CN106833642A - A kind of polyion activation single-matrix white fluorescent material being applied in WLED devices and preparation method thereof - Google Patents
A kind of polyion activation single-matrix white fluorescent material being applied in WLED devices and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 22
- 239000011159 matrix material Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229920000831 ionic polymer Polymers 0.000 title claims abstract description 14
- 230000004913 activation Effects 0.000 title abstract description 4
- -1 europium ion Chemical class 0.000 claims abstract description 20
- 239000000126 substance Substances 0.000 claims abstract description 7
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 6
- 150000001342 alkaline earth metals Chemical group 0.000 claims abstract description 4
- 150000002500 ions Chemical class 0.000 claims abstract description 4
- 238000005245 sintering Methods 0.000 claims description 34
- 238000000227 grinding Methods 0.000 claims description 33
- 150000001875 compounds Chemical class 0.000 claims description 24
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- 239000004327 boric acid Substances 0.000 claims description 10
- 239000004570 mortar (masonry) Substances 0.000 claims description 10
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 10
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 claims description 9
- 229910052733 gallium Inorganic materials 0.000 claims description 9
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 7
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 6
- 229910052796 boron Inorganic materials 0.000 claims description 6
- 150000001341 alkaline earth metal compounds Chemical class 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 150000002910 rare earth metals Chemical class 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 claims description 2
- 239000006227 byproduct Substances 0.000 claims description 2
- 230000004907 flux Effects 0.000 claims description 2
- 229910001195 gallium oxide Inorganic materials 0.000 claims description 2
- VGTPKLINSHNZRD-UHFFFAOYSA-N oxoborinic acid Chemical compound OB=O VGTPKLINSHNZRD-UHFFFAOYSA-N 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 2
- 244000025254 Cannabis sativa Species 0.000 claims 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 229910052684 Cerium Inorganic materials 0.000 abstract description 10
- 229910052693 Europium Inorganic materials 0.000 abstract description 7
- 239000000843 powder Substances 0.000 abstract description 6
- 238000001228 spectrum Methods 0.000 abstract description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 2
- 238000010189 synthetic method Methods 0.000 abstract description 2
- 230000003407 synthetizing effect Effects 0.000 abstract 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 24
- 229910000019 calcium carbonate Inorganic materials 0.000 description 12
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 8
- 238000001816 cooling Methods 0.000 description 8
- 229910052593 corundum Inorganic materials 0.000 description 8
- 239000010431 corundum Substances 0.000 description 8
- HEQHIXXLFUMNDC-UHFFFAOYSA-N O.O.O.O.O.O.O.[Tb].[Tb].[Tb].[Tb] Chemical compound O.O.O.O.O.O.O.[Tb].[Tb].[Tb].[Tb] HEQHIXXLFUMNDC-UHFFFAOYSA-N 0.000 description 7
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 7
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 7
- 229910001940 europium oxide Inorganic materials 0.000 description 7
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 7
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000000292 calcium oxide Substances 0.000 description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 229910000420 cerium oxide Inorganic materials 0.000 description 4
- 239000000395 magnesium oxide Substances 0.000 description 4
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910000018 strontium carbonate Inorganic materials 0.000 description 4
- 229910052771 Terbium Inorganic materials 0.000 description 3
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 3
- 239000002585 base Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 229910052571 earthenware Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000083879 Polyommatus icarus Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000002186 photoactivation Effects 0.000 description 1
- 238000012216 screening Methods 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
- 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
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7797—Borates
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses a kind of polyion activation single-matrix white fluorescent material being applied in WLED devices and preparation method thereof, its chemical formula is：M3Ga3‑mY1‑nB4O15:xCe3+,yTb3+,zEu3+, M is alkaline-earth metal case,x、yWithzRespectively Doped ions mol ratio coefficient, span is respectively：0.001≤x≤0.999、0.001≤y≤ 0.999 and 0.001≤z≤ 0.999 and meetx + y + z=m + n < 0.999.WLED of the invention activates single-matrix white fluorescent material with polyion, on the premise of architectural characteristic is ensured, the variation of valence of trivalent europium ion is successfully avoid while realizing and tetravalence cerium ion is effectively reduced, the made material white light for obtaining possesses the chromaticity coordinates and color temperature parameters for being easy to regulation.The white-light spectrum narrow emission peak of material occupies wholesale proportion, compared with display field is more suitable for for broad peak transmitting, to show broader colour gamut.The present invention emphasizes to sinter synthetizing phosphor powder using multistep to the control of reducing atmosphere, and synthetic method is simple unique and is applicable the scale for producing.
