CN104449683B - Copper-cladding Aluminum Bar lattice strain quantum dot and preparation method thereof - Google Patents
Copper-cladding Aluminum Bar lattice strain quantum dot and preparation method thereof Download PDFInfo
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- CN104449683B CN104449683B CN201310436855.4A CN201310436855A CN104449683B CN 104449683 B CN104449683 B CN 104449683B CN 201310436855 A CN201310436855 A CN 201310436855A CN 104449683 B CN104449683 B CN 104449683B
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 41
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 26
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000005253 cladding Methods 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- RWSXRVCMGQZWBV-WDSKDSINSA-N glutathione Chemical compound OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O RWSXRVCMGQZWBV-WDSKDSINSA-N 0.000 claims abstract description 23
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- 108010024636 Glutathione Proteins 0.000 claims abstract description 13
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 13
- 229960003180 glutathione Drugs 0.000 claims abstract description 10
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 230000004044 response Effects 0.000 claims abstract description 7
- 239000004246 zinc acetate Substances 0.000 claims abstract description 7
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims abstract description 6
- 230000001105 regulatory effect Effects 0.000 claims abstract description 6
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000011592 zinc chloride Substances 0.000 claims abstract description 3
- 235000005074 zinc chloride Nutrition 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 25
- 239000002243 precursor Substances 0.000 description 24
- 239000003643 water by type Substances 0.000 description 12
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 9
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 9
- 229910052725 zinc Inorganic materials 0.000 description 9
- 239000011701 zinc Substances 0.000 description 9
- 239000010949 copper Substances 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 6
- 229910052793 cadmium Inorganic materials 0.000 description 6
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 3
- DIWNCNINVWYUCD-UHFFFAOYSA-N acetyl acetate;zinc Chemical compound [Zn].CC(=O)OC(C)=O DIWNCNINVWYUCD-UHFFFAOYSA-N 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
- 238000003384 imaging method Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 239000008346 aqueous phase Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 229910000059 tellane Inorganic materials 0.000 description 2
- PWKSKIMOESPYIA-BYPYZUCNSA-N L-N-acetyl-Cysteine Chemical compound CC(=O)N[C@@H](CS)C(O)=O PWKSKIMOESPYIA-BYPYZUCNSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- 239000000090 biomarker Substances 0.000 description 1
- 150000001661 cadmium Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- XONPDZSGENTBNJ-UHFFFAOYSA-N molecular hydrogen;sodium Chemical compound [Na].[H][H] XONPDZSGENTBNJ-UHFFFAOYSA-N 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000004054 semiconductor nanocrystal Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- 125000003396 thiol group Chemical class [H]S* 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention discloses a kind of Copper-cladding Aluminum Bar lattice strain quantum dot and preparation method thereof, its preparation method comprises the following steps：（1）Caddy or cadmium acetate, zinc acetate or zinc chloride, copper chloride dihydrate and glutathione are pressed 1:1.5‑4：0.025‑0.05:5 10 mol ratio is soluble in water to obtain mixed solution, wherein the concentration of the caddy or cadmium acetate is 0.2 0.6mmol/L；（2）Regulating step（1）The pH value of obtained mixed solution to 10.5 11.5, then by mixed solution at 93 98 DEG C the 120min of heating response 30, be down to room temperature, produce the Copper-cladding Aluminum Bar lattice strain quantum dot.The launch wavelength of the invention for using one step of metal bath heating to prepare small particle adjustable quantum dot from visible ray near infrared region, easy with method, reaction condition is gentle, and the time is short, favorable reproducibility, the advantages of monodispersity is good.
Description
Technical field
The present invention relates to technical field of inorganic nanometer material, more particularly to a kind of Copper-cladding Aluminum Bar lattice strain quantum dot and its
Preparation method.
Background technology
Quantum dot（Quantum dots, QDs）Also known as semiconductor nanocrystal is one kind by II-IV race or III-V race
The nanocrystal of element composition.Quantum dot is due to its excellent physicochemical properties, such as quantum size effect, luminescent properties and change
Processability is learned, and is received much concern in the application in the fields such as biomarker, bio-sensing, photoelectronics and solar cell.
