CN116004227A - Ultraviolet excited blue light emitting fluorescent powder and preparation method and application thereof - Google Patents
Ultraviolet excited blue light emitting fluorescent powder and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to ultraviolet excited blue light emitting fluorescent powder and a preparation method and application thereof. The blue light fluorescent powder belongs to AO-B 2 O 3 ‑SnO 2 ‑SiO 2 ‑Ce 2 O 3 A system, wherein A is one or more of Ca, sr and Ba; b is one or more of Ga and In, and the components of the B are as follows In mass percent of oxides: AO is more than or equal to 20.44% and less than or equal to 44.86%, B is more than or equal to 18.31% 2 O 3 ≤33.76％，20.29％≤SnO 2 ≤30.88％，13.49％≤SiO 2 ≤20.52％，0.11％≤Ce 2 O 3 Less than or equal to 0.468 percent. Compared with the prior art, the fluorescent powder disclosed by the invention is oxide-based fluorescent powder, has the outstanding advantages of stable physical and chemical properties, simplicity and convenience in preparation, low cost and the like, and is suitable for application of ultraviolet chip white light LEDs, ultraviolet chip solar light LEDs, ultraviolet chip full-spectrum LEDs, ultraviolet chip high-quality white light LEDs and the like.
Description
Technical Field
The invention belongs to the technical field of fluorescent powder preparation, and particularly relates to ultraviolet excited blue light emitting fluorescent powder and a preparation method and application thereof.
Background
In solid state lighting, white light emitting diodes (W-LEDs) have been widely used because of their high efficiency, low power consumption, small size, and the like. The common method for realizing white light at present is to combine an InGaN blue light chip with yellow fluorescent powder Y 3 Al 5 O 12 :Ce 3+ (YAG:Ce 3+ ) And (3) combining. However, the intense blue emission of blue chips can cause serious "blue hazards" that create health problems. An effective way to solve the problem is to select near ultraviolet and ultraviolet LED chips to replace blue light chips, so as to reduce the blue light emission intensity in the artificial light source. The emission wavelength of the InGaN chip has gradually developed to near ultraviolet region, which can provide larger excitation energy for fluorescent material, and further improve the light intensity of white light LED. And because ultraviolet light is invisible, the three-color (red, green and blue) fluorescent powder plays an important role in the color stability and the color rendering index of the white light LED. Therefore, the blue light fluorescent powder with strong absorption in the near ultraviolet region is synthesized and plays an important role in healthy illumination.
Meanwhile, with the development of the LED, the LED has higher requirements on the cost and stability of the fluorescent conversion material. Therefore, development of an oxide-based blue phosphor capable of being excited by ultraviolet/near ultraviolet and excellent in performance is critical to development of white LEDs. The luminescence characteristics of the phosphor are largely dependent on the crystal structure of the host material, and variations in the structure are liable to affect the energy transfer process, crystal field strength, and covalent properties. Thus Ce 3+ Blue light emitted by the doped phosphor begins to enter the human visual field, while Ce 3+ Is a rare earth ion with excellent luminescence property, and its electron base configuration is [ Xe ]]4f, its 4f orbit receives the electron shielding effect of the outer layer (5 d), the external environment is small to the influence of 4f orbit, and 5d orbit is exposed in the outermost layer, its electron is greatly influenced by crystal field environment, its f-d transition is the transition that the space name permits, the transition intensity is the hundred times of f-f transition, therefore has already been used in the phosphor material extensively.
The property can just meet the requirements of white light LEDs, sunlight-like LEDs, full-spectrum LEDs, high-color-rendering white LEDs and the like on spectrum continuity, no light spectrum loss and the like, and becomes a widely used rare earth activator. Due to Ce 3+ The 4f-5d transition of (2) shows strong absorption in the near ultraviolet wavelength range, and can emit blue light under the excitation of the near ultraviolet wavelength. And the spectrum of which is significantly changed with the composition and structure of the matrix material, thus Ce 3+ Ions have become important candidate doping ions for rare earth doped phosphors.
Disclosure of Invention
The invention provides ultraviolet excited blue light emitting fluorescent powder and a preparation method and application thereof, so as to meet the urgent requirements of the current white light LED/solar light-like LED/full-spectrum LED/healthy illumination LED light source.
