CN102703057A - Application of polyamide-amine (PAMAM) dendrimer coated ZnX semiconductor quantum dots in fingerprint development - Google Patents
Application of polyamide-amine (PAMAM) dendrimer coated ZnX semiconductor quantum dots in fingerprint development Download PDFInfo
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Abstract
The invention relates to application of polyamide-amine (PAMAM) dendrimer coated ZnX (X=S, Se, Te) semiconductor quantum dots in fingerprint development, belonging to the technical field of material preparation. The method comprises the following steps: synthesizing a PAMAM dendrimer coated ZnX semiconductor quantum dot solution; and carrying out fluorescence labeling on latent fingerprints by using the PAMAM dendrimer coated ZnX semiconductor quantum dot solution. The method provided by the invention avoids the problem of toxicity of heavy metal ion Cd<2+> in the existing developing reagent, and the PAMAM dendrimer coated ZnX semiconductor quantum dots are harmless to the environment and users; the addition of the metal ion M<2+> can further enhance the fluorescence-emission strength of the ZnX semiconductor quantum dots; and by using the interaction between the PAMAM dendrimer and the fingerprint residue, the invention reserves the high development efficiency in the physical development method, and overcomes the defect of insufficient detailed development of fingerprint lines in the physical development method, thereby enhancing the precision and accuracy of the latent fingerprint development.
Description
Technical field
The present invention relates to the application of ZnX (X=S, Se, Te) semiconductor-quantum-point in fingerprint manifestation that a kind of polyamide-amide (PAMAM) dendrimer coats; Belong to technical field of material, use the ZnX semiconductor-quantum-point of the polyamide-amide dendrimer coating of present method preparation that the laten fingerprints residue is had target property and fluorescent appear effect.
Background technology
Fingerprint is also claimed impression of the hand, and the branch of broad sense and narrow sense is arranged.The generalized fingerprint comprises finger line, dactylus line and palmmprint.The fingerprint of narrow sense is meant that people's finger tips inboard refers to the surface detail of ball, and it begins growth in the 3rd～April that the human embryo grows, and is completed into June.
Everyone fingerprint all is its distinctive a kind of symbol, varies with each individual, different because of finger, has uniqueness; Under no special external force effect, mastoid process decorative pattern form and streakline minutia do not change because of the change at age, have lifelong unchangeability; Finger tips is quick of perception, and is maximum with the chance of object contact, and skin surface is covered with sweat and sebum, touches thing and stays trace; In addition, refer to that the neat rule of ball surface detail figure is easy to manifest, therefore for criminal case, the offender is retained in on-the-spot fingerprint, discloses the best evidence of its crime and its identity of locking exactly.And fingerprint also always is known as " king of evidence " by judicial circuit.
" plasticity-fingerprint " and " visible fingerprint " found easily and extracted, but for the just necessary utilization reliable method of laten fingerprints, it is manifested.1877, Charles Robert Richet Aubert was coated in silver nitrate solution and has shown sweat fingerprint on the paper, thereby become the technological founder of fingerprint manifestation in the process of research tetter and glandular secretion.Through 100 years of development, the fingerprint manifestation technology has developed into multi-door natural science professional techniques such as comprehensive physics, chemistry, bio-science.Wherein, Photoluminescence method is a kind of a kind of novel finger print process for show that just grows up in recent years; Have that cost is low, safe, selective power is strong, highly sensitive, the advantage that can detect single photon, therefore receive forensic science staff's favor.
Photoluminescence method manifests in the research of laten fingerprints, and embedded photoluminescent material commonly used is an organic fluorescent dye, like rhodamine 6G, Viola crystallina, Methylene blue etc.They have shortcomings such as excitation spectrum is narrow, emmission spectrum is wide, the laser coefficient is little, fluorescence intensity is low, optical stability is poor, bleach-resistant ability; Problems such as the fingerprint that manifests can exist that unclear, the false unique point of lines is many, the contrast gradient of fingerprint lines and substrate is little can't satisfy the high-precision requirement that at present fingerprint manifestation is proposed.Therefore, the research and development that the technical work personnel have invested the photoluminescent material with emphasis, semiconductor-quantum-point is wherein important a kind of.
