CN102504814A - Direct white light fluorescent material excited by ultraviolet light and preparation method and application thereof - Google Patents
Direct white light fluorescent material excited by ultraviolet light and preparation method and application thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 71
- YUZILKLGVPUFOT-YHPRVSEPSA-L disodium;5-[(6-anilino-4-oxo-1h-1,3,5-triazin-2-yl)amino]-2-[(e)-2-[4-[(6-anilino-4-oxo-1h-1,3,5-triazin-2-yl)amino]-2-sulfonatophenyl]ethenyl]benzenesulfonate Chemical compound [Na+].[Na+].C=1C=C(\C=C\C=2C(=CC(NC=3NC(NC=4C=CC=CC=4)=NC(=O)N=3)=CC=2)S([O-])(=O)=O)C(S(=O)(=O)[O-])=CC=1NC(N1)=NC(=O)N=C1NC1=CC=CC=C1 YUZILKLGVPUFOT-YHPRVSEPSA-L 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 53
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 239000011521 glass Substances 0.000 claims abstract description 14
- 229910052582 BN Inorganic materials 0.000 claims abstract description 9
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 5
- 239000002131 composite material Substances 0.000 claims abstract description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 9
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 229910052753 mercury Inorganic materials 0.000 abstract description 2
- 230000005284 excitation Effects 0.000 description 13
- 238000001228 spectrum Methods 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000007669 thermal treatment Methods 0.000 description 8
- 229910003564 SiAlON Inorganic materials 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 241001062009 Indigofera Species 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000000695 excitation spectrum Methods 0.000 description 3
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
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- 230000001105 regulatory effect Effects 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 229910017639 MgSi Inorganic materials 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910002795 Si–Al–O–N Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 239000003086 colorant Substances 0.000 description 1
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- -1 rare earth ion Chemical class 0.000 description 1
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- 239000002994 raw material Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
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Abstract
The invention discloses a direct white light fluorescent material excited by ultraviolet light and a preparation method and an application thereof. The material adopts a composite material comprising yellow fluorescent powder and amorphous glass phase; and the amorphous glass phase is covered on the surfaces of yellow fluorescent powder particles and is formed by performing heat treatment of the nanometer oxide and the yellow fluorescent powder. The preparation method comprises the following steps: the yellow fluorescent powder and the nanometer oxide are weighed in proportion, uniformly mixed and then put into a boron nitride pot; and the yellow fluorescent powder and the nanometer oxide are conducted to heat treatment in a nitrogen atmosphere, cooled and ground. As the fluorescent material adopts single fluorescent material which can emit blue light and yellow light at the same time, the fluorescent material can be applied to ultraviolet base white light LED (light-emitted diode) and mercury discharge ultraviolet light excited white light emitting devices. In addition, the method is not only simple in the preparation process and is suitable for large-scale production, but also can obtain direct white light for emitting, with different color temperatures, and has industrial application prospect and value.
Description
Technical field
The present invention relates to a kind of direct white light fluorescent material of ultraviolet excitation, belongs to the photovaltaic material technical field.
Background technology
Under global low-carbon (LC), energy-conservation overall background, the illumination of efficient reduce power consumption, show that white light parts has received the very big concern of various countries.Europe, Japan announce to adopt electricity-saving lamp or white light LEDs to replace the incandescent light of high energy consumption in succession.Incandescent light is a kind of heat radiation light source, and 95% energy is that the form with heat has lost.And electricity-saving lamp and white light LEDs are cold light sources, have efficient, low in power consumption, particularly white light LEDs and also have long service life, pollution-free, advantage such as volume is little.Electricity-saving lamp and white light LED part all are under a kind of irradiation of short-wavelength light, are converted to white light emission through fluor light.For example electricity-saving lamp is the ultraviolet ray excited three primary colors fluorescent powder of emitting with mercury vapor discharge, and white light LEDs modal be to excite yellow fluorescent powder with the InGaN blue chip.