Compared with traditional organic fluorescent dye, quantum dot has many excellent spectrum properties, is led in biology, medical science
Domain shows wide application prospect, near infrared fluorescence quantum point especially developed in recent years, due to having to tissue
There is strong penetration power, be particularly suitable for internal Noninvasive visible.And existing near-infrared quantum dots have particle diameter compared with
Greatly, it can not transport and be metabolized well in vivo, this strongly limits near-infrared quantum dots answering in living imaging
With.
At present, near-infrared quantum dots make its fluorescence emission wavelengths cover near infrared region mainly in the way of size control,
Synthesis is at present organometallic synthesis method and aqueous phase synthesis method using more method.The quantum dot stability of organic synthesis,
Though surface modifying preferably have poorly water-soluble, prepare the shortcomings of complicated, cost is higher, its application is limited.And aqueous phase is closed
Have the advantages that lower cost, simple to operate, reaction condition are gentle into method, easily regulate and control.
Alloy ratio is often used in existing quantum dot band engineering, core shell structure is transition metal element doped, or
The mode of lattice strain, the adjustable amplitude of fluorescence emission wavelengths is less or stronger to particle diameter accordance with tolerance, and in bio-imaging
Practical application in, the quantum dot of big particle diameter is not very practical.
The content of the invention
Based on this, it is an object of the invention to provide a kind of preparation method of Copper-cladding Aluminum Bar lattice strain quantum dot.
Specific technical scheme is as follows：
A kind of preparation method of Copper-cladding Aluminum Bar lattice strain quantum dot, comprises the following steps：
（1）Caddy or cadmium acetate, zinc acetate or zinc chloride, copper chloride dihydrate and glutathione are pressed 1:1.5-4:
0.025-0.05:5-10 mol ratio is soluble in water to obtain mixed solution, wherein the concentration of the caddy or cadmium acetate is 0.2-
0.6mmol/L；
（2）Regulating step（1）Then the pH value of obtained mixed solution heats mixed solution to 11 at 93-98 DEG C
30-120min is reacted, room temperature is down to, produces the Copper-cladding Aluminum Bar lattice strain quantum dot.
In one of the embodiments, the step（1）Middle caddy, zinc acetate, copper chloride dihydrate and glutathione
Mol ratio be 1：1.5：0.025-0.05：5-10 or 1：4：0.04-0.06：5-10.
In one of the embodiments, the step（1）Middle caddy, zinc acetate, copper chloride dihydrate and glutathione
Mol ratio be 1：1.5：0.025：5 or 1：4：0.05：10.
In one of the embodiments, the step（2）Middle mixed solution heating response 30-120min at 95 DEG C.
It is a further object of the present invention to provide a kind of Copper-cladding Aluminum Bar lattice strain quantum dot.
Specific technical scheme is as follows：
The Copper-cladding Aluminum Bar lattice strain quantum dot that above-mentioned preparation method is prepared.
In one of the embodiments, its launch wavelength is 600-750nm.
Advantages of the present invention is as follows：
Alloy ratio is often used in existing quantum dot band engineering, core shell structure is transition metal element doped, or
The mode of lattice, the adjustable amplitude of fluorescence emission wavelengths is little（Need to realize by changing particle diameter）Or to particle diameter according to
Patience is stronger, and in the practical application of bio-imaging, big particle diameter（The particle diameter of existing quantum dot is general>5nm）Quantum dot
It is very unpractical.The present invention is to combine alloy ratio, transition metal element doped, the advantage of lattice strain, using metal bath
Heat a step and prepare small particle（<5nm）Launch wavelength from visible ray near infrared region（600nm to 750nm）Adjustable amount
Sub-, easy with method, reaction condition is gentle, and the time is short, favorable reproducibility, the advantages of monodispersity is good.
Brief description of the drawings
Fig. 1 is the synthesis schematic diagram of preparation method of the present invention；
Fig. 2 is the XRD diffraction patterns for the product that embodiment 1-3 is prepared（1,2,3 represent embodiment 1,2,3 in figure）；
Fig. 3 is the transmission electron microscope photo for the product that embodiment 1 is prepared；
Fig. 4 is the transmission electron microscope photo for the product that embodiment 2 is prepared；
Fig. 5 is the transmission electron microscope photo for the product that embodiment 3 is prepared；
Fig. 6 is the product abosrption spectrogram that embodiment 1-3 is prepared（1,2,3 represent embodiment 1,2,3 in figure）；
Fig. 7 is the product launching light spectrogram that embodiment 1-3 is prepared（1,2,3 represent embodiment 1,2,3 in figure）.