The invention selects Ce 3+ As the luminescence center of the fluorescent powder, a novel unreported ultraviolet excitation Ce is synthesized 3+ Doped oxide base 471nm blue light emitting fluorescent material.
The aim of the invention can be achieved by the following technical scheme:
the invention provides ultraviolet excited blue light emitting fluorescent powder which is ultraviolet excited Ce 3+ Doped oxide-based 471nm blue light emitting phosphor, which is AO-B 2 O 3 -SnO 2 -SiO 2 -Ce 2 O 3 Wherein A is one or more of Ca, sr or Ba; b is one or more of Ga or In, and the mass percentage of the components is 20.44% or more and less than or equal to AO or less than or equal to 44.86% and 18.31% or less and less than or equal to B 2 O 3 ≤33.76％，20.29％≤SnO 2 ≤30.88％，13.49％≤SiO 2 ≤20.52％，0.11％≤Ce 2 O 3 ≤0.468％。
Preferably, the phosphor is AO-B 2 O 3 -SnO 2 -SiO 2 -Ce 2 O 3 Wherein A is one or more of Ca, sr or Ba; b is one or more of Ga or In, and the molar ratio of the component A to the component B to the component Sn to the component Si to the component Ce is (2.975-2.995:2:1.5:2.5:0.005-0.025).
Still further preferably, the phosphor is AO-B 2 O 3 -SnO 2 -SiO 2 -Ce 2 O 3 Wherein A is one or more of Ca, sr or Ba; b is one or more of Ga or In, wherein the mol ratio of component A to B to Si to Ce=2.995 to 1.5 to 2.5 to 0.005, or the mol ratio of component A to B to Si to Ce=2.99 to 2 to 1.5 to 2.5 to 0.01, or the mol ratio of component A to B to Si to Ce=2.985 to 2 to 1.5 to 2.5 to 0.015, or the mol ratio of component A to B to Sn to Si to Ce=2.98 to 2 to 1.5 to 2.5 to 0.02, or the mol ratio of component A to B to Sn to Si to Ce=2.975 to 2 to 1.5 to 2.5 to 0.025.
The ultraviolet excited blue light emitting fluorescent powder can emit blue light with a spectrum range covering 425-700 nm and a center wavelength at 471nm under ultraviolet excitation.
The invention further provides a preparation method of the ultraviolet excited blue light emitting fluorescent powder, which comprises the following steps:
(1) Weighing a proper amount of a compound containing A, a compound containing B, a compound containing Sn, a compound containing Si and a compound containing Ce as raw material powder;
(2) Grinding and uniformly mixing the mixture obtained in the step (1);
(3) Placing the ground raw material powder into an alumina crucible, calcining the alumina crucible filled with the raw material in an air atmosphere, and naturally cooling to room temperature;
(4) And (3) sufficiently grinding the mixed product obtained after calcining in the step (3) uniformly again, placing the mixed product in a reducing atmosphere mixed with hydrogen and nitrogen for sintering, and then cooling to room temperature to finally obtain the ultraviolet excited blue light emitting fluorescent powder.
In some embodiments of the invention, the compound containing a In step (1) is an oxide, halide or carbonate of Ca, sr or Ba, the compound containing B is an oxide or halide of Ga and In, the compound containing Sn is an oxide containing Sn, the compound containing Si is an oxide containing Si, silicate or silicic acid, and the compound containing Ce is an oxide or halide containing Ce.
In some embodiments of the invention, the milling in step (2) and step (4) is performed for a period of 20 to 50 minutes.
In some embodiments of the invention, the sintering temperature in the air atmosphere described in step (2) is 400 to 800 ℃ and the sintering time is 3 to 15 hours.
In some embodiments of the invention, the reduction sintering temperature in step (4) is 1100 to 1500 ℃ and the sintering time is 5 to 24 hours.
In some embodiments of the invention, the reduction sintering described in step (4) is 5%H 2 -95％N 2 Is reduced in a hydrogen-nitrogen mixed atmosphere.
