because of particle diameter, it is impossible to fully combined with impression of the hand material, therefore the impression of the hand in old impression of the hand and permeability object is shown
Existing effect on driving birds is not good.To improve the sensitivity of finger mark detection, researcher utilizes some semiconductor nanos(Quantum dot), rare earth material
Manifest potential impression of the hand Deng as fluorometric reagent, though obtaining better effects, how toxic such reagent is, and need to be set by means of complexity
Standby, operation sequence is cumbersome, is not easy to the popularization of engineering department of basic unit.Also there are the noble metal nanometer materials such as partial report gold, silver can
The sensitivity that Bio-imprinting manifests, but the method high cost are improved, laboratory stage is currently limited to.
It can be seen that, in existing finger mark appearing technique, there is problems with:
1st, conventional powder method is to the fingerprint displaying effect on driving birds is not good in old impression of the hand and permeability object.
2nd, semiconductor nano(Quantum dot)Or rare earth material is toxic, and need to by means of complex device, operation sequence compared with
It is cumbersome, it is not easy to the popularization of engineering department of basic unit.
3rd, the noble metal nanometer material high cost such as gold, silver, is currently limited to laboratory stage.
The content of the invention
In order to solve that existing conventional powder method is present to the fingerprint displaying effect in old impression of the hand and permeability object
Not good problem, the present invention proposes preparation and its finger mark process for show of a kind of copper/chromium composite black nanometer powder.
A kind of preparation of copper/chromium composite black nanometer powder of the present invention, comprises the following steps:
S1, prepare copper-chromium salt solution:Cu (the N0 of 24.2g are weighed respectively3)2·3H2Cr (the N0 of 0 and 80g3)3·9H20 solid,
It is made into 200mL hybrid metal saline solutions, ultrasonic mixing is uniform, and transfers them to flask;
S2, prepare citric acid solution:Weigh 76.9g citric acid solid, will its be made into the 200mL aqueous solution;
S3, prepare copper-chrome lemon hydrochlorate:The flask of step S1 is placed in thermostat water bath, it is 85 DEG C to set bath temperature,
Under strong stirring, citric acid solution obtained by step S2 is slowly instilled by flask by dropping funel, until completion of dropping;
S4, prepare gel:The Surfactant PEG 400 of 5.21g is added in the copper obtained by step S3-chrome lemon hydrochlorate, after
Continuous stirring, until moisture is evaporated in solution, forms the gel of clear, stops stirring;
S5 prepares precursor powder:Gel obtained by step S4 is placed in vacuum drying chamber, 1h is dried in 95 DEG C, can obtained dark green
Color xerogel, precursor powder is can be prepared by by xerogel grind into powder;
S6, Muffle furnace calcining:Precursor powder obtained by step S5 is placed in Muffle furnace, is calcined and is incubated at 700 DEG C
1h, is finally cooled to room temperature, that is, obtain CuCr2O4Black nano powder.
Further, in the step S4, mixing time is 4 hours.
Present invention additionally comprises the finger mark process for show of above-mentioned copper/chromium composite black nanometer powder, including aobvious method is directly brushed, spread
Powder trembles aobvious method and the aobvious method of suspension spray.
Further, described directly brush shows method, including, amount of copper/chromium composite black nanometer powder is dipped with fingerprint brush,
Swept from the bottom up along vertical roofing, powder is adhered to object plane, after streakline is seen, the powder that hair loss is painted is played, with hair
Brush aobvious along a direction brush along the flow direction of streakline, until streakline is clear;This method is applied on smooth impermeability object dives
In manifesting for impression of the hand.
Further, aobvious method is trembled in the dusting, including, amount of copper/chromium composite black nanometer powder is dipped with fingerprint brush,
Attack brush holder makes powder be covered in object plane;Then both hands hold two relative edges of object makes it shake up and down, allows powder to streak doubtful
There is the object plane of impression of the hand, you can show impression of the hand;Excessive powder is withdrawn into container, then gently the attack object back side is shaked off and floats on small plough
Powder in ditch;This method is applied to permeability or the semipermeability objects such as paper, true qualities wood.
Further, the aobvious method of suspension spray:Comprise the following steps:
S1, suspension preparation:First the neopelex of 0.5 g is dissolved in 50 mL deionized waters, stirring to table
After face activating agent neopelex is completely dissolved, the copper/chromium composite black nanometer powder CuCr of 5 g is added2O4With 50
ML deionized waters, stirring until powder be uniformly dispersed, it is not stratified.
