CN110234736A - A kind of fluorescent material and its made light emitting device - Google Patents
A kind of fluorescent material and its made light emitting device Download PDFInfo
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- CN110234736A CN110234736A CN201880008182.3A CN201880008182A CN110234736A CN 110234736 A CN110234736 A CN 110234736A CN 201880008182 A CN201880008182 A CN 201880008182A CN 110234736 A CN110234736 A CN 110234736A
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- fluorescent material
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- 239000000463 material Substances 0.000 title claims abstract description 55
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 12
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 9
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 9
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 8
- 229910052788 barium Inorganic materials 0.000 claims abstract description 5
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 5
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 4
- 229910052796 boron Inorganic materials 0.000 claims abstract description 4
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 4
- 229910020068 MgAl Inorganic materials 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 3
- 239000004065 semiconductor Substances 0.000 claims description 2
- 230000005284 excitation Effects 0.000 abstract description 11
- 239000004973 liquid crystal related substance Substances 0.000 abstract description 3
- 239000000843 powder Substances 0.000 description 6
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
- 238000000695 excitation spectrum Methods 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002284 excitation--emission spectrum Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 238000005303 weighing 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
- C09K11/62—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing gallium, indium or thallium
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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
- C09K11/63—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing boron
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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
- C09K11/64—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing aluminium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
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Abstract
The present invention provides a kind of fluorescent material and its made light emitting devices.The group of the fluorescent material is divided into xABmOn·y(aAl2O3BAlN), wherein, two or more combination of the A in Ca, Sr, Ba, Mg, Zn, Mn, Si element, and Mn element must be contained, B is selected from the combination of one or more of Al, B, Ga element, and 1.8≤m≤2.2,3.5≤n≤4.5,0.5≤x≤1,0.22≤b≤0.35, x+y=1, a+b=1.Fluorescent material of the invention can issue the green light between 510-540nm, and excitation purity is high, is expected to meet the application demand of high colour gamut liquid crystal display white LED device under 400~470nm excitation.
Description
The application requires the priority of the Chinese patent application based on the Chinese patent application proposition application No. is the 201711159723.6, applying date on November 20th, 2017, and the application is incorporated herein as reference in the full content of the Chinese patent application.
The present invention relates to a kind of fluorescent material and its made light emitting devices, belong to white light LEDs illumination field.
White light LEDs have the advantages such as green, environmental protection, long-life, are widely used in illumination and display field.At present for the producing method of white light LEDs, mainly based on the implementation of chip cooperation fluorescent powder.Therefore, the luminescent properties of fluorescent powder directly affect and determine the performance of white light LED part.
In recent years, one kind is with high-melting-point, stiff stability, the adjustable MgAl of optical band gap
2O
4Or ZnAl
2O
4For luminous host, with Mn
2+For the novel MgAl of activator
2O
4:Mn
2+Or ZnAl
2O
4:Mn
2+Fluorescent powder is concerned, such as: using Mn
2+The MgAl of activation
2O
4、ZnAl
2O
4Green light can be issued in the wavelength region of 510-540nm by the light excitation by the ultraviolet wide range of wavelengths to blue light, and excitation purity is high.Therefore, as the fluorophor that can be used for white light LEDs, deep explore and study has been carried out to it.As US20060243197A1 discloses transient metal Mn doped MgAl
2O
4Fluorescent material, preparation method and the laser equipment containing it.Wherein, Mg
1-xMn
xAlO
4(0.003≤x≤0.01) realizes the green emitting of 520nm under the blue light excitation of 450nm.Jiao Xuechen et al. has researched and developed a series of MgAl
2O
4:xMn
2+Fluorescent material, under the blue light excitation of 450nm, Mn
2+Occur
4T
1→
6A
1Transition realizes that green emitting, transmitting light reach maximum luminousing brightness (Chinese of journal of luminescence, 2011,32,1139-1142) when x is 10% content.It is the Zn doped with metal nanoparticle that CN103849383A, which provides chemical formula,
1-xAl
2O
4:Mn
2+ x(0 x≤0.1 <) luminescent material, passes through the luminescent properties of metal nano particle-doped reinforcing material.