Semiconductor-quantum-point and photoluminescence method are manifested the imagination that laten fingerprints combines derive from the widely used fluorescence quantum point mark technology of biological technical field.This technological ultimate principle is; Modified the fluorescence quantum of functional organic substance; The exposed functional groups in its outer end can carry out target with the target organism material and combine, thereby will be quantum dot-labeled on it, excites time generation fluoroscopic image at specific light source then.Theoretically, this semiconductor-quantum-point fluorescent marker method portable is applied to the developing latent finger prints using field.Therefore; From 2000, the technician of court began to be applied to developing latent finger prints using, like (Patent No.:US 09 487 702 such as Menzel; 2000, Patent No.:US 6; 30662B1,2001) reported that the pl-property CdS quantum dot that coats with the pamam dendrimer molecule carries out the research of developing latent finger prints using, has started the beginning that the fluorescence semiconductor-quantum-point that coats with dendrimer carries out developing latent finger prints using.
But Cd
2+Ion is a heavy metal ion, in use staff and environment is had certain injury, and the fingerprint presentation reagent of therefore studying environment-friendly type is very important.
Summary of the invention
The objective of the invention is in order to propose the application of ZnX semiconductor-quantum-point in fingerprint manifestation that a kind of polyamide-amide dendrimer coats.
The objective of the invention is to realize through following technical scheme.
The application of ZnX semiconductor-quantum-point in fingerprint manifestation that a kind of polyamide-amide dendrimer of the present invention coats; Adopt the pamam dendrimer molecule to coat the ZnX semiconductor-quantum-point; X is a kind of among S, Se or the Te; Pamam dendrimer exposed terminated groups type is amido, ester group, hydroxyl or carboxyl, and algebraically is 3.0～7.0; Concrete steps are:
1) ZnX (X=S, Se, Te) the semiconductor-quantum-point solution of synthetic pamam dendrimer molecule coating;
I) be 1 * 10 to concentration
-5MolL
-1～1 * 10
-4MolL
-1, pH is that to add concentration in 5.0～9.0 the pamam dendrimer molecular solution be 0.01molL
-1～0.1molL
-1Zn
2+Solion makes Zn
2+The mole ratio of ion and pamam dendrimer molecule is 0.5: 1～40: 1, and complexing 3～48h under 5 ℃～45 ℃ condition is until Zn
2+Ion and pamam dendrimer molecule coordination balance obtain Zn
2+The complex solution of ion and pamam dendrimer molecule;
The employed solvent of described pamam dendrimer molecular solution is a kind of in mixture or the DMSO 99.8MIN. of methyl alcohol, water, methyl alcohol and water; Described Zn
2+Ion comes from a kind of in liquor zinci chloridi, acetic acid zinc solution or the zinc nitrate solution;
Ii) X
2-The preparation in source
Work as X
2-The source is S
2-During the source, directly adopt sodium sulfide solution, potassium sulfide solution or hydrogen sulfide solution;
Work as X
2-The source is Se
2-During the source, be to place deionized water in 1: 1～1: 8 with mol ratio, stir selenium powder and Peng Qinghuana, 0 ℃～40 ℃ down reaction to generate concentration be 0.002molL
-1～0.2molL
-1Sodium hydrogen selenide solution;
Work as X
2-The source is Te
2-During the source, be to place deionized water in 1: 1～1: 8 with mol ratio, stir tellurium powder and Peng Qinghuana, 0 ℃～40 ℃ down reaction to generate concentration be 0.002molL
-1～0.2molL
-1Sodium hydrogen telluride solution;
Iii) to step I) in the complex solution that obtains, add step I i) X of preparation
2-Source solution, wherein, the X of adding
