CN106315558A - Preparation method of phosphorus and sulfur doped carbon quantum dots - Google Patents
Preparation method of phosphorus and sulfur doped carbon quantum dots Download PDFInfo
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- CN106315558A CN106315558A CN201610698084.XA CN201610698084A CN106315558A CN 106315558 A CN106315558 A CN 106315558A CN 201610698084 A CN201610698084 A CN 201610698084A CN 106315558 A CN106315558 A CN 106315558A
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- sodium phosphate
- brucite
- dimethyl sulfydryl
- carbon quantum
- hydrotalcite
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/70—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus
- C09K11/701—Chalcogenides
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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Abstract
The invention discloses a preparation method of phosphorus and sulfur doped carbon quantum dots. The preparation method successively comprises the following steps: adding hydrotalcite which is sieved by a sieve with meshes of 20-50 meshes in O,O-dimethyl sulfydryl sodium phosphate solution with the mass percentage concentration of 0.1%-1% under the condition that every gram of the hydrotalcite corresponds to 1-1.5 mmol of O,O-dimethyl sulfydryl sodium phosphate; stirring and ageing in water bath at the constant temperature of 60-70 DEG C; then carrying out solid-liquid separation; washing precipitate for 2-3 times with deionized water and drying to obtain O,O-dimethyl sulfydryl sodium phosphate modified hydrotalcite; placing the obtained O,O-dimethyl sulfydryl sodium phosphate modified hydrotalcite in a vacuum tubular furnace; heating to the temperature of 400-600 DEG C under vacuum; calcining for 2-4 hours under vacuum and then cooling to room temperature; adding calcined powder in a hydrochloric acid solution with the mass percentage concentration of 20%-40%, wherein every gram of powder corresponds to 10-15 milliliters of the hydrochloric acid solution; stirring for 3-4 hours under nitrogen protection; and after a hydrotalcite lamellas are totally dissolved, centrifuging at high speed to obtain the phosphorus and sulfur doped carbon quantum dots. The method is simple in material and gentle in condition.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, particularly relate to the preparation side of a kind of phosphorus sulfur doping carbon quantum dot
Method.
Background technology
Quantum dot is at the nanometer semiconductor structure that exciton is held onto on three direction in spaces.This constraint can be returned
Tie in electrostatic potential (by outside electrode, doping, strain, impurity produces), the interface of two kinds of different semi-conducting materials (such as:
In group quantum dot), the surface (such as: semiconductor nanocrystal) of quasiconductor, or the combination of above three.Quantum dot has
The quantized power spectrum separated.Corresponding wave function is spatially positioned in quantum dot, but extends in several lattice period.
It is unit that one quantum dot has a small amount of electronics of (1-100) integer, electric hole or electronics electricity hole pair, i.e. its electricity carried
The integral multiple of electric charge.
Carbon quantum dot is similar with various metal quantum points, and carbon quantum dot can emit a brilliant light in the case of illumination.
Before it has application in the widest field including improvement biosensor, medical imaging devices and small light emitting diode
Scape.Because carbon nano-particles has the biggest surface area, so scientists thinks this nanoparticle phase for a long time always
Than macroscopical carbon, there is the most peculiar chemical and physical features.
Quantum dot usually extracts from the mixture of lead, cadmium and silicon, but these quantum dots are the most poisonous, to ring
Also there is the biggest harm in border.So scientists seeks to extract quantum dot in the compound that some are optimum.Opposing metallic quantum
For Dian, carbon quantum dot nonhazardous effect, the harm to environment is the least, and preparation cost is cheap.Its research represents luminescence and receives
Rice corpuscles research enters a new stage.
Layered di-hydroxyl composite metal oxidate (Layered Double Hydroxides is called for short LDH), also known as neatly
Stone, is the important inorganic functional material of a class.The layer structure of its uniqueness and laminate element and the adjustable degeneration of interlayer anion
Get more and more people's extensive concerning, introduce new object anion through ion exchange to interlayer and layer structure and composition can be made to produce phase
The change answered, thus a big class can be prepared there is the functional material of special nature.Hydrotalcite material belongs to anion type laminated
Compound.Lamellar compound refers to have layer structure, interlayer ion has a compounds of interchangeability, utilizes laminarization
Intercalation that compound main body is had under highly polar molecular action and the interchangeability of interlayer ion, by some functional visitors
Body material introduces bedding void and laminate distance is strutted thus form layer-pillared compound.