Usually need excite three kinds of fluorescent material of red, green, blue with the ultraviolet LED chip in order to obtain the high-color rendering low color temperature white light LED.Yet, adopt the mixed light conversion of white light technology of many components fluor to come with some shortcomings like this, such as: the specific refractory power of each composition fluorescent grain of micron order is inconsistent, causes the propagation attenuation of photon energy between different crystalline lattice; The absorption of each composition fluor, excite with emmission spectrum, light decay and efficient inconsistently, cause the colour stability of device poor; Directly there is the re-absorbed problem of light in each composition fluorescent powder grain; And complicated mixed powder craft problem.To above-mentioned background, adopt direct white light (single-phase panchromatic or single-phase white) fluorescent material effectively to overcome and mix the problem that the whitewash optical tech exists, be a kind of innovation that tradition is mixed the whitewash optical tech.Therefore the research that is used for the direct white light fluorescent material of burst of ultraviolel of white light LEDs and electricity-saving lamp becomes a research focus of field of light emitting materials and has obtained extensive studies.
Reported be suitable for ultraviolet excitation single mutually directly the white light fluorescent material have a lot, for example: application number is that in the Chinese invention patent of CN200910087495 a kind of its ingredient formula to be provided be Ca
1-xPr
xMO
4The white emitting fluorescent powder of single component, under the exciting of single excitaton source, lighting system can be sent the white light of low colour temperature; Application number is the preparation method that the single white emitting fluorescent powder of a kind of ultraviolet excitation is provided in the Chinese invention patent of CN 200710170433, and the structural formula of fluorescent material is Sr
1-xEu
xZn
2-yMn (PO
4)
2Application number is that in the Chinese invention patent of CN 200510016743 a kind of expression formula to be provided be Eu
XySr
Y-xyMgSi
zO
2x+y+1White emitting fluorescent powder.Can find out from prior art, at present the color matching strategy of emission white light and the research of material system are variation, the direct white light emission system of indigo plant+yellow two waveband based on multiple luminescence center is wherein arranged; Based on Eu
2+-Mn
2+Mix the red+direct white light emission system of green+blue (or indigo plant+Huang) of transmission ofenergy altogether; Based on the whole color fluorescent material of conjugation rare earth ion to an electronic migration; Synthesize the direct white light emission that accompanying impurities is realized mutually based on original position; Based on direct white light fluorescent material system of mixing valency Eu codoped or the like.Industrial community and each big research institution have given great attention to the direct white light fluorescent material of burst of ultraviolel, are particularly thought to obtain the developing direction of high-color rendering, white light LED part that colour temperature is adjustable by industry with the direct white light fluorescent material of ultraviolet chips incorporate.
Summary of the invention
The technical problem that the present invention will solve provides a kind of direct white light fluorescent material of ultraviolet excitation.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is following:
A kind of direct white light fluorescent material of ultraviolet excitation; It is a kind of matrix material by yellow fluorescent powder and amorphous glass phase composite; Described amorphous glass is coated on the particle surface of yellow fluorescent powder mutually, is to be formed through thermal treatment by nano-oxide and yellow fluorescent powder.
Further, the composition general formula of described yellow fluorescent powder is Ca
M/2Si
12-m-nAl
M+nO
nN
16-n: Eu
x, 0＜m wherein≤3,0＜n≤1.5,0.005≤x≤0.2.
Further, the composition general formula of described yellow fluorescent powder is Ca
1-xSi
9Al
3ON
15: Eu
x, 0.005≤x wherein≤0.2.
Further, described nano-oxide is nanometer SiO
2, nanometer A1
2O
3, nanometer B
2O
3In any one or a few mixture.
A kind of direct white light Preparation of Fluorescent Material method of described ultraviolet excitation comprises the steps: to take by weighing in proportion yellow fluorescent powder and nano-oxide, and uniform mixing is placed in the boron nitride crucible, in nitrogen atmosphere, heat-treats, and cooling is ground.
The mass ratio of described yellow fluorescent powder and nano-oxide is recommended as 1: 0.01～and 1: 2, be preferably 1: 0.1～1: 1.
Described heat-treat condition is recommended as at 1200～1500 ℃ and handled 30～100 minutes.
Because material of the present invention is under the exciting of the UV-light of 250～420nm; Can launch the blue light of 380～460nm and the orange light of 470～600nm simultaneously; And then be mixed into white light; For direct white light fluorescent material, therefore, can be applicable in the white light emitting device of ultraviolet base white light LEDs and mercury discharge ultraviolet excitation.