S2, spray are aobvious:Carrying out spraying aobvious at blood latent fingerprint 20cm with the spray bottle equipped with suspension, solution is filled with sample
Tap is touched, and is observed again after slowly being rinsed with clear water after 30s and is manifested effect, is repeated if effect on driving birds is not good, until showing reason
Sample is dried up with hair dryer after thinking effect.
Copper/chromium composite black nanometer powder prepared by this method has certain dispersiveness in organic phase, residual with impression of the hand
Stay thing binding ability stronger;Its particle diameter is small, good with impression of the hand residue adhesiveness in nanoscale;And this compound is due to choosing
Selecting property is high, only with impression of the hand streakline on grease or hemoglobin occur adhesive attraction, handprint images ambient interferences can be reduced
Effect, strengthens contrast.Although powder is made up of metallic elements such as titanium, cobalts, the two has formed gold by high temperature sintering
Category ion solid solution, will not separate out under normal temperature and pressure, therefore possess environmental protection feature, harmless to operator.Therefore present invention tool
There are following Advantageous Effects:
1st, it is good to the fingerprint displaying effect in old impression of the hand and permeability object.
2nd, product possesses environmental protection feature, harmless to operator.
3rd, preparation method is simple and easy to apply, it is easy to popularization and application.
Brief description of the drawings
Fig. 1 is the X-ray diffraction spectrogram of the copper/chromium composite black nanometer powder prepared by the present invention.
Fig. 2 is the transmission electron microscope picture of the copper/chromium composite black nanometer powder prepared by the present invention.
Fig. 3 is the elementary analysis figure of the copper/chromium composite black nanometer powder prepared by the present invention.
Fig. 4 is that the copper/chromium composite black nanometer powder prepared by the present invention manifests design sketch for diving hand print with perspiration on paper.
Fig. 5 is that the copper/chromium composite black nanometer powder prepared by the present invention manifests design sketch for diving hand print with perspiration on ceramic tile.
Fig. 6 is that the copper/chromium composite black nanometer powder prepared by the present invention manifests effect for blood latent fingerprint on artificial leather
Figure.
Fig. 7 is that the copper/chromium composite black nanometer powder prepared by the present invention manifests design sketch for blood latent fingerprint on plastics.
Specific embodiment
Fig. 1 is the X-ray diffraction spectrogram of the copper/chromium composite black nanometer powder prepared by the present invention, and the figure shows mainly
Crystal face characteristic diffraction peak and standard card JCPDS:34-0424 is basically identical.
Fig. 2 is the transmission electron microscope picture of the copper/chromium composite black nanometer powder prepared by the present invention.The prepared powder of display
Particle diameter is mainly distributed 50 rans, and dispersiveness is preferably.
Fig. 3 is the elementary analysis figure of the copper/chromium composite black nanometer powder prepared by the present invention.Show powder by copper, chromium,
Three kinds of element compositions of oxygen, compositional purity is high, free from admixture.
Fig. 4 is that the copper/chromium composite black nanometer powder prepared by the present invention manifests design sketch for diving hand print with perspiration on paper,
Fig. 5 is that the copper/chromium composite black nanometer powder prepared by the present invention manifests design sketch for diving hand print with perspiration on ceramic tile, and Fig. 6 is this
Prepared copper/chromium composite black the nanometer powder of invention is used for blood latent fingerprint on artificial leather and manifests design sketch, and Fig. 7 is institute of the present invention
The copper of preparation/chromium composite black nanometer powder is used for blood latent fingerprint on plastics and manifests design sketch.From Fig. 4-Fig. 7:The present invention
The effect that prepared copper/chromium composite black nanometer powder manifests outmoded finger mark is good, and its finger mark mastoid process streakline is smooth, spillikin, small
The minutias such as point are protruded, and reagent is shown better than traditional powder.
