CN106590639B - A kind of adjustable inorganic fluorescent substances of fluorescence spectrum and preparation method thereof - Google Patents
A kind of adjustable inorganic fluorescent substances of fluorescence spectrum and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of adjustable inorganic fluorescent substances of fluorescence spectrum and preparation method thereof.The inorganic fluorescent substances are prepared by citric acid, boric acid and urea for raw material.Its element composition are as follows: 1~15wt% of carbon, 16~43wt% of boron element, 8~28wt% of nitrogen, 21~45wt% of oxygen element, wherein the carbon is few layer graphene film made of being decomposed and restored as citric acid.The preparation method comprises the following steps: in air atmosphere, the citric acid solution is reacted 3~10min under the conditions of the microwave power of 600W~900W；The reaction system is mixed with the boric acid with the mixed solution of urea, under the conditions of the microwave power of 400W~900W react 10~90min, be cooled to room temperature, by the solid abrasive being collected at powder to get.The present invention prepares inorganic fluorescent substances using two step microwave methods, easy to operate to be easily achieved, and can produce polychromatic photoinduced luminous material by control raw material ratio and microwave power and each step reaction time.
Description
Technical field
The invention belongs to technical field of function materials, and in particular to a kind of adjustable inorganic fluorescent substances of fluorescence spectrum
And preparation method thereof.
Background technique
Luminescent substance has become important materials indispensable in people's production and living, and the matrix of luminescent material is main at present
There are following a few class compounds: sulphur system, silicate, aluminate, phosphate, borate etc..For luminescent material, matrix material is removed
Material is outer, and activator or coactivator are also extremely important, and usual activator selects rare earth element, but rare earth element is expensive, closes
At temperature high (900 DEG C), protective atmosphere (nitrogen or argon gas) or reducing atmosphere (hydrogen) is needed to be sintered and its oxide and chlorine
Compound has larger toxicity (Journal of The Electrochemical Society, 2009,156 (5): 81~84.).Its
His some luminescent materials then need the higher preparation condition such as high temperature and pressure (J.Electrochem.Soc., 2010,157 (10):
329~333.).Therefore, the preparation and application of economic and environment-friendly luminescent material necessitate.BCNO is a kind of non-rear-earth-doped hair
The fluorescent material of light, it has, and low toxic and environment-friendly, synthesis cost is low, synthesis technology is simple, luminous efficiency is high, emission wavelength is adjustable
Equal many advantages, thus become luminescent material of new generation outstanding person (Adv.Mater., 2008,20 (17): 3235~
3238.)。
Application No. is 201310097837.8 Chinese invention patent applications to disclose a kind of wide excitation and emission spectra
The preparation method of BCNO fluorescent powder, it prepares BCNO fluorescent powder by raw material of melamine, boric acid and second triol, but when its reaction
Between it is longer, resulting materials luminous efficiency is lower；Application No. is 201410724748.6 Chinese invention patent and application No. is
The Chinese invention patent SEPARATE APPLICATION of 201410719862.X discloses a kind of orange-red light and the adjustable BCNO of red light emission is glimmering
The preparation method of light powder, both preparation method reaction steps are more, and preparation process is relative complex.
Summary of the invention
The technical problem to be solved by the present invention is to overcome defect of the existing technology, provide a kind of raw material and easily obtain
It takes, inorganic fluorescent substances of preparation method simplicity and preparation method thereof.
In order to solve the above-mentioned technical problems, the present invention provides a kind of inorganic fluorescent substances.
Inorganic fluorescent substances provided by the present invention are prepared by citric acid, boric acid and urea for raw material, yuan
Element composition are as follows: 1~15wt% of carbon, 16~43wt% of boron element, 8~28wt% of nitrogen, 21~45wt% of oxygen element,
In, the carbon is few layer graphene film made of being decomposed and restored as citric acid.
