CN106566549B - A kind of semiconductor green fluorescent powder and preparation method thereof - Google Patents
A kind of semiconductor green fluorescent powder and preparation method thereof Download PDFInfo
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- CN106566549B CN106566549B CN201610982001.XA CN201610982001A CN106566549B CN 106566549 B CN106566549 B CN 106566549B CN 201610982001 A CN201610982001 A CN 201610982001A CN 106566549 B CN106566549 B CN 106566549B
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- fluorescent powder
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- 239000000843 powder Substances 0.000 title claims abstract description 59
- 239000004065 semiconductor Substances 0.000 title claims abstract description 22
- 108010043121 Green Fluorescent Proteins Proteins 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 32
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 23
- 239000011787 zinc oxide Substances 0.000 claims description 23
- 150000001875 compounds Chemical class 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 4
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 2
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 2
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 230000005284 excitation Effects 0.000 abstract description 22
- 239000000463 material Substances 0.000 abstract description 11
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000001228 spectrum Methods 0.000 description 10
- 238000000695 excitation spectrum Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 229910002651 NO3 Inorganic materials 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 229910009253 Y(NO3)3 Inorganic materials 0.000 description 4
- BXJPTTGFESFXJU-UHFFFAOYSA-N yttrium(3+);trinitrate Chemical compound [Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O BXJPTTGFESFXJU-UHFFFAOYSA-N 0.000 description 4
- 239000012190 activator Substances 0.000 description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241001062009 Indigofera Species 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 230000003081 coactivator Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Classifications
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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
- C09K11/7712—Borates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/12—Borates
- C01B35/128—Borates containing plural metal or metal and ammonium
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Luminescent Compositions (AREA)
Abstract
The present invention relates to luminescent material technical fields.A kind of semiconductor green fluorescent powder, the fluorescent powder have following chemical representation: (Bi1‑xYx)2ZnO(BO3)2, the value range of x is 0 x≤1 <.The beneficial effects of the invention are as follows fluorescent powders to be free of the rare earth element of price costly, and preparation condition is mild, high temperature and reducing atmosphere are not needed, being able to achieve the green emitting phosphor that green emission obtains has wide excitation bandwidth, cover ultraviolet, purple light and blue region, excitation peak is located near 410nm, fine with the transmitting overlap of peaks of ultraviolet chip, can effectively be excited.
Description
Technical field
The present invention relates to luminescent material technical fields, more particularly, to semiconductor green fluorescent powder and preparation method thereof.
Background technique
White light LEDs are a kind of solid-state semiconductor device for converting electrical energy into white light, also known as semiconductor lighting, have efficiency
High, small in size, many advantages, such as service life is long, safety, low-voltage, energy-saving and environmental protection, by people regard as after incandescent lamp, fluorescent lamp,
Forth generation lighting source after high-voltage gas discharging light is the main product in the following illumination market.
There are various white light LEDs preparation methods at present, wherein blue-light LED chip and yellow fluorescent material group
It closes, blue-light LED chip is combined with red and green fluorescent material, purple LED chip with fluorescent material with three basic colour combines these three
Method is low with price, preparation simply becomes the main method for preparing white light LEDs.Blue-light LED chip is combined with yellow fluorescent material
It is research earliest and most mature method, the white light LEDs luminous efficiency of preparation develops the color and refer to considerably beyond incandescent lamp
Number is low, and colour temperature is high, cannot function as room lighting use.In order to improve the colour rendering of white light LEDs, scientists from all over the world have developed blue light
LED chip is combined with red, green fluorescent material and purple LED chip combines other two kinds with red, green, blue fluorescent material with three basic colour
The method for realizing white light LEDs.
The launch wavelength of InGaN chip has moved near ultraviolet region at present, and higher excitation energy can be provided for fluorescent powder
Amount, further increases the light intensity of white light LEDs.Since ultraviolet light is invisible, the color of burst of ultraviolel white light LEDs can only be by fluorescence
Powder determines that therefore colour stable, colour rendering index is high, glimmering using near ultraviolet InGaN chip and indigo plant, Huang fluorescent powder or with three primary colours
The scheme that light powder combines to realize white light becomes the emphasis of current white light LEDs industry development.Green emitting phosphor be in the program not
The ingredient that can lack.