Description
Technical field
The present invention relates to phosphor technologies field, specifically, it is related to a kind of polyion being applied in WLED devices to swash
Single-matrix white fluorescent material living and preparation method thereof.
Background technology
It can be seen that optical chip is combined with YAG yellow fluorescent powders, after being partially absorbed to LED chip light using chip blue light and YAG
The gold-tinted for being converted, can form outdoor lighting white light.But because the white-light spectrum covering domain for combining is limited, red color light component
Missing have a strong impact on the performance indications of white light.It is lifting white light quality, expands the application category of white light, makes to be not limited to that low
End outdoor lighting, has more been applicable the technical fields such as room lighting, high accuracy display, studies the new available fluorescent material of WLED devices
It is one of emerging problem.
For the more traditional three primary colors fluorescent powder of single-matrix white fluorescent material, can be effectively prevented between different substrates to having radiated
The re-absorption of energy, meanwhile, because of matrix components uniformity, the environmental difference of each centre of luminescence is small, so as to largely keep away
Exempted from caused by matrix difference it is photochromic do not cooperate with, obtained white light can be allowed to possess color stability higher.Swash for polyion
Single-matrix white fluorescent material living, due to that can carry out ion screening according to purposes, adaptability is more broad.Trivalent cerium, terbium and europium from
Son is common blue, green and red photoactivation agent.In same matrix, do not reduce or over reduction is to the final of cerium and europium ion
Chemical valence produces influence, therefore it is still the key for obtaining high quality white light to realize that trivalent cerium and europium ion coexist in particular substrate
Technical problem.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided one kind can be excited by near ultraviolet LED chip, light
Fully, the wider array of polyion of the scope of application activates single-matrix white fluorescent material to spectrum covering domain.
Another mesh of the invention is to provide the preparation method of above-mentioned single-matrix white fluorescent material.
To achieve these goals, the present invention is adopted the following technical scheme that：
A kind of polyion activates single-matrix white fluorescent material, and its chemical formula is：M3Ga3-mY1-nB4O15: xCe3+,yTb3+,zEu3+,
M is alkaline-earth metal case,x、yWithzRespectively Doped ions mol ratio coefficient, span is respectively：0.001≤x≤
0.999、0.001≤y≤ 0.999 and 0.001≤z≤ 0.999 and meetx + y + z = m + n < 0.999。
In above-mentioned polyion activation single-matrix white fluorescent material, the M is Ca3-p-q Mg p Ba q Wherein 0≤p≤
0.100,0≤q≤ 0.100 andp + q ≤ 0.10。
Above-mentioned polyion activates the preparation method of single-matrix white fluorescent material, comprises the following steps：
Raw material is weighed by chemical composition, is added flux in mortar and is fully ground and treat uniform mixing, then reduced in gradient
Multistep sintering is carried out in atmosphere, after be cooled to room temperature, by product grinding obtain product.
