CN105385436A - Nontoxic diluted-magnetic quantum dot material with fluorescence and room temperature ferromagnetism, and preparation method thereof - Google Patents
Nontoxic diluted-magnetic quantum dot material with fluorescence and room temperature ferromagnetism, and preparation method thereof Download PDFInfo
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- CN105385436A CN105385436A CN201510882258.3A CN201510882258A CN105385436A CN 105385436 A CN105385436 A CN 105385436A CN 201510882258 A CN201510882258 A CN 201510882258A CN 105385436 A CN105385436 A CN 105385436A
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 47
- 239000000463 material Substances 0.000 title claims abstract description 26
- 231100000252 nontoxic Toxicity 0.000 title claims abstract description 22
- 230000003000 nontoxic effect Effects 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 230000005307 ferromagnetism Effects 0.000 title abstract 3
- 150000002500 ions Chemical class 0.000 claims abstract description 6
- 230000005291 magnetic effect Effects 0.000 claims description 27
- 230000005294 ferromagnetic effect Effects 0.000 claims description 24
- 239000011701 zinc Substances 0.000 claims description 16
- -1 n-dodecyl Chemical group 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 229910021595 Copper(I) iodide Inorganic materials 0.000 claims description 7
- LSXDOTMGLUJQCM-UHFFFAOYSA-M copper(i) iodide Chemical compound I[Cu] LSXDOTMGLUJQCM-UHFFFAOYSA-M 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 3
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- VBXWCGWXDOBUQZ-UHFFFAOYSA-K diacetyloxyindiganyl acetate Chemical compound [In+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VBXWCGWXDOBUQZ-UHFFFAOYSA-K 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims description 3
- 238000010899 nucleation Methods 0.000 claims description 3
- 229920001187 thermosetting polymer Polymers 0.000 claims description 3
- 239000004246 zinc acetate Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 238000005979 thermal decomposition reaction Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000005418 spin wave Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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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
- C09K11/62—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing gallium, indium or thallium
- C09K11/621—Chalcogenides
- C09K11/623—Chalcogenides with zinc or cadmium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/0551—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0552—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 in the form of particles, e.g. rapid quenched powders or ribbon flakes with a protective layer
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Power Engineering (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses a nontoxic diluted-magnetic quantum dot material with fluorescence and room temperature ferromagnetism, and a preparation method thereof. The quantum dot material is Co: CuInS2 coated by two to four layers of a ZnS shell and has a structural formula of Co: CuInS2@ZnS, wherein Co exists in quantum dots in the form of ions. The preparation method comprises the following steps: (1) preparation of a Co: CuInS2 core with room temperature ferromagnetism; and (2) injecting a Zn source at room temperature and wrapping the core with a proper thickness of the ZnS shell layers. The preparation method adopts a single-pot thermal decomposition process, is simple in process, easy to operate, convenient in raw material supply and cheap in raw materials, can be completed in a common chemical laboratory and is easy to promote.
Description
Technical field
The invention belongs to quantum dot light emitting Material Field, particularly a kind ofly have nontoxic rare coupled magnetic quantum dot material of fluorescence and room-temperature ferromagnetic and preparation method thereof concurrently.
Background technology
Rare coupled magnetic quantum dot is by being combined with quantum dot by magnetic ion, makes it possess optical characteristics and magnetism characteristic.Utilize these characteristics to prepare self-spining device, and in order to make self-spining device at room temperature use, namely the harsh condition of the rare coupled magnetic quantum dot demand fulfillment one prepared at room temperature possesses ferromegnetism.And prepare the two problems that exists of rare magnon traditionally, one is prepare based on this kind of toxic heavy metal of Cd, and two great majority cannot realize room-temperature ferromagnetic.Therefore to prepare without Cd and rare coupled magnetic quantum dot with room-temperature ferromagnetic just seems particularly important.
Summary of the invention
Object of the present invention provides a kind of and has nontoxic rare coupled magnetic quantum dot material of fluorescence and room-temperature ferromagnetic and preparation method thereof concurrently, to solve traditional rare coupled magnetic quantum dot not to have room-temperature ferromagnetic problem containing Cd and great majority.
For achieving the above object, the present invention is by the following technical solutions:
Have a nontoxic rare coupled magnetic quantum dot material for fluorescence and room-temperature ferromagnetic concurrently, it is the Co:CuInS wrapped up by 2 to 4 layers of ZnS shell
2, structural formula is: Co:CuInS
2znS, Co exist in the form of an ion in quantum dot inside.
Have a preparation method for nontoxic rare coupled magnetic quantum dot material of fluorescence and room-temperature ferromagnetic concurrently, adopt non-toxic material Co, Cu, In, prepare rare magnetic Co:CuInS in accordance with the following steps
2znS quantum dot: add Co in a nitrogen environment in the DDT solution of n-dodecyl mereaptan
2+, Cu
+ ,in
3+, add thermosetting Co:CuInS
2quantum dot core; And then reduce temperature Zn presoma is dispersed in Co:CuInS
2in core solution; Reheat subsequently, until ZnS shell has grown.