2-The mole number in source and Zn
2+The ionic mole number is identical; X
2-Be S
2-, Se
2-Or Te
2-A kind of in the ion; At 5 ℃～45 ℃ following stirring reaction 5min～60min; Using molecular weight cut-off is that 2000～5000 dialysis tubing carries out dialysis; Obtain the ZnX semiconductor-quantum-point solution that clarifying pamam dendrimer molecule coats, the wavelength of its maximum fluorescence emission intensity correspondence is adjustable in 450nm～750nm scope;
2) the ZnX semiconductor-quantum-point solution of pamam dendrimer molecule coating is to the fluorescent mark of laten fingerprints;
The substrate that is loaded with laten fingerprints directly is immersed in 1min～12h in the ZnX semiconductor-quantum-point solution that the pamam dendrimer molecule coats; Then substrate is taken out, use deionized water rinsing, natural airing; Obtain being loaded with the substrate of waiting to manifest laten fingerprints; And be placed in the darkroom, in 300nm～400nm scope, take pictures under the ultraviolet excitation, obtain the fluorescence fingerprint;
Above-mentioned steps 1) the ZnX semiconductor-quantum-point solution of middle synthetic pamam dendrimer molecule coating can also further be modified, i.e. the ZnXM of pamam dendrimer molecule coating
2+Semiconductor-quantum-point solution, M
2+Be Mn
2+, Co
2+, Zn
2+Or Cu
2+In a kind of; Concrete steps are:
Under 5 ℃～45 ℃, with M
2+Solion joins in the ZnX semiconductor-quantum-point solution that pamam dendrimer molecule that step 1) obtains coats, and the ZnX semiconductor-quantum-point is modified doping, makes M
2+The mole ratio of ion and ZnX semiconductor-quantum-point is 1: 1～8: 1, stirs 10min, obtains the ZnXM that the pamam dendrimer molecule coats
2+Quantum dot;
Described ZnXM
2+Be M
2+Ionic adsorption is on ZnX semiconductor-quantum-point surface.
Beneficial effect
Method preparation technology of the present invention is simple, and it is easy to manifest process, is easy to produce in enormous quantities and popularize;
Method of the present invention has avoided manifesting at present heavy metal ion Cd in the reagent
2+Toxicity problem, harmless to environment and user;
Metal ions M in the method for the present invention
2+Adding can further improve the fluorescent emission intensity of ZnX semiconductor-quantum-point;
Method of the present invention is utilized the interaction (physisorption and chemical coupling effect) between pamam dendrimer molecule and fingerprint residues thing; Both kept the physics process for show higher manifest efficient; Remedy the physics appearance method again the fingerprint ridge details has been manifested insufficient shortcoming, improved the precision and the accuracy of developing latent finger prints using.
Description of drawings
Fig. 1 Zn under the different complexing times
2+The UV-Vis abosrption spectrogram of/pamam dendrimer molecular complex;
Fig. 2 is the interval partial enlarged drawing of 260nm～300nm for absorbing wavelength among Fig. 1;
Fig. 3 Zn
2+The complexing action synoptic diagram of ion and pamam dendrimer molecule;
The preparation principle synoptic diagram of the ZnS semiconductor-quantum-point that Fig. 4 pamam dendrimer molecule coats;
The UV-Vis abosrption spectrogram of the ZnS semiconductor-quantum-point of Fig. 5 pamam dendrimer molecule and coating thereof;
The fluorescence emission spectrogram of the ZnS semiconductor-quantum-point of Fig. 6 pamam dendrimer molecule and coating thereof;
The ZnS semiconductor-quantum-point that Fig. 7 pamam dendrimer molecule coats is to the fluorescent mark photo of laten fingerprints;
The ZnSZn of Fig. 8 pamam dendrimer molecule and coating thereof
2+The fluorescence emission spectrogram of quantum dot.