Brucite chemical structure of general formula is: [M2+ 1-xM3+x(OH)2]x+[(An-)x/n·mH2O], wherein M2+For Mg2+、Ni2+、
Mn2+、Zn2+、Ca2+、Fe2+、Cu2+Deng divalent metal；M3+For Al3+、Cr3+、Fe3+、Co3+Deng trivalent metal cation；
An-For anion, such as CO3 2-、NO3 -、Cl-、OH-、SO4 2-、PO4 3-、C6H4(COO)2 2-Etc. inorganic and organic ion and complexation from
Son, when interlevel inorganic anion is different, and the interlamellar spacing of brucite is different.
Summary of the invention
It is an object of the invention to as overcoming complicated process of preparation in prior art, expensive etc. deficiency, it is provided that a kind of
The preparation method of phosphorus sulfur doping carbon quantum dot.
To this end, the invention provides techniques below scheme, the preparation method of a kind of phosphorus sulfur doping carbon quantum dot, include successively
Following steps:
1) according to the amount of corresponding 1～1.5mmol O, the O-dimethyl sulfydryl sodium phosphate of every gram of brucite, by 20-50 mesh sieve
Brucite join in the O that mass percent concentration is 0.1%～1%, O-dimethyl sulfydryl sodium radio-phosphate,P-32 solution, 60～70
DEG C water bath with thermostatic control stirs 5～6h, aging 12～24h, then solid-liquid separation, it is washed with deionized water precipitate 2～3 times, dries,
To the brucite that O, O-dimethyl sulfydryl sodium phosphate is modified；
2) brucite of the O that will obtain, O-dimethyl sulfydryl sodium phosphate modification is put in vacuum tube furnace, at vacuum condition
Under be heated to 400～600 DEG C, vacuum calcining 2～4h, be then cooled to room temperature；
3) powder after calcining is joined in the hydrochloric acid solution that mass percent concentration is 20%～40%, every gram of powder
Corresponding 10～15 milliliters of hydrochloric acid solutions, stirring 3～4h, treats that brucite lamella all dissolves, after high speed centrifugation under nitrogen protection
Obtain phosphorus sulfur doping carbon quantum dot.
Compared with prior art, the present invention has a following useful technique effect:
1. preparing this quanta point material source simple, utilizing acylate O, O-dimethyl sulfydryl sodium phosphate is raw material, should
The structure of matter is regular, it is possible to obtain the preferable carbon quantum dot of pattern.
2. utilize the special construction of brucite, by anion exchange effect, O, O-dimethyl sulfydryl phosphate radical is exchanged to
Hydrotalcite layers, and it is fixed on interlayer.Guarantee that interlayer Organic substance is being with electric charge point position monomolecular dispersion, at 400～600 DEG C of carbon
Granulated carbon structure is formed after change.
3. the material after carbonization is after overpickling, brucite itself destructurized, and metal-oxide is molten by acid
Solving, the charcoal quantum dot of interlayer presents naturally, and process is simple, gentle.
Detailed description of the invention
Describe the present invention in detail below in conjunction with embodiment, but the present invention is not limited to this.
Embodiment 1
According to the amount of every gram of commercially available magnesium aluminum-hydrotalcite correspondence 1.5mmol O, O-dimethyl sulfydryl sodium phosphate, by 50 mesh sieves
Brucite join in the O that mass percent concentration is 1%, O-dimethyl sulfydryl sodium radio-phosphate,P-32 solution, 70 DEG C of waters bath with thermostatic control
Middle stirring 6h, aging 24h, then solid-liquid separation, it is washed with deionized water precipitate 3 times, dries, obtain O, O-dimethyl sulfydryl phosphoric acid
The brucite that sodium is modified；The brucite of the O that will obtain, O-dimethyl sulfydryl sodium phosphate modification is put in vacuum tube furnace, very
600 DEG C it are heated under empty condition, vacuum calcining 4h, it is then cooled to room temperature；Powder after calcining is joined mass percent
Concentration is in the hydrochloric acid solution of 40%, every gram of corresponding 15 milliliters of hydrochloric acid solutions of powder, stirs 4h under nitrogen protection, treats brucite
Lamella all dissolves, and obtains phosphorus sulfur doping carbon quantum dot after high speed centrifugation.
Embodiment 2
According to the amount of every gram of commercially available zinc-aluminum hydrotalcite correspondence 1mmol O, O-dimethyl sulfydryl sodium phosphate, 20 mesh sieves will be crossed
Brucite joins in the O that mass percent concentration is 0.1%, O-dimethyl sulfydryl sodium radio-phosphate,P-32 solution, 60 DEG C of waters bath with thermostatic control
Middle stirring 5h, aging 12h, then solid-liquid separation, it is washed with deionized water precipitate 2 times, dries, obtain O, O-dimethyl sulfydryl phosphoric acid
The brucite that sodium is modified；The brucite of the O that will obtain, O-dimethyl sulfydryl sodium phosphate modification is put in vacuum tube furnace, very
400 DEG C it are heated under empty condition, vacuum calcining 2h, it is then cooled to room temperature；Powder after calcining is joined mass percent
Concentration is in the hydrochloric acid solution of 20%, every gram of corresponding 10 milliliters of hydrochloric acid solutions of powder, stirs 3h under nitrogen protection, treats brucite
Lamella all dissolves, and obtains phosphorus sulfur doping carbon quantum dot after high speed centrifugation.