However, limiting MgAl at present
2O
4:Mn
2+Or ZnAl
2O
4:Mn
2+The outstanding problem of fluorescent material application is still that its luminous efficiency is low.
Summary of the invention
For this purpose, the fluorescent material has more preferably Photochromic Properties one of the objects of the present invention is to provide a kind of fluorescent material.
In order to achieve the above object, the present invention adopts the following technical scheme:
The chemical formula of a kind of fluorescent material, the substance is following formula I:
xAB
mO
n·y(aAl
2O
3·bAlN) I
Wherein two or more combination of the A in Ca, Sr, Ba, Mg, Zn, Mn, Si element, and Mn element must be contained；
B is selected from the combination of one or more of Al, B, Ga element；
And 1.8≤m≤2.2,3.5≤n≤4.5,0.5≤x≤1,0.22≤b≤0.35, x+y=1, a+b=1.
Fluorescent material of the invention can issue the green light between 510-540nm, and excitation purity is high, is expected to meet the application demand of high colour gamut liquid crystal display white LED device under 400~470nm excitation.
Preferably, the fluorescent material has and MgAl
2O
4Identical crystal structure.
Preferably, A is Mn and Zn element or Mn and Mg element.By by MgAl
2O
4:Mn
2+Or ZnAl
2O
4:Mn
2+(the aAl of fluorescent material and similar structure and luminescent properties
2O
3BAlN) fluorescent material carries out two-phase solid solution, the fluorescent material of more high brightness is formed, to meet the application demand of high colour gamut liquid crystal display white LED device.
Preferably, molar percentage z of the Mn element in element A meets 0.1%≤z≤20%.
Preferably, B is Al element.
Preferably, 0.38≤b/a≤0.44.
Preferably, A contains Si element.Ca, Sr, Ba in fluorescent powder of the invention, in A, Mg, Zn are diads, and occupy the position B (such as B, the Al of trivalent, Ga), the Si that therefore will cause vacancy, therefore add tetravalence in A can play the role of valence state balance, to keep the performance that fluorescent powder is made more excellent.
Preferably, molar percentage d of the Si element in element A meets 10%≤d≤50%.
Preferably, A is Si, Mn and Zn element or Si, Mn and Mg element.
Preferably, molar percentage z of the Mn element in element A meets 0.1%≤z≤20%.
Preferably, B is Al element.
Preferably, 0.38≤b/a≤0.44.
The prior art can be used in the preparation method of fluorescent material of the invention or in the future prepared by the new technology of discovery.
Such as fluorescent material of the invention can be used following method and be prepared: by Al
2O
3、AlN、MnCO
3And other respective metal oxides or metal carbonate mixed after roast under an inert atmosphere；Product of roasting is crushed, is classified, post-process after obtain fluorescent material of the present invention.
Other respective metal oxides or metal carbonate can be determined according to the selected element of A, B, and if A also contains Mg, when B is Al, then other above-mentioned respective metal oxides are MgO or MgCO
3, when also containing Si such as A, then other above-mentioned respective metal oxides are SiO
2。
The temperature of roasting can be 1600-2000 DEG C, and preferably 1800 DEG C, the time of roasting is 2h or more, preferably 4h.The pressure of roasting can be 0.3-0.8Mpa, preferably 0.5Mpa.
It roasts in a preferred embodiment under an inert atmosphere, under 1800 DEG C of temperature, the pressure of 0.5Mpa roast 4h.
An object of the present invention, which also resides in, provides a kind of light emitting device, and the light emitting device includes excitaton source and fluorescent material of the present invention, and the excitaton source is that launch wavelength range is 400~430nm or the semiconductor chip of 430~470nm.
Fluorescent material xAB of the invention
mO
n·y(aAl
2O
3BAlN it) can be excited in the large-scale wavelength region of 400-470nm and issue green light, and regulated and controled by solid solubility (x and y value) linkage between two-phase fluorescent material, it can be obviously improved the luminous intensity of fluorescent material, with green emitting phosphor be highly beneficial as white light LED part.Fluorescent material good thermal stability of the invention can come individually or with other phosphor combinations for various light-emitting components, particularly using ultraviolet LED or blue led as the white light LEDs of light source.
