CN105154073A - Blue/green fluorescent powder suitable for ultraviolet light/near ultraviolet light excitated white LED and preparation method for blue/green fluorescent powder - Google Patents

Blue/green fluorescent powder suitable for ultraviolet light/near ultraviolet light excitated white LED and preparation method for blue/green fluorescent powder Download PDF

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Publication number
CN105154073A
CN105154073A CN201510427130.8A CN201510427130A CN105154073A CN 105154073 A CN105154073 A CN 105154073A CN 201510427130 A CN201510427130 A CN 201510427130A CN 105154073 A CN105154073 A CN 105154073A
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fluorescent powder
blue
green fluorescent
preparation
ultraviolet light
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林君
李凯
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Changchun Institute of Applied Chemistry of CAS
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Changchun Institute of Applied Chemistry of CAS
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Abstract

The invention relates to blue/green fluorescent powder suitable for an ultraviolet light/near ultraviolet light excitated white LED and a preparation method for the blue/green fluorescent powder and belongs to the field of light emitting materials. The blue/green fluorescent powder solves the technical problems that the white light color temperature is on the high side, the color rendering index is low and the thermal characteristic is poor as the existing YAG fluorescent powder for realizing the white light LED is short of red light components. The chemical composition of the blue/green fluorescent powder is as follows: Ca(1.65-y)Sr(0.35-x)Si(1-z)O4: Eux, Cey/Lz, wherein x is 0.001-0.08, y is 0.001-0.15, z is 0-0.5, and L is one or more of Al, Ga and B. The invention further provides the preparation method for the material. The blue/green fluorescent powder excitated at 365 nm has broadband transmission without L doping, wherein the emitting peaks are positioned at 436 nm and 508 nm. The positions and full width at half maximum(FWHM) of the emitting peaks of the blue fluorescent powder are increased as the content of L is increased. The emitting intensity is enhanced in some L doping conditions. The FWHM of the green fluorescent powder is about 87 nm. The product has certain promotional value for preparing a light emitting material for an efficient white light LED with potential applicability.

