CN104726097A - Novel yellow fluorescent powder and preparation method thereof - Google Patents

Novel yellow fluorescent powder and preparation method thereof Download PDF

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Publication number
CN104726097A
CN104726097A CN201510130781.0A CN201510130781A CN104726097A CN 104726097 A CN104726097 A CN 104726097A CN 201510130781 A CN201510130781 A CN 201510130781A CN 104726097 A CN104726097 A CN 104726097A
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powder
preparation
luminescent material
roasting
fluorescent powder
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刘光辉
刘茜
周真真
万洁琼
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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Abstract

The invention relates to novel yellow fluorescent powder and a preparation method thereof. A luminescent material is Ce3 + doped Ca3Ga2O6, and the chemical formula is Ca3 (1-x) Ga2O6:3xCe, wherein the value range of x is 0.5-10%. A novel fluorescent material Ce:Ca3Ga2O6 is obtained through a high temperature solid phase roasting method in the invention, the fluorescent powder material emits yellow light under the excitation of blue light at a 460 nm waveband, and thus the yellow fluorescent powder has a high application value. Compared with the prior art, the fluorescent material prepared in the invention has the advantages that the sintering temperature is lower, and the reaction conditions are relatively moderate, so as to meet the development requirements of novel luminescent materials, and thus the novel yellow fluorescent powder is suitable for industrial production and can be applied to industrial fields such as LED illumination and photoelectric display screens.