The invention further provides application of the ultraviolet excited blue light emitting fluorescent powder, and the ultraviolet excited blue light emitting fluorescent powder is used for preparing an ultraviolet chip white light LED, an ultraviolet chip solar light LED, an ultraviolet chip full spectrum LED or an ultraviolet chip healthy lighting LED.
Compared with the prior art, the invention has the advantages and beneficial effects that:
(1) The fluorescent powder can emit blue light with a spectrum range covering 425-700 nm and a center wavelength of 471nm under ultraviolet excitation, and is not reported.
(2) Compared with the prior art, the fluorescent powder is Ce 3+ The doped oxide-based blue light emitting fluorescent powder has the advantage of stable physical and chemical properties, can be prepared by adopting a conventional solid phase reaction method, has a simple preparation process, is beneficial to industrial production, and can be a good candidate material for wide application.
(3) The fluorescent powder can be well matched with the existing commercial near ultraviolet LED chip, and is suitable for application of ultraviolet chip white light LEDs, ultraviolet chip solar light LEDs, ultraviolet chip full spectrum LEDs, ultraviolet chip high-quality white light LEDs and the like.
Drawings
Fig. 1 is a photo-excitation-emission spectrum of example 1 of the present invention.
Fig. 2 shows photoluminescence spectra of examples 1, 2 and 3 according to the present invention.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples.
Example 1:
1. SrCO is selected for use 3 、Ga 2 O 3 、SnO 2 、SiO 2 、CeO 2 As starting materials, five materials were weighed respectively corresponding to x=0.005, and the total mass of the raw material mixture was controlled to be 5g of mixed raw materials.
2. Grinding the raw material mixture in an agate mortar for 20 to 50 minutes, loading the mixture into an alumina crucible after the materials are uniformly mixed, calcining the alumina crucible filled with the raw material at 400 ℃ for 3 hours in an air atmosphere, and naturally cooling to room temperature; and then, after the obtained mixed product is sufficiently and uniformly ground again, placing the mixed product in a reducing atmosphere mixed with hydrogen and nitrogen, calcining at 1100 ℃ for 5 hours, and then cooling to room temperature to obtain the target product.
3. The spectral properties of the phosphor of this system were tested using a fluorescence spectrometer (HITACHI F-7000), as shown in FIGS. 1 and 2. The result shows that the fluorescent powder of the system has wider excitation band, covers ultraviolet and purple light areas, has a peak value near 365nm and higher spectrum peak value, and can be effectively excited by ultraviolet and purple light chips and well matched with an n-UV LED chip. Under the excitation of 365nm ultraviolet light source, the fluorescent powder emits bright blue light, and the emission spectrum is composed of a wider emission band (425-700 nm), and the peak value is 471nm.
Example 2:
1. SrCO is selected for use 3 、Ga 2 O 3 、SnO 2 、SiO 2 、CeO 2 As starting materials, five materials were weighed respectively corresponding to x=0.01, and the total mass of the raw material mixture was controlled to be 5g of mixed raw materials.
2. Grinding the raw material mixture in an agate mortar for 20 to 50 minutes, loading the mixture into an alumina crucible after the materials are uniformly mixed, calcining the alumina crucible filled with the raw material at 500 ℃ for 6 hours in an air atmosphere, and naturally cooling to room temperature; and then, after the obtained mixed product is sufficiently and uniformly ground again, placing the mixed product in a reducing atmosphere mixed with hydrogen and nitrogen, calcining the mixed product at 1200 ℃ for 9 hours, and then cooling the mixed product to room temperature to obtain the target product.
3. The spectral properties of the phosphor of this system were tested using a fluorescence spectrometer (HITACHI F-7000), as shown in FIG. 2. The result shows that under the excitation of 365nm ultraviolet light source, the fluorescent powder emits bright blue light, and the emission spectrum is composed of a wider emission band (425-700 nm), and the peak value is 471nm.
Example 3:
1. SrCO is selected for use 3 、Ga 2 O 3 、SnO 2 、SiO 2 、CeO 2 As starting materials, five materials were weighed respectively corresponding to x=0.015 and the total mass of the raw material mixture was controlled to be 5g of mixed raw material.