Description

A kind of white light LEDs indigo plant/green emitting phosphor being applicable to ultraviolet/near ultraviolet excitation and preparation method thereof
Technical field
The present invention relates to field of light emitting materials, be specifically related to a kind of white light LEDs indigo plant/green emitting phosphor being applicable to ultraviolet/near ultraviolet excitation and preparation method thereof.
Background technology
White light emitting diode (LED), as a kind of novel solid state illumination technology, because its luminous efficiency is high, long service life, the features such as environmental friendliness, have more energy-conservation advantage, this technology will progressively replace the luminescent lamp of the larger incandescent light of power consumption and mercury pollution, and therefore corresponding measures and tactics has all been formulated to develop white light LEDs in many countries and regions.At present, white light LEDs mainly contains three kinds of implementations, and one is combination red, green and blue three kinds of LED, and two is adopt blue-ray LED combination yellow fluorescent powder (Y 3al 5o 12, YAG), three is adopt ultraviolet near-ultraviolet light LED combination red, green, blue fluorescent material.But, really reach commercial and only have the second way.Fluorescence transition material is as one of the critical material of white light LEDs, most important to the development of high efficiency semiconductor illumination.Before this, white light LEDs mainly adopts blue-ray LED to combine YAG yellow fluorescent powder, and namely a part of blue-light excited fluorescent material produces gold-tinted, and gold-tinted and some blue light combine and realize white light.But widely use YAG fluorescent powder at present, because it lacks ruddiness component, it is higher to adopt the white light colour temperature obtained in this way, and colour rendering index is low, and thermal property neither be fine.Thus, in order to overcome these shortcomings, the third above-mentioned scheme realizing white light LEDs is paid close attention to widely.The exploitation of novel indigo plant/green emitting phosphor is a wherein very important part.
Summary of the invention
The present invention to solve in prior art adopt blue-ray LED combine YAG yellow fluorescent powder realize white light LEDs use YAG fluorescent powder due to the white light colour temperature lacking ruddiness component and cause obtaining higher, colour rendering index is low, the technical problem that thermal property is bad, provides a kind of white light LEDs indigo plant/green emitting phosphor being applicable to ultraviolet/near ultraviolet excitation and preparation method thereof.
In order to solve the problems of the technologies described above, technical scheme of the present invention is specific as follows:
Be applicable to white light LEDs indigo plant/green emitting phosphor of ultraviolet/near ultraviolet excitation, its chemical constitution is: Ca 1.65-ysr 0.35-xsi 1-zo 4: Eu x, Ce y/ L z, in formula, x=0.001-0.08, y=0.001-0.15, z=0-0.5, L are one or more in Al, Ga and B.
Be applicable to a preparation method for the white light LEDs indigo plant/green emitting phosphor of ultraviolet/near ultraviolet excitation, comprise the following steps:
Material is chosen according to chemical formula Ca 1.65-ysr 0.35-xsi 1-zo 4: Eu x, Ce y/ L zanalytically pure CaCO is taken respectively according to its molar percentage 3, SrCO 3, SiO 2, Al (OH) 3, Ga 2o 3and H 3bO 3in one or more, and high-purity CeO 2and/or Eu 2o 3, then add appropriate ethanol and fully grind post-drying, then grind, in reducing atmosphere H at temperature of reaction is 1100-1300 DEG C 2/ N 2lower sintering 8-10h, takes out after cooling, can obtain final product.
In technique scheme, the described time of grinding again is 1 minute.
In technique scheme, described temperature of reaction is 1200-1250 DEG C, and sintering time is 8h.
In technique scheme, described H 2/ N 2per-cent be 20%:80%.
The invention has the beneficial effects as follows:
White light LEDs indigo plant/the green emitting phosphor being applicable to ultraviolet/near ultraviolet excitation provided by the invention compared with existing blue BAM fluorescent material, see the known prepared blue Ca of Fig. 1-Fig. 3 1.65-ysr 0.35si 1-zo 4: Ce y/ L zexcite wider, the position of excitation peak is about 370nm, is more suitable for mating ultraviolet chip.The green Ca of preparation 1.65sr 0.35-xsiO 4: Eu xfluorescent material and (Ba, Sr) 2siO 4compare, excite wider can better and ultraviolet/near-ultraviolet light LED chip match.Simultaneously under 365nm excites, the emission peak launching the strongest sample is the broadband emission being positioned at 436 and 508nm respectively.The position of blue colour fluorescent powder emission peak and halfwidth can increase along with the increase of the content of L.And its emissive porwer can strengthen under some L doping condition.The emission peak positions of green emitting phosphor is at about 510nm, and its halfwidth is about 87nm.Its under 150 DEG C of intensity are about normal temperature 66%, be better than (Ba, Sr) 2siO 449%, sample does not carry out subsequent disposal, and luminous quantum efficiency can reach 69%.This product has certain promotional value to the white light LEDs luminescent material that preparation is efficient, have potential applicability.
Preparation method of the present invention synthesizes the europium and/or cerium ion-doped silicate luminescent material that obtain, and chemical constitution is Ca 1.65-ysr 0.35-xsi 1-zo 4: Eu x, Ce y/ L z, in formula, x=0.001-0.08, y=0.001-0.15, z=0-0.5, L are one or more in Al, Ga and B.Under ultraviolet/near-ultraviolet light (250-420nm) excites, sample can launch bright indigo plant/green glow.Obtained fluorescent material is expected to the LED chip that is rear and ultraviolet/near-ultraviolet light with rouge and powder mixing and is encapsulated into white light emitting diode, is applied to illumination.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Fig. 1 is the XRD figure spectrum of the indigo plant/green emitting phosphor prepared by embodiment of the present invention 1-6, the a-f figure respectively in corresponding diagram 1;