Traditional phosphor material powder all relies on greatly activator or coactivator shines, and activator usually selects rare earth first
Element, rare earth element price is higher and its oxide, chloride and sal limonis are toxic, furthermore phosphor material powder prepare it is past
It is past to need the more exacting terms such as high temperature reducing atmospheres.Therefore, it the preparation of economic and environment-friendly fluorescent powder and is applied in order to must
It wants.
Summary of the invention
It is a kind of with the wide semiconductor green fluorescent powder of excitation bandwidth and preparation method thereof the purpose of the present invention is disclosing.
To achieve the above object, the technical solution used in the present invention is: the fluorescent powder has following chemical representation:
(Bi1-xYx)2ZnO(BO3)2, the value range of x is 0 x≤1 <.
Preferably, the value range of x is 0 < x < 1.
A kind of preparation method of semiconductor green fluorescent powder, includes the following steps:
(1) with the compound containing Bi, the compound containing Y, zinc oxide and boric acid, by chemical expression (Bi1-xYx)2ZnO
(BO3)2Molar ratio weigh the raw material, the value range of x is 0 x≤1 <, obtains mixture；
(2) by the mixture be packed into crucible, be sintered 2~7 hours under the conditions of 600~850 DEG C in high temperature furnace, after be cooled to
Room temperature obtains the semiconductor green fluorescent powder.
Further, the compound containing Bi is any one in bismuth nitrate and bismuth oxide.
Further: the compound containing Y is any one in yttrium nitrate and yttrium oxide.
Compared with prior art, the beneficial effects of the present invention are: (1) fluorescent powder of the invention without price costly
Rare earth element, and preparation condition is mild, does not need high temperature and reducing atmosphere；(2) present invention is in borate semiconductor material (Bi1- xYx)2ZnO(BO3)2In, it is able to achieve green emission, under Bi and Y Coexistence Situation, high-intensitive green emission is able to achieve, obtains
Green emitting phosphor has wide excitation bandwidth, covers ultraviolet, purple light and blue region, excitation peak and is located near 410nm, and ultraviolet
The transmitting overlap of peaks of chip is fine, can effectively be excited.
Detailed description of the invention
Fig. 1 is fluorescent powder exciting light spectrogram (518 nanometers of supervisory wavelength) prepared by embodiment 1 provided by the invention；
Fig. 2 is fluorescent powder launching light spectrogram (410 nanometers of excitation wavelength) prepared by embodiment 1 provided by the invention；
Fig. 3 is fluorescent powder launching light spectrogram (410 nanometers of excitation wavelength) prepared by embodiment 6 provided by the invention.
Specific embodiment
Comparative example
According to Bi2ZnO(BO3)2Weigh Bi (NO3)3, ZnO and H3BO3, the molar ratio between them is 2:1:2, is sufficiently ground
Mill after mixing, place crucible in, then high temperature furnace 600 DEG C roast 7 hours, after be cooled to room temperature, obtained powder is in purple
Outside, under purple light and blue light excitation, VISIBLE LIGHT EMISSION is had no.
Embodiment 1
According to (Bi0.995Y0.005)2ZnO(BO3)2Weigh Bi (NO3)3、Y(NO3)3, ZnO and H3BO3, rubbing between them
Your ratio is 1.99:0.01:1:2, is fully ground after mixing, places in crucible, then high temperature furnace roasts 6 hours at 620 DEG C, after
It is cooled to room temperature, obtains semiconductor green fluorescent powder.