In above-mentioned preparation method, the raw material is：Rare earth compound, alkaline earth metal compound, gallium element compound
Or boron element compound.The rare earth compound is in rare earth oxide, rare-earth oxalate, rare earth carbonate, rare earth nitrades
Any one compound or multiple compounds composition mixture.The alkaline earth metal compound is alkaline earth oxide carbon
The mixing of any one compound or the multiple compounds composition in hydrochlorate, alkali metal bicarbonates, alkali earth metal phosphate
Thing.The gallium element compound is any one compound or multiple compounds in gallium oxide, gallium carbonate, gallium oxalates
The mixture of composition.The boron element compound is any one or more in boric acid, metaboric acid and other boron-containing compounds
Compound group into mixture.
In above-mentioned preparation method, first step sintering temperature is 800 ~ 1000 DEG C, and the time is 10 ~ 20 h；Second step burns
Junction temperature is 1000 ~ 1200 DEG C, and sintering time is 10 ~ 20h；3rd step sintering temperature is 1000 ~ 1200 DEG C, and sintering time is 10
~20 h。
Compared with prior art, the present invention possesses following beneficial effect：
WLED of the invention with polyion activate single-matrix white fluorescent material, ensure architectural characteristic on the premise of, realize it is right
Tetravalence cerium ion successfully avoid the variation of valence of trivalent europium ion while effectively reduction, the made material white light for obtaining possesses just
In the chromaticity coordinates and color temperature parameters of regulation.The white-light spectrum narrow emission peak of material occupies wholesale proportion, for broad peak transmitting
Display field is more suitable for, to show broader colour gamut.The present invention is emphasized to be sintered the control of reducing atmosphere using multistep and closed
Into fluorescent material, synthetic method is simple unique and is applicable the scale for producing.
Brief description of the drawings
Fig. 1 is the X-ray powder diffraction pattern of the white fluorescent powder prepared by embodiment 1 ~ 2.
Fig. 2 is the fluorescence emission collection of illustrative plates of the white fluorescent powder prepared by embodiment 2.
Specific embodiment
Embodiment 1
Calcium carbonate is weighed respectively（CaCO3）0.3003 g, boric acid（(H3BO3）0.2600 g, gallium oxide（Ga2O3）0.2812 g,
Yittrium oxide（Y2O3）0.1129 g, above-mentioned raw materials are ground in agate mortar, corundum crucible are put into after grinding is uniform, 800
First step sintering is carried out in DEG C reducing atmosphere, constant temperature time is 10 h.Grinding is taken out after end, then Primordial Qi is gone back at 1000 DEG C
Second step sintering is carried out in atmosphere, constant temperature time is 10 h.Grinding is taken out after end, the 3rd step burning is carried out at 1000 DEG C again
Knot, constant temperature time is 10 h.Its natural cooling is treated after 3rd EOS, grinding is uniform and obtains product.Product x-ray powder spreads out
Penetrate result as shown in Figure 1.As shown in spectral line 1 in Fig. 1, all diffraction maximums can be with Ca3Ga3YB4O15Base peak（ICSD No.
17-2155）Correspondence, shows that the preparation scheme that multistep sintering is carried out in gradient reducing atmosphere will not mutually be impacted to thing.
Embodiment 2
Calcium carbonate is weighed respectively（CaCO3）0.3003 g, boric acid（(H3BO3）0.2600 g, gallium oxide（Ga2O3）0.2812 g,
Cerium oxide（CeO2）0.0037 g, terbium oxide（Tb4O7）0.0373 g, europium oxide（Eu2O3）0.0053 g, yittrium oxide（Y2O3）
0.0847 g, above-mentioned raw materials are ground in agate mortar, corundum crucible are put into after grinding is uniform, in 800 DEG C of reducing atmospheres
First step sintering is carried out, constant temperature time is 10 h.Grinding is taken out after end, second is then carried out in 1000 DEG C of reducing atmospheres
Step sintering, constant temperature time is 10 h.Grinding is taken out after end, the 3rd step sintering is carried out at 1000 DEG C again, constant temperature time is
10 h.Its natural cooling is treated after 3rd EOS, grinding is uniform and obtains product.Product X-ray powder diffraction result such as Fig. 1 institutes
Show.As shown in spectral line 2 in Fig. 1, all diffraction maximums and base peak（ICSD No. 17-2155）Control be as good as substantially, show cerium,
The introducing of terbium and europium ion can't mutually cause to significantly affect on the original.Fluorescence emission spectrogram of compound is as shown in Fig. 2 white light comes from
The common transmitting of cerium, terbium and europium ion.
