CN106318385A - Method for preparing silicon nitrogen doped carbon quantum dots - Google Patents
Method for preparing silicon nitrogen doped carbon quantum dots Download PDFInfo
- Publication number
- CN106318385A CN106318385A CN201610688861.2A CN201610688861A CN106318385A CN 106318385 A CN106318385 A CN 106318385A CN 201610688861 A CN201610688861 A CN 201610688861A CN 106318385 A CN106318385 A CN 106318385A
- Authority
- CN
- China
- Prior art keywords
- brucite
- carbon quantum
- doped carbon
- hydrotalcite
- silica
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Biophysics (AREA)
- Optics & Photonics (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a method for preparing silicon nitrogen doped carbon quantum dots. The method sequentially comprises the following steps: adding hydrotalcite capable of passing through a sieve with the granularity of 20-50 meshes into a sodium trimethylsilyl aminoacetate liquid with the mass concentration of 0.1-1% according to the amount that the hydrotalcite per gram corresponds to 1-1.5mmol sodium trimethylsilyl aminoacetate, stirring in a thermostatic waterbath at the temperature of 60-70 DEG C for 5-6 hours, ageing for 12-24 hours, performing solid-liquid separation, and washing the precipitate for 2-3 times by using deionized water, thereby obtaining the sodium trimethylsilyl aminoacetate modified hydrotalcite; adding the obtained sodium trimethylsilyl aminoacetate modified hydrotalcite into a vacuum tube furnace, heating to the temperature of 400-600 DEG C under vacuum conditions, performing vacuum calcination for 2-4 hours, and cooling to room temperature; adding the calcined powder into a hydrochloric acid liquid with the mass concentration of 20-40%, wherein the powder per gram corresponds to 10-15ml of the hydrochloric acid liquid; stirring under nitrogen protection for 3-4 hours, and centrifuging at a high speed after the hydrotalcite sheet layer is totally dissolved, thereby obtaining the silicon sulfur doped carbon quantum dots. The method is simple in materials and mild in conditions.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, particularly relate to the preparation side of a kind of silicon nitrogen-doped 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 silicon nitrogen-doped carbon quantum dot.
To this end, the invention provides techniques below scheme, the preparation method of a kind of silicon nitrogen-doped carbon quantum dot, include successively
Following steps:
1) according to the amount of the corresponding 1～1.5mmol silica-based Sodium Glycinate of trimethyl of every gram of brucite, by 20-50 mesh sieve
Brucite join in the silica-based Sodium Glycinate solution of trimethyl that mass percent concentration is 0.1%～1%, 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 the silica-based Sodium Glycinate of trimethyl is modified；
2) brucite that silica-based for the trimethyl obtained Sodium Glycinate is modified 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 silicon nitrogen-doped 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 the silica-based Sodium Glycinate of acylate trimethyl 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, silica-based for trimethyl glycine root 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 silica-based Sodium Glycinate of correspondence 1.5mmol trimethyl, by 50 mesh sieves
Brucite join in the silica-based Sodium Glycinate solution of trimethyl that mass percent concentration is 1%, 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 the silica-based glycine of trimethyl
The brucite that sodium is modified；The brucite that silica-based for the trimethyl obtained Sodium Glycinate is modified 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 silicon nitrogen-doped carbon quantum dot after high speed centrifugation.