Description

A kind of novel yellow fluorescent material and preparation method thereof
Technical field
The present invention relates to a kind of novel Ce:Ca 3ga 2o 6luminescent material, belongs to optical function material technical field.
Background technology
In illumination market, white light LEDs developed one of the swiftest and the most violent technology in recent years.Compared with traditional lighting mode (incandescent osram lamp and energy-saving fluorescent lamp), white light LEDs has the longer life-span, the advantages such as higher luminous efficiency.In order to realize LED white-light illuminating, following scheme can be adopted: 1. the luminescence of three primary colours (red, green, blue) chip portfolio realizes white light; 2. blue chip (GaN/InGaN) is in conjunction with yellow fluorescent powder (appropriate introducing green emitting phosphor and red fluorescence powder), realizes white-light illuminating; 3. near ultraviolet chip realizes white light emission in conjunction with three primary colors fluorescent powder.
In such scheme, the second is one of mode most widely used in current market, blue chip (GaN/InGaN) and appropriate yellow fluorescent powder (as Ce:YAG etc.) is in harmonious proportion to realize white light emission.In this technical scheme, the acquisition of high performance yellow fluorescent material is one of key factor wherein.Ce:YAG yellow fluorescent powder quantum yield is high, and can coincide preferably with blue chip thus obtain white light, be applied widely, but the deficiency of its aspect such as colour rendering index and high temperature stability performance, can not meet on market that (high-temperature stability is good for the demand of high performance yellow fluorescent material, high colour rendering index, low colour temperature etc.).Therefore, the yellow fluorescent powder developing performance more excellent also becomes technical requirements new in white light LEDs field.
Summary of the invention
The present invention is intended to the performance deficiency overcoming existing yellow fluorescent powder, the invention provides a kind of novel yellow fluorescent powder Ce:Ca 3ga 2o 6and preparation method thereof.
The invention provides a kind of Ce 3+the luminescent material of doping, described luminescent material is Ce 3+the Ca of doping 3ga 2o 6, chemical formula is Ca 3 (1-x)ga 2o 6: 3xCe, wherein, the span of x is between 0.5%-10%.
Preferably, the luminescence center of described luminescent material is from Ce 3+the feature of ion excites.
Preferably, described luminescent material under blue-light excited, can launch gold-tinted.
Again, present invention also offers a kind of preparation method of above-mentioned luminescent material, comprising:
1) according to the chemical formula of described luminescent material, Ga is taken respectively 2o 3powder, Ca source powder and Ce source powder, wherein Ca source powder is CaO powder and/or CaCO 3powder, Ce source powder are CeO 2powder and/or Ce (NO 3) 3powder, after Homogeneous phase mixing, as material powder;
2) by material powder 1000-1350 DEG C, under reducing atmosphere high temperature solid-state roasting obtain described luminescent material.
Preferably, the high temperature solid-state roasting time of material powder is 2-6 hour.
Preferably, by material powder at Ar/H 2roasting 2-6 hour at atmosphere, 1150-1300 DEG C.
Preferably, by material powder roasting 3-5 hour at gac atmosphere, 1100-1350 DEG C.
Preferably, by material powder at NH 3roasting 3-5 hour at atmosphere, 1000-1150 DEG C.
Beneficial effect of the present invention:
The present invention, by the method for high temperature solid-state roasting, obtains a kind of novel fluorescent material Ce:Ca 3ga 2o 6, this phosphor material powder, at the blue-light excited lower transmitting gold-tinted of 460nm wave band, is a kind of yellow fluorescent powder having using value.Compared with prior art, fluorescent material prepared by the present invention, sintering temperature is lower, and reaction conditions is relatively gentle, meets the demand for development of advanced luminescent material, is applicable to suitability for industrialized production, can be used for the industrial circle such as LED illumination, photo-electric display.
Accompanying drawing explanation
Fig. 1 shows the Ce:Ca of the various ce ion doping prepared in embodiment 1-6 3ga 2o 6the luminous collection of illustrative plates of fluorescent material;
Fig. 2 shows the Ce:Ca of preparation in embodiment 1 3ga 2o 6the XRD figure spectrum of fluorescent material (x=0.5mol%);
Fig. 3 shows the Ce:Ca of preparation in embodiment 5 3ga 2o 6the chromaticity coordinates collection of illustrative plates of fluorescent material (x=7.5mol%);
Fig. 4 shows in embodiment 7 to sinter under gac atmosphere and obtains Ce:Ca 3ga 2o 6the luminous collection of illustrative plates of fluorescent material (x=1mol%);