Embodiment
The application of ZnS semiconductor-quantum-point in fingerprint manifestation that a kind of polyamide-amide dendrimer coats adopts the pamam dendrimer molecule to coat the ZnS semiconductor-quantum-point, and the pamam dendrimer exposed terminated groups is an amido, and algebraically is 5.0; Concrete steps are:
1) the ZnS semiconductor-quantum-point solution of synthetic pamam dendrimer molecule coating;
I) be 1 * 10 to 100mL concentration
-5MolL
-1, pH is that to add 0.25mL concentration in 7.0 the pamam dendrimer molecule methanol solution be 0.1molL
-1Liquor zinci chloridi, complexing 7h under 25 ℃ condition obtains Zn then
2+The complex solution of ion and pamam dendrimer molecule, in its complexing process to Zn
2+The complex solution of ion and pamam dendrimer molecule carries out the UV-Vis absorption spectrum and characterizes, and the result is as shown in Figure 1, and Fig. 2 is the interval partial enlarged drawing of 260nm～300nm for absorbing wavelength among Fig. 1; Can find out that by Fig. 1 and Fig. 2 the complexing time, the pamam dendrimer molecular solution had two big absorption peaks at 230nm and 280nm place when being 0h, they by in the pamam dendrimer molecule-CO-NH-(amido linkage) in N go up n → π that lone-pair electron shift to luminophore-C=O
*Transition causes; Along with the prolongation of complexing time, the pamam dendrimer molecular solution reduces at the uv-absorbing peak intensity at 280nm place gradually, reaches Schwellenwert behind the 6h;
Add Zn
2+Behind the ion, Zn
2+The ligand complex effect has taken place in ion and pamam dendrimer molecule, PAMAM-CO-NH-(amido linkage) in lone-pair electron on the N transit to Zn
2+Ionic d unoccupied orbital (Zn
2+The saturated ligancy of ionic typical case is 6, i.e. a Zn
2+Ion can be had an effect with 6 N at most, and is as shown in Figure 3), produce the charge transfer transition (LMCT) of part → metals ion, reduced lone-pair electron on self N to the n → π of the last π track transfer of luminophore-C=O
*Transition probability, so its uv-absorbing peak intensity at the 280nm place reduces gradually, up to balance;
During complexing 7h, Zn
2+The absorption peak of/pamam dendrimer molecular complex overlaps during almost with 6h, can think Zn under 35 ℃ of conditions
2+The coordination starting time of ion and pamam dendrimer molecule is 6～7h, shows Zn this moment
2+Ion has been broken through the obstruction of the peripheral limb of pamam dendrimer molecule fully, gets into its inside and has carried out coordination with the N part;
Ii) to step I) to add 0.25mL concentration in the complex solution that obtains be 0.1molL
-1Sodium sulfide solution; Stirring reaction 10min under 25 ℃ of conditions then; The use molecular weight cut-off is dialysis tubing dialysis in methyl alcohol of 3500, obtains the ZnS semiconductor-quantum-point solution that the pamam dendrimer molecule coats, and the corresponding wavelength of its maximum fluorescence emission intensity is positioned at 450nm; Fig. 4 is the concrete preparation principle synoptic diagram of the ZnS semiconductor-quantum-point of pamam dendrimer molecule coating.Therefrom can find out, at Zn
2+Ion and pamam dendrimer molecule take place to stablize on the basis of ligand complex effect, toward Zn
2+Add an amount of Na in the/pamam dendrimer molecular complex solution
2S solution is with obtaining a bigger nano-cluster, i.e. ZnS semiconductor-quantum-point.Though Na
2The moment that S solution adds can obtain a plurality of ZnS molecules that the pamam dendrimer molecule coats, but because the surface energy of single ZnS molecule is bigger, therefore is easy at pamam dendrimer intramolecule reunion cluster;
Fig. 5 is 25 o'clock for duty ratio, the uv-visible absorption spectra (ratio of the mol ratio of ZnS semiconductor-quantum-point and pamam dendrimer molecule is called duty ratio) of the ZnS semiconductor-quantum-point solution of pamam dendrimer molecule and coating thereof.As can beappreciated from fig. 5:
At Zn
2+Add S in the/pamam dendrimer molecular complex solution
