CN104140084B - A kind of preparation method of carbonitride quantum dot - Google Patents
A kind of preparation method of carbonitride quantum dot Download PDFInfo
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- CN104140084B CN104140084B CN201410375843.XA CN201410375843A CN104140084B CN 104140084 B CN104140084 B CN 104140084B CN 201410375843 A CN201410375843 A CN 201410375843A CN 104140084 B CN104140084 B CN 104140084B
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Abstract
A preparation method for carbonitride quantum dot, comprises the following steps: (1) gets the raw materials ready; (2) dry and compressing tablet; (3) heat; (4) be separated; (5) dry.Template used in the present invention is sodium chloride crystal, and preparation technology is simple, and cost is low, can remove by water dissolution easily; Adopt trimeric cyanamide as raw material, melamine molecule inherently has ring-type carbonitride basic structural unit to exist, and prepare quantum dot productive rate high, product size homogeneity is good; The quantum dot specific surface area of preparation is high, and good water solubility, good dispersity, has the radiation of Naked eye visible hyperfluorescenceZeng Yongminggaoyingguang, be with a wide range of applications in fields such as fluorescence detection, luminescent device, biomarkers.
Description
Technical field
The present invention relates to a kind of preparation method of carbonitride quantum dot, particularly one prepares graphite phase carbon nitride (g-C
3n
4) method of quantum dot, belong to field of material preparation.
Background technology
Carbonitride by carbon and two kinds, nitrogen elementary composition, rich reserves, wide material sources, simple synthetic method, good economy performance and be easy to obtain.Graphite phase carbon nitride (g-C
3n
4) belonging to narrow gap semiconductor, its band gap width is about 2.7eV, nontoxic, not containing metal.Meanwhile, g-C
3n
4also there is the strong and electron transfer rate advantages of higher of good mechanical property, thermostability, acid-alkali-corrosive-resisting (all having good stability the aqueous solution of pH from 0 to 14) and oxidation capacity.Based on above-mentioned advantage, g-C
3n
4it is a kind of novel visible light catalyst, can be applied in the reactions such as photochemical catalysis, electrocatalysis, organic oxygenation dehydrogenation, simultaneously at other field, as energy transformation, gas storage and catch, the aspect such as purification, solar cell of water pollutant also applies well.
The preparation method that carbonitride is conventional mainly contains hot high pressure solution, vapour deposition process, ion implantation, hydro-thermal or solvent-thermal process method and electrochemical deposition technique etc.Recently, a kind of method of the organic matter precursors such as direct heating condensation polymerization cyanamide, cyanamid dimerization and trimeric cyanamide, becomes the many preparation g-C applied in recent years
3n
4the method of crystal.But block materials specific surface area prepared by this method is often less than 10m
2/ g, practical ranges is limited.
For this reason, usually consider to introduce the adjustable pore structure in aperture in body phase carbon nitride, or change the nanometer particle size of carbonitride and pattern increases its specific surface area.2005, (" Preparationandcharacterizationofwell-orderedhexagonalmes oporouscarbonnitride " AdvMater such as Vinu, 2005,17:1648) take mesoporous SBA-15 as hard template, prepare the carbonitride MCN-1 with ordered mesopore structure, but porous g-C
3n
4after synthesis, need to remove hard template, often need HF or NH using severe toxicity
4hF
2, larger to the injury of human body.Except vesicular structure, also can utilize space confinement method, synthesis smashes method, hot stripping method, solvent stripping method etc. and prepare the carbonitride quantum dot of a series of different-shape, nano wire, nanotube, nano belt, nanometer rod, nano particle, nanometer ball, nano-cluster (see " preparations and applicatio of high-specific surface area greying carbonitride ", petroleum journal, 2014,30:158).
Quantum dot is all subject to the impact of confinement effect in three directions, and diameter is generally less than 10nm, and because electronics and hole are by quantum confinement, continuous print energy band structure becomes the discrete energy levels structure with molecular characterization, can emitting fluorescence after being excited.Based on quantum effect, quantum dot is with a wide range of applications in fields such as solar cell, luminescent device, optical bio marks.