Fig. 1 is the XRD spectrum for the fluorescent material that the embodiment of the present invention 1 obtains；
Fig. 2 is the excitation spectrum and emission spectrum for the fluorescent material that the embodiment of the present invention 1 obtains.
Fluorescent material of the invention is further illustrated as embodiment below, it will help further understanding of the invention, protection scope of the present invention are not limited to the examples, and protection scope is determined by claims.
In order to overcome MgAl
2O
4:Mn
2+Or ZnAl
2O
4:Mn
2+The low outstanding problem of luminous efficiency in fluorescent material application, the present invention provides fluorescent materials a kind of novel and with higher photoluminescence efficiency.Fluorescent material in the present invention is with general formula xAB
mO
n·y(aAl
2O
3BAlN) the two-phase solid solution indicated, wherein two or more combination of the A in Ca, Sr, Ba, Mg, Zn, Mn, Si element, and Mn element must be contained, B is selected from the combination of one or more of Al, B, Ga element, preferably one or two kinds of, and 1.8≤m≤2.2,3.5≤n≤4.5,0.5≤x≤1,0.22≤b≤0.35, x+y=1, a+b=1.The fluorescent material preferably has and MgAl
2O
4Identical crystal structure.
Based on the above invention, made experiment and effect are as described in specific embodiment, and wherein test condition is as follows:
Test condition:
Blue light with wavelength for 460nm excites the fluorescent material in embodiment 1, and measures intensity of emission spectra and the relative luminous brightness of fluorescent material.
The test of XRD is carried out with Co target (λ=1.78892nm), operating voltage 40kV, operating current 40mA.
Comparative example 1
40g MgO, 101.96g Al are weighed according to stoichiometric ratio
2O
3With 3.44g MnCO
3And it is mixed；By said mixture under an inert atmosphere, 1450 DEG C of roasting temperature 4h；The fluorescent material MgAl of comparative example 1 is obtained after above-mentioned product of roasting is crushed, is classified, is post-processed
2O
4: 0.03Mn
2+。
Comparative example 2
30g ZnO, 37.58g Al are weighed according to stoichiometric ratio
2O
3With 1.69g MnCO
3It is mixed；By said mixture under an inert atmosphere, 1750 DEG C of roasting temperature 2h；The fluorescent material ZnAl of comparative example 2 is obtained after above-mentioned product of roasting is crushed, is classified, is post-processed
2O
4: 0.04Mn
2+。
Embodiment 1
Accurately weigh 115.21g Al
2O
3,18.45g AlN,20.69g MnCO
3And 7.25g MgO is mixed；Said mixture is roasted into 4h under an inert atmosphere, under 1800 DEG C of temperature, the pressure of 0.5Mpa；The fluorescent material 0.6MgMn of embodiment 1 is obtained after above-mentioned product of roasting is crushed, is classified, is post-processed
0.15Al
2O
4·0.4(0.72Al
2O
3·0.28AlN)。
As shown in Figure 1, excitation and emission spectra is as shown in Figure 2 (wherein excitation wavelength is 460nm, and the Detection wavelength of excitation spectrum is 520nm) by XRD of the above-mentioned fluorescent material under Co target (λ=0.178892nm) test condition.It will be seen from figure 1 that material made from the embodiment of the present invention 1 is 0.6MgMn
0.15Al
2O
4·0.4(0.72Al
2O
30.28AlN) fluorescent material, Fig. 2 then can be seen that material made from embodiment 1 can emit the light of 520nm under the excitation of 460nm.
Embodiment 2-15
According to step shown in embodiment 1, the raw material for weighing corresponding chemical metering ratio is roasted and is post-processed, and obtains corresponding phosphor substance shown in embodiment 2-15.
The composition of fluorescent powder is shown in Table 1, and the test result of light emission luminance and Emission Spectrum Peals wavelength is shown in Table 2.
Fluorescent material ingredient prepared by table 1.
The luminescent properties of 2 fluorescent material of table
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.For those of ordinary skill in the art, other different forms of changes or modifications may be made based on the above description.There is no necessity and possibility to exhaust all the enbodiments.And obvious changes or variations extended from this are still within the protection scope of the invention.