Embodiment 1:
The preparation of copper/chromium composite black nanometer powder, comprises the following steps:
S1, to prepare copper-chromic salts molten:Cu (the N0 of 24.2g are weighed respectively3)2·3H2Cr (the N0 of 0 and 80g3)3·9H20 solid, matches somebody with somebody
Into 200mL hybrid metal saline solutions, ultrasonic mixing is uniform, and transfers them to flask;
S2, prepare citric acid solution:Weigh 76.9g citric acid solid, will its be made into the 200mL aqueous solution;
S3, prepare copper-chrome lemon hydrochlorate:The flask of step S1 is placed in thermostat water bath, it is 85 DEG C to set bath temperature,
Under strong stirring, citric acid solution obtained by step S2 is slowly instilled by flask by dropping funel, until completion of dropping;
S4, prepare gel:The Surfactant PEG 400 of 5.21g is added in the copper obtained by step S3-chrome lemon hydrochlorate, after
Continuous stirring, until moisture is evaporated in solution, forms the gel of clear, stops stirring;Wherein, to be used as colloidal sol steady for PEG400
Determine agent;The mixing time for preparing gel is 4 hours;
S5, prepare precursor powder:Gel obtained by step S4 is placed in vacuum drying chamber, 1h is dried in 95 DEG C, depth can be obtained
Green xerogel, precursor powder is can be prepared by by xerogel grind into powder;
S6, Muffle furnace calcining:Precursor powder obtained by step S5 is placed in Muffle furnace, is calcined and is incubated at 700 DEG C
1h, is finally cooled to room temperature, that is, obtain CuCr2O4Black nano powder.
Embodiment 2:
By the finger mark process for show of the copper obtained by the present invention/chromium composite black nanometer powder:
Directly brush aobvious method:Appropriate powder is dipped with fingerprint brush, is swept from the bottom up along vertical roofing, powder is adhered to thing
Face, after streakline is seen, plays the powder that hair loss is painted, and the flow direction along streakline is aobvious along a direction brush, until streakline is clear.
Embodiment 3:
By the finger mark process for show of the copper obtained by the present invention/chromium composite black nanometer powder:
Aobvious method is trembled in dusting:Appropriate powder is dipped with fingerprint brush, attack brush holder makes powder be covered in object plane;Then both hands are held
Two relative edges of object make it shake up and down, allow powder to streak the object plane for being suspected to have impression of the hand, you can to show impression of the hand.By excessive powder
Container is withdrawn, then gently the powder floated in small ditch dug with a plow is shaked off at the attack object back side.
Embodiment 4:
By the finger mark process for show of the copper obtained by the present invention/chromium composite black nanometer powder:
The aobvious method of suspension spray:Comprise the following steps:
S1, suspension preparation:First the neopelex of 0.5 g is dissolved in 50 mL deionized waters, stirring to table
After face activating agent neopelex is completely dissolved, the copper/chromium composite black nanometer powder CuCr of 5 g is added2O4With
50 mL deionized waters, stirring until powder be uniformly dispersed, it is not stratified.
S2, spray are aobvious:Carrying out spraying aobvious at blood latent fingerprint 20cm with the spray bottle equipped with suspension, solution is filled with sample
Tap is touched, and is observed again after slowly being rinsed with clear water after 30s and is manifested effect, is repeated if effect on driving birds is not good, until showing reason
Sample is dried up with hair dryer after thinking effect.
Copper/chromium composite black nanometer powder prepared by this method can fast and efficiently manifest outmoded finger mark.The preparation method
It is simple for process, it is easy to popularization and application;Its particle diameter is small, good with impression of the hand residue adhesiveness in nanoscale;And it is this compound
Thing due to selective height, only with impression of the hand streakline on grease or hemoglobin there is adhesive attraction, the handprint images back of the body can be reduced
The effect of scape interference, strengthens contrast, so to the good developing effect of outmoded finger mark.Although powder is by the metals such as titanium, cobalt unit
Element composition, but the two is by high temperature sintering, has been formed and will not separate out under metal ion solid solution, normal temperature and pressure, therefore has possessed green
Color characteristic of environmental protection, it is harmless to operator.
Finally, in addition it is also necessary to it is noted that listed above is only several specific embodiments of the invention.Obviously, this hair
Bright to be not limited to above example, one of ordinary skill in the art can directly derive from present disclosure or associate
All technical schemes, are considered as within protection scope of the present invention.