2-Behind the ion, system new absorption peak occurred at the 272nm place.This peak is caused by ZnS semiconductor-quantum-point surface plasma body resonant vibration, shows that title product ZnS semiconductor-quantum-point generates;
Fig. 6 is 25 o'clock for duty ratio; The fluorescence emission spectrogram of the ZnS semiconductor-quantum-point solution of pamam dendrimer molecule and coating thereof; Therefrom can find out; Duty ratio is 25 o'clock, and the fluorescent emission intensity of the ZnS semiconductor-quantum-point that PAMAM coats is far longer than the fluorescent emission intensity of pamam dendrimer molecule self, shows that title product ZnS quantum dot generates;
2) the ZnS semiconductor-quantum-point solution of pamam dendrimer molecule coating is to the fluorescent mark of laten fingerprints;
The volunteer at first uses soap to give a baby a bath on the third day after its birth all over hand under flowing water, dries naturally, wipes and rubs forehead for several times, on tinfoil, restrains oily laten fingerprints sample respectively and preserves;
In the 1h presentation time; The tinfoil that is loaded with volunteer's laten fingerprints is dipped in the ZnS semiconductor-quantum-point solution that pamam dendrimer molecule that step 1) obtains coats fully, reacts 30min under the room temperature, then tinfoil is taken out; With tap water flushing 3 times; Dry, place to excite under the 365nm light source and take pictures fixingly, it is as shown in Figure 7 to obtain fingerprint.Can find out that therefrom under ultraviolet excitation, the laten fingerprints behind the mark is launched bright blue-fluorescence, the fingerprint lines is clear to link up, obvious with the substrate contrast.Reason is some organic constituent in the laten fingerprints, and like grease, electrostatic adsorption or aminolysis reaction have taken place the amine end groups peripheral with the pamam dendrimer molecule, and the ZnS semiconductor-quantum-point target that makes the pamam dendrimer molecule coat is combined on the mastoid process line of fingerprint.
1) the ZnS semiconductor-quantum-point solution of synthetic pamam dendrimer molecule coating;
I) be 1 * 10 to 100mL concentration
-5MolL
-1, pH is that to add 0.25mL concentration in 7.0 the pamam dendrimer molecule methanol solution be 0.1molL
-1Liquor zinci chloridi, complexing 7h under 25 ℃ condition obtains Zn then
2+The complex solution of ion and pamam dendrimer molecule;
Ii) to step I) to add 0.25mL concentration in the complex solution that obtains be 0.1molL
-1Sodium sulfide solution, stirring reaction 10min under 25 ℃ of conditions then, using molecular weight cut-off is dialysis tubing dialysis in methyl alcohol of 3500, obtains the ZnS semiconductor-quantum-point solution that the pamam dendrimer molecule coats;
2) under 25 ℃, be 0.1molL with the concentration of 0.375mL
-1Liquor zinci chloridi join in the ZnX semiconductor-quantum-point solution that pamam dendrimer molecule that step 1) obtains coats, the ZnX semiconductor-quantum-point is modified doping, stir 10min, obtain the ZnXM that the pamam dendrimer molecule coats
2+Quantum dot solution, and with fluorescence emission spectrum it is characterized, as shown in Figure 8; Therefrom can find out, add Zn
2+Behind the ion, the fluorescent emission intensity of the ZnS semiconductor-quantum-point solution that the pamam dendrimer molecule coats significantly strengthens; Reason is that the ZnS semiconductor-quantum-point is had the N in the pamam dendrimer molecule of stabilization, the O atom can with Zn
2+Ion coordination makes Zn
2+Ion is attached to ZnS semiconductor-quantum-point surface, saturated its surperficial S
2-Outstanding key, so fluorescent emission intensity strengthens.Show an amount of Metal Zn
2+Ionic adds the fluorescent emission performance that can effectively improve quantum dot.
3) ZnXM that the pamam dendrimer molecule that obtains is coated
2+Quantum dot solution carries out fluorescent mark to laten fingerprints.
The present invention includes but be not limited to above embodiment, every within spirit of the present invention and principle, done any local change, be equal to replacement all will be regarded as within protection scope of the present invention.