2. Grinding the raw material mixture in an agate mortar for 20 to 50 minutes, loading the mixture into an alumina crucible after the materials are uniformly mixed, calcining the alumina crucible filled with the raw material at 600 ℃ for 10 hours in an air atmosphere, and naturally cooling to room temperature; and (3) sufficiently grinding the obtained mixed product again uniformly, placing the mixed product in a reducing atmosphere mixed with hydrogen and nitrogen, calcining at 1300 ℃ for 14 hours, and cooling to room temperature to obtain the target product.
3. The spectral properties of the phosphor of this system were tested using a fluorescence spectrometer (HITACHI F-7000), as shown in FIG. 2. The result shows that under the excitation of 365nm ultraviolet light source, the fluorescent powder emits bright blue light, and the emission spectrum is composed of a wider emission band (425-700 nm), and the peak value is 471nm.
Example 4:
1. by SrCO 3 、Ga 2 O 3 、SnO 2 、SiO 2 、CeO 2 As starting materials, five materials were weighed respectively corresponding to x=0.02, and the total mass of the raw material mixture was controlled to be 5g of mixed raw material.
2. Grinding the raw material mixture in an agate mortar for 20 to 50 minutes, loading the mixture into an alumina crucible after the materials are uniformly mixed, calcining the alumina crucible filled with the raw material at 800 ℃ for 15 hours in an air atmosphere, and naturally cooling to room temperature; after the obtained mixed product was sufficiently ground again, it was calcined at 1500 ℃ for 24 hours in a reducing atmosphere mixed with hydrogen and nitrogen, and then cooled to room temperature, to obtain the objective product, the fluorescence spectrum properties of which were similar to those of example 1.
Example 5:
1. by SrCO 3 、Ga 2 O 3 、SnO 2 、SiO 2 、CeO 2 As starting materials, five materials were weighed respectively corresponding to x=0.025, and the total mass of the raw material mixture was controlled to be 5g of mixed raw materials.
2. Grinding the raw material mixture in an agate mortar for 20 to 50 minutes, loading the mixture into an alumina crucible after the materials are uniformly mixed, calcining the alumina crucible filled with the raw material at 800 ℃ for 15 hours in an air atmosphere, and naturally cooling to room temperature; after the obtained mixed product was sufficiently ground again, it was calcined at 1500 ℃ for 24 hours in a reducing atmosphere mixed with hydrogen and nitrogen, and then cooled to room temperature, to obtain the objective product, the fluorescence spectrum properties of which were similar to those of example 1.
Example 6:
1. by BaCO 3 、Ga 2 O 3 、SnO 2 、SiO 2 、CeO 2 As starting materials, ba: ga: sn: si: ce=2.995:2:1.5:2.5:0.005 (molar ratio), corresponding to x=0.005, five materials were weighed respectively, and the total mass of the raw material mixture was controlled to be 5g of mixed raw material.
2. Grinding the raw material mixture in an agate mortar for 20 to 50 minutes, loading the mixture into an alumina crucible after the materials are uniformly mixed, calcining the alumina crucible filled with the raw material at 700 ℃ for 8 hours in an air atmosphere, and naturally cooling to room temperature; after the obtained mixed product was sufficiently ground again to uniformity, it was calcined at 1400 ℃ for 6 hours in a reducing atmosphere mixed with hydrogen and nitrogen, and then cooled to room temperature, to obtain the objective product, the fluorescence spectrum properties of which were similar to those of example 1.
Example 7:
1. by CaCO 3 、Ga 2 O 3 、SnO 2 、SiO 2 、CeO 2 As starting materials, ca: ga: sn: si: ce=2.995:2:1.5:2.5:0.005 (molar ratio), corresponding to x=0.005, five materials were weighed respectively, and the total mass of the raw material mixture was controlled to be 5g of mixed raw material.
2. Grinding the raw material mixture in an agate mortar for 20 to 50 minutes, loading the mixture into an alumina crucible after the materials are uniformly mixed, calcining the alumina crucible filled with the raw material at 700 ℃ for 8 hours in an air atmosphere, and naturally cooling to room temperature; after the obtained mixed product was sufficiently ground again to uniformity, it was calcined at 1400 ℃ for 7 hours in a reducing atmosphere mixed with hydrogen and nitrogen, and then cooled to room temperature, to obtain the objective product, the fluorescence spectrum properties of which were similar to those of example 1.