Embodiment 3：
Strontium carbonate is weighed respectively（SrCO3）0.0147 g, calcium carbonate（CaCO3）0.2903 g, boric acid（(H3BO3）0.2600 g,
Gallium oxide（Ga2O3）0.2812 g, cerium oxide（CeO2）0.0037 g, terbium oxide（Tb4O7）0.0373 g, europium oxide（Eu2O3）
0.0053 g, yittrium oxide（Y2O3）0.0847 g, above-mentioned raw materials are ground in agate mortar, and corundum earthenware is put into after grinding is uniform
Crucible, carries out first step sintering in 800 DEG C of reducing atmospheres, and constant temperature time is 10 h.Grinding is taken out after end, then 1000
Second step sintering is carried out in DEG C reducing atmosphere, constant temperature time is 10 h.Grinding is taken out after end, is carried out at 1000 DEG C again
3rd step is sintered, and constant temperature time is 10 h.Its natural cooling is treated after 3rd EOS, grinding is uniform and obtains product.
Embodiment 4：
Magnesia is weighed respectively（MgO）0.0040 g, calcium carbonate（CaCO3）0.2903 g, boric acid（(H3BO3）0.2600 g, oxygen
Change gallium（Ga2O3）0.2812 g, cerium oxide（CeO2）0.0037 g, terbium oxide（Tb4O7）0.0373 g, europium oxide（Eu2O3）
0.0053 g, yittrium oxide（Y2O3）0.0847 g, above-mentioned raw materials are ground in agate mortar, and corundum earthenware is put into after grinding is uniform
Crucible, carries out first step sintering in 800 DEG C of reducing atmospheres, and constant temperature time is 10 h.Grinding is taken out after end, then 1000
Second step sintering is carried out in DEG C reducing atmosphere, constant temperature time is 10 h.Grinding is taken out after end, is carried out at 1000 DEG C again
3rd step is sintered, and constant temperature time is 10 h.Its natural cooling is treated after 3rd EOS, grinding is uniform and obtains product.
Embodiment 5：
Magnesia is weighed respectively（MgO）0.0020 g, strontium carbonate（SrCO3）0.0074 g, calcium carbonate（CaCO3）0.2903 g,
Boric acid（(H3BO3）0.2600 g, gallium oxide（Ga2O3）0.2812 g, cerium oxide（CeO2）0.0037 g, terbium oxide（Tb4O7）
0.0373 g, europium oxide（Eu2O3）0.0053 g, yittrium oxide（Y2O3）0.0847 g, above-mentioned raw materials are ground in agate mortar
Mill, corundum crucible is put into after grinding is uniform, and first step sintering is carried out in 800 DEG C of reducing atmospheres, and constant temperature time is 10 h.Knot
Grinding is taken out after beam, second step sintering is then carried out in 1000 DEG C of reducing atmospheres, constant temperature time is 10 h.Taken out after end
Grinding, carries out the 3rd step sintering at 1000 DEG C again, and constant temperature time is 10 h.Its natural cooling is treated after 3rd EOS, is ground
Mill is uniform and obtains product.
