CN108219791A - A kind of fluorescent crystal material and its preparation process flow based on rare earth oxide - Google Patents
A kind of fluorescent crystal material and its preparation process flow based on rare earth oxide Download PDFInfo
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- CN108219791A CN108219791A CN201810079072.8A CN201810079072A CN108219791A CN 108219791 A CN108219791 A CN 108219791A CN 201810079072 A CN201810079072 A CN 201810079072A CN 108219791 A CN108219791 A CN 108219791A
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- rare earth
- earth oxide
- iodide
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7704—Halogenides
Abstract
The invention discloses a kind of fluorescent crystal material based on rare earth oxide, including following composition by weight：12 15 parts of iodide, 10 18 parts of halide, 12 18 parts of sulfide, 8 15 parts of pyrazine, 22 30 parts of rare earth oxide, 11 17 parts of porphyrins, PH adjust 18 24 parts of liquid, 58 parts of ethyl alcohol, 12 18 parts of butane.A kind of preparation process flow of the fluorescent crystal material based on rare earth oxide, it is characterised in that：Include the following steps：S1：Mixed solution makes；S2：The stirring of mixed solution；S3：Mixed solution calcination processing；S4：Crystal pro cessing processing.Present invention saves its process times to correspond to the required energy expended, achievees the effect that environmental protection.
Description
Technical field
The present invention relates to fluorescent crystal manufacture technology field, specially a kind of fluorescent crystal based on rare earth oxide
Material and its preparation process flow.
Background technology
Realize the sub- yield of higher amount of luminescent material, must be requested that optical material is capable of the energy by absorption of maximum possible
Amount is converted into photon rather than is converted into thermal energy by non-radiative relaxation.And reduce the non-radiative relaxation of material, it is necessary to which material has
There are smaller phonon energy, preferable crystallinity, larger light transmission rate etc..Therefore, optical crystal material, due to its compared with
Good crystallization property and larger light transmission rate and smaller phonon energy so that it is benefited from extensively.But in the prior art
The preparation method complex steps of fluorescent crystal, not only waste time, and waste of resource so that entirely process in this way
Process is not environmentally.
Invention content
The purpose of the present invention is to provide a kind of fluorescent crystal materials and its preparation process based on rare earth oxide
Flow, to solve the problems mentioned in the above background technology.
To achieve the above object, the present invention provides following technical solution：A kind of fluorescence based on rare earth oxide is brilliant
Body material, including following composition by weight：12-15 parts of iodide, 10-18 parts of halide, 12-18 parts of sulfide, 8-15 parts of pyrazine,
22-30 parts of rare earth oxide, 11-17 parts of porphyrins, PH adjust 18-24 parts of liquid, 5-8 parts of ethyl alcohol, butane 12-
18 parts.
Preferably, the iodide include hydrogen iodide, potassium iodide and ammonium iodide any of which or a variety of combinations.
Preferably, the halide include fluoride, chloride, bromide, iodide and certain interhalogen compounds its
In any one or a variety of combinations.
Preferably, the sulfide is thioether (R-S-R), thiophenol/mercaptan (Ar/R-SH), thioaldehydes (R-CSH), thio carboxylic
Acid or disulphide (R-S-S-R).
A kind of preparation process flow of the fluorescent crystal material based on rare earth oxide, includes the following steps：
S1：Mixed solution makes, by iodide, halide, sulfide, pyrazine, rare earth oxide and porphyrin
Object is closed to be respectively put into reaction kettle, and to iodide, halide, sulfide, pyrazine, rare earth oxide and porphyrin chemical combination
PH is added in the solution of object and adjusts liquid and ethyl alcohol, then to pressurizeing in reaction kettle, and adds butane, and right to being filled in reaction kettle
Any channel in addition to filling and adding butane channel is sealed；
S2：The stirring of mixed solution, interior agitating device in reaction kettle, is stirred mixed solution, agitating device can
With rotating, the rotating speed of rotating is 2000-3000r/min, is often rotated forward 10 minutes, that is, replaces direction and invert 10 minutes, stirring
Shi Changwei 2-3 hours；
S3：Mixed solution after stirring is placed in inside calcining furnace and carries out high-temperature calcination by mixed solution calcination processing, calcining
Temperature for 1000-1800 DEG C, be fired to crystal precipitation, stop calcining after 2-3 hour, obtain yellow crystals；
S4：Crystal pro cessing processing, the obtained yellow crystals after calcining are cleaned rapidly, and drain by clear water.
Preferably, the pressure that reaction kettle pressurizes in the step S1 is 1000-2000Kpa.
