CN106590639A - Inorganic photoluminescence material with adjustable fluorescence spectrum and preparation method of inorganic photoluminescence material - Google Patents
Inorganic photoluminescence material with adjustable fluorescence spectrum and preparation method of inorganic photoluminescence material Download PDFInfo
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Abstract
The invention provides an inorganic photoluminescence material with an adjustable fluorescence spectrum and a preparation method of the inorganic photoluminescence material. The inorganic photoluminescence material is prepared from citric acid, boric acid and urea as raw materials. The inorganic photoluminescence material consists of the following elements: 1-15wt% of a carbon element, 16-43wt% of a boron element, 8-28wt% of a nitrogen element and 21-45wt% of an oxygen element, wherein the carbon element is a small-layer graphene sheet which is prepared by decomposing and reducing the citric acid. The preparation method comprises the following steps: in the presence of an air atmosphere, enabling a citric acid solution to react for 3-10 minutes under a microwave power condition of 600-900W; and mixing a reaction system with a mixed solution of the boric acid and the urea, enabling the mixture to react for 10-90 minutes under a microwave power condition of 400-900W, cooling to the room temperature, and grinding a collected solid into powder, thereby obtaining the inorganic photoluminescence material. As the inorganic photoluminescence material is prepared by using two steps of microwave methods, the operation is simple and easy to achieve, and moreover, multi-color photoluminescence materials can be prepared by controlling raw material ratios, microwave power and reaction times of different steps.
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 technology
Luminescent substance has become important materials indispensable in people's productive life, and the substrate of current luminescent material is main
There are following a few class compounds:Sulfur system, silicate, aluminate, phosphate, borate etc..For luminescent material,
In addition to host material, activator or coactivator are also extremely important, and usual activator selects rare earth element, but rare earth unit
Plain expensive, synthesis temperature high (900 DEG C), need protective atmosphere (nitrogen or argon) or reducing atmosphere (hydrogen
Gas) sintering and its oxide and chloride have larger toxicity (Journal of The Electrochemical Society, 2009,
156(5):81~84.).Some other luminescent material then needs the higher preparation condition (J.Electrochem. such as High Temperature High Pressure
Soc.,2010,157(10):329~333.).Therefore, the preparation of economic and environment-friendly luminescent material and application necessitates.
BCNO is a kind of non-rear-earth-doped luminous fluorescent material, and it has low toxic and environment-friendly, synthesis low cost, synthesis technique
Simply, many advantages such as luminous efficiency height, emission wavelength scalable, thus become the outstanding person of luminescent material of new generation
(Adv.Mater.,2008,20(17):3235~3238.).
The Chinese invention patent application of Application No. 201310097837.8 discloses a kind of wide excitation and emission spectra
The preparation method of BCNO fluorescent powder, it prepares BCNO fluorescent powder by raw material of tripolycyanamide, boric acid and second triol,
But its response time is longer, resulting materials luminous efficiency is relatively low;The Chinese invention of Application No. 201410724748.6 is special
The Chinese invention patent SEPARATE APPLICATION of profit and Application No. 201410719862.X discloses a kind of orange-red light and redness
Light launches the preparation method of adjustable BCNO fluorescent powder, and both preparation method reactions steps are more, and preparation process is relative
It is complicated.
The content of the invention
The technical problem to be solved is the defect for overcoming prior art to exist, there is provided a kind of raw material is easily obtained
Take, inorganic fluorescent substances of preparation method is simple and preparation method thereof.
In order to solve above-mentioned technical problem, the invention provides a kind of inorganic fluorescent substances.
Inorganic fluorescent substances provided by the present invention, are prepared by citric acid, boric acid and carbamide for raw material, its
It is elementary composition to be:1~15wt% of carbon, 16~43wt% of boron element, 8~28wt% of nitrogen, oxygen element 21~
45wt%, wherein, the carbon is the few layer graphene piece for being decomposed by citric acid and being reduced.