Embodiment
The application is further elaborated by the following examples.
Embodiment 1
A kind of preparation method of Copper-cladding Aluminum Bar lattice strain quantum dot of the present embodiment, comprises the following steps：
（1）Precursor storing solution A：Anhydrous caddy 0.183g is weighed, is dissolved in 10ml ultra-pure waters；
（2）Precursor storing solution B：Acetic anhydride zinc 0.183g is weighed, is dissolved in 10ml ultra-pure waters；
（3）Precursor storing solution C：Copper chloride dihydrate 0.175g is weighed, is dissolved in 10ml ultra-pure waters；
（4）Precursor storing solution D：Reduced glutathione 0.123g is weighed, is dissolved in 10ml ultra-pure waters；
（5）0.4ml precursor storing solution A are taken, correspondence adds 0.6ml precursor storing solution B, adds 0.01ml precursor storing solutions
C, 5ml precursor storing solution D, are settled to 100ml（Anhydrous caddy, acetic anhydride zinc, copper chloride dihydrate and glutathione rub
You are than being 1:1.5：0.025:5）；
（6）Regulating step（5）The pH value of obtained mixed solution to 11, then by mixed solution at 95 DEG C heating response
30min, is down to room temperature, produces the Copper-cladding Aluminum Bar lattice strain quantum dot（Synthesize schematic diagram as shown in Figure 1）.
The result for the Copper-cladding Aluminum Bar lattice strain quantum dot elementary analysis that above-mentioned preparation method is obtained is as follows：
| Zinc/cadmium molar ratio | Copper/(zinc+cadmium) | Particle diameter |
| 0.91 | 0.51% | 3.5nm |
XRD is as shown in Figure 2, transmission electron microscope photo is as shown in figure 3, absorption spectrum is as shown in fig. 6, emission spectrum such as Fig. 7
It is shown.
Embodiment 2
A kind of preparation method of Copper-cladding Aluminum Bar lattice strain quantum dot of the present embodiment, comprises the following steps：
（1）Precursor storing solution A：Anhydrous caddy 0.183g is weighed, is dissolved in 10ml ultra-pure waters；
（2）Precursor storing solution B：Acetic anhydride zinc 0.183g is weighed, is dissolved in 10ml ultra-pure waters；
（3）Precursor storing solution C：Copper chloride dihydrate 0.175g is weighed, is dissolved in 10ml ultra-pure waters；
（4）Precursor storing solution D：Reduced glutathione 0.123g is weighed, is dissolved in 10ml ultra-pure waters；
（5）0.2ml precursor storing solution A are taken, correspondence adds 0.8ml precursor storing solution B, adds 0.01ml precursor storing solutions
C, 5ml precursor storing solution D, are settled to 100ml（Anhydrous caddy, acetic anhydride zinc, copper chloride dihydrate and glutathione rub
You are than being 1:4：0.05:10）；
（6）Regulating step（5）The pH value of obtained mixed solution to 11, then by mixed solution at 95 DEG C heating response
90min, is down to room temperature, produces the Copper-cladding Aluminum Bar lattice strain quantum dot.
The result for the Copper-cladding Aluminum Bar lattice strain quantum dot elementary analysis that above-mentioned preparation method is obtained is as follows：
| Zinc/cadmium molar ratio | Copper/(zinc+cadmium) | Particle diameter |
| 3.85 | 0.07% | 3.5nm |
XRD is as shown in Figure 2, transmission electron microscope photo is as shown in figure 4, absorption spectrum is as shown in fig. 6, emission spectrum such as Fig. 7
It is shown.