Preferably, when being sealed in the step S1 to any channel in addition to filling and adding butane channel, what is used is close
Encapsulation method is rubber stopper seal.
Compared with prior art, the beneficial effects of the invention are as follows：The present invention is with rare earth oxide as fluorescence crystalline substance
One of raw material prepared by body, iodide, halide, sulfide, pyrazine and porphyrins are inwardly filled and are added as auxiliary
Butane and ethyl alcohol reduce time of the crystal raw material during preparation, save its process time correspondence as activator
The energy of required consuming achievees the effect that environmental protection.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical solution in the embodiment of the present invention is clearly and completely retouched
It states, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, the every other implementation that those of ordinary skill in the art are obtained without making creative work
Example, shall fall within the protection scope of the present invention.
Embodiment one
The present invention provides a kind of technical solution：A kind of fluorescent crystal material based on rare earth oxide, including following
Composition by weight：12 parts of iodide, 10 parts of halide, 12 parts of sulfide, 8 parts of pyrazine, 22 parts of rare earth oxide, porphyrin
Close 11 parts of object, PH adjusts 18 parts of liquid, 5 parts of ethyl alcohol, 12 parts of butane.
Further, the iodide include hydrogen iodide, potassium iodide and ammonium iodide any of which or a variety of
Combination.
Further, the halide is mutually changed including fluoride, chloride, bromide, iodide and certain halogens
Object any of which or a variety of combinations.
Further, the sulfide is thioether (R-S-R), thiophenol/mercaptan (Ar/R-SH), thioaldehydes (R-CSH), sulphur
For carboxylic acid or disulphide (R-S-S-R).
A kind of preparation process flow of the fluorescent crystal material based on rare earth oxide, includes the following steps：
S1：Mixed solution makes, by iodide, halide, sulfide, pyrazine, rare earth oxide and porphyrin
Object is closed to be respectively put into reaction kettle, and to iodide, halide, sulfide, pyrazine, rare earth oxide and porphyrin chemical combination
PH is added in the solution of object and adjusts liquid and ethyl alcohol, then to pressurizeing in reaction kettle, and adds butane, and right to being filled in reaction kettle
Any channel in addition to filling and adding butane channel is sealed；
S2：The stirring of mixed solution, interior agitating device in reaction kettle, is stirred mixed solution, agitating device can
With rotating, the rotating speed of rotating is 2000r/min, is often rotated forward 10 minutes, that is, replaces direction and invert 10 minutes, and when stirring is a length of
2 hours；
S3：Mixed solution after stirring is placed in inside calcining furnace and carries out high-temperature calcination by mixed solution calcination processing, calcining
Temperature for 1000 DEG C, be fired to crystal precipitation, stop calcining after 2 hours, obtain yellow crystals；
S4：Crystal pro cessing processing, the obtained yellow crystals after calcining are cleaned rapidly, and drain by clear water.
Further, the pressure that reaction kettle pressurizes in the step S1 is 1000Kpa.
Further, it when being sealed in the step S1 to any channel in addition to filling and adding butane channel, uses
Encapsulating method be rubber stopper seal.
Further, one of raw material that the present invention is prepared with silver chlorate as fluorescent crystal, iodide, metal vulcanization
Object, pyrazine, porphyrins, rare earth oxide are as auxiliary so that this crystal raw material cost during preparation
It is cheap, environment protecting is good, and shortens a series of technological process, save a large amount of time.
Embodiment two
A kind of fluorescent crystal material based on rare earth oxide, including following composition by weight：15 parts of iodide, halogen
18 parts of compound, 18 parts of sulfide, 15 parts of pyrazine, 30 parts of rare earth oxide, 17 parts of porphyrins, PH adjust liquid 24
Part, 8 parts of ethyl alcohol, 18 parts of butane.
Further, the iodide include hydrogen iodide, potassium iodide and ammonium iodide any of which or a variety of
Combination.
Further, the halide is mutually changed including fluoride, chloride, bromide, iodide and certain halogens
Object any of which or a variety of combinations.
Further, the sulfide is thioether (R-S-R), thiophenol/mercaptan (Ar/R-SH), thioaldehydes (R-CSH), sulphur
For carboxylic acid or disulphide (R-S-S-R).