Because fluorescent material provided by the invention is a kind of single fluorescent material that can launch blue light and gold-tinted simultaneously; Therefore than adopting ultraviolet excitation red, green, blue or indigo plant, the mixed whitewash light prior art of yellow multiple fluorescent material on micro-meter scale; The light that can overcome between different fluorescent powder grains heavily absorbs and complicated defect problems such as mixed powder craft; Not only technology is simple; Be fit to large-scale production; And can obtain the direct white light emission of different-colour, have prospects for commercial application and value.
Description of drawings
Fig. 1 is the yellow fluorescent powder (Ca of the different Eu doping contents of embodiment 1 preparation
1-xSi
9Al
3ON
15: Eu
x, x=0.02,0.04,0.06,0.08,0.10) and emmission spectrum under the ultraviolet excitation of 365nm;
Fig. 2 is the emmission spectrum of the direct white light fluorescent material formed of the difference of embodiment 2 preparation;
Fig. 3 reaches the XRD diffracting spectrum of the direct white light fluorescent material that under the different heat treatment temperature, prepares for embodiment 3 used yellow fluorescent powders;
The TEM of the direct white light fluorescent material that Fig. 4 prepares for embodiment 3, HRTEM photo and EDS ultimate analysis collection of illustrative plates.
Fig. 5 reaches the excitation spectrum and the emmission spectrum of the direct white light fluorescent material that under the different heat treatment temperature, prepares for embodiment 3 used yellow fluorescent powders;
Fig. 6 reaches the chromaticity coordinates figure of the direct white light fluorescent material that under the different heat treatment temperature, prepares for embodiment 3 used yellow fluorescent powders;
Fig. 7 reaches the emmission spectrum of the direct white light fluorescent material for preparing under the time in different heat treatment for embodiment 4 used yellow fluorescent powders;
Fig. 8 is the SEM photo of used yellow fluorescent powder (a) of embodiment 5 and the direct white light fluorescent material (b) for preparing.
Embodiment
The progress of substantive distinguishing features of the present invention and significance is described below in conjunction with specific embodiment and accompanying drawing.Should be understood that these embodiment only are used for the present invention is further specified, can not be interpreted as restriction protection domain of the present invention.The experimental technique of unreceipted actual conditions in the following example usually according to normal condition, for example is the condition in the workshop manual, or the condition of advising according to manufacturer.
Embodiment 1
According to Ca
1-xSi
9Al
3ON
15: Eu
xThe stoichiometric ratio of (x=0.02,0.04,0.06,0.08,0.10) accurately takes by weighing CaCO
3, Si
3N
4, AlN, Eu
2O
3, in dislocation boron nitride crucible behind the uniform mixing in the agate grinding, the concrete weight of various raw materials is as shown in table 1; Then boron nitride crucible is placed high frequency furnace, under nitrogen protection atmosphere,, obtain the yellow fluorescent powder of different Eu doping contents behind the naturally cooling, be designated as: Ca-SiAlON:Eu in 1700 ℃ of sintering reactions 2 hours
2+
Table 1
| Chemical formula | CaCO 3(g) | Si 3N 4(g) | AlN(g) | Eu 2O 3(g) |
| Ca 0.98Si 9Al 3ON 15:Eu 0.02 | 0.0901 | 1.7534 | 0.9225 | 0.0176 |
| Ca 0.96Si 9Al 3ON 15:Eu 0.04 | 0.1802 | 1.7534 | 0.9225 | 0.0352 |
| Ca 0.94Si 9Al 3ON 15:Eu 0.06 | 0.2703 | 1.7534 | 0.9225 | 0.0528 |
| Ca 0.92Si 9Al 3ON 15:Eu 0.08 | 0.3604 | 1.7534 | 0.9225 | 0.0704 |
| Ca 0.90Si 9Al 3ON 15:Eu 0.10 | 0.4504 | 1.7534 | 0.9225 | 0.0880 |
Fig. 1 is the yellow fluorescent powder (Ca of the prepared different Eu doping contents of present embodiment
1-xSi
9Al
3ON
15: Eu
x, x=0.02,0.04; 0.06; 0.08,0.10) and emmission spectrum figure under the ultraviolet excitation of 365nm, visible by Fig. 1: along with the increase of Eu doping content; Red shift has taken place in the emission peak of sample, has moved to the orange light of 575nm of doping content x=0.10 from the 555nm yellow green light of doping content x=0.02.
