CN104140084A - Method for preparing carbon nitride quantum dots - Google Patents
Method for preparing carbon nitride quantum dots Download PDFInfo
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- CN104140084A CN104140084A CN201410375843.XA CN201410375843A CN104140084A CN 104140084 A CN104140084 A CN 104140084A CN 201410375843 A CN201410375843 A CN 201410375843A CN 104140084 A CN104140084 A CN 104140084A
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Abstract
A method for preparing carbon nitride quantum dots comprises the following steps of (1) material preparation, (2) drying and tabletting, (3) heating, (4) separation and (5) drying. Sodium chloride crystals are used as a template, the preparing process is simple and low in cost, and the sodium chloride crystals can be easily removed through water dissolution; melamine is used as the raw material, and annular carbon nitride basic structural units exist in melamine molecules, so that the yield of preparing the quantum dots is high, and product size uniformity is good; the prepared quantum dots are high in specific area, good in water solubility and good in dispersity, have strong fluorescent radiation visible under naked eyes, and have wide application prospects in the fields of fluorescence detection, light emitting devices, biomarker and the like.
Description
Technical field
The present invention relates to a kind of preparation method of carbonitride quantum dot, particularly one is prepared graphite-phase carbonitride (g-C
3n
4) method of quantum dot, belong to field of material preparation.
Background technology
Carbonitride is elementary composition by carbon and two kinds, nitrogen, and reserves are abundant, wide material sources, simple synthetic method, good economy performance and be easy to obtain.Graphite-phase carbonitride (g-C
3n
4) belonging to narrow gap semiconductor, its band gap width is about 2.7 eV, 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 thering is 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 the storage of energy transformation, gas 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 synthesis 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 many preparation g-C of application in recent years
3n
4the method of crystal.But block materials specific surface area prepared by this method is often less than 10 m
2/ g, practical ranges is limited.
For this reason, conventionally consider to introduce the adjustable pore structure in aperture in body phase carbon nitride, or nanometer particle size and the pattern of change carbonitride increase its specific surface area.2005, (" Preparation and characterization of well-ordered hexagonal mesoporous carbon nitride " the Adv Mater such as Vinu, 2005,17:1648) taking mesoporous SBA-15 as hard template, prepare the carbonitride MCN-1 with order mesoporous structure, but porous g-C
3n
4after synthetic, hard template be need to remove, hypertoxic HF or NH often needed to use
4hF
2, larger to the injury of human body.Except vesicular structure, also can utilize space confinement method, synthetic carbonitride quantum dot that method, hot stripping method, solvent stripping method etc. prepare a series of different-shapes, nano wire, nanotube, nano belt, nanometer rod, nano particle, nanometer ball, the nano-cluster smashed (referring to " preparation and the application 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, diameter is generally less than 10nm, and because electronics and hole are by quantum confinement, continuous 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.
Aspect carbonitride quantum dot, the people such as Liu (" Preparation of photoluminescent carbon nitride dots from CCl
4and 1,2-ethylenediamine:A heat-treatment-based strategy " J Mater Chem, 2011,21:11726) utilize CCl
4with quadrol be raw material, obtained having the carbonitride quantum dot of fluorescent characteristic by mixture heat processing; The people such as Liu (" Acid-driven; microwave-assisted production of photoluminescent carbon nitride dots from N; N-dimethylformamide " RSC Adv, 2011,1:951) utilize N, dinethylformamide is presoma, by the microwave treatment under acidic conditions, has obtained having the carbonitride quantum dot compared with strong fluorescent properties; The people such as Liu (" A general strategy for the production of photoluminescent carbon nitride dots from organic amines and their application as novel peroxide-like catalysts for colorimetric detection of H
2o
2and glucose " RSC Adv, 2012,2:411) utilize organic amine to prepare carbonitride quantum dot for presoma, and explored the purposes that catalysis is surveyed; The people such as Xiao (" Microwave-assisted one-step green synthesis of amino-functionalized fluorescent carbon nitride dots from chitosan " Luminescence, 2013,28:612) from chitosan, utilize microwave treatment technology to obtain the carbonitride quantum dot of amino functional; The people such as Zhou (" A low-temperature solid-phase method to synthesize highly fluorescent carbon nitride dots with tunable emission " Chem Commun, 2013,49:8605) utilize urea and Trisodium Citrate at lower temperature, to prepare carbonitride quantum dot, find that its fluorescence can regulate and control; The people such as Tang (" Carbon nitride quantum dots:a novel chemiluminescence system for selective detection of free chlorine in water " Anal Chem, 2014,86:4528) utilize Guanidinium hydrochloride and EDTA to prepare carbonitride quantum dot for presoma, discovery can be in order to survey the free chlorine in water; The people such as Zhang (" Polymer nanodots of graphitic carbon nitride as effective fluorescent probes for the detection of Fe
3+and Cu
2+ions " Nanoscale, 2014,6,4157) by block g-C
3n
4after processing by hydrothermal technique, obtain few layer of azotized carbon nano point, find that it is at Fe
3+and Cu
2+detection aspect has excellent properties.