Above-mentioned inorganic fluorescent substances are prepared by the method comprising the following steps:
1) mixed solution of citric acid solution, boric acid and urea is prepared respectively；
2) in air atmosphere, by the citric acid solution 600W~900W (preferably 700W~850W) microwave power
Under the conditions of react 3~10min, obtain the reaction system of containing graphene；By the reaction system of the containing graphene and the boric acid
Mixed with the mixed solution of urea, under the conditions of the microwave power of 400W~900W (preferably 700W~850W) react 10~
90min is cooled to room temperature, and by the solid abrasive being collected at powder, obtains inorganic fluorescent substances.
In above method step 1), in the mixed solution of the boric acid and urea the mass ratio of boric acid and urea be 1:3~
20；The mass ratio of citric acid in the gross mass of the boric acid and urea and the citric acid solution is 300~150:1.
The citric acid solution can be prepared according to the method included the following steps: first by citric acid be dissolved in 40ml from
In sub- water, then through 5~20min ultrasonic treatment, obtain uniform and stable solution, wherein the power of the ultrasound is 30~70W, frequency
Rate is 30~70KHz.
The mixed solution of the boric acid and urea can be prepared according to the method included the following steps: by boric acid, urea
It is added in deionized water 50ml, then is ultrasonically treated through 10~60min, obtain the mixed solution of evenly dispersed boric acid and urea,
Wherein, the ultrasonic power is 30~70W, frequency is 30~70KHz.
In the present invention, raw material proportioning and reaction condition have a major impact the luminescent spectrum of material, feed change proportion, micro-
The embedded photoluminescent material of different colours spectrum can be obtained in wave power, reaction time.
Further, the boric acid and urea quality ratio are 1:11；The matter of the gross mass and citric acid of the boric acid and urea
Amount is than being 300:1, in the step 2), under the conditions of " 790~820W " (preferably 800W) microwave power, and citric acid solution microwave
After reacting 5min, mixed with the boric acid with the mixed solution of urea, in " 790W~820W " (preferably 800W) microwave power item
30min is reacted under part, obtains pale powder, under ultraviolet (365nm) excitation, blue-fluorescence is presented.
Further, the boric acid and urea quality ratio are 1:5；The quality of the gross mass and citric acid of the boric acid and urea
Than for 150:1, in the step 2), under the conditions of " 790~820W " (preferably 800W) microwave power, citric acid solution microwave is anti-
It after answering 3min, is mixed with the boric acid with the mixed solution of urea, in " 790W~820W " (preferably 800W) microwave power condition
Lower reaction 25min, obtains pale powder, and under ultraviolet (365nm) excitation, purple fluorescence is presented.
Further, the boric acid and urea quality ratio are 1:3；The quality of the gross mass and citric acid of the boric acid and urea
Than for 200:1, in the step 2), under the conditions of " 690~710W " (preferably 700W) microwave power, citric acid solution microwave is anti-
It after answering 10min, is mixed with the boric acid with the mixed solution of urea, in " 690~710W " (preferably 700W) microwave power condition
Lower reaction 50min, obtains grey powder, and under ultraviolet (365nm) excitation, yellow fluorescence is presented.
Further, the boric acid and urea quality ratio are 1:9；The quality of the gross mass and citric acid of the boric acid and urea
Than for 250:1, in the step 2), under the conditions of " 840~870W " (preferably 850W) microwave power, citric acid solution microwave is anti-
It after answering 8min, is mixed with the boric acid with the mixed solution of urea, under the conditions of " 840~870W " (preferably 850W) microwave power
30min is reacted, grey powder is obtained, under ultraviolet (365nm) excitation, weak blue fluorescence is presented.
Further, the boric acid and urea quality ratio are 1:5；The quality of the gross mass and citric acid of the boric acid and urea
Than for 120:1, in the step 2), under the conditions of " 790~820W " (preferably 800W) microwave power, citric acid solution microwave is anti-
It after answering 6min, is mixed with the boric acid with the mixed solution of urea, under the conditions of " 790~820W " (preferably 800W) microwave power
40min is reacted, grey powder is obtained, under ultraviolet (365nm) excitation, orange fluorescence is presented.