By present embodiment the yellow fluorescent powder that can obtain different emission through the doping content that changes Eu can be described.
The Ca that embodiment 1 is obtained
0.98Si
9Al
3ON
15: Eu
0.02Yellow fluorescent powder and nano-oxide (SiO
2, Al
2O
3, B
2O
3) in one or more by the certain mass ratio uniform mixing, concrete mass ratio is as shown in table 2; Material after mixing is put into boron nitride crucible, in high frequency furnace, handles 45 minutes in 1200 ℃ under the nitrogen protection atmosphere.Behind the naturally cooling, promptly obtain the direct white light fluorescent material of ultraviolet excitation.
Table 2
| Sequence number | Ca 0.98Si 9Al 3ON 15:Eu 0.02(g) | SiO 2(g) | Al 2O 3(g) | B 2O 3(g) |
| 1 | 0.200 | 0 | 0 | 0 |
| 2 | 0.200 | 0 | 0 | 0.065 |
| 3 | 0.200 | 0 | 0.075 | 0 |
| 4 | 0.200 | 0.075 | 0 | 0 |
| 5 | 0.200 | 0 | 0.075 | 0.065 |
| 6 | 0.200 | 0.075 | 0.065 | 0 |
| 7 | 0.200 | 0 | 0.040 | 0.052 |
| 8 | 0.200 | 0.075 | 0.075 | 0.065 |
Fig. 2 is the emmission spectrum figure of the direct white light fluorescent material of the prepared difference composition of present embodiment, and is visible by Fig. 2: as not add the sample of nano-oxide, show the luminosity of yellow fluorescent powder; But added the sample of nano-oxide, blue emission peak in various degree occurred in 400～480nm zone, with Ca
0.98Si
9Al
3ON
15: Eu
0.02Yellow emission mix, and then obtain direct white light.
Can be explained that by present embodiment the fluorescent material that the present invention obtains can be launched blue light and gold-tinted simultaneously under the exciting of UV-light, and then mix the acquisition white light, be direct white light fluorescent material.
Take by weighing 0.60 gram Ca
0.98Si
9Al
3ON
15: Eu
0.02Yellow fluorescent powder and 0.225 gram nanometer SiO
2Be divided into 3 parts behind the uniform mixing and put into 3 boron nitride crucibles, in high frequency furnace, handled 45 minutes respectively at 1200 ℃, 1300 ℃, 1400 ℃ under the nitrogen protection atmosphere, behind the naturally cooling, obtain direct white light fluorescent material.
Fig. 3 reaches the XRD diffracting spectrum of the direct white light fluorescent material that under the different heat treatment temperature, prepares for the used yellow fluorescent powder of present embodiment; Visible by Fig. 3: Ca
0.98Si
9Al
3ON
15: Eu
0.02Yellow fluorescent powder is a typical C a-SiAlON structure, and the direct white light fluorescent material that obtains under the subzero treatment still keeps the Ca-SiAlON structure, along with the increase of thermal treatment temp, a spot of Si occurred
2N
2The diffraction peak of O impurity phase.The intensity step-down of the diffraction peak of the sample after all are handled, the percent crystallinity of interpret sample reduces, and has in other words occurred the amorphous glass phase in the sample, has formed yellow Ca-SiAlON fluorescent material and amorphous glass phase composite materials.
The TEM of the direct white light fluorescent material that Fig. 4 prepares for present embodiment, HRTEM photo and EDS ultimate analysis collection of illustrative plates.Can find out that by HRTEM coat the tangible amorphous glass phase of one deck on the crystal grain surface, the electron diffraction analysis result shows that crystal grain is Ca-SiAlON crystalline phase (being the yellow fluorescent powder that we prepare).Find that through the crystal grain of inside and the constituency EDS ultimate analysis of surface coated amorphous glass layer their composition all is Ca-Si-Al-O-N, this explanation amorphous glass is not by nanometer SiO mutually
2Simply be coated on the particle surface of fluorescent material, but the back forms through incorporating into the mutual diffusion mutually on fluorescent powder grain surface.In addition, the Si-O composition of amorphous glass phase will be higher than the corresponding composition of inner crystalline phase, and this has just explained that the formation of amorphous glass phase is because SiO
2Incorporate into and cause.