Above-mentioned inorganic fluorescent substances are prepared by the method comprising the following steps:
1) mixed solution of citric acid solution, boric acid and carbamide is prepared respectively;
2) in air atmosphere, by the citric acid solution 600W~900W's (preferred 700W~850W)
3~10min is reacted under the conditions of microwave power, the reaction system of graphene-containing is obtained;By the reactant of the graphene-containing
System mixes with the boric acid with the mixed solution of carbamide, in the microwave of 400W~900W (preferred 700W~850W)
10~90min is reacted under power condition, room temperature is cooled to, by the solid abrasive collected into powder, obtains inorganic photic
Luminescent material.
Said method step 1) in, the boric acid is 1 with the mass ratio of carbamide with the mixed solution mesoboric acid of carbamide:3~
20;The mass ratio of the citric acid in the gross mass of the boric acid and carbamide and the citric acid solution is 300~150:1.
The citric acid solution can be prepared according to the method for comprising the steps:First by citric acid be dissolved in 40ml from
In sub- water, then Jing 5~20min supersound process, uniform and stable solution is obtained, wherein, the power of the ultrasound is 30~
70W, frequency are 30~70KHz.
The boric acid can be prepared with the mixed solution of carbamide according to the method for comprising the steps:By boric acid, carbamide
In adding deionized water 50ml, then Jing 10~60min supersound process, obtain homodisperse boric acid mixed with carbamide
Solution is closed, wherein, the ultrasonic power is 30~70W, frequency is 30~70KHz.
In the present invention, proportioning raw materials have a major impact with reaction condition to the luminescent spectrum of material, feed change proportioning,
Microwave power, response time are obtained the embedded photoluminescent material of different colours spectrum.
Further, the boric acid and urea quality ratio are 1:11;The boric acid and the gross mass of carbamide and the matter of citric acid
Amount is than being 300:1, the step 2) in, under the conditions of " 790~820W " (preferred 800W) microwave power, lemon
After lemon acid solution microwave reaction 5min, mix with the boric acid with the mixed solution of carbamide, at " 790W~820W "
30min is reacted under the conditions of (preferred 800W) microwave power, pale powder is obtained, it swashs at ultraviolet (365nm)
Give, blue-fluorescence is presented.
Further, the boric acid and urea quality ratio are 1:5;The boric acid and the gross mass of carbamide and the quality of citric acid
Than for 150:1, the step 2) in, under the conditions of " 790~820W " (preferred 800W) microwave power, Fructus Citri Limoniae
After acid solution microwave reaction 3min, mix with the boric acid with the mixed solution of carbamide, it is (excellent at " 790W~820W "
Select 800W) react 25min under the conditions of microwave power, obtain pale powder, its in the case where ultraviolet (365nm) is excited,
Purple fluorescence is presented.
Further, the boric acid and urea quality ratio are 1:3;The boric acid and the gross mass of carbamide and the quality of citric acid
Than for 200:1, the step 2) in, under the conditions of " 690~710W " (preferred 700W) microwave power, Fructus Citri Limoniae
After acid solution microwave reaction 10min, mix with the boric acid with the mixed solution of carbamide, it is (excellent at " 690~710W "
Select 700W) react 50min under the conditions of microwave power, obtain Lycoperdon polymorphum Vitt powder, its in the case where ultraviolet (365nm) is excited,
Yellow fluorescence is presented.
Further, the boric acid and urea quality ratio are 1:9;The boric acid and the gross mass of carbamide and the quality of citric acid
Than for 250:1, the step 2) in, under the conditions of " 840~870W " (preferred 850W) microwave power, Fructus Citri Limoniae
After acid solution microwave reaction 8min, mix with the boric acid with the mixed solution of carbamide, at " 840~870W " (preferably
30min 850W) is reacted under the conditions of microwave power, Lycoperdon polymorphum Vitt powder is obtained, it is in the case where ultraviolet (365nm) is excited
Existing weak blue fluorescence.
Further, the boric acid and urea quality ratio are 1:5;The gross mass of the boric acid and carbamide and the quality of citric acid
Than for 120:1, the step 2) in, under the conditions of " 790~820W " (preferred 800W) microwave power, Fructus Citri Limoniae
After acid solution microwave reaction 6min, mix with the boric acid with the mixed solution of carbamide, at " 790~820W " (preferably
40min 800W) is reacted under the conditions of microwave power, Lycoperdon polymorphum Vitt powder is obtained, it is in the case where ultraviolet (365nm) is excited
Existing orange fluorescence.