Further, described Cu
+, Zn
2+, In
3+, Co
2+respectively from cuprous iodide (CuI), zinc acetate (Zn (OAc)
2), indium acetate (In (OAc)
3), Cobaltous diacetate (Co (OAc)
2); S source is: the n-dodecyl mereaptan decomposed under heating.
Further, Co
2+, Cu
+, In
3+the mol ratio of add-on be 1:2:2, Co
2+compare for 0.01mmol:12mL with the molecular volume of the DDT solution of n-dodecyl mereaptan.
Further, the mol ratio of Zn/ (Cu+In) is between 1.75 to 3.5.
Further, the mol ratio of Co/ (Cu+In) controls 2% to 10%.
Further, the mol ratio of Cu/ (Cu+In) controls between 33% to 66%, the Fluorescent peal of this quantum dot can be transferred to 555nm from 545nm.
Further, Co:CuInS
2nucleation temperature controls at 195-205 DEG C, and nucleus growth time controling is at 90-100Min.
Further, Zn presoma is dispersed in Co:CuInS
2temperature in core solution controls at 20-60 DEG C.
Further, the time controling that the temperature during growth of ZnS shell controls to grow at 220-235 DEG C, ZnS shell is at 100-120Min.
The invention has the beneficial effects as follows:
Quanta point material of the present invention had both had fluorescence and had had room-temperature ferromagnetic.Can realize Fluorescent peal by Cu/In ratio adjustable from 545-555nm, fluorescence quantum efficiency about 2% and maximum magnetic susceptibility are 4.996 × 10
-3to 13.457 × 10
-3between emu.And Co exists in the form of an ion in quantum dot inside, but not cluster form exists.Preparation method's required equipment simply, easily operates, raw material supplying is convenient, low in raw material price, all can complete at general chemical laboratory, is easy to promote; This not containing Cd and the material possessing room-temperature ferromagnetic be expected to prepare can room temperature use without cadmium self-spining device.
Accompanying drawing explanation
Fig. 1 is for having fluorescence and room-temperature ferromagnetic Co:CuInS
2the preparation flow figure of ZnS quantum dot;
Fig. 2 is the magnetic hysteresis loop figure under different Co/ (Cu+In) ratio;
Fig. 3 is that ZnS schemes at different PL;
Fig. 4 is Co:CuInS under different Cu/In
2znS quantum dot is PL figure under 3 layers of ZnS shell;
Fig. 5 is Co:CuInS under different Co/ (Cu+In) ratio
2znS quantum dot is PL figure under 3 layers of ZnS shell; Built-in picture to be Co doping be 2% Co:CuInS
2the pictorial diagram of ZnS quantum dot under the ultraviolet lamp of 365nm wavelength.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
As Fig. 1, the nontoxic rare coupled magnetic quantum dot material having fluorescence and room-temperature ferromagnetic concurrently of the present invention, it is the Co:CuInS wrapped up by 2 to 4 layers of ZnS shell
2, structural formula is: Co:CuInS
2znS, Co exist in the form of an ion in quantum dot inside.
The above-mentioned preparation method having nontoxic rare coupled magnetic quantum dot material of fluorescence and room-temperature ferromagnetic concurrently is: adopt non-toxic material Co, Cu, In, prepare rare magnetic Co:CuInS in accordance with the following steps
2znS quantum dot: add Co in a nitrogen environment in the DDT solution of n-dodecyl mereaptan
2+, Cu
+ ,in
3+, add thermosetting Co:CuInS
2quantum dot core; And then reduce temperature Zn presoma is dispersed in Co:CuInS
2in core solution; Reheat subsequently, until ZnS shell has grown.
In aforesaid method, Co:CuInS
2nucleation temperature controls at 195-205 DEG C, and nucleus growth time controling is at 90-100Min; Zn presoma is dispersed in Co:CuInS
2temperature in core solution controls at 20-60 DEG C; The time controling that temperature during the growth of ZnS shell controls to grow at 220-235 DEG C, ZnS shell is at 100-120Min.
Cu
+, Zn
2+, In
3+, Co
2+respectively from cuprous iodide (CuI), zinc acetate (Zn (OAc)
2), indium acetate (In (OAc)
3), Cobaltous diacetate (Co (OAc)
2); S source is: the n-dodecyl mereaptan decomposed under heating.
Co
2+, Cu
+, In
3+the mol ratio of add-on be 1:2:2, Co
2+compare for 0.01mmol:12mL with the molecular volume of the DDT solution of n-dodecyl mereaptan.
The mol ratio of control Zn/ (Cu+In) is between 1.75 to 3.5, and ZnS shell thickness is between 2 to 4 layers.
Mol ratio as Fig. 2 and Fig. 5, Co/ (Cu+In) controls 2% to 10%, to keep the fluorescence property of quantum dot.
Mol ratio as Fig. 4, Cu/ (Cu+In) controls between 33% to 66%, the Fluorescent peal of this quantum dot can be transferred to 555nm from 545nm.