Embodiment 3
A kind of preparation method of Copper-cladding Aluminum Bar lattice strain quantum dot of the present embodiment, comprises the following steps：
（1）Precursor storing solution A：Anhydrous caddy 0.183g is weighed, is dissolved in 10ml ultra-pure waters；
（2）Precursor storing solution B：Acetic anhydride zinc 0.183g is weighed, is dissolved in 10ml ultra-pure waters；
（3）Precursor storing solution C：Copper chloride dihydrate 0.175g is weighed, is dissolved in 10ml ultra-pure waters；
（4）Precursor storing solution D：Reduced glutathione 0.123g is weighed, is dissolved in 10ml ultra-pure waters；
（5）0.2ml precursor storing solution A are taken, correspondence adds 0.8ml precursor storing solution B, adds 0.01ml precursor storing solutions
C, 5ml precursor storing solution D, are settled to 100ml（Anhydrous caddy, acetic anhydride zinc, copper chloride dihydrate and glutathione rub
You are than being 1:4：0.05:10）；
（6）Regulating step（5）The pH value of obtained mixed solution to 11, then by mixed solution at 95 DEG C heating response
120min, is down to room temperature, produces the Copper-cladding Aluminum Bar lattice strain quantum dot.
The result for the Copper-cladding Aluminum Bar lattice strain quantum dot elementary analysis that above-mentioned preparation method is obtained is as follows：
| Zinc/cadmium molar ratio | Copper/(zinc+cadmium) | Particle diameter |
| 7.55 | 0.25% | 4.0nm |
XRD is as shown in Figure 2, transmission electron microscope photo is as shown in figure 5, absorption spectrum is as shown in fig. 6, emission spectrum such as Fig. 7
It is shown.
Comparative example 1
A kind of Cd of water-soluble Cu dopingxCu1-xThe preparation method of Te quantum dots.The operating procedure of the preparation method be
Under nitrogen protection, previously prepared obtained sodium hydrogen telluride NaHTe or hydrogen telluride potassium KHTe solution are injected into well prepared in advance
Cadmium salt, mantoquita are with the mixed liquor of water-soluble N-acetyl-L-cysteine, obtaining that fluorescence emission wavelengths are adjustable, fluorescent quantum production
The Cd of the high water-soluble Cu doping of ratexCu1-xTe quantum dots.The Cd of this method naked exposed on external layer completely, in actual applications easily
Cause Cd2+Release, and Te sources preparation process more take it is whard to control.And the method that the present invention is coated using zinc sulphide has
What is imitated inhibits Cd2+Release, and sulphur source is directly derived from ligand mercapto, without nitrogen protection, without being manufactured separately.
Embodiment described above only expresses the several embodiments of the present invention, and it describes more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (5)
1. a kind of preparation method of Copper-cladding Aluminum Bar lattice strain quantum dot, it is characterised in that comprise the following steps：
(1) caddy or cadmium acetate, zinc acetate or zinc chloride, copper chloride dihydrate and glutathione are pressed 1:1.5-4:0.025-
0.05:5-10 mol ratio is soluble in water to obtain mixed solution, wherein the concentration of the caddy or cadmium acetate is 0.2-
0.6mmol/L；
(2) then the pH value for the mixed solution that regulating step (1) is obtained adds mixed solution to 10.5-11.5 at 93-98 DEG C
Thermal response 30-120min, is down to room temperature, produces the Copper-cladding Aluminum Bar lattice strain quantum dot；The Copper-cladding Aluminum Bar lattice strain quantum
The launch wavelength of point is 600-750nm, particle diameter<5nm.
2. the preparation method of Copper-cladding Aluminum Bar lattice strain quantum dot according to claim 1, it is characterised in that the step
(1) caddy in, zinc acetate, the mol ratio of copper chloride dihydrate and glutathione are 1：1.5：0.025-0.05：5 or 1：4：
0.025-0.05：10.
3. the preparation method of Copper-cladding Aluminum Bar lattice strain quantum dot according to claim 2, it is characterised in that the step
(1) caddy in, zinc acetate, the mol ratio of copper chloride dihydrate and glutathione are 1：1.5：0.025：5 or 1：4：0.05：
10。
4. the preparation method of the Copper-cladding Aluminum Bar lattice strain quantum dot according to claim any one of 1-3, it is characterised in that institute
State mixed solution heating response 30-120min at 95 DEG C in step (2).
5. the Copper-cladding Aluminum Bar lattice strain quantum dot that any one of the claim 1-4 preparation methods are prepared.
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