Further, the boric acid and urea quality ratio are 1:6；The quality of the gross mass and citric acid of the boric acid and urea
Than for 180:1, in the step 2), under the conditions of " 840~870W " (preferably 850W) microwave power, citric acid solution microwave is anti-
It after answering 3min, is mixed with the boric acid with the mixed solution of urea, microwave reaction under the conditions of " 840~870W " (preferably 850W)
90min obtains grey powder, and under ultraviolet (365nm) excitation, red fluorescence is presented.
The present invention prepares inorganic fluorescent substances using two step microwave methods, easy to operate to be easily achieved, and can lead to
Control raw material ratio and microwave power and each step reaction time are spent, polychromatic photoinduced luminous material is produced.
Compared with prior art, the invention has the following advantages that (1) raw material are nontoxic, it is easily obtained；(2) it makes
Method is simple, will not cause damages to environment；(3) luminous intensity is high, good brightness；(4) it by control process conditions, can produce more
Coloured light electroluminescent material.Under ultraviolet light (365nm) excitation, crocus, yellow, blue, red, light blue is presented in fluorescence color
Deng.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph for the embedded photoluminescent material that the embodiment of the present invention 1 is prepared.
Fig. 2 is the scanning electron microscope (SEM) photograph for the embedded photoluminescent material that the embodiment of the present invention 2 is prepared.
Specific embodiment
The present invention will be described below by way of specific embodiments, but the present invention is not limited thereto.
Experimental method used in following embodiments is conventional method unless otherwise specified；Institute in following embodiments
Reagent, material etc., are commercially available unless otherwise specified.
Embodiment 1
The inorganic fluorescent substances of the present embodiment are to be generated by citric acid, boric acid and urea through two-step method microwave reaction,
Products therefrom is in pale powder.Element composition are as follows: carbon 6wt%, boron element 34wt%, nitrogen 19wt%, oxygen element
41wt%, wherein carbon is layer graphene film few made of citric acid is decomposed and restored (see Fig. 1).
The preparation method of the inorganic fluorescent substances of the present embodiment, comprising the following steps:
(1) raw material preparation: in proportion weigh citric acid 0.02g (citric acid decomposes and restores made of lack layer graphene film,
See document Carbon, 2012,50 (12): 4738~4743.), boric acid 0.5g and urea 5.5g, i.e. boric acid be with urea quality ratio
1:11；The mass ratio of boric acid and urea gross mass and citric acid is 300:1
(2) prepare citric acid solution: ready citric acid is dissolved in 40ml ionized water by step (1) be configured to it is molten
Liquid, it is ultrasonic (ultrasonic power is 60W, frequency 50KHz) through 15min, obtain uniform and stable solution；
(3) match preparing boric acid, urea mixed solution: weighing boric acid, urea by predetermined mass ratio, deionized water 50ml is added to prepare
It is ultrasonic (ultrasonic power is 60W, frequency 50KHz) through 30min at mixed solution, obtain evenly dispersed boric acid, urea
Mixed solution；
(4) microwave heating is reacted: citric acid solution obtained by step (2) is placed in the micro-wave oven full of air atmosphere,
5min is reacted under 800W power condition, citric acid decomposes and is reduced to graphene.Obtained material and step (3) is prepared
Boric acid, urea liquid mixing, react 30min under 800W power condition, be cooled to room temperature, by the solid abrasive being collected at
Powder obtains inorganic fluorescent substances.
Using the present embodiment inorganic fluorescent substances, powder is in canescence.Element composition are as follows: carbon 6wt%, boron member
Plain 34wt%, nitrogen 19wt%, oxygen element 41wt%, wherein carbon is few layer graphite made of citric acid is decomposed and restored
Alkene piece.Blue light is presented under ultraviolet (365nm) excitation in gained powder.Its luminous efficiency is higher (53%), and luminous intensity is good.