From figure 1 it appears that the fluorescent powder excitation spectrum of the present embodiment is a wide range, ultraviolet, purple light and blue light are covered
Region, excitation peak are located near 410nm, and spectrum peak is high, illustrate that the fluorescent powder of the present embodiment can be by ultraviolet and purple light chip
Effectively excitation.When the excitation wavelength of emission spectrum is 410nm, from figure 2 it can be seen that the fluorescent powder of the present embodiment is emitted as
Broadband green light transmitting, emission peak are located near 518nm, illustrate that the fluorescent powder of the present embodiment is suitble to do ultraviolet, purple light and blue light swashs
The green emitting phosphor of hair.
Embodiment 2
According to (Bi0.95Y0.05)2ZnO(BO3)2Weigh Bi (NO3)3、Y(NO3)3, ZnO and H3BO3, mole between them
Than for 1.9:0.1:1:2, being fully ground after mixing, place in crucible, then high temperature furnace roasts 6 hours at 650 DEG C, it is rear cooling
To room temperature, semiconductor green fluorescent powder is obtained.
The fluorescent powder excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue region, excitation peak is located at
Near 410nm, spectrum peak is high, illustrates that the fluorescent powder of the present embodiment can effectively be excited by ultraviolet and purple light chip.Work as transmitting
The excitation wavelength of spectrum is 410nm, and the fluorescent powder of the present embodiment is emitted as broadband green light transmitting, and it is attached that emission peak is located at 518nm
Closely, illustrate that the fluorescent powder of the present embodiment is suitble to do ultraviolet, purple light and blue light activated green emitting phosphor.
Embodiment 3
According to (Bi0.75Y0.25)2ZnO(BO3)2Weigh Bi (NO3)3、Y(NO3)3, ZnO and H3BO3, mole between them
Than for 1.5:0.5:1:2, being fully ground after mixing, place in crucible, then high temperature furnace roasts 5 hours at 650 DEG C, it is rear cooling
To room temperature, semiconductor green fluorescent powder is obtained.
The fluorescent powder excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue region, excitation peak is located at
Near 410nm, spectrum peak is high, illustrates that the fluorescent powder of the present embodiment can effectively be excited by ultraviolet and purple light chip.Work as transmitting
The excitation wavelength of spectrum is 410nm, and the fluorescent powder of the present embodiment is emitted as broadband green light transmitting, and it is attached that emission peak is located at 515nm
Closely, illustrate that the fluorescent powder of the present embodiment is suitble to do ultraviolet, purple light and blue light activated green emitting phosphor.
Embodiment 4
According to (Bi0.5Y0.5)2ZnO(BO3)2Weigh Bi (NO3)3、Y2O3, ZnO and H3BO3, the molar ratio between them is
1:0.5:1:2, be fully ground after mixing, place crucible in, then high temperature furnace 700 DEG C roast 4 hours, after be cooled to room
Temperature obtains semiconductor green fluorescent powder.
The fluorescent powder excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue region, excitation peak is located at
Near 410nm, spectrum peak is high, illustrates that the fluorescent powder of the present embodiment can effectively be excited by ultraviolet and purple light chip.Work as transmitting
The excitation wavelength of spectrum is 410nm, and the fluorescent powder of the present embodiment is emitted as broadband green light transmitting, and it is attached that emission peak is located at 510nm
Closely, illustrate that the fluorescent powder of the present embodiment is suitble to do ultraviolet, purple light and blue light activated green emitting phosphor.
Embodiment 5
According to (Bi0.25Y0.75)2ZnO(BO3)2Weigh Bi2O3、Y(NO3)3, ZnO and H3BO3, the molar ratio between them is
0.25:1.5:1:2, be fully ground after mixing, place crucible in, then high temperature furnace 750 DEG C roast 3 hours, after be cooled to
Room temperature obtains semiconductor green fluorescent powder.
The fluorescent powder excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue region, excitation peak is located at
Near 410nm, spectrum peak is high, illustrates that the fluorescent powder of the present embodiment can effectively be excited by ultraviolet and purple light chip.Work as transmitting
The excitation wavelength of spectrum is 410nm, and the fluorescent powder of the present embodiment is emitted as broadband green light transmitting, and it is attached that emission peak is located at 515nm
Closely, illustrate that the fluorescent powder of the present embodiment is suitble to do ultraviolet, purple light and blue light activated green emitting phosphor.