Embodiment 2
According to the amount of every gram of commercially available zinc-aluminum hydrotalcite silica-based Sodium Glycinate of correspondence 1mmol trimethyl, 20 mesh sieves will be crossed
Brucite joins in the silica-based Sodium Glycinate solution of trimethyl that mass percent concentration is 0.1%, 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 the silica-based glycine of trimethyl
The brucite that sodium is modified；The brucite that silica-based for the trimethyl obtained Sodium Glycinate is modified 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 silicon nitrogen-doped 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 the amount of every gram of brucite silica-based Sodium Glycinate of correspondence 1mmol trimethyl, the brucite crossing 50 mesh sieves is added
Enter in the silica-based Sodium Glycinate solution of the trimethyl that mass percent concentration is 0.5%, 70 DEG C of waters bath with thermostatic control stirred 6h,
Aging 24h, then solid-liquid separation, be washed with deionized water precipitate 3 times, dries, and obtains the modification of trimethyl silica-based Sodium Glycinate
Brucite；The brucite that silica-based for the trimethyl obtained Sodium Glycinate is modified 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 silicon nitrogen-doped carbon quantum dot after high speed centrifugation.
Claims (1)
1. the preparation method of a silicon nitrogen-doped carbon quantum dot, it is characterised in that: in turn include the following steps:
1) according to the amount of the corresponding 1～1.5mmol silica-based Sodium Glycinate of trimethyl of every gram of brucite, the water of 20-50 mesh sieve will be crossed
Talcum joins in the silica-based Sodium Glycinate solution of trimethyl that mass percent concentration is 0.1%～1%, 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 three
The brucite that methylsilyl Sodium Glycinate is modified；
2) brucite that silica-based for the trimethyl obtained Sodium Glycinate is modified is put in vacuum tube furnace, add 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
Silicon nitrogen-doped carbon quantum dot.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610688861.2A CN106318385A (en) | 2016-08-18 | 2016-08-18 | Method for preparing silicon nitrogen doped carbon quantum dots |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610688861.2A CN106318385A (en) | 2016-08-18 | 2016-08-18 | Method for preparing silicon nitrogen doped carbon quantum dots |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106318385A true CN106318385A (en) | 2017-01-11 |
Family
ID=57743202
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610688861.2A Pending CN106318385A (en) | 2016-08-18 | 2016-08-18 | Method for preparing silicon nitrogen doped carbon quantum dots |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106318385A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108333158A (en) * | 2018-01-24 | 2018-07-27 | 深圳大学 | Codope fluorescent carbon quantum dot and synthetic method and the method for detecting ferro concentration in serum |
| CN113277499A (en) * | 2021-05-07 | 2021-08-20 | 优彩科技(湖北)有限公司 | Preparation method and application of silicon-nitrogen co-doped graphene quantum dot |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103497762A (en) * | 2013-06-26 | 2014-01-08 | 上海交通大学 | Method for synthesizing nitrogen doped carbon quantum dot based on one-step monocomponent hydro-thermal synthesis |
| CN104140084A (en) * | 2014-08-01 | 2014-11-12 | 中国人民解放军国防科学技术大学 | Method for preparing carbon nitride quantum dots |
| CN104817063A (en) * | 2015-05-07 | 2015-08-05 | 常州大学 | Preparation method of two-dimension nitrogen- and phosphorus-doped graphene |
| CN104974749A (en) * | 2014-04-04 | 2015-10-14 | 中国科学院苏州纳米技术与纳米仿生研究所 | Nitrogen-doped carbon quantum dot with high fluorescence quantum yield and preparation method and application of nitrogen-doped carbon quantum dot |
-
2016
- 2016-08-18 CN CN201610688861.2A patent/CN106318385A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103497762A (en) * | 2013-06-26 | 2014-01-08 | 上海交通大学 | Method for synthesizing nitrogen doped carbon quantum dot based on one-step monocomponent hydro-thermal synthesis |