In carbonitride quantum dot, the people (" PreparationofphotoluminescentcarbonnitridedotsfromCCl such as Liu
4and1,2-ethylenediamine:Aheat-treatment-basedstrategy " JMaterChem, 2011,21:11726) utilize CCl
4be raw material with quadrol, obtained the carbonitride quantum dot with fluorescent characteristic by mixture heat process; The people such as Liu (" Acid-driven; microwave-assistedproductionofphotoluminescentcarbonnitr idedotsfromN; N-dimethylformamide " RSCAdv, 2011,1:951) utilize N, dinethylformamide is presoma, by the microwave treatment under acidic conditions, obtains the carbonitride quantum dot had compared with strong fluorescent properties; The people such as Liu (" Ageneralstrategyfortheproductionofphotoluminescentcarbon nitridedotsfromorganicaminesandtheirapplicationasnovelpe roxide-likecatalystsforcolorimetricdetectionofH
2o
2andglucose " RSCAdv, 2012,2:411) the carbonitride quantum dot that utilizes organic amine to be precursor power, and explore the purposes of catalysis detection; The people such as Xiao (" Microwave-assistedone-stepgreensynthesisofamino-function alizedfluorescentcarbonnitridedotsfromchitosan " Luminescence, 2013,28:612) from chitosan, microwave treatment technology is utilized to obtain the carbonitride quantum dot of amino functional; The people such as Zhou (" Alow-temperaturesolid-phasemethodtosynthesizehighlyfluor escentcarbonnitridedotswithtunableemission " ChemCommun, 2013,49:8605) utilize urea and Trisodium Citrate to prepare carbonitride quantum dot at a lower temperature, find that its fluorescence can regulate and control; The people such as Tang (" Carbonnitridequantumdots:anovelchemiluminescencesystemfo rselectivedetectionoffreechlorineinwater " AnalChem, 2014, the carbonitride quantum dot that 86:4528) utilizes Guanidinium hydrochloride and EDTA to be precursor power, finding can in order to detect the free chlorine in water; The people such as Zhang (" Polymernanodotsofgraphiticcarbonnitrideaseffectivefluore scentprobesforthedetectionofFe
3+andCu
2+ions " Nanoscale, 2014,6,4157) by block g-C
3n
4by obtaining few layer of azotized carbon nano point after hydrothermal technique process, find that it is at Fe
3+and Cu
2+detection aspect has excellent properties.
Visible, a lot of starting material can in order to prepare carbonitride quantum dot, and starting material used relate to and utilize the even block g-C of quadrol, DMF, organic amine, chitosan, EDTA, urea, Trisodium Citrate
3n
4above-mentioned carbonitride quantum dot also shows powerful application potential, but the homogeneity of above-mentioned preparation method's gained " quantum dot " size is desirable not to the utmost, size range comparatively large (5 ~ 80nm), so be commonly referred to as nano dot, and quantum dot mean diameter is generally less than 10nm; In addition, be small molecules mostly owing to using raw-material, so the productive rate of existing technology of preparing is lower, be generally no more than 50%, limit mass production and the application of product.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes the deficiencies in the prior art, and provide a kind of template to remove and be easier to, productive rate is higher, and cost is lower, the preparation method of the good carbonitride quantum dot of product size homogeneity.