Embodiment 6：
Calcium oxide is weighed respectively（CaO）0.1684 g, boric acid（(H3BO3）0.2600 g, gallium oxide（Ga2O3）0.2812 g, oxygen
Change cerium（CeO2）0.0037 g, terbium oxide（Tb4O7）0.0373 g, europium oxide（Eu2O3）0.0053 g, yittrium oxide（Y2O3）
0.0847 g, above-mentioned raw materials are ground in agate mortar, corundum crucible are put into after grinding is uniform, in 800 DEG C of reducing atmospheres
First step sintering is carried out, constant temperature time is 10 h.Grinding is taken out after end, second is then carried out in 1000 DEG C of reducing atmospheres
Step sintering, constant temperature time is 10 h.Grinding is taken out after end, the 3rd step sintering is carried out at 1000 DEG C again, constant temperature time is
10 h.Its natural cooling is treated after 3rd EOS, grinding is uniform and obtains product.
Embodiment 7：
Calcium oxide is weighed respectively（CaO）0.1684 g, boric acid（(H3BO3）0.2600 g, gallium oxide（Ga2O3）0.2812 g, oxygen
Change cerium（CeO2）0.0037 g, terbium oxide（Tb4O7）0.0373 g, europium oxide（Eu2O3）0.0053 g, yittrium oxide（Y2O3）
0.0847 g, above-mentioned raw materials are ground in agate mortar, corundum crucible are put into after grinding is uniform, in 800 DEG C of reducing atmospheres
First step sintering is carried out, constant temperature time is 10 h.Grinding is taken out after end, second is then carried out in 1000 DEG C of reducing atmospheres
Step sintering, constant temperature time is 10 h.Grinding is taken out after end, the 3rd step sintering is carried out at 1000 DEG C again, constant temperature time is
10 h.Its natural cooling is treated after 3rd EOS, grinding is uniform and obtains product.
Embodiment 8：
Calcium carbonate is weighed respectively（CaCO3）0.3003, boric acid（(H3BO3）0.2600 g, gallium oxide（Ga2O3）0.2800 g, oxygen
Change cerium（CeO2）0.0037 g, terbium oxide（Tb4O7）0.0373 g, europium oxide（Eu2O3）0.0053 g, yittrium oxide（Y2O3）
0.0858 g, above-mentioned raw materials are ground in agate mortar, corundum crucible are put into after grinding is uniform, in 800 DEG C of reducing atmospheres
First step sintering is carried out, constant temperature time is 10 h.Grinding is taken out after end, second is then carried out in 1000 DEG C of reducing atmospheres
Step sintering, constant temperature time is 10 h.Grinding is taken out after end, the 3rd step sintering is carried out at 1000 DEG C again, constant temperature time is
10 h.Its natural cooling is treated after 3rd EOS, grinding is uniform and obtains product.
Claims (9)
1. a kind of polyion activates single-matrix white fluorescent material, and its chemical formula is：M3Ga3-mY1-nB4O15: xCe3+,yTb3+,zEu3 +, M is alkaline-earth metal case,x、yWithzRespectively Doped ions mol ratio coefficient, span is respectively：0.001≤x≤
0.999、0.001≤y≤ 0.999 and 0.001≤z≤ 0.999 and meetx + y + z = m + n < 0.999。
2. polyion as claimed in claim 1 activates single-matrix white fluorescent material, it is characterised in that the M is Ca3-p- q Mg p Ba q Wherein 0≤p≤ 0.100,0≤q≤ 0.100 andp + q ≤ 0.10。
3. polyion described in claim 1 activates the preparation method of single-matrix white fluorescent material, it is characterised in that including following step
Suddenly：
Raw material is weighed by chemical composition, is added flux in mortar and is fully ground and treat uniform mixing, then reduced in gradient
Multistep sintering is carried out in atmosphere, after be cooled to room temperature, by product grinding obtain product.
4. preparation method as claimed in claim 3, it is characterised in that the raw material is：Rare earth compound, alkaline-earth metal chemical combination
Thing, gallium element compound or boron element compound.
5. preparation method as claimed in claim 4, it is characterised in that the rare earth compound is rare earth oxide, rare earth grass
The mixture of any one compound or the multiple compounds composition in hydrochlorate, rare earth carbonate, rare earth nitrades.