Fig. 5 shows in embodiment 8 at NH 3the Ce:Ca obtained is sintered under atmosphere 3ga 2o 6the luminous collection of illustrative plates of fluorescent material (x=2mol%).
Embodiment
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that accompanying drawing and following embodiment are only for illustration of the present invention, and unrestricted the present invention.
The invention discloses a kind of cerium (Ce 3+) Ca of ion doping 3ga 2o 6luminescent material and preparation method thereof, this luminescent material is blue-light excited (about 460nm), launch gold-tinted (about 550nm), can with commercial blue-light LED chip (InGaN, 460nm) combine preferably, thus obtain white light LEDs.The luminescence center of described luminescent material comes from Ce 3+the feature of ion excites (5d-4f), is to adopt Ce 3+ion, as luminescent activator, realizes yellow emission.
The preparation process of this luminescent material is:
Ca will be formed 3ga 2o 6raw material Ga 2o 3, CaO (or CaCO 3) according to 1:3 (1-x) mol ratio batching, then take CeO 2/ Ce (NO 3) 3, Ce 3+ion doping concentration is x (the molar weight sum relative to Ca atom and Ce atom), and x is between 0.5%-10%;
Dry mixed is even, and put into electric furnace under reducing atmosphere condition, through high temperature sintering, maturing temperature scope is 1000-1350 DEG C, roasting time 2-6h, finally cools to room temperature with the furnace, can obtain final sample after grinding.
Adopt reducing atmosphere during solid phase roasting, one of adoptable reducing atmosphere is: argon gas/hydrogen mixed gas (Ar/H 2, H 2volume content is 5%).Adopt high temperature solid-state roasting method, at Ar/H 2sinter under atmosphere, at 1150-1300 DEG C of temperature, insulation 2-6h, finally cools to room temperature with the furnace, grinding.
Adopting gac and buried charcoal method, is one of method obtaining reducing atmosphere.Adopt high temperature solid-state roasting method, sinter under gac atmosphere, at 1100-1350 DEG C of temperature, insulation 3-5h, finally cools to room temperature with the furnace, grinding.
Adopt reducing atmosphere during solid phase roasting, in sintering process, pass into appropriate NH 3it is one of method obtaining reducing atmosphere.Adopt high temperature solid-state roasting method, at NH 3sinter under atmosphere, at 1000-1150 DEG C of temperature, insulation 3-5h, finally cools to room temperature with the furnace, grinding.
Prepared fluorescent material Ce:Ca 3ga 2o 6belong to blue-light excited acquisition yellow emission, can combine preferably with commercial blue-light LED chip (InGaN, 460nm), thus obtain white light LEDs.This fluorescent material can be applicable to white-light illuminating field or other photoelectron display lighting field.
This patent proposes, Ce:Ca 3ga 2o 6yellow fluorescent material, Ce 3+the feature of ion excites (5d-4f) to be positioned at about 460nm, emission wavelength about 550nm, can combine preferably with commercial blue-light LED chip (InGaN, 460nm), thus obtains white light LEDs.Known through investigating, for Ce 3+the Ca of ion doping 3ga 2o 6the research of yellow fluorescent material, is not reported both at home and abroad.This patent applies for that protection content is for pioneering sex work.
Exemplify embodiment below further to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The processing parameter etc. that following example is concrete is also only an example in OK range, and namely those skilled in the art can be done in suitable scope by explanation herein and select, and do not really want the concrete numerical value being defined in Examples below.
Embodiment 1
By raw material Ga 2o 3, CaO takes according to 1:3 (1-x) mol ratio, CeO 2/ Ce (NO 3) 3take by x=0.5mol%, by even for raw material dry mixed.Above-mentioned mixing raw material is put into electric furnace, at Ar/H 2roasting 4h at gas mixture atmosphere 1200 DEG C, furnace cooling, to room temperature, takes out grinding;
Fig. 1 shows obtained fluorescent material (x=0.5mol%) Ce:Ca 3ga 2o 6luminous collection of illustrative plates, visible, the main emission peak of the phosphor material powder obtained by the present embodiment is about 548nm, and apparent is yellow fluorescent powder.Fig. 2 is its XRD test result, and collection of illustrative plates display fits like a glove with PDF card #41-0856, and namely gained sample is the Ca of orthorhombic phase 3ga 2o 6.
Embodiment 2
By raw material Ga 2o 3, CaO takes according to 1:3 (1-x) mol ratio, CeO 2/ Ce (NO 3) 3take by x=1mol%, by even for raw material dry mixed.Above-mentioned mixing raw material is put into electric furnace, at Ar/H 2roasting 4h at gas mixture atmosphere 1200 DEG C, furnace cooling, to room temperature, takes out grinding;
Fig. 1 shows obtained fluorescent material (x=1mol%) Ce:Ca 3ga 2o 6luminous collection of illustrative plates, visible, the main emission peak of the phosphor material powder obtained by the present embodiment is about 550nm, and the sample that luminous intensity is prepared in embodiment 1 strengthens.XRD test result and PDF card #41-0856 fit like a glove, and namely gained sample is the Ca of orthorhombic phase 3ga 2o 6.