Further, the boric acid and urea quality ratio are 1:6;The boric acid and the gross mass of carbamide and the quality of citric acid
Than for 180:1, the step 2) in, under the conditions of " 840~870W " (preferred 850W) microwave power, Fructus Citri Limoniae
After acid solution microwave reaction 3min, mix with the boric acid with the mixed solution of carbamide, at " 840~870W " (preferably
Microwave reaction 90min under the conditions of 850W), obtains Lycoperdon polymorphum Vitt powder, and it is presented red in the case where ultraviolet (365nm) is excited
Color fluorescence.
The present invention prepares inorganic fluorescent substances using two step microwave methods, simple to operate to be easily achieved, and can lead to
Cross control raw material ratio and microwave power and respectively walk the response time, produce polychromatic photoinduced luminous material.
Compared with prior art, the present invention has advantages below:(1) raw material is nontoxic, it is easy to obtain;(2)
Manufacture method is simple, and environment will not be worked the mischief;(3) luminous intensity is high, good brightness;(4) by control technique
Condition, can produce polychromatic photoinduced luminous material.In the case where ultraviolet (365nm) is excited, fluorescence color presentation crocus,
Yellow, blueness, redness, light blue etc..
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the embedded photoluminescent material that the embodiment of the present invention 1 is prepared.
Fig. 2 is the scanning electron microscope (SEM) photograph of the embedded photoluminescent material that the embodiment of the present invention 2 is prepared.
Specific embodiment
Below by specific embodiment, the present invention will be described, but the invention is not limited in this.
Experimental technique used in following embodiments if no special instructions, is conventional method;Institute in following embodiments
Reagent, material etc., if no special instructions, commercially obtain.
Embodiment 1
The inorganic fluorescent substances of the present embodiment are generated by citric acid, boric acid and carbamide Jing two-step methods microwave reaction,
Products therefrom is in pale powder.It is elementary composition to be:Carbon 6wt%, boron element 34wt%, nitrogen 19wt%,
Oxygen element 41wt%, wherein carbon are few layer graphene pieces that citric acid decomposes and reduces (see Fig. 1).
The preparation method of the inorganic fluorescent substances of the present embodiment, comprises the following steps:
(1) raw material prepares:Citric acid 0.02g (few layer graphenes that citric acid decomposes and reduces are weighed in proportion
Piece, is shown in document Carbon, 2012,50 (12):4738~4743.), boric acid 0.5g and carbamide 5.5g, i.e. boric acid and carbamide
Mass ratio is 1:11;Boric acid is 300 with the mass ratio of citric acid with carbamide gross mass:1
(2) citric acid solution is prepared:Ready citric acid is dissolved in 40ml ionized waters by step (1) and is configured to
Solution, Jing 15min ultrasounds (ultrasonic power is 60W, frequency is 50KHz), obtains uniform and stable solution;
(3) with preparing boric acid, carbamide mixed solution:Boric acid, carbamide, plus deionized water 50ml are weighed by predetermined mass ratio
Mixed solution is configured to, Jing 30min ultrasounds (ultrasonic power is 60W, frequency is 50KHz) obtain uniform
Scattered boric acid, carbamide mixed solution;
(4) microwave heating reaction:Step (2) gained citric acid solution is positioned over into the microwave oven full of air atmosphere
In, 5min is reacted under 800W power conditions, citric acid decomposes and is reduced to Graphene.By gained material and step
(3) boric acid, the urea liquid mixing prepared, under 800W power conditions 30min is reacted, and is cooled to room temperature,
By the solid abrasive collected into powder, inorganic fluorescent substances are obtained.
Using the present embodiment inorganic fluorescent substances, powder is in canescence.It is elementary composition to be:Carbon 6wt%,
Boron element 34wt%, nitrogen 19wt%, wherein oxygen element 41wt%, carbon are that citric acid decomposes and reduces and forms
Few layer graphene piece.Gained powder excites lower presentation blue light at ultraviolet (365nm).Its luminous efficiency is higher
(53%), luminous intensity is good.