Embodiment 6
According to Y2ZnO(BO3)2Weigh Y2O3, ZnO and H3BO3, the molar ratio between them is 1:1:2, is fully ground mixed
Close uniformly after, place crucible in, then high temperature furnace 850 DEG C roast 2 hours, after be cooled to room temperature, obtain semiconductor green fluorescence
Powder.
The fluorescent powder sintering temperature of the present embodiment is apparently higher than the (Bi containing Bi1-xYx)2ZnO(BO3)2Fluorescent powder, excitation
Spectrum is a wide range, covers ultraviolet, purple light and blue region, excitation peak is located near 410nm.From figure 3, it can be seen that when hair
The excitation wavelength for penetrating spectrum is 410nm, and the fluorescent powder of the present embodiment is emitted as broadband green light transmitting, and emission peak is located at 518nm
Near, luminous intensity is about the (Bi containing Bi1-xYx)2ZnO(BO3)2The 50% of fluorescent powder.
Above-described embodiment is used to illustrate the present invention, rather than limits the invention, in spirit of the invention and
In scope of protection of the claims, to any modifications and changes that the present invention makes, protection scope of the present invention is both fallen within.
Claims (5)
1. a kind of semiconductor green fluorescent powder, which is characterized in that the fluorescent powder has following chemical representation: (Bi1-xYx)2ZnO
(BO3)2, the value range of x is 0 x≤1 <.
2. a kind of semiconductor green fluorescent powder as described in claim 1, which is characterized in that the value range of x is 0 < x < 1.
3. a kind of preparation method of semiconductor green fluorescent powder as claimed in claim 1 or 2, it is characterised in that including walking as follows
It is rapid:
(1) with the compound containing Bi, the compound containing Y, zinc oxide and boric acid, by chemical expression (Bi1-xYx)2ZnO(BO3)2
Molar ratio weigh the raw material, the value range of x is 0 x≤1 <, obtains mixture；
(2) by the mixture be packed into crucible, be sintered 2~7 hours under the conditions of 600~850 DEG C in high temperature furnace, after be cooled to room
Temperature obtains the semiconductor green fluorescent powder.
4. the preparation method of semiconductor green fluorescent powder as claimed in claim 3, it is characterised in that: the compound containing Bi
For any one in bismuth nitrate and bismuth oxide.
5. the preparation method of semiconductor green fluorescent powder as claimed in claim 3, it is characterised in that: the compound containing Y
For any one in yttrium nitrate and yttrium oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610982001.XA CN106566549B (en) | 2016-11-09 | 2016-11-09 | A kind of semiconductor green fluorescent powder and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610982001.XA CN106566549B (en) | 2016-11-09 | 2016-11-09 | A kind of semiconductor green fluorescent powder and preparation method thereof |
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| CN106566549A CN106566549A (en) | 2017-04-19 |
| CN106566549B true CN106566549B (en) | 2018-12-28 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104845617A (en) * | 2015-04-30 | 2015-08-19 | 陕西师范大学 | Simple preparation method of Zn4B6O13: Eu3 + luminescent material |
-
2016
- 2016-11-09 CN CN201610982001.XA patent/CN106566549B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104845617A (en) * | 2015-04-30 | 2015-08-19 | 陕西师范大学 | Simple preparation method of Zn4B6O13: Eu3 + luminescent material |
Non-Patent Citations (3)
| Title |
|---|
| ZHANG Qiuhong等.Synthesis and luminescent properties of Ln3+ (Ln3+ = Eu3+, Dy3+)-doped Bi2ZnB2O7 phosphors.《RARE METALS》.2012, * |
| 张季 等.Bi2ZnOB2O6单晶偏振拉曼光谱.《物理学报》.2013, * |
| 石琳琳 等.组合优化设计制备Y3+/Dy3+共掺Bi2ZnB2O7新型荧光粉发光性质的研究.《光子学报》.2014, * |
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