Claims (10)
- A kind of fluorescent material, which is characterized in that the chemical formula of the substance is following formula I:xAB mO n·y(aAl 2O 3·bAlN) IWherein two or more combination of the A in Ca, Sr, Ba, Mg, Zn, Mn, Si element, and Mn element must be contained；B is selected from the combination of one or more of Al, B, Ga element；And 1.8≤m≤2.2,3.5≤n≤4.5,0.5≤x≤1,0.22≤b≤0.35, x+y=1, a+b=1.
- Fluorescent material according to claim 1, which is characterized in that the fluorescent material has MgAl 2O 4Same crystal structure.
- Fluorescent material according to claim 1 or claim 2, which is characterized in that A is Mn and Zn element or Mn and Mg element.
- Fluorescent material according to claim 1 or claim 2, which is characterized in that A contains Si element.
- Fluorescent material according to claim 4, which is characterized in that molar percentage d of the Si element in element A meets 10%≤d≤50%.
- Any one of -5 fluorescent material according to claim 1, which is characterized in that A Si, Mn and Zn element or Si, Mn and Mg element.
- Any one of -6 fluorescent material according to claim 1, which is characterized in that B is Al element.
- Any one of -7 fluorescent material according to claim 1, which is characterized in that molar percentage z of the Mn element in element A is to meet 0.1%≤z≤20%.
- Any one of -8 fluorescent material according to claim 1, which is characterized in that 0.38≤b/a≤0.44.
- A kind of light emitting device, which is characterized in that including excitaton source and the described in any item fluorescent materials of claim 1-9；Preferably, it is 400~430nm or the semiconductor chip of 430~470nm that excitaton source, which is launch wavelength range,.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2017111597236 | 2017-11-20 | ||
| CN201711159723 | 2017-11-20 | ||
| PCT/CN2018/115637 WO2019096204A1 (en) | 2017-11-20 | 2018-11-15 | Fluorescent substance and light-emitting device made therefrom |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110234736A true CN110234736A (en) | 2019-09-13 |
Family
ID=66538898
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201880008182.3A Withdrawn CN110234736A (en) | 2017-11-20 | 2018-11-15 | A kind of fluorescent material and its made light emitting device |
| CN201811363126.XA Active CN109810695B (en) | 2017-11-20 | 2018-11-15 | Fluorescent substance and light-emitting device made of same |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811363126.XA Active CN109810695B (en) | 2017-11-20 | 2018-11-15 | Fluorescent substance and light-emitting device made of same |
Country Status (2)
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|---|---|
| CN (2) | CN110234736A (en) |
| WO (1) | WO2019096204A1 (en) |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100589405B1 (en) * | 2003-11-20 | 2006-06-14 | 삼성에스디아이 주식회사 | A green emitting phosphor for vuvvacuum ultraviolet excited light emitting device, a preparation method thereof and a light emitting device comprising the same |
| CN101157854B (en) * | 2007-07-02 | 2010-10-13 | 北京宇极科技发展有限公司 | Oxynitrides luminescent material, preparation method and uses thereof |
| CN101781560B (en) * | 2010-03-23 | 2012-11-14 | 中国计量学院 | Fluorescent powder using silicon-aluminum base nitrogen oxides as base materials and preparation method thereof |
| CN102433114B (en) * | 2011-12-13 | 2015-06-10 | 北京晶创达科技有限公司 | Fluorescent powder, and preparation method and application thereof |
| CN108531166A (en) * | 2018-04-24 | 2018-09-14 | 武汉理工大学 | A kind of preparation method of the regulatable divalent manganesetion doping MgAlON green emitting phosphors of optical property |
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2018
- 2018-11-15 WO PCT/CN2018/115637 patent/WO2019096204A1/en active Application Filing
- 2018-11-15 CN CN201880008182.3A patent/CN110234736A/en not_active Withdrawn
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Also Published As
| Publication number | Publication date |
|---|---|
| CN109810695A (en) | 2019-05-28 |
| WO2019096204A1 (en) | 2019-05-23 |
| CN109810695B (en) | 2022-03-11 |
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Application publication date: 20190913 |