Example 8:
1. by SrCO 3 、In 2 O 3 、SnO 2 、SiO 2 、CeO 2 As starting materials, sr: in: sn: si: ce=2.995:2:1.5:2.5:0.005 (molar ratio), five materials were weighed respectively corresponding to x=0.005, and the total mass of the raw material mixture was controlled to be 5g of mixed raw material.
2. Grinding the raw material mixture in an agate mortar for 20 to 50 minutes, loading the mixture into an alumina crucible after the materials are uniformly mixed, calcining the alumina crucible filled with the raw material at 700 ℃ for 8 hours in an air atmosphere, and naturally cooling to room temperature; after the obtained mixed product was sufficiently ground again to uniformity, it was calcined at 1400 ℃ for 8 hours in a reducing atmosphere mixed with hydrogen and nitrogen, and then cooled to room temperature, to obtain the objective product, the fluorescence spectrum properties of which were similar to those of example 1.
Example 9:
1. by BaCO 3 、In 2 O 3 、SnO 2 、SiO 2 、CeO 2 As starting materials, ba: in: sn: si: ce=2.995:2:1.5:2.5:0.005 (molar ratio), five materials were weighed respectively corresponding to x=0.005, and the total mass of the raw material mixture was controlled to be 5g of mixed raw material.
2. Grinding the raw material mixture in an agate mortar for 20 to 50 minutes, loading the mixture into an alumina crucible after the materials are uniformly mixed, calcining the alumina crucible filled with the raw material at 700 ℃ for 8 hours in an air atmosphere, and naturally cooling to room temperature; after the obtained mixed product was sufficiently ground again to uniformity, it was calcined at 1400 ℃ for 9 hours in a reducing atmosphere mixed with hydrogen and nitrogen, and then cooled to room temperature, to obtain the objective product, the fluorescence spectrum properties of which were similar to those of example 1.
Example 10:
1. by CaCO 3 、In 2 O 3 、SnO 2 、SiO 2 、CeO 2 As starting material, ca: in: sn: si: ce=2.995:2:1.5:2.5:0.005 (molar ratio), corresponding to x=0.005, minutesFive raw materials are weighed separately, and the total mass of the raw material mixture is controlled to be 5 g.
2. Grinding the raw material mixture in an agate mortar for 20 to 50 minutes, loading the mixture into an alumina crucible after the materials are uniformly mixed, calcining the alumina crucible filled with the raw material at 700 ℃ for 8 hours in an air atmosphere, and naturally cooling to room temperature; after the obtained mixed product was sufficiently ground again to uniformity, it was calcined at 1400 ℃ for 10 hours in a reducing atmosphere mixed with hydrogen and nitrogen, and then cooled to room temperature, to obtain the objective product, the fluorescence spectrum properties of which were similar to those of example 1.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (10)
1. An ultraviolet excited blue light emitting fluorescent powder is characterized in that the ultraviolet excited blue light emitting fluorescent powder is ultraviolet excited Ce 3+ Doped oxide-based 471nm blue light emitting phosphor, which is AO-B 2 O 3 -SnO 2 -SiO 2 -Ce 2 O 3 Wherein A is one or more of Ca, sr or Ba; b is one or more of Ga or In, and the mass percentage of the components is 20.44% or more and less than or equal to AO or less than or equal to 44.86% and 18.31% or less and less than or equal to B 2 O 3 ≤33.76％，20.29％≤SnO 2 ≤30.88％，13.49％≤SiO 2 ≤20.52％，0.11％≤Ce 2 O 3 ≤0.468％。
2. The ultraviolet excited blue light emitting phosphor of claim 1, wherein the phosphor is AO-B 2 O 3 -SnO 2 -SiO 2 -Ce 2 O 3 Wherein A is one or more of Ca, sr or Ba; b is one or more of Ga or In, and the molar ratio of the component A to the component B to the component Sn to the component Si to the component Ce is (2.975-2.995:2:1.5:2.5:0.005-0.025).