6. preparation method as claimed in claim 4, it is characterised in that the alkaline earth metal compound is alkaline earth oxide
It is mixed that any one compound or multiple compounds in carbonate, alkali metal bicarbonates, alkali earth metal phosphate are constituted
Compound.
7. preparation method as claimed in claim 4, it is characterised in that the gallium element compound is gallium oxide, gallium carbonic acid
The mixture of any one compound or the multiple compounds composition in salt, gallium oxalates.
8. preparation method as claimed in claim 4, it is characterised in that the boron element compound be boric acid, metaboric acid and its
Any one or more compound group in his boron-containing compound into mixture.
9. preparation method as claimed in claim 3, it is characterised in that the multistep sintering is divided into three steps, first step sintering temperature
It is 800 ~ 1000 DEG C to spend, and the time is 10 ~ 20 h；Second step sintering temperature is 1000 ~ 1200 DEG C, and sintering time is 10 ~ 20h；The
Three step sintering temperatures are 1000 ~ 1200 DEG C, and sintering time is 10 ~ 20 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710008355.9A CN106833642A (en) | 2017-01-05 | 2017-01-05 | A kind of polyion activation single-matrix white fluorescent material being applied in WLED devices and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107353900A (en) * | 2017-07-31 | 2017-11-17 | 广东工业大学 | A kind of niobates fluorescent material, its preparation method and light emitting diode |
| CN107746709A (en) * | 2017-11-20 | 2018-03-02 | 山东省科学院新材料研究所 | A kind of tunable luminescence rare earth ion doping Mg2Al4Si5O18Fluorescent material and preparation method thereof |
| CN115011342A (en) * | 2022-05-09 | 2022-09-06 | 广东省科学院资源利用与稀土开发研究所 | Bi 3+ Doped cyan fluorescent powder and preparation method thereof |
| CN115477321A (en) * | 2022-09-06 | 2022-12-16 | 五邑大学 | Red fluorescent powder and preparation method and application thereof |
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2017
- 2017-01-05 CN CN201710008355.9A patent/CN106833642A/en active Pending
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| CHIEN-HAO HUANG ET AL.: "A Novel Single-Composition Trichromatic White-Light Ca3Y(GaO)3(BO3)4:Ce3+,Mn2+,Tb3+ Phosphor for UV-Light Emitting Diodes", 《J. PHYS. CHEM. C》 * |
| JUN ZHOU ET AL.: "Luminescence color tuning of Ce3+, Tb3+ and Eu3+ codoped and tri-doped BaY2Si3O10 phosphors via energy transfer", 《J. MATER. CHEM. C》 * |
| WASIM ULLAH KHAN ET AL.: "Efficient energy transfer and luminescence properties of Ca3Y(GaO)3(BO3)4:Tb3+,Eu3+ as a green-to-red colour tunable phosphor under near-UV excitation", 《DALTON TRANSACTIONS》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107353900A (en) * | 2017-07-31 | 2017-11-17 | 广东工业大学 | A kind of niobates fluorescent material, its preparation method and light emitting diode |
| CN107746709A (en) * | 2017-11-20 | 2018-03-02 | 山东省科学院新材料研究所 | A kind of tunable luminescence rare earth ion doping Mg2Al4Si5O18Fluorescent material and preparation method thereof |
| CN115011342A (en) * | 2022-05-09 | 2022-09-06 | 广东省科学院资源利用与稀土开发研究所 | Bi 3+ Doped cyan fluorescent powder and preparation method thereof |
| CN115011342B (en) * | 2022-05-09 | 2023-04-07 | 广东省科学院资源利用与稀土开发研究所 | Bi 3+ Doped cyan fluorescent powder and preparation method thereof |
| CN115477321A (en) * | 2022-09-06 | 2022-12-16 | 五邑大学 | Red fluorescent powder and preparation method and application thereof |
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