The technical scheme that the present invention solves the employing of its technical problem is:
A preparation method for carbonitride quantum dot, comprises the following steps:
(1) get the raw materials ready: weigh trimeric cyanamide and sodium chloride crystal in proportion, wherein trimeric cyanamide and sodium chloride crystal mass ratio are the preferred 1:2-4 of 1:1 ~ 5(, more preferably 1:3); Be dissolved in deionized water by trimeric cyanamide and sodium chloride crystal, the quality of described deionized water is equivalent to 6 ~ 12 times (preferably 7 ~ 10 times of sodium chloride crystal quality; More preferably 8-9 doubly);
(2) dry and compressing tablet: by step (1) obtained aqueous solution at-40 ~-10 DEG C (preferably-30 ~-20 DEG C, more preferably-28 ~-22 DEG C) lyophilize 10 ~ 48h(preferably 20 ~ 24h) to constant weight, be placed in mould, utilize tabletting machine at 5 ~ 20MPa(preferably 10 ~ 15MPa) pressure becomes thickness to be the preferred 1-2cm of 0.5 ~ 3cm() sheet material;
(object of compressing tablet reduces gap, and compressing tablet is gordian technique of the present invention, otherwise can not get quantum dot)
(3) heat: step (2) resulting sheet is placed in porcelain boat, be placed in tube furnace, with 1 ~ 10ml/min(preferably 2 ~ 6ml/min, more preferably 3-4ml/min) flow velocity lead to nitrogen, with 1 ~ 30 DEG C/min(preferably 5 ~ 20 DEG C/min, more preferably 10-15 DEG C/min) temperature rise rate be raised to 400 ~ 700 DEG C (preferably 500 ~ 600 DEG C) and be incubated 1 ~ 2h, then be chilled to room temperature with stove;
(4) be separated: step (3) products therefrom is placed in the preferred 15-20min of mortar grinding 10 ~ 30min(), be dissolved in the deionized water being equivalent to raw material sodium chloride crystal quality 6 ~ 12 times (preferred 8-10 doubly) again, the preferred 20-40min of ultrasonic 10 ~ 60min(, more preferably 28-32min), with the preferred 600-800rpm of 500 ~ 1000rpm(, more preferably 650-750rpm) centrifugation rate removing precipitation, molecular weight is used to be the preferred 1000-2000 of 500 ~ 3000(, more preferably 1500-1800) dialysis tubing dialysis 24 ~ 48h(preferred 30-40h, more preferably 32-35h) remove sodium-chlor, obtain the aqueous solution containing quantum dot,
(5) dry: by step (4) obtained aqueous solution at-40 ~-10 DEG C of (preferably-30 ~-20 DEG C) the preferred 15-40h of lyophilize 10 ~ 48h(, more preferably 20 ~ 24h) to constant weight, obtain carbonitride quantum dot powder.
The present invention has the following advantages:
(1) template used is sodium chloride crystal, and preparation technology is simple, and cost is low, can remove by water dissolution easily;
(2) trimeric cyanamide, is commonly called as melamine, extract of protein, is the tripolymer of cyanamide, be a kind of triazines nitrogen heterocyclic ring organic compound, melamine molecule inherently has ring-type carbonitride basic structural unit to exist, and the present invention adopts trimeric cyanamide as raw material, research shows, at preparation g-C
3n
4quantum dot aspect has unique advantage, quantum dot productive rate high (90 ~ 96%), product size homogeneity good (4 ~ 16nm, mean value is less than 10nm); In addition, it is industrial chemicals, and cost is low, but is not useable for food-processing or food additives, for developing quantum dot, will significantly expand the purposes of trimeric cyanamide.
(3) high (300 ~ 340m of quantum dot specific surface area for preparing of the present invention
2/ g), good water solubility, good dispersity, has the radiation of Naked eye visible hyperfluorescenceZeng Yongminggaoyingguang, is with a wide range of applications in fields such as fluorescence detection, luminescent device, biomarkers.
Accompanying drawing explanation
Fig. 1 is the variation diagram in the embodiment of the present invention 1 " quantum dot " preparation process;
Fig. 2 is the transmission electron microscope picture of the embodiment of the present invention 1 " quantum dot ";
Fig. 3 is the size distribution plot of the embodiment of the present invention 1 " quantum dot ".