Embodiment
The CuI used in the present embodiment, Co (OAc)
2, Zn (OAc)
2, In (OAc)
3the starting material such as powder are analytical reagent, and solvent and part are the DDT solution of n-dodecyl mereaptan, with deionized water rinse three times final vacuum dryings before glassware used uses.
It is the Co:CuInS of 2% that preparation has the Co doping that fluorescence and room-temperature ferromagnetic wrap up 3 layers of ZnS
2znS quantum dot, comprises the steps:
(1) there is ferromegnetism Co:CuInS
2core: add Co in a nitrogen environment in the DDT solution of 12mL n-dodecyl mereaptan
2+(0.01mmol), Cu
+(0.2mmol)
,in
3+(0.2mmol), be then heated to 200 DEG C, keep 90Min at 200 DEG C afterwards, finally go out thermal source cool to room temperature under normal temperature environment, carry out ZnS involucrum;
(2) ZnS involucrum: 1mmolZn presoma is joined the Co:CuInS under normal temperature
2in core solution, be then warmed up to 230 DEG C, keep 120Min at such a temperature afterwards.Complete to this Quantum Dots Growth.After cooling to room temperature, purify with the mixed solution of toluene and methyl alcohol 1:3, be finally dispersed in toluene.
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. have a nontoxic rare coupled magnetic quantum dot material for fluorescence and room-temperature ferromagnetic concurrently, it is characterized in that: it is the Co:CuInS wrapped up by 2 to 4 layers of ZnS shell
2, structural formula is: Co:CuInS
2znS, Co exist in the form of an ion in quantum dot inside.
2. have a preparation method for nontoxic rare coupled magnetic quantum dot material of fluorescence and room-temperature ferromagnetic concurrently, it is characterized in that: adopt non-toxic material Co, Cu, In, prepare rare magnetic Co:CuInS in accordance with the following steps
2znS quantum dot: add Co in a nitrogen environment in the DDT solution of n-dodecyl mereaptan
2+, Cu
+, In
3+, add thermosetting Co:CuInS
2quantum dot core; And then reduce temperature Zn presoma is dispersed in Co:CuInS
2in core solution; Reheat subsequently, until ZnS shell has grown.
3. have the preparation method of nontoxic rare coupled magnetic quantum dot material of fluorescence and room-temperature ferromagnetic as claimed in claim 2 concurrently, it is characterized in that: described Cu
+, Zn
2+, In
3+, Co
2+respectively from cuprous iodide (CuI), zinc acetate (Zn (OAc)
2), indium acetate (In (OAc)
3), Cobaltous diacetate (Co (OAc)
2); S source is: the n-dodecyl mereaptan decomposed under heating.
4. have the preparation method of nontoxic rare coupled magnetic quantum dot material of fluorescence and room-temperature ferromagnetic as claimed in claim 2 concurrently, it is characterized in that: Co
2+, Cu
+, In
3+the mol ratio of add-on be 1:2:2, Co
2+compare for 0.01mmol:12mL with the molecular volume of the DDT solution of n-dodecyl mereaptan.
5. have the preparation method of nontoxic rare coupled magnetic quantum dot material of fluorescence and room-temperature ferromagnetic as claimed in claim 2 concurrently, it is characterized in that: the mol ratio of Zn/ (Cu+In) is between 1.75 to 3.5.
6. have the preparation method of nontoxic rare coupled magnetic quantum dot material of fluorescence and room-temperature ferromagnetic as claimed in claim 2 concurrently, it is characterized in that: the mol ratio of Co/ (Cu+In) controls 2% to 10%.
7. have the preparation method of nontoxic rare coupled magnetic quantum dot material of fluorescence and room-temperature ferromagnetic as claimed in claim 2 concurrently, it is characterized in that: the mol ratio of Cu/ (Cu+In) controls between 33% to 66%, the Fluorescent peal of this quantum dot can be transferred to 555nm from 545nm.
8. have the preparation method of nontoxic rare coupled magnetic quantum dot material of fluorescence and room-temperature ferromagnetic as claimed in claim 2 concurrently, it is characterized in that: Co:CuInS
2nucleation temperature controls at 195-205 DEG C, and nucleus growth time controling is at 90-100Min.
9. have the preparation method of nontoxic rare coupled magnetic quantum dot material of fluorescence and room-temperature ferromagnetic as claimed in claim 2 concurrently, it is characterized in that: Zn presoma is dispersed in Co:CuInS
2temperature in core solution controls at 20-60 DEG C.
10. have the preparation method of nontoxic rare coupled magnetic quantum dot material of fluorescence and room-temperature ferromagnetic as claimed in claim 2 concurrently, it is characterized in that: the time controling that the temperature during growth of ZnS shell controls to grow at 220-235 DEG C, ZnS shell is at 100-120Min.
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|---|---|---|---|
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|---|---|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019119924A1 (en) * | 2017-12-18 | 2019-06-27 | 京东方科技集团股份有限公司 | Quantum dots and synthesis method therefor |
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| WO2019119924A1 (en) * | 2017-12-18 | 2019-06-27 | 京东方科技集团股份有限公司 | Quantum dots and synthesis method therefor |
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