Embodiment 2
The inorganic fluorescent substances of the present embodiment are to be reacted to give birth to through two step microwave heating methods by citric acid, boric acid and urea
At products therefrom is in pale powder.Element composition are as follows: carbon 5wt%, boron element 40wt%, nitrogen 21wt%, oxygen member
Plain 34wt%, wherein carbon is layer graphene film few made of citric acid is decomposed and restored (see Fig. 2).
The inorganic fluorescent substances of the present embodiment are compared with the preparation method of 1 inorganic fluorescent substances of embodiment, institute
It states boric acid and urea quality ratio is 1:5, the mass ratio of the gross mass and citric acid of boric acid and urea is 150:1.The step (4)
In, 3min is reacted under 800W power condition, citric acid decomposes and is reduced to graphene.Obtained material and boric acid, urea is molten
Liquid mixing, reacts 25min under 800W power condition, is cooled to room temperature, by the solid abrasive being collected at powder, obtain inorganic light
Electroluminescent material.Remaining method is same as Example 1.
It is in pale powder using the present embodiment inorganic fluorescent substances.Element composition are as follows: carbon 5wt%, boron member
Plain 40wt%, nitrogen 21wt%, oxygen element 34wt%, wherein carbon is few layer graphite made of citric acid is decomposed and restored
Alkene piece.Purple fluorescence is presented under ultraviolet light (365nm) excitation.Its luminous efficiency is higher (45%), and luminous intensity is bright.
Embodiment 3
The inorganic fluorescent substances of the present embodiment are to be reacted to give birth to through two step microwave heating methods by citric acid, boric acid and urea
At products therefrom gray powder.Element composition are as follows: carbon 12wt%, boron element 27wt%, nitrogen 26wt%, oxygen member
Plain 35wt%, wherein carbon is few layer graphene film made of citric acid is decomposed and restored.
The inorganic fluorescent substances of the present embodiment are compared with the preparation method of 1 inorganic fluorescent substances of embodiment, institute
It states boric acid and urea quality ratio is 1:3, the mass ratio of the gross mass and citric acid of the boric acid and urea is 200:1.The step
Suddenly in (4), 10min is reacted under 700W power condition, citric acid decomposes and is reduced to graphene.By obtained material and boric acid,
Urea liquid mixing, reacts 50min under identical power conditions, is cooled to room temperature, by the solid abrasive being collected at powder, obtain
Inorganic fluorescent substances.Remaining method is same as Example 1.
Use the present embodiment inorganic fluorescent substances, gray powder.Element composition are as follows: carbon 12wt%, boron member
Plain 27wt%, nitrogen 26wt%, oxygen element 35wt%, wherein carbon is few layer graphite made of citric acid is decomposed and restored
Alkene piece.Yellow fluorescence is presented under ultraviolet light (365nm) excitation.Its luminous efficiency is higher (58%), and luminous intensity is bright.
Embodiment 4
The inorganic fluorescent substances of the present embodiment are to be reacted to give birth to through two step microwave heating methods by citric acid, boric acid and urea
At products therefrom is in pale powder.Element composition are as follows: carbon 5wt%, boron element 32wt%, nitrogen 18wt%, oxygen member
Plain 45wt%, wherein carbon is few layer graphene film made of citric acid is decomposed and restored.
The inorganic fluorescent substances of the present embodiment are compared with the preparation method of 1 inorganic fluorescent substances of embodiment, institute
It states boric acid and urea quality ratio is 1:9, the mass ratio of the gross mass and citric acid of boric acid and urea is 250:1.The step (4)
In, 8min is reacted under 850W power condition, citric acid decomposes and is reduced to graphene.Obtained material and boric acid, urea is molten
Liquid mixing, reacts 30min under identical power conditions, is cooled to room temperature, and the solid abrasive being collected into is arrived at powder inorganic
Embedded photoluminescent material.Remaining method is same as Example 1.