Fig. 5 reaches the excitation spectrum and the emmission spectrum figure of the direct white light fluorescent material that under the different heat treatment temperature, prepares for the used yellow fluorescent powder of present embodiment; Visible by Fig. 5: along with the rising of thermal treatment temp, the direct white light fluorescent material for preparing strengthens at the blue-light-emitting peak of 400～480nm, reduces at the Yellow luminous peak of 480～600nm.When thermal treatment temp was 1400 ℃, the blue emission peak of the direct white light fluorescent material for preparing accounted for leading; From excitation spectrum, the PLE of blue emission and the PLE of yellow emission have well overlapping in 250～400nm UV-light zone, explain that the material of preparation can be launched blue light and gold-tinted simultaneously with ultraviolet excitation, and then mix the acquisition white light.
Fig. 6 reaches the chromaticity coordinates figure of the direct white light fluorescent material that under the different heat treatment temperature, prepares for the used yellow fluorescent powder of present embodiment; Visible by Fig. 6: Ca
0.98Si
9Al
3ON
15: Eu
0.02The chromaticity coordinates of yellow fluorescent powder drops on the gold-tinted zone, and along with the rising of thermal treatment temp, directly the chromaticity coordinates of white light fluorescent material moves toward white light field.When thermal treatment temp is 1300 ℃; The chromaticity coordinates of the direct white light fluorescent material for preparing is (0.33,0.36), near equal-energy white luminous point (0.33; 0.33); And when thermal treatment temp was 1400 ℃, the chromaticity coordinates of the direct white light fluorescent material for preparing had moved to blue white light field, explained that the blue light ingredient of this moment is too much.
Can explain through regulating thermal treatment temp, the direct white light fluorescent material that can obtain to have different photochromic performances by present embodiment.
Embodiment 4
Take by weighing 0.60 gram Ca
0.98Si
9Al
3ON
15: Eu
0.02Yellow fluorescent powder and 0.225 gram nanometer SiO
2, be divided into 3 parts behind the uniform mixing and put into 3 boron nitride crucibles, in high frequency furnace, handled respectively 30 minutes, 45 minutes, 60 minutes in 1300 ℃ under the nitrogen protection atmosphere, behind the naturally cooling, obtain direct white light fluorescent material.
Fig. 7 reaches the emmission spectrum figure of the direct white light fluorescent material for preparing under the time in different heat treatment for the used yellow fluorescent powder of present embodiment; Visible by Fig. 7: along with the increase of heat treatment time; The blue emission peak of the direct white light fluorescent material for preparing strengthens; And the yellow emission peak weakens, and explains through regulating the color quality that heat treatment time can change white light emission.
Embodiment 5
Take by weighing 0.20 gram Ca
0.98Si
9Al
3ON
15: Eu
0.02Yellow fluorescent powder and 0.07 gram property nanometer B
2O
3, uniform mixing is placed in the boron nitride crucible, under high frequency furnace nitrogen protection atmosphere, in 1400 ℃ of processing 30 minutes, behind the naturally cooling, obtains direct white light fluorescent material.
Fig. 8 is for the SEM photo of used yellow fluorescent powder (a) of present embodiment and the direct white light fluorescent material (b) for preparing, and is visible by Fig. 8: Ca
0.98Si
9Al
3ON
15: Eu
0.02The yellow fluorescent powder grain diameter is about 2～3 microns; And about about 5 microns of the grain diameter of the direct white light fluorescent material for preparing, this be since mutual diffusion mutually between nano-oxide and the yellow fluorescent powder surface and the amorphous glass of incorporating formation into to be coated on the yellow fluorescent powder particle surface mutually caused.
Claims (10)
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| CN106883842A (en) * | 2017-02-24 | 2017-06-23 | 河北利福光电技术有限公司 | A kind of highly reliable silicate fluorescent powder and its surface modification method |
| CN106883842B (en) * | 2017-02-24 | 2019-12-06 | 河北利福光电技术有限公司 | High-reliability silicate fluorescent powder and surface modification method thereof |
| CN110118312A (en) * | 2018-02-07 | 2019-08-13 | 深圳光峰科技股份有限公司 | Wavelength converter |
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| CN102504814B (en) | 2013-11-20 |
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