Embodiment 2
The inorganic fluorescent substances of the present embodiment are given birth to by the reaction of citric acid, boric acid and the step microwave heating methods of carbamide Jing two
Into products therefrom is in pale powder.It is elementary composition to be:Carbon 5wt%, boron element 40wt%, nitrogen 21wt%,
Oxygen element 34wt%, wherein carbon are few layer graphene pieces that citric acid decomposes and reduces (see Fig. 2).
The inorganic fluorescent substances of the present embodiment compared with the preparation method of the inorganic fluorescent substances of embodiment 1, institute
It is 1 that boric acid is stated with urea quality ratio:5, boric acid is 150 with the mass ratio of citric acid with the gross mass of carbamide:1.The step
Suddenly in (4), 3min is reacted under 800W power conditions, citric acid decomposes and be reduced to Graphene.By gains
Matter mixes with boric acid, urea liquid, and under 800W power conditions 25min is reacted, and is cooled to room temperature, will collect
Solid abrasive into powder, obtain inorganic fluorescent substances.Remaining method is same as Example 1.
Using the present embodiment inorganic fluorescent substances, in pale powder.It is elementary composition to be:Carbon 5wt%,
Boron element 40wt%, nitrogen 21wt%, wherein oxygen element 34wt%, carbon are that citric acid decomposes and reduces and forms
Few layer graphene piece.Lower presentation purple fluorescence is excited in ultraviolet (365nm).Its luminous efficiency higher (45%),
Luminous intensity is bright.
Embodiment 3
The inorganic fluorescent substances of the present embodiment are given birth to by the reaction of citric acid, boric acid and the step microwave heating methods of carbamide Jing two
Into products therefrom gray powder.It is elementary composition to be:Carbon 12wt%, boron element 27wt%, nitrogen 26wt%,
Oxygen element 35wt%, wherein carbon are few layer graphene pieces that citric acid decomposes and reduces.
The inorganic fluorescent substances of the present embodiment compared with the preparation method of the inorganic fluorescent substances of embodiment 1, institute
It is 1 that boric acid is stated with urea quality ratio:3, the boric acid is 200 with the mass ratio of citric acid with the gross mass of carbamide:1.Institute
In stating step (4), 10min is reacted under 700W power conditions, citric acid decomposes and be reduced to Graphene.By institute
Obtain material to mix with boric acid, urea liquid, 50min is reacted under identical power conditions, be cooled to room temperature, will collect
The solid abrasive for arriving obtains inorganic fluorescent substances into powder.Remaining method is same as Example 1.
Using the present embodiment inorganic fluorescent substances, gray powder.It is elementary composition to be:Carbon 12wt%, boron
Element 27wt%, nitrogen 26wt%, wherein oxygen element 35wt%, carbon are that citric acid decomposes and reduces and forms
Few layer graphene piece.Lower presentation yellow fluorescence is excited in ultraviolet (365nm).Its luminous efficiency higher (58%),
Luminous intensity is bright.
Embodiment 4
The inorganic fluorescent substances of the present embodiment are given birth to by the reaction of citric acid, boric acid and the step microwave heating methods of carbamide Jing two
Into products therefrom is in pale powder.It is elementary composition to be:Carbon 5wt%, boron element 32wt%, nitrogen 18wt%,
Oxygen element 45wt%, wherein carbon are few layer graphene pieces that citric acid decomposes and reduces.
The inorganic fluorescent substances of the present embodiment compared with the preparation method of the inorganic fluorescent substances of embodiment 1, institute
It is 1 that boric acid is stated with urea quality ratio:9, boric acid is 250 with the mass ratio of citric acid with the gross mass of carbamide:1.The step
Suddenly in (4), 8min is reacted under 850W power conditions, citric acid decomposes and be reduced to Graphene.By gains
Matter mixes with boric acid, urea liquid, and 30min is reacted under identical power conditions, is cooled to room temperature, by what is collected
Solid abrasive obtains inorganic fluorescent substances into powder.Remaining method is same as Example 1.