Use the present embodiment inorganic fluorescent substances, gray powder.Element composition are as follows: carbon 5wt%, boron element
32wt%, nitrogen 18wt%, oxygen element 45wt%, wherein carbon is few layer graphene made of citric acid is decomposed and restored
Piece.Weak blue fluorescence is presented under ultraviolet light (365nm) excitation.Its luminous efficiency is higher (62%), and luminous intensity is bright.
Embodiment 5
The inorganic fluorescent substances of the present embodiment are to be reacted to give birth to through two step microwave heating methods by citric acid, boric acid and urea
At products therefrom is in pale powder.Element composition are as follows: carbon 10wt%, boron element 27wt%, nitrogen 20wt%, oxygen
Element 43wt%, wherein carbon is few layer graphene film made of citric acid is decomposed and restored.
The inorganic fluorescent substances of the present embodiment are compared with the preparation method of 1 inorganic fluorescent substances of embodiment, institute
It states boric acid and urea quality ratio is 1:5, the mass ratio of the gross mass and citric acid of boric acid and urea is 120:1.The step (4)
In, 6min is reacted under 800W power condition, citric acid decomposes and is reduced to graphene.Obtained material and boric acid, urea is molten
Liquid mixing, reacts 40min under identical power conditions, is cooled to room temperature, and the solid abrasive being collected into is arrived at powder inorganic
Embedded photoluminescent material.Remaining method is same as Example 1.
It is in pale powder using the present embodiment inorganic fluorescent substances.Element composition are as follows: carbon 10wt%, boron
Element 27wt%, nitrogen 20wt%, oxygen element 43wt%, wherein carbon is few layer stone made of citric acid is decomposed and restored
Black alkene piece.Orange fluorescence is presented under ultraviolet light (365nm) excitation.Its luminous efficiency is higher (48%), and luminous intensity is bright.
Embodiment 6
The inorganic fluorescent substances of the present embodiment are to be reacted to give birth to through two step microwave heating methods by citric acid, boric acid and urea
At products therefrom is in pale powder.Element composition are as follows: carbon 13wt%, boron element 29wt%, nitrogen 19wt%, oxygen
Element 39wt%, wherein carbon is few layer graphene film made of citric acid is decomposed and restored.
The inorganic fluorescent substances of the present embodiment are compared with the preparation method of 1 inorganic fluorescent substances of embodiment, institute
It states boric acid and urea quality ratio is 1:6, the mass ratio of the gross mass and citric acid of boric acid and urea is 180:1.The step (4)
In, 3min is reacted under 850W power condition, citric acid decomposes and is reduced to graphene.Obtained material and boric acid, urea is molten
Liquid mixing, reacts 90min under identical power conditions, is cooled to room temperature, and the solid abrasive being collected into is arrived at powder inorganic
Embedded photoluminescent material.Remaining method is same as Example 1.
It is in pale powder using the present embodiment inorganic fluorescent substances.Element composition are as follows: carbon 13wt%, boron
Element 29wt%, nitrogen 19wt%, oxygen element 39wt%, wherein carbon is few layer stone made of citric acid is decomposed and restored
Black alkene piece.Red fluorescence is presented under ultraviolet light (365nm) excitation.Its luminous efficiency is higher (43%), and luminous intensity is bright.
Claims (7)
1. a kind of preparation method of inorganic fluorescent substances, includes the following steps:
1) mixed solution of citric acid solution, boric acid and urea is prepared respectively；
2) in air atmosphere, the citric acid solution is reacted to 3~10min under the conditions of the microwave power of 600W~900W,
Obtain the reaction system of containing graphene；The reaction system of the containing graphene and the mixed solution of the boric acid and urea are mixed
Close, under the conditions of the microwave power of 400W~900W react 10~90min, be cooled to room temperature, by the solid abrasive being collected at
Powder to get arrive inorganic fluorescent substances；
The inorganic fluorescent substances are prepared by citric acid, boric acid and urea for raw material, element composition, with quality
Percentage composition meter, are as follows: 1~15wt% of carbon, 16~43wt% of boron element, 8~28wt% of nitrogen, 21~45wt% of oxygen element,
Wherein, the carbon is few layer graphene film made of being decomposed and restored as citric acid；
In step 1), the mass ratio of boric acid and urea is 1:3~20 in the mixed solution of the boric acid and urea；The boric acid with
The mass ratio of citric acid in the gross mass of urea and the citric acid solution is 300~150:1.