| CN104974749A (en) * | 2014-04-04 | 2015-10-14 | 中国科学院苏州纳米技术与纳米仿生研究所 | Nitrogen-doped carbon quantum dot with high fluorescence quantum yield and preparation method and application of nitrogen-doped carbon quantum dot |
| CN104140084A (en) * | 2014-08-01 | 2014-11-12 | 中国人民解放军国防科学技术大学 | Method for preparing carbon nitride quantum dots |
| CN104817063A (en) * | 2015-05-07 | 2015-08-05 | 常州大学 | Preparation method of two-dimension nitrogen- and phosphorus-doped graphene |
Non-Patent Citations (1)
| Title |
|---|
| 史文颖等，: ""二维限域空间内碳点的制备及性能调控"", 《中国化学会第30届学术年会摘要集-第二十一分会：Π-共轭材料》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108333158A (en) * | 2018-01-24 | 2018-07-27 | 深圳大学 | Codope fluorescent carbon quantum dot and synthetic method and the method for detecting ferro concentration in serum |
| CN108333158B (en) * | 2018-01-24 | 2020-12-08 | 深圳大学 | Double-doped fluorescent carbon quantum dot and synthetic method thereof |
| CN113277499A (en) * | 2021-05-07 | 2021-08-20 | 优彩科技(湖北)有限公司 | Preparation method and application of silicon-nitrogen co-doped graphene quantum dot |
| CN113277499B (en) * | 2021-05-07 | 2022-11-08 | 优彩科技(湖北)有限公司 | Preparation method and application of silicon-nitrogen co-doped graphene quantum dots |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106315557A (en) | Preparation method for nitrogen and phosphorus-doped carbon quantum dots | |
| Yang et al. | Crystal defect-mediated {0 1 0} facets of Bi2MoO6 nanosheets for removal of TC: enhanced mechanism and degradation pathway | |
| CN104817063B (en) | A kind of preparation method of two dimension nitrogen phosphorus doping Graphene | |
| CN102910622B (en) | Preparation method of two-dimensional nano-graphene | |
| Wang et al. | Enhanced visible light-driven photocatalytic activities and photoluminescence characteristics of BiOF nanoparticles determined via doping engineering | |
| Anilkumar et al. | Bio-inspired route for the synthesis of spherical shaped MgO: Fe3+ nanoparticles: Structural, photoluminescence and photocatalytic investigation | |
| Yang et al. | High-quality Cu2ZnSnS4 and Cu2ZnSnSe4 nanocrystals hybrid with ZnO and NaYF4: Yb, Tm as efficient photocatalytic sensitizers | |
| CN106318389A (en) | Preparation method of silicon-boron doped carbon quantum dots | |
| Bae et al. | Novel environment-friendly yellow pigments based on praseodymium (III) tungstate | |
| Liu et al. | Enhanced photoresponse of monolayer MoS2 through hybridization with carbon quantum dots as efficient photosensitizer | |
| CN106318385A (en) | Method for preparing silicon nitrogen doped carbon quantum dots | |
| CN106315556A (en) | Preparation method for nitrogen and chlorine-doped carbon quantum dots | |
| CN106318387A (en) | Preparation method of boron-sulfur doped carbon quantum dots | |
| CN106365143A (en) | Production method of boron doped carbon quantum dots | |
| Guzmán-Carrillo et al. | Facile control of ZnO nanostructures by varying molar concentration of zinc acetate | |
| CN106398689A (en) | A preparing method of a boron nitrogen doped carbon quantum dot | |
| CN106318383A (en) | Preparation method of sulfur-doped carbon quantum dots | |
| CN106315558A (en) | Preparation method of phosphorus and sulfur doped carbon quantum dots | |
| CN106318386A (en) | Preparation method of boron-chlorine doped carbon quantum dots | |
| CN106318391A (en) | Preparation method of silicon-phosphorous doped carbon quantum dots | |
| CN106335893A (en) | Preparation method of phosphorus-doped carbon quantum dots | |
| CN106350066A (en) | Method for preparing carbon quantum dots doped with phosphorus and chlorine | |
| CN106335894A (en) | Preparation method of silicon-doped carbon quantum dots | |
| Cho et al. | Quantum dot–layered double hydroxide composites for near-infrared emitting codes | |
| CN106318384A (en) | Preparation method of chlorine-doped carbon quantum dots |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170111 |
|
| WD01 | Invention patent application deemed withdrawn after publication |