Claims (5)
1. the application of ZnX semiconductor-quantum-point in fingerprint manifestation that the polyamide-amide dendrimer coats; Adopt the pamam dendrimer molecule to coat the ZnX semiconductor-quantum-point; X is a kind of among S, Se or the Te; Pamam dendrimer exposed terminated groups type is amido, ester group, hydroxyl or carboxyl, and algebraically is 3.0～7.0; It is characterized in that concrete steps are:
1) the ZnX semiconductor-quantum-point solution of synthetic pamam dendrimer molecule coating;
I) be 1 * 10 to concentration
-5MolL
-1～1 * 10
-4MolL
-1, pH is that to add concentration in 5.0～9.0 the pamam dendrimer molecular solution be 0.01molL
-1～0.1molL
-1Zn
2+Solion makes Zn
2+The mole ratio of ion and pamam dendrimer molecule is 0.5: 1～40: 1, and complexing 3～48h under 5 ℃～45 ℃ condition is until Zn
2+Ion and pamam dendrimer molecule coordination balance obtain Zn
2+The complex solution of ion and pamam dendrimer molecule;
The employed solvent of described pamam dendrimer molecular solution is a kind of in mixture or the DMSO 99.8MIN. of methyl alcohol, water, methyl alcohol and water; Described Zn
2+Ion comes from a kind of in liquor zinci chloridi, acetic acid zinc solution or the zinc nitrate solution;
Ii) prepare X
2-The source
Iii) to step I) in the complex solution that obtains, add step I i) X of preparation
2-Source solution, wherein, the X of adding
2-The mole number in source and Zn
2+The ionic mole number is identical; X
2-Be S
2-, Se
2-Or Te
2-A kind of in the ion; At 5 ℃～45 ℃ following stirring reaction 5min～60min, using molecular weight cut-off is that 2000～5000 dialysis tubing carries out dialysis, obtains the ZnX semiconductor-quantum-point solution that clarifying pamam dendrimer molecule coats;
2) the ZnX semiconductor-quantum-point solution of pamam dendrimer molecule coating is to the fluorescent mark of laten fingerprints;
The substrate that is loaded with laten fingerprints directly is immersed in 1min～12h in the ZnX semiconductor-quantum-point solution that the pamam dendrimer molecule coats; Then substrate is taken out, use deionized water rinsing, natural airing; Obtain being loaded with the substrate of waiting to manifest laten fingerprints; And be placed in the darkroom, in 300nm～400nm scope, take pictures under the ultraviolet excitation, obtain the fluorescence fingerprint.
2. the application of ZnX semiconductor-quantum-point in fingerprint manifestation that a kind of polyamide-amide dendrimer according to claim 1 coats is characterized in that: X step I i)
2-The source is S
2-Sodium sulfide solution, potassium sulfide solution or hydrogen sulfide solution are directly adopted in the source.
3. the application of ZnX semiconductor-quantum-point in fingerprint manifestation that a kind of polyamide-amide dendrimer according to claim 1 coats is characterized in that: X step I i)
2-The source is Se
2-The source, the preparation method is: is to place deionized water in 1: 1～1: 8 with selenium powder and Peng Qinghuana with mol ratio, stir, 0 ℃～40 ℃ down reaction to generate concentration be 0.002molL
-1～0.2molL
-1Sodium hydrogen selenide solution.
4. the application of ZnX semiconductor-quantum-point in fingerprint manifestation that a kind of polyamide-amide dendrimer according to claim 1 coats is characterized in that: X step I i)
2-The source is Te
2-The source, the preparation method is: is to place deionized water in 1: 1～1: 8 with tellurium powder and Peng Qinghuana with mol ratio, stir, 0 ℃～40 ℃ down reaction to generate concentration be 0.002molL
-1～0.2molL
-1Sodium hydrogen telluride solution.
5. the application of ZnX semiconductor-quantum-point in fingerprint manifestation that a kind of polyamide-amide dendrimer according to claim 1 coats; It is characterized in that: the ZnX semiconductor-quantum-point solution to synthetic pamam dendrimer molecule in the step 1) coats is further modified, and concrete steps are:
Under 5 ℃～45 ℃, with M
2+Solion joins in the ZnX semiconductor-quantum-point solution that pamam dendrimer molecule that step 1) obtains coats, and the ZnX semiconductor-quantum-point is modified doping, makes M
2+The mole ratio of ion and ZnX semiconductor-quantum-point is 1: 1～8: 1, stirs 10min, obtains the ZnXM that the pamam dendrimer molecule coats
2+Quantum dot;
M
2+Be Mn
2+, Co
2+, Zn
2+Or Cu
2+In a kind of; ZnXM
2+Be M
2+Ionic adsorption is on ZnX semiconductor-quantum-point surface.
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