Using the present embodiment inorganic fluorescent substances, gray powder.It is elementary composition to be:Carbon 5wt%, boron
Element 32wt%, nitrogen 18wt%, wherein oxygen element 45wt%, carbon are that citric acid decomposes and reduces and forms
Few layer graphene piece.Lower presentation weak blue fluorescence is excited in ultraviolet (365nm).Its luminous efficiency higher (62%),
Luminous intensity is bright.
Embodiment 5
The inorganic fluorescent substances of the present embodiment are given birth to by the reaction of citric acid, boric acid and the step microwave heating methods of carbamide Jing two
Into products therefrom is in pale powder.It is elementary composition to be:Carbon 10wt%, boron element 27wt%, nitrogen 20wt%,
Oxygen element 43wt%, wherein carbon are few layer graphene pieces that citric acid decomposes and reduces.
The inorganic fluorescent substances of the present embodiment compared with the preparation method of the inorganic fluorescent substances of embodiment 1, institute
It is 1 that boric acid is stated with urea quality ratio:5, boric acid and the gross mass of carbamide and the mass ratio of citric acid are 120:1.The step
Suddenly in (4), 6min is reacted under 800W power conditions, citric acid decomposes and be reduced to Graphene.By gains
Matter mixes with boric acid, urea liquid, and 40min is reacted under identical power conditions, is cooled to room temperature, by what is collected
Solid abrasive obtains inorganic fluorescent substances into powder.Remaining method is same as Example 1.
Using the present embodiment inorganic fluorescent substances, in pale powder.It is elementary composition to be:Carbon 10wt%,
Boron element 27wt%, nitrogen 20wt%, wherein oxygen element 43wt%, carbon are that citric acid decomposes and reduces and forms
Few layer graphene piece.Lower presentation orange fluorescence is excited in ultraviolet (365nm).Its luminous efficiency higher (48%),
Luminous intensity is bright.
Embodiment 6
The inorganic fluorescent substances of the present embodiment are given birth to by the reaction of citric acid, boric acid and the step microwave heating methods of carbamide Jing two
Into products therefrom is in pale powder.It is elementary composition to be:Carbon 13wt%, boron element 29wt%, nitrogen 19wt%,
Oxygen element 39wt%, wherein carbon are few layer graphene pieces that citric acid decomposes and reduces.
The inorganic fluorescent substances of the present embodiment compared with the preparation method of the inorganic fluorescent substances of embodiment 1, institute
It is 1 that boric acid is stated with urea quality ratio:6, boric acid is 180 with the mass ratio of citric acid with the gross mass of carbamide:1.The step
Suddenly in (4), 3min is reacted under 850W power conditions, citric acid decomposes and be reduced to Graphene.By gains
Matter mixes with boric acid, urea liquid, and 90min is reacted under identical power conditions, is cooled to room temperature, by what is collected
Solid abrasive obtains inorganic fluorescent substances into powder.Remaining method is same as Example 1.
Using the present embodiment inorganic fluorescent substances, in pale powder.It is elementary composition to be:Carbon 13wt%,
Boron element 29wt%, nitrogen 19wt%, wherein oxygen element 39wt%, carbon are that citric acid decomposes and reduces and forms
Few layer graphene piece.Lower presentation red fluorescence is excited in ultraviolet (365nm).Its luminous efficiency higher (43%),
Luminous intensity is bright.
Claims (10)
1. a kind of inorganic fluorescent substances, are prepared by citric acid, boric acid and carbamide for raw material, its element
Composition, in terms of weight/mass percentage composition, be:1~15wt% of carbon, 16~43wt% of boron element, nitrogen 8~
28wt%, 21~45wt% of oxygen element, wherein, the carbon is the few layer for being decomposed by citric acid and being reduced
Graphene film.
2. the preparation method of the inorganic fluorescent substances described in claim 1, comprises the steps:
1) mixed solution of citric acid solution, boric acid and carbamide is prepared respectively;
2) in air atmosphere, the citric acid solution is reacted under the conditions of the microwave power of 600W~900W
3~10min, obtains the reaction system of graphene-containing;By the reaction system of the graphene-containing and the boric acid and urine
The mixed solution mixing of element, reacts 10~90min under the conditions of the microwave power of 400W~900W, is cooled to room
Temperature, by the solid abrasive collected into powder, that is, obtains inorganic fluorescent substances.