Embodiment 3
By raw material Ga 2o 3, CaO takes according to 1:3 (1-x) mol ratio, CeO 2/ Ce (NO 3) 3take by x=2mol%, by even for raw material dry mixed.Above-mentioned mixing raw material is put into electric furnace, at Ar/H 2roasting 4h at gas mixture atmosphere 1200 DEG C, furnace cooling, to room temperature, takes out grinding;
Fig. 1 shows obtained fluorescent material (x=2mol%) Ce:Ca 3ga 2o 6luminous collection of illustrative plates, visible, the main emission peak of the phosphor material powder obtained by the present embodiment is 550nm, and the sample that sample luminous intensity prepared by embodiment 3 is prepared than embodiment 2 strengthens.XRD test result and PDF card #41-0856 fit like a glove, and namely gained sample is the Ca of orthorhombic phase 3ga 2o 6.
Embodiment 4
By raw material Ga 2o 3, CaO takes according to 1:3 (1-x) mol ratio, CeO 2/ Ce (NO 3) 3take by x=4mol%, by even for raw material dry mixed.Above-mentioned mixing raw material is put into electric furnace, at Ar/H 2roasting 4h at gas mixture atmosphere 1200 DEG C, furnace cooling, to room temperature, takes out grinding;
Fig. 1 shows obtained fluorescent material (x=4mol%) Ce:Ca 3ga 2o 6luminous collection of illustrative plates, visible, the main emission peak of the phosphor material powder obtained by the present embodiment is 550nm, and the sample that sample luminous intensity prepared by embodiment 4 is prepared than embodiment 3 strengthens.XRD test result and PDF card #41-0856 fit like a glove, and namely gained sample is the Ca of orthorhombic phase 3ga 2o 6.
Embodiment 5
By raw material Ga 2o 3, CaO takes according to 1:3 (1-x) mol ratio, CeO 2/ Ce (NO 3) 3take by x=7.5mol%, by even for raw material dry mixed.Above-mentioned mixing raw material is put into electric furnace, at Ar/H 2roasting 4h at gas mixture atmosphere 1200 DEG C, furnace cooling, to room temperature, takes out grinding;
Fig. 1 shows obtained fluorescent material (x=7.5mol%) Ce:Ca 3ga 2o 6luminous collection of illustrative plates, visible, the main emission peak of the phosphor material powder obtained by the present embodiment is 550nm, and the sample that sample luminous intensity prepared by embodiment 5 is prepared than embodiment 4 has further enhancing.Fig. 3 is this fluorescent material (x=7.5mol%) Ce:Ca 3ga 2o 6chromaticity coordinates, chromaticity coordinates value is (0.423,0.534), apparent upper be gold-tinted.XRD test result and PDF card #41-0856 fit like a glove, and namely gained sample is the Ca of orthorhombic phase 3ga 2o 6.
Embodiment 6
By raw material Ga 2o 3, CaO takes according to 1:3 (1-x) mol ratio, CeO 2/ Ce (NO 3) 3take by x=10mol%, by even for raw material dry mixed.Above-mentioned mixing raw material is put into electric furnace, at Ar/H 2roasting 4h at gas mixture atmosphere 1200 DEG C, furnace cooling, to room temperature, takes out grinding;
Fig. 1 shows obtained fluorescent material (x=10mol%) Ce:Ca 3ga 2o 6luminous collection of illustrative plates, visible, the main emission peak of the phosphor material powder obtained by the present embodiment is 550nm, and Quenching has appearred in the sample luminous intensity that sample luminous intensity prepared by embodiment 6 is prepared than embodiment 5, illustrates that 7.5%mol concentration is close to optimum doping concentration.XRD test result and PDF card #41-0856 fit like a glove, and namely gained sample is the Ca of orthorhombic phase 3ga 2o 6.
Embodiment 7
By raw material Ga 2o 3, CaO takes according to 1:3 (1-x) mol ratio, CeO 2/ Ce (NO 3) 3take by x=1mol%, by even for raw material dry mixed.Above-mentioned mixing raw material is put into electric furnace, roasting 4h at gac atmosphere 1200 DEG C, furnace cooling, to room temperature, takes out grinding;
In Fig. 4, curve is obtained fluorescent material (x=1mol%) Ce:Ca 3ga 2o 6luminous collection of illustrative plates, visible, the main emission peak of the phosphor material powder obtained by the present embodiment is 547nm.XRD test result and PDF card #41-0856 fit like a glove, and namely gained sample is the Ca of orthorhombic phase 3ga 2o 6.
Embodiment 8
By raw material Ga 2o 3, CaO takes according to 1:3 (1-x) mol ratio, CeO 2/ Ce (NO 3) 3take by x=2mol%, by even for raw material dry mixed.Above-mentioned mixing raw material is put into electric furnace, at NH 3roasting 3h at atmosphere 1100 DEG C, furnace cooling, to room temperature, takes out grinding;
In Fig. 5, curve is obtained fluorescent material (x=2mol%) Ce:Ca 3ga 2o 6luminous collection of illustrative plates, visible, the main emission peak of the phosphor material powder obtained by the present embodiment is 550nm, and apparent is above gold-tinted.XRD test result and PDF card #41-0856 fit like a glove, and namely gained sample is the Ca of orthorhombic phase 3ga 2o 6.