Embodiment
Below with reference to Figure of description and specific embodiment, the present invention is described in further details.
embodiment 1
The preparation method of the carbonitride quantum dot of the present embodiment, comprises the following steps:
(1) get the raw materials ready: weigh trimeric cyanamide 1g, sodium chloride crystal 3g(and trimeric cyanamide and sodium chloride crystal mass ratio are 1:3), trimeric cyanamide and sodium chloride crystal are dissolved in 30g deionized water;
(2) dry and compressing tablet: by step (1) obtained aqueous solution at-30 DEG C of lyophilize 24h to constant weight, be placed in mould, utilize the sheet material that tabletting machine becomes thickness to be 1cm at 10MPa pressure;
(3) heat: step (2) resulting sheet is placed in porcelain boat, is placed in tube furnace, lead to nitrogen with the flow velocity of 5ml/min, be raised to 600 DEG C with the temperature rise rate of 10 DEG C/min and be incubated 2h, being chilled to room temperature with stove;
(4) be separated: step (3) products therefrom is placed in mortar and grinds 20min, be dissolved in 30g deionized water again, ultrasonic 30min, with the centrifugation rate of 800rpm removing precipitation, use molecular weight is the dialysis tubing dialysis 30h removing sodium-chlor of 2000, obtains the aqueous solution containing quantum dot;
(5) dry: by step (4) obtained aqueous solution at-30 DEG C of lyophilize 30h to constant weight, obtain carbonitride quantum dot powder.
The present embodiment gained nitrogenize lateral size of dots is 5 ~ 16nm(average out to 9.0nm), specific surface area is 340m
2/ g, productive rate is 96wt%.Fig. 1 is the variation diagram in the present embodiment " quantum dot " preparation process; Fig. 2 is the transmission electron microscope picture of the present embodiment " quantum dot "; Fig. 3 is the size distribution plot of the embodiment of the present invention " quantum dot ".
embodiment 2
Only be with the difference of embodiment 1, in the present embodiment, trimeric cyanamide and sodium chloride crystal mass ratio are 1:1, namely trimeric cyanamide 1g is weighed in step (1), sodium chloride crystal 1g, trimeric cyanamide and sodium chloride crystal are dissolved in 10g deionized water, step (4) is also dissolved in 10g deionized water, and other are identical with embodiment 1.
The present embodiment gained nitrogenize lateral size of dots is 5 ~ 16nm(average out to 8.8nm), specific surface area is 300m
2/ g, productive rate is 92wt%.
embodiment 3
Only be with the difference of embodiment 1, in the present embodiment, trimeric cyanamide and sodium chloride crystal mass ratio are 1:5, namely trimeric cyanamide 1g is weighed in step (1), sodium chloride crystal 5g, trimeric cyanamide and sodium chloride crystal are dissolved in 50g deionized water, step (4) is also dissolved in 50g deionized water, and other are identical with embodiment 1.
The present embodiment gained nitrogenize lateral size of dots is 4 ~ 13nm(average out to 7.3nm), specific surface area is 310m
2/ g, productive rate is 94wt%.
embodiment 4
Only be with the difference of embodiment 1, in step (2), by step (1) obtained aqueous solution at-20 DEG C of lyophilize 48h to constant weight, be placed in mould, utilize the sheet material that tabletting machine becomes thickness to be 2cm at 20MPa pressure, other are identical with embodiment 1.
The present embodiment gained nitrogenize lateral size of dots is 4 ~ 14nm(average out to 8.0nm), specific surface area is 320m
2/ g, productive rate is 91wt%.
embodiment 5
Only be with the difference of embodiment 1, in step (2), by step (1) obtained aqueous solution at-40 DEG C of lyophilize 10h to constant weight, be placed in mould, utilize the sheet material that tabletting machine becomes thickness to be 0.5cm at 5MPa pressure, other are identical with embodiment 1.
The present embodiment gained nitrogenize lateral size of dots is 4 ~ 15nm(average out to 9.2nm), specific surface area is 330m
2/ g, productive rate is 90wt%.
embodiment 6
Only be with the difference of embodiment 1, in step (3), step (2) sheet material be placed in porcelain boat, be placed in tube furnace, lead to nitrogen with the flow velocity of 1ml/min, be raised to 500 DEG C with the temperature rise rate of 1 DEG C/min and be incubated 1h, be chilled to room temperature with stove, other are identical with embodiment 1.