A kind of preparation process flow of the fluorescent crystal material based on rare earth oxide, includes the following steps：
S1：Mixed solution makes, by iodide, halide, sulfide, pyrazine, rare earth oxide and porphyrin
Object is closed to be respectively put into reaction kettle, and to iodide, halide, sulfide, pyrazine, rare earth oxide and porphyrin chemical combination
PH is added in the solution of object and adjusts liquid and ethyl alcohol, then to pressurizeing in reaction kettle, and adds butane, and right to being filled in reaction kettle
Any channel in addition to filling and adding butane channel is sealed；
S2：The stirring of mixed solution, interior agitating device in reaction kettle, is stirred mixed solution, agitating device can
With rotating, the rotating speed of rotating is 3000r/min, is often rotated forward 10 minutes, that is, replaces direction and invert 10 minutes, and when stirring is a length of
3 hours；
S3：Mixed solution after stirring is placed in inside calcining furnace and carries out high-temperature calcination by mixed solution calcination processing, calcining
Temperature for 1800 DEG C, be fired to crystal precipitation, stop calcining after 3 hours, obtain yellow crystals；
S4：Crystal pro cessing processing, the obtained yellow crystals after calcining are cleaned rapidly, and drain by clear water.
Further, the pressure that reaction kettle pressurizes in the step S1 is 2000Kpa.
Further, it when being sealed in the step S1 to any channel in addition to filling and adding butane channel, uses
Encapsulating method be rubber stopper seal.
Further, one of raw material that the present invention is prepared with silver chlorate as fluorescent crystal, iodide, metal vulcanization
Object, pyrazine, porphyrins, rare earth oxide are as auxiliary so that this crystal raw material cost during preparation
It is cheap, environment protecting is good, and shortens a series of technological process, save a large amount of time.
Embodiment three
A kind of fluorescent crystal material based on rare earth oxide, including following composition by weight：15 parts of iodide, halogen
11 parts of compound, 16 parts of sulfide, 12 parts of pyrazine, 25 parts of rare earth oxide, 15 parts of porphyrins, PH adjust liquid 20
Part, 7 parts of ethyl alcohol, 16 parts of butane.
Further, the iodide include hydrogen iodide, potassium iodide and ammonium iodide any of which or a variety of
Combination.
Further, the halide is mutually changed including fluoride, chloride, bromide, iodide and certain halogens
Object any of which or a variety of combinations.
Further, the sulfide is thioether (R-S-R), thiophenol/mercaptan (Ar/R-SH), thioaldehydes (R-CSH), sulphur
For carboxylic acid or disulphide (R-S-S-R).
A kind of preparation process flow of the fluorescent crystal material based on rare earth oxide, includes the following steps：
S1：Mixed solution makes, by iodide, halide, sulfide, pyrazine, rare earth oxide and porphyrin
Object is closed to be respectively put into reaction kettle, and to iodide, halide, sulfide, pyrazine, rare earth oxide and porphyrin chemical combination
PH is added in the solution of object and adjusts liquid and ethyl alcohol, then to pressurizeing in reaction kettle, and adds butane, and right to being filled in reaction kettle
Any channel in addition to filling and adding butane channel is sealed；
S2：The stirring of mixed solution, interior agitating device in reaction kettle, is stirred mixed solution, agitating device can
With rotating, the rotating speed of rotating is 2500r/min, is often rotated forward 10 minutes, that is, replaces direction and invert 10 minutes, and when stirring is a length of
2.5 hours；
S3：Mixed solution after stirring is placed in inside calcining furnace and carries out high-temperature calcination by mixed solution calcination processing, calcining
Temperature for 1500 DEG C, be fired to crystal precipitation, stop calcining after 2.5 hours, obtain yellow crystals；
S4：Crystal pro cessing processing, the obtained yellow crystals after calcining are cleaned rapidly, and drain by clear water.
Further, the pressure that reaction kettle pressurizes in the step S1 is 1500Kpa.
Further, it when being sealed in the step S1 to any channel in addition to filling and adding butane channel, uses
Encapsulating method be rubber stopper seal.
Further, one of raw material that the present invention is prepared with silver chlorate as fluorescent crystal, iodide, metal vulcanization
Object, pyrazine, porphyrins, rare earth oxide are as auxiliary so that this crystal raw material cost during preparation
It is cheap, environment protecting is good, and shortens a series of technological process, save a large amount of time.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (7)
1. a kind of fluorescent crystal material based on rare earth oxide, it is characterised in that：Including following composition by weight：Iodide
12-15 parts, 10-18 parts of halide, 12-18 parts of sulfide, 8-15 parts of pyrazine, 22-30 parts of rare earth oxide, porphyrin
Close 11-17 parts of object, PH adjusts 18-24 parts of liquid, 5-8 parts of ethyl alcohol, 12-18 parts of butane.