2. according to the method described in claim 1, it is characterized by: the boric acid and urea quality ratio are 1:11；The boric acid
It is 300:1 with the gross mass of urea and the mass ratio of citric acid；
In step 2, under the conditions of 790~820W microwave power, after citric acid solution microwave reaction 5min, with the boric acid with
The mixed solution of urea mixes, and reacts 30min under the conditions of 790W~820W microwave power, pale powder is obtained, in purple
Under outer excitation, blue-fluorescence is presented.
3. according to the method described in claim 1, it is characterized by: the boric acid and urea quality ratio are 1:5；The boric acid with
The gross mass of urea and the mass ratio of citric acid are 150:1；
In step 2, under the conditions of 790~820W microwave power, after citric acid solution microwave reaction 3min, with the boric acid with
The mixed solution of urea mixes, and reacts 25min under the conditions of 790W~820W microwave power, pale powder is obtained, in purple
Under outer excitation, purple fluorescence is presented.
4. according to the method described in claim 1, it is characterized by: the boric acid and urea quality ratio are 1:3；The boric acid with
The gross mass of urea and the mass ratio of citric acid are 200:1；
It is and described after citric acid solution microwave reaction 10min under the conditions of 690~710W microwave power in the step 2
Boric acid is mixed with the mixed solution of urea, is reacted 50min under the conditions of 690~710W microwave power, is obtained grey powder,
Under burst of ultraviolel, yellow fluorescence is presented.
5. according to the method described in claim 1, it is characterized by: the boric acid and urea quality ratio are 1:9；The boric acid with
The gross mass of urea and the mass ratio of citric acid are 250:1；
In the step 2, under the conditions of 840~870W microwave power, after citric acid solution microwave reaction 8min, with the boron
Acid is mixed with the mixed solution of urea, is reacted 30min under the conditions of 840~870W microwave power, grey powder is obtained, in purple
Under outer excitation, weak blue fluorescence is presented.
6. according to the method described in claim 1, it is characterized by: the boric acid and urea quality ratio are 1:5；The boric acid and
The gross mass of urea and the mass ratio of citric acid are 120:1；
In the step 2, under the conditions of 790~820W microwave power, after citric acid solution microwave reaction 6min, with the boron
Acid is mixed with the mixed solution of urea, is reacted 40min under the conditions of 790~820W microwave power, grey powder is obtained, in purple
Under outer excitation, orange fluorescence is presented.
7. according to the method described in claim 1, it is characterized by: the boric acid and urea quality ratio are 1:6；The boric acid with
The gross mass of urea and the mass ratio of citric acid are 180:1；
In the step 2, under the conditions of 840~870W microwave power, after citric acid solution microwave reaction 3min, with the boron
Acid is mixed with the mixed solution of urea, and microwave reaction 90min under the conditions of 840~870W obtains grey powder, is swashed ultraviolet
It gives, red fluorescence is presented.
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Non-Patent Citations (2)
| Title |
|---|
| Green and simple route toward boron doped carbon dots with significantly enhanced non-linear optical properties;Athanasios B. Bourlinos et al.;《CARBON》;20141121;173-179 |
| Microwave synthesis of homogeneous and highly luminescent BCNO nanoparticles for the light emitting polymer materials;Hideharu Iwasaki等;《Journal of Luminescence》;20150523;第166卷;148-155 |
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