Fig. 2 is exciting and utilizing emitted light spectrogram of the indigo plant/green emitting phosphor prepared by embodiment of the present invention 1-6, the a-f figure respectively in corresponding diagram 1;
Fig. 3 is sample Ca 1.65sr 0.35-xsiO 4: Eu xalong with Eu under 365nm excites 2+doped parameterx increases the chromaticity coordinates variation diagram of d.
Embodiment
Raw material used in the present invention is analytically pure CaCO 3, SrCO 3, SiO 2, Al (OH) 3/ Ga 2o 3/ H 3bO 3with high-purity CeO 2or Eu 2o 3(99.99%), in conjunction with embodiment, the present invention is described in more detail, but the present invention is not limited to these embodiments.
Embodiment 1
Material is chosen according to chemical formula Ca 1.60sr 0.35siO 4: Ce 0.05, take analytically pure CaCO respectively according to its molar percentage 3, SrCO 3, SiO 2with high-purity CeO 2(99.99%), add after appropriate ethanol fully grinds, grind one minute after drying, load in crucible at 1250 DEG C of reducing atmosphere H 2/ N 2sinter 8h under (20%/80%), take out after cooling, after grinding, can final product be obtained.
Embodiment 2
Material is chosen according to chemical formula Ca 1.60sr 0.35si 0.7o 4: Ce 0.05/ 0.30Al, takes analytically pure CaCO respectively according to its molar percentage 3, SrCO 3, SiO 2, Al (OH) 3with high-purity CeO 2(99.99%), add after appropriate ethanol fully grinds, grind one minute after drying, load in crucible at 1250 DEG C of reducing atmosphere H 2/ N 2sinter 8h under (20%/80%), take out after cooling, after grinding, can final product be obtained.
Embodiment 3
Material is chosen according to chemical formula Ca 1.60sr 0.35si 0.7o 4: Ce 0.05/ 0.30Ga, takes analytically pure CaCO respectively according to its molar percentage 3, SrCO 3, SiO 2, Ga 2o 3with high-purity CeO 2(99.99%), add after appropriate ethanol fully grinds, grind one minute after drying, load in crucible at 1250 DEG C of reducing atmosphere H 2/ N 2sinter 8h under (20%/80%), take out after cooling, after grinding, can final product be obtained.
Embodiment 4
Material is chosen according to chemical formula Ca 1.60sr 0.35si 0.7o 4: Ce 0.05/ 0.30B, takes analytically pure CaCO respectively according to its molar percentage 3, SrCO 3, SiO 2, H 3bO 3with high-purity CeO 2(99.99%), add after appropriate ethanol fully grinds, grind one minute after drying, load in crucible at 1300 DEG C of reducing atmosphere H 2/ N 2sinter 8h under (20%/80%), take out after cooling, after grinding, can final product be obtained.
Embodiment 5
Material is chosen according to chemical formula Ca 1.65sr 0.34siO 4: Eu 0.01, take analytically pure CaCO respectively according to its molar percentage 3, SrCO 3, SiO 2with high-purity Eu 2o 3(99.99%), add after appropriate ethanol fully grinds, grind one minute after drying, load in crucible at 1250 DEG C of reducing atmosphere H 2/ N 2sinter 8h under (20%/80%), take out after cooling, after grinding, can final product be obtained.
Embodiment 6
Material is chosen according to chemical formula Ca 1.60sr 0.34siO 4: Eu 0.01, Ce 0.05, take analytically pure CaCO respectively according to its molar percentage 3, SrCO 3, SiO 2with high-purity Eu 2o 3(99.99%), CeO 2(99.99%), add after appropriate ethanol fully grinds, grind one minute after drying, load in crucible at 1100 DEG C of reducing atmosphere H 2/ N 2sinter 10h under (20%/80%), take out after cooling, after grinding, can final product be obtained.
Known see Fig. 1-Fig. 3, the blue Ca prepared by above-described embodiment 1.65-ysr 0.35si 1-zo 4: Ce y/ L zexcite wider, the position of excitation peak is about 370nm, is more suitable for mating ultraviolet chip.The green Ca of preparation 1.65sr 0.35-xsiO 4: Eu xfluorescent material and (Ba, Sr) 2siO 4compare, excite wider can better and ultraviolet/near-ultraviolet light LED chip match.Simultaneously under 365nm excites, the emission peak launching the strongest sample is the broadband emission being positioned at 436 and 508nm respectively.The position of blue colour fluorescent powder emission peak and halfwidth can increase along with the increase of the content of L.And its emissive porwer can strengthen under some L doping condition.The emission peak positions of green emitting phosphor is at about 510nm, and its halfwidth is about 87nm.
Embodiment 7
Material is chosen according to chemical formula Ca 1.60sr 0.35si 0.80o 4: Ce 0.05, Al 0.10, Ga 0.10analytically pure CaCO is taken respectively according to its molar percentage 3, SrCO 3, SiO 2, Ga 2o 3, Al (OH) 3with high-purity CeO 2(99.99%), add after appropriate ethanol fully grinds, grind one minute after drying, load in crucible at 1200 DEG C of reducing atmosphere H 2/ N 2sinter 9h under (20%/80%), take out after cooling, after grinding, can final product be obtained.
Embodiment 8
Material is chosen according to chemical formula Ca 1.60sr 0.35si 0.70o 4: Ce 0.05, Al 0.10, Ga 0.10,b 0.10analytically pure CaCO is taken respectively according to its molar percentage 3, SrCO 3, SiO 2, Ga 2o 3, Al (OH) 3, H 3bO 3with high-purity CeO 2(99.99%), add after appropriate ethanol fully grinds, grind one minute after drying, load in crucible at 1250 DEG C of reducing atmosphere H 2/ N 2sinter 9h under (20%/80%), take out after cooling, after grinding, can final product be obtained.
White light LEDs indigo plant/the green emitting phosphor of ultraviolet/near ultraviolet excitation not prepared by all the other embodiments, as long as chemical constitution is Ca 1.65-ysr 0.35-xsi 1-zo 4: Eu x, Ce y/ L z, in formula, x=0.001-0.08, y=0.001-0.15, z=0-0.5, L are one or more in Al, Ga and B.Indigo plant/the green emitting phosphor meeting above-mentioned condition all can prepare under condition disclosed in above-described embodiment, will not enumerate here.
Obviously, above-described embodiment is only for clearly example being described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And thus the apparent change of extending out or variation be still among the protection domain of the invention.