3. An ultraviolet excited blue light emitting phosphor according to claim 2, wherein the phosphor is AO-B 2 O 3 -SnO 2 -SiO 2 -Ce 2 O 3 Wherein A is one or more of Ca, sr or Ba; b is one or more of Ga or In, wherein the mol ratio of component A to B to Si to Ce=2.995 to 1.5 to 2.5 to 0.005, or the mol ratio of component A to B to Si to Ce=2.99 to 2 to 1.5 to 2.5 to 0.01, or the mol ratio of component A to B to Si to Ce=2.985 to 2 to 1.5 to 2.5 to 0.015, or the mol ratio of component A to B to Sn to Si to Ce=2.98 to 2 to 1.5 to 2.5 to 0.02, or the mol ratio of component A to B to Sn to Si to Ce=2.975 to 2 to 1.5 to 2.5 to 0.025.
4. An ultraviolet excited blue light emitting phosphor according to claim 1, 2 or 3, wherein the ultraviolet excited blue light emitting phosphor emits blue light with a spectral range of 425-700 nm and a center wavelength of 471nm under ultraviolet excitation.
5. A method for preparing the ultraviolet excited blue light emitting phosphor according to any one of claims 1 to 3, comprising the steps of:
(1) Weighing a proper amount of a compound containing A, a compound containing B, a compound containing Sn, a compound containing Si and a compound containing Ce as raw material powder;
(2) Grinding and uniformly mixing the mixture obtained in the step (1);
(3) Placing the ground raw material powder into an alumina crucible, calcining the alumina crucible filled with the raw material in an air atmosphere, and naturally cooling to room temperature;
(4) And (3) sufficiently grinding the mixed product obtained after calcining in the step (3) uniformly again, placing the mixed product in a reducing atmosphere mixed with hydrogen and nitrogen for sintering, and then cooling to room temperature to finally obtain the ultraviolet excited blue light emitting fluorescent powder.
6. The method of preparing ultraviolet excited blue light emitting phosphor according to claim 5, wherein the compound a In step (1) is an oxide, halide or carbonate of Ca, sr or Ba, the compound B is an oxide or halide of Ga and In, the compound Sn is an oxide of Sn, the compound Si is an oxide, silicate or silicic acid of Si, and the compound Ce is an oxide or halide of Ce.
7. The method for preparing ultraviolet excited blue light emitting phosphor according to claim 5, wherein the grinding time in the step (2) and the step (4) is 20 to 50min;
the sintering temperature in the air atmosphere in the step (2) is 400-800 ℃ and the sintering time is 3-15 h.
8. The method for preparing ultraviolet excited blue light emitting phosphor according to claim 5, wherein the reduction sintering temperature in the step (4) is 1100-1500 ℃ and the sintering time is 5-24 h.
9. The method of preparing ultraviolet excited blue light emitting phosphor according to claim 5, wherein the reduction sintering in step (4) is 5%H 2 -95％N 2 Is reduced in a hydrogen-nitrogen mixed atmosphere.
10. The use of an ultraviolet excited blue light emitting phosphor according to any one of claims 1 to 3, wherein the ultraviolet excited blue light emitting phosphor is used for the preparation of an ultraviolet chip white light LED, an ultraviolet chip solar light LED, an ultraviolet chip full spectrum LED or an ultraviolet chip health lighting LED.
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| CN101781560A (en) * | 2010-03-23 | 2010-07-21 | 中国计量学院 | Fluorescent powder using silicon-aluminum base nitrogen oxides as base materials and preparation method thereof |
| CN102010710A (en) * | 2010-11-26 | 2011-04-13 | 四川新力光源有限公司 | Blue fluorescent powder and preparation method thereof |
| CN109650725A (en) * | 2018-12-29 | 2019-04-19 | 上海应用技术大学 | A kind of production method of blue-fluorescence glass ceramics |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101077973A (en) * | 2006-05-26 | 2007-11-28 | 大连路明发光科技股份有限公司 | Silicate luminescent material, preparation method thereof and luminescent device using the same |
| CN101781560A (en) * | 2010-03-23 | 2010-07-21 | 中国计量学院 | Fluorescent powder using silicon-aluminum base nitrogen oxides as base materials and preparation method thereof |
| CN102010710A (en) * | 2010-11-26 | 2011-04-13 | 四川新力光源有限公司 | Blue fluorescent powder and preparation method thereof |
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