Visible, a lot of starting material can be 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 has also shown powerful application potential, but the homogeneity of above-mentioned preparation method's gained " quantum dot " size is desirable not to the utmost, and size range is 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, provides a kind of template to remove and is easier to, and 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 its technical problem employing is:
A preparation method for carbonitride quantum dot, comprises the following steps:
(1) get the raw materials ready: weigh in proportion trimeric cyanamide and sodium chloride crystal, wherein trimeric cyanamide and sodium chloride crystal mass ratio are the preferred 1:2-4 of 1:1～5(, more preferably 1:3); Trimeric cyanamide and sodium chloride crystal are dissolved in deionized water, and 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) preferably 20～24h of lyophilize 10～48h() to constant weight, be placed in mould, utilize tabletting machine at preferably 10～15 MPa of 5～20MPa() to depress to thickness be the preferred 1-2cm of 0.5～3cm(to pressure) sheet material;
(object of compressing tablet is to reduce gap, and compressing tablet is gordian technique of the present invention, otherwise can not get quantum dot)
(3) heating: step (2) resulting sheet is placed in porcelain boat, be placed in tube furnace, with preferably 2 ~ 6 ml/min of 1～10ml/min(, more preferably 3-4 ml/min) the logical nitrogen of flow velocity, with preferably 5 ~ 20 DEG C/min of 1～30 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) separate: step (3) products therefrom is placed in to mortar and grinds the preferred 15-20min of 10～30min(), be dissolved in again in the deionized water that is equivalent to 6～12 times of raw material sodium chloride crystal quality (preferably 8-10 doubly), the preferred 20-40min of ultrasonic 10～60min(, more preferably 28-32min), with the preferred 600-800 rpm of 500 ~ 1000rpm(, more preferably 650-750 rpm) centrifugation rate remove precipitation, using molecular weight is the preferred 1000-2000 of 500～3000(, more preferably 1500-1800) the preferred 30-40h of dialysis tubing dialysis 24～48h(, more preferably 32-35h) remove sodium-chlor, obtain the aqueous solution that contains quantum dot,
(5) dry: by step (4) obtained aqueous solution at-40～-10 DEG C of (preferably-30～-20 DEG C) 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 using 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 itself just 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 (300～340 m of quantum dot specific surface area that prepared by the present invention
2/ g), and 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.
Brief description of the drawings
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(is that 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 tabletting machine to depress at 10MPa pressure the sheet material that thickness is 1cm;
(3) heating: step (2) resulting sheet is placed in porcelain boat, is placed in tube furnace, with the logical nitrogen of the flow velocity of 5ml/min, be raised to 600 DEG C and be incubated 2h with the temperature rise rate of 10 DEG C/min, be chilled to room temperature with stove;
(4) separate: step (3) products therefrom is placed in to mortar and grinds 20min, be dissolved in 30g deionized water, ultrasonic 30min, removes precipitation with the centrifugation rate of 800rpm again, use the dialysis tubing dialysis 30h that molecular weight is 2000 to remove sodium-chlor, obtain the aqueous solution that contains 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 340 m
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, be in step (1), to weigh trimeric cyanamide 1g, 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 300 m
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, be in step (1), to weigh trimeric cyanamide 1g, 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 310 m
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 tabletting machine to depress at 20MPa pressure the sheet material that thickness is 2cm, 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 320 m
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 tabletting machine to depress at 5MPa pressure the sheet material that thickness is 0.5cm, 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 330 m
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, with the logical nitrogen of the flow velocity of 1ml/min, be raised to 500 DEG C and be incubated 1h with the temperature rise rate of 1 DEG C/min, 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 325 m
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, with the logical nitrogen of the flow velocity of 10ml/min, be raised to 700 DEG C and be incubated 2h with the temperature rise rate of 30 DEG C/min, 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 335 m
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 to mortar and grinds 30min, be dissolved in 30g deionized water, ultrasonic 60min, removes precipitation with the centrifugation rate of 1000rpm, uses the dialysis tubing dialysis 48h that molecular weight is 3000 to remove sodium-chlor, obtain the aqueous solution that contains 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 310 m
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 to mortar and grinds 10min, be dissolved in 30g deionized water, ultrasonic 10min, removes precipitation with the centrifugation rate of 500rpm, uses the dialysis tubing dialysis 24h that molecular weight is 500 to remove sodium-chlor, obtain the aqueous solution that contains 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 330 m
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 305 m
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 320 m
2/ g, productive rate is 93wt%.
Below be only the preferred embodiment of the present invention, protection scope of the present invention is also 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 in proportion trimeric cyanamide and sodium chloride crystal, wherein trimeric cyanamide and sodium chloride crystal mass ratio are 1:1～5; Trimeric cyanamide and sodium chloride crystal are dissolved in deionized water, and 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 depress at 5～20MPa pressure the sheet material that thickness is 0.5～3cm;
(3) heating: step (2) resulting sheet is placed in porcelain boat, is placed in tube furnace, with the logical nitrogen of the flow velocity of 1～10ml/min, be raised to 400～700 DEG C and be incubated 1～2h with the temperature rise rate of 1～30 DEG C/min, then be chilled to room temperature with stove;
(4) separate: step (3) products therefrom is placed in to mortar and grinds 10～30min; be dissolved in again in the deionized water that is equivalent to 6～12 times of raw material sodium chloride crystal quality; ultrasonic 10～60min; centrifugation rate with 500 ~ 1000rpm is removed precipitation; use dialysis tubing dialysis 24～48h that molecular weight is 500～3000 to remove sodium-chlor, obtain the aqueous solution that contains 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 that passes into nitrogen is 2 ~ 6 ml/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 compressing tablet is 10～15 MPa.
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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