Embodiment 3
It is first according to document (Hydrotalcite by Hydrothermal Method synthesizes, applied chemistry, 2001,18,70-72) synthesis and prepares magnalium
Type brucite；Brucite is crossed 40 mesh sieves, standby.
According to every gram of brucite correspondence 1mmol O, the amount of O-dimethyl sulfydryl sodium phosphate, the brucite crossing 50 mesh sieves is added
Entering to mass percent concentration is in the O of 0.5%, O-dimethyl sulfydryl sodium radio-phosphate,P-32 solution, stirs 6h in 70 DEG C of waters bath with thermostatic control,
Aging 24h, then solid-liquid separation, be washed with deionized water precipitate 3 times, dries, and obtains the modification of O, O-dimethyl sulfydryl sodium phosphate
Brucite；The brucite of the O that will obtain, O-dimethyl sulfydryl sodium phosphate modification is put in vacuum tube furnace, under vacuum
It is heated to 500 DEG C, vacuum calcining 4h, it is then cooled to room temperature；Powder after calcining is joined mass percent concentration is
In the hydrochloric acid solution of 40%, every gram of corresponding 15 milliliters of hydrochloric acid solutions of powder, stir 4h under nitrogen protection, treat that brucite lamella is complete
Portion dissolves, and obtains phosphorus sulfur doping carbon quantum dot after high speed centrifugation.
Claims (1)
1. the preparation method of a phosphorus sulfur doping carbon quantum dot, it is characterised in that: in turn include the following steps:
1) according to the amount of corresponding 1～1.5mmol O, the O-dimethyl sulfydryl sodium phosphate of every gram of brucite, the water of 20-50 mesh sieve will be crossed
Talcum joins in the O that mass percent concentration is 0.1%～1%, O-dimethyl sulfydryl sodium radio-phosphate,P-32 solution, 60～70 DEG C of perseverances
Tepidarium stirs 5～6h, aging 12～24h, then solid-liquid separation, it is washed with deionized water precipitate 2～3 times, dries, obtain O,
The brucite that O-dimethyl sulfydryl sodium phosphate is modified；
2) brucite of the O that will obtain, O-dimethyl sulfydryl sodium phosphate modification is put in vacuum tube furnace, adds under vacuum
Hot to 400～600 DEG C, vacuum calcining 2～4h, it is then cooled to room temperature；
3) powder after calcining is joined in the hydrochloric acid solution that mass percent concentration is 20%～40%, every gram of powder correspondence
10～15 milliliters of hydrochloric acid solutions, stirring 3～4h, treats that brucite lamella all dissolves, obtains after high speed centrifugation under nitrogen protection
Phosphorus sulfur doping carbon quantum dot.
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| JPWO2021235025A1 (en) * | 2020-05-21 | 2021-11-25 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104817077A (en) * | 2015-05-07 | 2015-08-05 | 常州大学 | Preparation method of nitrogen- and phosphorus-doped graphene sheet |
| CN104817080A (en) * | 2015-05-07 | 2015-08-05 | 常州大学 | Preparation method of nitrogen-, sulfur- and phosphorus-doped graphene sheet |
| CN104817063A (en) * | 2015-05-07 | 2015-08-05 | 常州大学 | Preparation method of two-dimension nitrogen- and phosphorus-doped graphene |
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- 2016-08-18 CN CN201610698084.XA patent/CN106315558A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104817077A (en) * | 2015-05-07 | 2015-08-05 | 常州大学 | Preparation method of nitrogen- and phosphorus-doped graphene sheet |
| CN104817080A (en) * | 2015-05-07 | 2015-08-05 | 常州大学 | Preparation method of nitrogen-, sulfur- and phosphorus-doped graphene sheet |
| CN104817063A (en) * | 2015-05-07 | 2015-08-05 | 常州大学 | Preparation method of two-dimension nitrogen- and phosphorus-doped graphene |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2021235025A1 (en) * | 2020-05-21 | 2021-11-25 | ||
| WO2021235025A1 (en) * | 2020-05-21 | 2021-11-25 | 株式会社クレハ | Composition and method for producing same |
| JP7197750B2 (en) | 2020-05-21 | 2022-12-27 | 株式会社クレハ | Composition and method for producing same |
| US11898077B2 (en) | 2020-05-21 | 2024-02-13 | Kureha Corporation | Composition and method for producing same |
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