Claims (8)

1. a Ce 3+the luminescent material of doping, it is characterized in that, described luminescent material is Ce 3+the Ca of doping 3ga 2o 6, chemical formula is Ca 3 (1-x)ga 2o 6: 3xCe, wherein, the span of x is between 0.5%-10%.
2. luminescent material according to claim 1, is characterized in that, the luminescence center of described luminescent material is from Ce 3+the feature of ion excites.
3. luminescent material according to claim 1 and 2, is characterized in that, described luminescent material under blue-light excited, can launch gold-tinted.
4. the preparation method of arbitrary described luminescent material in claim 1-3, is characterized in that, comprising:
1) according to the chemical formula of described luminescent material, Ga is taken respectively 2o 3powder, Ca source powder and Ce source powder, wherein Ca source powder is CaO powder and/or CaCO 3powder, Ce source powder are CeO 2powder and/or Ce (NO 3) 3powder, after Homogeneous phase mixing, as material powder;
2) by material powder 1000-1350 DEG C, under reducing atmosphere high temperature solid-state roasting obtain described luminescent material.
5. preparation method according to claim 4, is characterized in that, the high temperature solid-state roasting time of material powder is 2-6 hour.
6. the preparation method according to claim 4 or 5, is characterized in that, by material powder at Ar/H 2roasting 2-6 hour at atmosphere, 1150-1300 DEG C.
7. the preparation method according to claim 4 or 5, is characterized in that, by material powder roasting 3-5 hour at gac atmosphere, 1100-1350 DEG C.
8. the preparation method according to claim 4 or 5, is characterized in that, by material powder at NH 3roasting 3-5 hour at atmosphere, 1000-1150 DEG C.
CN201510130781.0A 2015-03-24 2015-03-24 Novel yellow fluorescent powder and preparation method thereof Pending CN104726097A (en)

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN105131478A (en) * 2015-08-04 2015-12-09 浙江工商大学 Composite fluorescent agent microporous material
CN107760301A (en) * 2016-08-15 2018-03-06 中国科学院上海硅酸盐研究所 The Ca of Pr ion dopings3Ga2O6Blue-green fluorescent powder and preparation method thereof
CN108546510A (en) * 2018-05-15 2018-09-18 深圳瑞欧光技术有限公司 A kind of low biohazard transparent coatings of LED lamp
CN108662553A (en) * 2018-05-15 2018-10-16 深圳瑞欧光技术有限公司 It is a kind of to hinder blue coating with low biohazard and use the LED lamp of the coating
CN115710089A (en) * 2022-12-23 2023-02-24 景德镇陶瓷大学 Yellow semitransparent fluorescent glass ceramic and preparation method thereof

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105131478A (en) * 2015-08-04 2015-12-09 浙江工商大学 Composite fluorescent agent microporous material
CN107760301A (en) * 2016-08-15 2018-03-06 中国科学院上海硅酸盐研究所 The Ca of Pr ion dopings3Ga2O6Blue-green fluorescent powder and preparation method thereof
CN107760301B (en) * 2016-08-15 2020-09-18 中国科学院上海硅酸盐研究所 Pr ion doped Ca3Ga2O6Blue-green fluorescent powder and preparation method thereof
CN108546510A (en) * 2018-05-15 2018-09-18 深圳瑞欧光技术有限公司 A kind of low biohazard transparent coatings of LED lamp
CN108662553A (en) * 2018-05-15 2018-10-16 深圳瑞欧光技术有限公司 It is a kind of to hinder blue coating with low biohazard and use the LED lamp of the coating
CN115710089A (en) * 2022-12-23 2023-02-24 景德镇陶瓷大学 Yellow semitransparent fluorescent glass ceramic and preparation method thereof
CN115710089B (en) * 2022-12-23 2024-02-27 景德镇陶瓷大学 Yellow semitransparent fluorescent microcrystalline glass and preparation method thereof

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Application publication date: 20150624