Claims (5)

1. be applicable to white light LEDs indigo plant/green emitting phosphor of ultraviolet/near ultraviolet excitation, it is characterized in that, its chemical constitution is: Ca 1.65-ysr 0.35-xsi 1-zo 4: Eu x, Ce y/ L z, in formula, x=0.001-0.08, y=0.001-0.15, z=0-0.5, L are one or more in Al, Ga and B.
2. the preparation method being applicable to the white light LEDs indigo plant/green emitting phosphor of ultraviolet/near ultraviolet excitation according to claim 1, is characterized in that, comprise the following steps:
Material is chosen according to chemical formula Ca 1.65-ysr 0.35-xsi 1-zo 4: Eu x, Ce y/ L zanalytically pure CaCO is taken respectively according to its molar percentage 3, SrCO 3, SiO 2, Al (OH) 3, Ga 2o 3and H 3bO 3in one or more, and high-purity CeO 2and/or Eu 2o 3, then add appropriate ethanol and fully grind post-drying, then grind, in reducing atmosphere H at temperature of reaction is 1100-1300 DEG C 2/ N 2lower sintering 8-10h, takes out after cooling, can obtain final product.
3. preparation method according to claim 2, is characterized in that, the described time of grinding again is 1 minute.
4. preparation method according to claim 2, is characterized in that, described temperature of reaction is 1200-1250 DEG C, and sintering time is 8h.
5. preparation method according to claim 2, is characterized in that, described H 2/ N 2per-cent be 20%:80%.
CN201510427130.8A 2015-07-20 2015-07-20 Blue/green fluorescent powder suitable for ultraviolet light/near ultraviolet light excitated white LED and preparation method for blue/green fluorescent powder Pending CN105154073A (en)

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Publication number Priority date Publication date Assignee Title
CN107358780A (en) * 2017-07-30 2017-11-17 王旭兰 Intelligent electric spark detection warning system based on PN junction chip and preparation method thereof
CN107603605A (en) * 2017-09-30 2018-01-19 五邑大学 A kind of white light LEDs blue green luminescent material suitable for ultraviolet/near ultraviolet excitation
CN111994914A (en) * 2020-08-10 2020-11-27 苏州鼎安科技有限公司 Ion co-doped beta-dicalcium silicate powder, preparation method and application

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107358780A (en) * 2017-07-30 2017-11-17 王旭兰 Intelligent electric spark detection warning system based on PN junction chip and preparation method thereof
CN107358780B (en) * 2017-07-30 2020-01-03 王旭兰 Intelligent electric spark detection alarm system based on PN junction chip and preparation method thereof
CN107603605A (en) * 2017-09-30 2018-01-19 五邑大学 A kind of white light LEDs blue green luminescent material suitable for ultraviolet/near ultraviolet excitation
CN111994914A (en) * 2020-08-10 2020-11-27 苏州鼎安科技有限公司 Ion co-doped beta-dicalcium silicate powder, preparation method and application
CN111994914B (en) * 2020-08-10 2023-11-28 苏州鼎安科技有限公司 Ion co-doped beta-dicalcium silicate powder, preparation method and application

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