2. a kind of fluorescent crystal material based on rare earth oxide, it is characterised in that：The iodide include hydrogen iodide, iodine
Change potassium and ammonium iodide any of which or a variety of combinations.
3. a kind of fluorescent crystal material based on rare earth oxide, it is characterised in that：The halide includes fluoride, chlorine
Compound, bromide, iodide and certain interhalogen compounds any of which or a variety of combinations.
4. a kind of fluorescent crystal material based on rare earth oxide, it is characterised in that：The sulfide is thioether (R-S-
R), thiophenol/mercaptan (Ar/R-SH), thioaldehydes (R-CSH), thiocarboxylic acid or disulphide (R-S-S-R).
5. a kind of preparation process flow of the fluorescent crystal material based on rare earth oxide, it is characterised in that：Including following
Step：
S1：Mixed solution makes, by iodide, halide, sulfide, pyrazine, rare earth oxide and porphyrins
It is respectively put into reaction kettle, and to iodide, halide, sulfide, pyrazine, rare earth oxide and porphyrins
PH is added in solution and adjusts liquid and ethyl alcohol, then to pressurizeing in reaction kettle, and adds butane, and fill to removing to being filled in reaction kettle
Any channel except butane channel is added to be sealed；
S2：The stirring of mixed solution, interior agitating device in reaction kettle, is stirred mixed solution, agitating device can be just
Reversion, the rotating speed of rotating is 2000-3000r/min, is often rotated forward 10 minutes, that is, replaces direction and invert 10 minutes, stir duration
For 2-3 hour；
S3：Mixed solution after stirring is placed in inside calcining furnace and carries out high-temperature calcination by mixed solution calcination processing, the temperature of calcining
It is 1000-1800 DEG C to spend, and is fired to crystal precipitation, stops calcining after 2-3 hours, obtain yellow crystals；
S4：Crystal pro cessing processing, the obtained yellow crystals after calcining are cleaned rapidly, and drain by clear water.
6. a kind of fluorescent crystal material and its preparation process stream based on rare earth oxide according to claim 5
Journey, it is characterised in that：The pressure that reaction kettle pressurizes in the step S1 is 1000-2000Kpa.
7. a kind of fluorescent crystal material and its preparation process stream based on rare earth oxide according to claim 1
Journey, it is characterised in that：In the step S1 to except fill plus butane channel in addition to any channel be sealed when, the sealing that uses
Method is rubber stopper seal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810079072.8A CN108219791A (en) | 2018-01-26 | 2018-01-26 | A kind of fluorescent crystal material and its preparation process flow based on rare earth oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810079072.8A CN108219791A (en) | 2018-01-26 | 2018-01-26 | A kind of fluorescent crystal material and its preparation process flow based on rare earth oxide |
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| CN108219791A true CN108219791A (en) | 2018-06-29 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102453229A (en) * | 2010-10-19 | 2012-05-16 | 海洋王照明科技股份有限公司 | Metalloporphyrin-thienopyrazine organic semiconductor material, preparation method thereof and application thereof |
| CN102533247A (en) * | 2010-12-12 | 2012-07-04 | 陈文通 | Dysprosium-contained fluorescent crystal and preparation method thereof |
| CN103588817A (en) * | 2013-11-14 | 2014-02-19 | 沈阳化工大学 | Method for preparing complex crystal with biological activity |
| CN105418686A (en) * | 2015-12-24 | 2016-03-23 | 北京北达聚邦科技有限公司 | Pyrazine phosphorescent iridium complex, preparation method and application thereof |
-
2018
- 2018-01-26 CN CN201810079072.8A patent/CN108219791A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102453229A (en) * | 2010-10-19 | 2012-05-16 | 海洋王照明科技股份有限公司 | Metalloporphyrin-thienopyrazine organic semiconductor material, preparation method thereof and application thereof |
| CN102533247A (en) * | 2010-12-12 | 2012-07-04 | 陈文通 | Dysprosium-contained fluorescent crystal and preparation method thereof |
| CN103588817A (en) * | 2013-11-14 | 2014-02-19 | 沈阳化工大学 | Method for preparing complex crystal with biological activity |
| CN105418686A (en) * | 2015-12-24 | 2016-03-23 | 北京北达聚邦科技有限公司 | Pyrazine phosphorescent iridium complex, preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 黄燕等: "共沉淀-熔盐焙烧法制备Y2O3:Eu及其发光性能的研究", 《中国稀土学报》 * |
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Application publication date: 20180629 |
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