Claims (6)
1. the preparation method of a kind of copper/chromium composite black nanometer powder, it is characterised in that the method is comprised the following steps:
S1, prepare copper-chromium salt solution:Cu (the N0 of 24.2g are weighed respectively3)2·3H2Cr (the N0 of 0 and 80g3)3·9H20 solid,
It is made into 200mL hybrid metal saline solutions, ultrasonic mixing is uniform, and transfers them to flask;
S2, prepare citric acid solution:Weigh 76.9g citric acid solid, will its be made into the 200mL aqueous solution;
S3, prepare copper-chrome lemon hydrochlorate:The flask of step S1 is placed in thermostat water bath, it is 85 DEG C to set bath temperature,
Under strong stirring, citric acid solution obtained by step S2 is slowly instilled by flask by dropping funel, until completion of dropping;
S4, prepare gel:The Surfactant PEG 400 of 5.21g is added in the copper obtained by step S3-chrome lemon hydrochlorate, after
Continuous stirring, until moisture is evaporated in solution, forms the gel of clear, stops stirring;
S5 prepares precursor powder:Gel obtained by step S4 is placed in vacuum drying chamber, 1h is dried in 95 DEG C, can obtained dark green
Color xerogel, precursor powder is can be prepared by by xerogel grind into powder;
S6, Muffle furnace calcining:Precursor powder obtained by step S5 is placed in Muffle furnace, is calcined and is incubated at 700 DEG C
1h, is finally cooled to room temperature, that is, obtain CuCr2O4Black nano powder.
2. preparation method according to claim 1, it is characterised in that:In the step S4, mixing time is 4 hours.
3. a kind of finger mark process for show, it is characterised in that the copper/chromium prepared using the preparation method described in claim 1 or 2 is multiple
Conjunction black nano powder carries out finger mark to be manifested, including directly brushes aobvious method, and aobvious method and the aobvious method of suspension spray are trembled in dusting.
4. the finger mark process for show according to claim 3, it is characterised in that described directly to brush aobvious method, including, use fingerprint
Hairbrush dips amount of copper/chromium composite black nanometer powder, is swept from the bottom up along vertical roofing, powder is adhered to object plane,
After streakline is seen, the powder that hair loss is painted is played, the flow direction with hairbrush along streakline brushes aobvious along a direction, until streakline is clear
It is clear;This method is applied to potential impression of the hand on smooth impermeability object and manifests.
5. the finger mark process for show according to claim 3, it is characterised in that:Aobvious method is trembled in the dusting, including, use fingerprint
Hairbrush dips amount of copper/chromium composite black nanometer powder, and attack brush holder makes powder be covered in object plane;Then both hands hold object two
Individual relative edge makes it shake up and down, allows powder to streak the object plane for being suspected to have impression of the hand, you can to show impression of the hand;Excessive powder is withdrawn and is held
Device, then gently the powder floated in small ditch dug with a plow is shaked off at the attack object back side;This method is applied to the permeability such as paper, true qualities wood
Or semipermeability object.
6. the finger mark process for show according to claim 3, it is characterised in that:The aobvious method of suspension spray:Including following
Step:
S1, suspension preparation:First the neopelex of 0.5g is dissolved in 50 mL deionized waters, stirring to surface
After activating agent neopelex is completely dissolved, the copper/chromium composite black nanometer powder CuCr of 5 g is added2O4With 50
ML deionized waters, stirring until powder be uniformly dispersed, it is not stratified;
S2, spray are aobvious:Carrying out spraying aobvious at blood latent fingerprint 20cm with the spray bottle equipped with suspension, solution is fully connect with sample
Touch, observed again after slowly being rinsed with clear water after 30s and manifest effect, repeated if effect on driving birds is not good, until showing preferable effect
Sample is dried up with hair dryer after fruit.
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Cited By (2)
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CN108059187A (en) * | 2017-12-29 | 2018-05-22 | 华南协同创新研究院 | Copper-chrome black and preparation method and application is precipitated in a kind of low Cr VI |
CN108102427A (en) * | 2017-12-29 | 2018-06-01 | 华南协同创新研究院 | A kind of sub-micron ceramic pigment color containing cobalt black and its preparation method and application |
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108059187A (en) * | 2017-12-29 | 2018-05-22 | 华南协同创新研究院 | Copper-chrome black and preparation method and application is precipitated in a kind of low Cr VI |
CN108102427A (en) * | 2017-12-29 | 2018-06-01 | 华南协同创新研究院 | A kind of sub-micron ceramic pigment color containing cobalt black and its preparation method and application |
CN108059187B (en) * | 2017-12-29 | 2020-03-24 | 华南协同创新研究院 | Low hexavalent chromium separated copper-chromium black pigment and preparation method and application thereof |
CN108102427B (en) * | 2017-12-29 | 2020-10-09 | 华南协同创新研究院 | Submicron cobalt-containing black ceramic pigment and preparation method and application thereof |
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