3. method according to claim 2, it is characterised in that:Step 1) in, the boric acid and carbamide
Mixed solution mesoboric acid is 1 with the mass ratio of carbamide:3~20;Gross mass and the Fructus Citri Limoniae of the boric acid with carbamide
The mass ratio of the citric acid in acid solution is 300~150:1.
4. according to the method in claim 2 or 3, it is characterised in that:The boric acid is with urea quality ratio
1:11;The boric acid is 300 with the mass ratio of citric acid with the gross mass of carbamide:1;
Step 2) in, under the conditions of 790~820W microwave powers, after citric acid solution microwave reaction 5min,
Mix with the boric acid with the mixed solution of carbamide, under the conditions of 790W~820W microwave powers 30min reacted,
Pale powder is obtained, it is presented blue-fluorescence under burst of ultraviolel.
5. according to the method in claim 2 or 3, it is characterised in that:The boric acid is with urea quality ratio
1:5;The boric acid is 150 with the mass ratio of citric acid with the gross mass of carbamide:1;
Step 2) in, under the conditions of 790~820W microwave powers, after citric acid solution microwave reaction 3min,
Mix with the boric acid with the mixed solution of carbamide, under the conditions of 790W~820W microwave powers 25min reacted,
Pale powder is obtained, it is presented purple fluorescence under burst of ultraviolel.
6. according to the method in claim 2 or 3, it is characterised in that:The boric acid is with urea quality ratio
1:3;The boric acid is 200 with the mass ratio of citric acid with the gross mass of carbamide:1;
The step 2) in, under the conditions of 690~710W microwave powers, citric acid solution microwave reaction 10min
Afterwards, mix with the boric acid with the mixed solution of carbamide, under the conditions of 690~710W microwave powers 50min reacted,
Lycoperdon polymorphum Vitt powder is obtained, it is presented yellow fluorescence under burst of ultraviolel.
7. according to the method in claim 2 or 3, it is characterised in that:The boric acid is with urea quality ratio
1:9;The boric acid is 250 with the mass ratio of citric acid with the gross mass of carbamide:1;
The step 2) in, under the conditions of 840~870W microwave powers, citric acid solution microwave reaction 8min
Afterwards, mix with the boric acid with the mixed solution of carbamide, under the conditions of 840~870W microwave powers 30min reacted,
Lycoperdon polymorphum Vitt powder is obtained, it is presented weak blue fluorescence under burst of ultraviolel.
8. according to the method in claim 2 or 3, it is characterised in that:The boric acid is with urea quality ratio
1:5;The gross mass of the boric acid and carbamide is 120 with the mass ratio of citric acid:1;
The step 2) in, under the conditions of 790~820W microwave powers, citric acid solution microwave reaction 6min
Afterwards, mix with the boric acid with the mixed solution of carbamide, under the conditions of 790~820W microwave powers 40min reacted,
Lycoperdon polymorphum Vitt powder is obtained, it is presented orange fluorescence under burst of ultraviolel.
9. according to the method in claim 2 or 3, it is characterised in that:The boric acid is with urea quality ratio
1:6;The boric acid is 180 with the mass ratio of citric acid with the gross mass of carbamide:1;
The step 2) in, under the conditions of 840~870W microwave powers, citric acid solution microwave reaction 3min
Afterwards, mix with the boric acid with the mixed solution of carbamide, the microwave reaction 90min under the conditions of 840~870W is obtained
To Lycoperdon polymorphum Vitt powder, it is presented red fluorescence under burst of ultraviolel.
10. the inorganic fluorescent substances that the method any one of claim 2-9 is prepared.
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CN114890637A (en) * | 2022-05-24 | 2022-08-12 | 龙岩学院 | Method for treating sludge and method for preparing environment-friendly bricks from obtained solid waste sludge |
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CN111978959A (en) * | 2020-08-22 | 2020-11-24 | 东北农业大学 | Preparation method and application of fluorescent carbon dots capable of rapidly detecting survival state of yeast cells |
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CN114890637A (en) * | 2022-05-24 | 2022-08-12 | 龙岩学院 | Method for treating sludge and method for preparing environment-friendly bricks from obtained solid waste sludge |
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