The present embodiment gained nitrogenize lateral size of dots is 5 ~ 15nm(average out to 8.5nm), specific surface area is 325m
2/ g, productive rate is 95wt%.
embodiment 7
Only be with the difference of embodiment 1, in step (3), step (2) sheet material be placed in porcelain boat, be placed in tube furnace, lead to nitrogen with the flow velocity of 10ml/min, be raised to 700 DEG C with the temperature rise rate of 30 DEG C/min and be incubated 2h, be chilled to room temperature with stove, other are identical with embodiment 1.
The present embodiment gained nitrogenize lateral size of dots is 5 ~ 16nm(average out to 9.3nm), specific surface area is 335m
2/ g, productive rate is 92wt%.
embodiment 8
Only be with the difference of embodiment 1, in step (4), step (3) products therefrom is placed in mortar and grinds 30min, be dissolved in 30g deionized water, ultrasonic 60min, with the centrifugation rate of 1000rpm removing precipitation, use molecular weight is the dialysis tubing dialysis 48h removing sodium-chlor of 3000, obtain the aqueous solution containing quantum dot, other are identical with embodiment 1.
The present embodiment gained nitrogenize lateral size of dots is 5 ~ 15nm(average out to 8.2nm), specific surface area is 310m
2/ g, productive rate is 91wt%.
embodiment 9
Only be with the difference of embodiment 1, in step (4), step (3) products therefrom is placed in mortar and grinds 10min, be dissolved in 30g deionized water, ultrasonic 10min, with the centrifugation rate of 500rpm removing precipitation, use molecular weight is the dialysis tubing dialysis 24h removing sodium-chlor of 500, obtain the aqueous solution containing quantum dot, other are identical with embodiment 1.
The present embodiment gained nitrogenize lateral size of dots is 4 ~ 16nm(average out to 9.4nm), specific surface area is 330m
2/ g, productive rate is 92wt%.
embodiment 10
Only be with the difference of embodiment 8, in step (5), by step (4) obtained aqueous solution at-40 DEG C of lyophilize 10h to constant weight, can obtain carbonitride quantum dot powder, other are identical with embodiment 1.
The present embodiment gained nitrogenize lateral size of dots is 4 ~ 16nm(average out to 8.5nm), specific surface area is 305m
2/ g, productive rate is 94wt%.
embodiment 11
Only be with the difference of embodiment 9, in step (5), by step (4) obtained aqueous solution at-10 DEG C of lyophilize 48h to constant weight, can obtain carbonitride quantum dot powder, other are identical with embodiment 1.
The present embodiment gained nitrogenize lateral size of dots is 4 ~ 16nm(average out to 9.2nm), specific surface area is 320m
2/ g, productive rate is 93wt%.
Below be only the preferred embodiment of the present invention, protection scope of the present invention be not only confined to above-described embodiment, conceives various process programs without substantial differences all in protection scope of the present invention with the present invention.
Claims (9)
1. a preparation method for carbonitride quantum dot, is characterized in that, comprises the following steps:
(1) get the raw materials ready: weigh trimeric cyanamide and sodium chloride crystal in proportion, wherein trimeric cyanamide and sodium chloride crystal mass ratio are 1:1 ~ 5; Be dissolved in deionized water by trimeric cyanamide and sodium chloride crystal, the quality of described deionized water is equivalent to 6 ~ 12 times of sodium chloride crystal quality;
(2) dry and compressing tablet: by step (1) obtained aqueous solution at-40 ~-10 DEG C of lyophilize 10 ~ 48h to constant weight, be placed in mould, utilize tabletting machine to become thickness to be the sheet material of 0.5 ~ 3cm at 5 ~ 20MPa pressure;
(3) heat: step (2) resulting sheet is placed in porcelain boat, is placed in tube furnace, lead to nitrogen with the flow velocity of 1 ~ 10mL/min, be raised to 400 ~ 700 DEG C with the temperature rise rate of 1 ~ 30 DEG C/min and be incubated 1 ~ 2h, then being chilled to room temperature with stove;
(4) be separated: step (3) products therefrom is placed in mortar grinding 10 ~ 30min; be dissolved in the deionized water being equivalent to raw material sodium chloride crystal quality 6 ~ 12 times again; ultrasonic 10 ~ 60min; with the centrifugation rate of 500 ~ 1000rpm removing precipitation; use molecular weight is dialysis tubing dialysis 24 ~ 48h removing sodium-chlor of 500 ~ 3000, obtains the aqueous solution containing quantum dot;
(5) dry: by step (4) obtained aqueous solution at-40 ~-10 DEG C of lyophilize 10 ~ 48h to constant weight, obtain carbonitride quantum dot powder.
2. the preparation method of carbonitride quantum dot according to claim 1, is characterized in that, in step (3), the flow velocity passing into nitrogen is 2 ~ 6mL/min.
3. the preparation method of carbonitride quantum dot according to claim 1 and 2, is characterized in that, in step (3), temperature rise rate is 5 ~ 20 DEG C/min.
4. the preparation method of carbonitride quantum dot according to claim 1 and 2, is characterized in that, in step (3), is warmed up to 500 ~ 600 DEG C.
5. the preparation method of carbonitride quantum dot according to claim 1 and 2, is characterized in that, in step (2), cryodesiccated temperature is-30 ~-20 DEG C.
6. the preparation method of carbonitride quantum dot according to claim 1 and 2, is characterized in that, in step (2), the cryodesiccated time is 20 ~ 24h.
7. the preparation method of carbonitride quantum dot according to claim 1 and 2, is characterized in that, in step (2), the pressure of tabletting machine is 10 ~ 15MPa.
8. the preparation method of carbonitride quantum dot according to claim 1 and 2, is characterized in that, in step (5), cryodesiccated temperature is-30 ~-20 DEG C.
9. the preparation method of carbonitride quantum dot according to claim 1 and 2, is characterized in that, in step (5), the cryodesiccated time is 20 ~ 24h.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992282A (en) * | 2012-11-08 | 2013-03-27 | 南京大学 | Mesoporous C3N4 photocatalytic material prepared by using molten salt method and application thereof in photocatalysis field |
| CN103359727A (en) * | 2013-07-24 | 2013-10-23 | 云南师范大学 | Preparation method of oxygen and chlorine co-doped graphene quantum dots |
| CN103601162A (en) * | 2013-11-26 | 2014-02-26 | 天津大学 | Preparation method of graphite type carbon nitride nanotubes |
| CN103787290A (en) * | 2014-01-16 | 2014-05-14 | 大连民族学院 | High-performance humidity-sensitive material based on C3N4 nanosheet having intercalated structure and preparation method of high-performance humidity-sensitive material |
| CN103861632A (en) * | 2014-04-07 | 2014-06-18 | 吉林大学 | Preparation method for multi-hole carbon nitride photocatalytic material doped with sulphur |
-
2014
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992282A (en) * | 2012-11-08 | 2013-03-27 | 南京大学 | Mesoporous C3N4 photocatalytic material prepared by using molten salt method and application thereof in photocatalysis field |
| CN103359727A (en) * | 2013-07-24 | 2013-10-23 | 云南师范大学 | Preparation method of oxygen and chlorine co-doped graphene quantum dots |
| CN103601162A (en) * | 2013-11-26 | 2014-02-26 | 天津大学 | Preparation method of graphite type carbon nitride nanotubes |
| CN103787290A (en) * | 2014-01-16 | 2014-05-14 | 大连民族学院 | High-performance humidity-sensitive material based on C3N4 nanosheet having intercalated structure and preparation method of high-performance humidity-sensitive material |
| CN103861632A (en) * | 2014-04-07 | 2014-06-18 | 吉林大学 | Preparation method for multi-hole carbon nitride photocatalytic material doped with sulphur |
Non-Patent Citations (3)
| Title |
|---|
| "g-C3N4 quantum dots: direct synthesis upconversion properties and photocatalytic application";Wanjun Wang et al.;《ChemComm》;20140709;第50卷;第10148-10150页 * |
| "氮化碳材料的研究进展";李述中等;《河南师范大学学报(自然科学版)》;20060228;第34卷(第1期);第67-72页 * |
| "高比表面积石墨化氮化碳的制备及应用";李敏等;《石油学报（石油加工）》;20140228;第30卷(第1期);第158-168页 * |
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