CN112662400A - Energy-storage luminescent material and preparation method thereof - Google Patents
Energy-storage luminescent material and preparation method thereof Download PDFInfo
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- CN112662400A CN112662400A CN202011208865.9A CN202011208865A CN112662400A CN 112662400 A CN112662400 A CN 112662400A CN 202011208865 A CN202011208865 A CN 202011208865A CN 112662400 A CN112662400 A CN 112662400A
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- 239000000463 material Substances 0.000 title claims abstract description 39
- 238000004146 energy storage Methods 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 38
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 239000010453 quartz Substances 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004327 boric acid Substances 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000000197 pyrolysis Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 4
- 239000012190 activator Substances 0.000 abstract description 3
- 238000005054 agglomeration Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- 230000003993 interaction Effects 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract 1
- 238000005056 compaction Methods 0.000 abstract 1
- 229910017604 nitric acid Inorganic materials 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 8
- 229910052593 corundum Inorganic materials 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 229910001845 yogo sapphire Inorganic materials 0.000 description 8
- 238000000227 grinding Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001917 fluorescence detection Methods 0.000 description 1
- 238000003018 immunoassay Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 238000005390 triboluminescence Methods 0.000 description 1
- 238000004875 x-ray luminescence Methods 0.000 description 1
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- Luminescent Compositions (AREA)
Abstract
本发明公开了一种蓄能发光材料，该发光材料组成成分包括如下重量份数原料：Sr2O3，Al2O3，Y203，Si02，Yb203和Er203，其制备方法，包括以下步骤：步骤1:称取Al2O3，Y203，Si02放入反应容器中适量的硝酸加入到反应容器中；步骤5：将干燥后的原料放入玛瑙研钵中，充分研磨20‑25min，装入坩埚中压实，加入干燥后的原料同体积的5‑15%的碳粉覆盖在混合物上面，容器加盖后密封，然后将坩埚置于石英管中；将石英管在高温炉中灼烧，得出成品。经此发明提供的方法得出的发光材料，在同等条件下，余辉时间较长，可达到700min以上，属于超长余辉，具有良好的蓄能效果，同时Yb3+作敏化剂，Er3+作激活剂，其Yb‑Er体系相对较为稳定，粒子间的相互作用增大，相互吸附团聚增多，能大大降低制备难度。The invention discloses an energy storage luminescent material. The luminescent material comprises the following raw materials in parts by weight: Sr 2 O 3 , Al 2 O 3 , Y 2 0 3 , SiO 2 , Yb 2 0 3 and Er 2 0 3 , and its preparation method includes the following steps: Step 1: Weigh Al 2 O 3 , Y 2 O 3 , SiO 2 and put it into the reaction vessel. An appropriate amount of nitric acid is added to the reaction vessel; Step 5: The dried raw materials are put into the reaction vessel. In an agate mortar, fully grind for 20-25min, put it into a crucible for compaction, add 5-15% carbon powder of the same volume of the dried raw materials to cover the mixture, cover the container and seal it, and then place the crucible on the quartz In the tube; burn the quartz tube in a high temperature furnace to obtain the finished product. The luminescent material obtained by the method provided by the invention has a longer afterglow time under the same conditions, which can reach more than 700min , which belongs to the ultra - long afterglow and has a good energy storage effect. + As an activator, its Yb-Er system is relatively stable, the interaction between particles increases, and the mutual adsorption and agglomeration increases, which can greatly reduce the difficulty of preparation.
Description
Technical Field
The invention relates to the field of materials, in particular to an energy storage luminescent material and a preparation method thereof.
Background
A substance capable of emitting light after being excited by the outside is called a luminescent material, and the luminescent material is one of functional materials. The luminous substance is not strange to people and can be seen almost everywhere at home or in public places. The core part of the X-ray security check instrument of the airport, the display of the computer and the like is the luminescent material, and the luminescent material which plays the role of anti-counterfeiting is also contained in paper money which is commonly used, not only in expensive equipment. Luminescent materials have long become indispensable materials in people's daily life, and are widely used in large-screen color display panels, lighting devices, computer monitors, fluorescence detection immunoassays, and the like. Luminescent materials can be excited by various forms of energy. Chemiluminescence is excited by the energy of a chemical reaction; electroluminescent light is excited by a voltage; photoluminescence is excited by electromagnetic radiation; the triboluminescence is excited by mechanical energy; the cathode ray luminescence is excited by a high-energy electron beam; the X-ray luminescence is excited by X-rays.
The energy storage time of the existing luminescent material is short in the actual use process, basically about 500min, and the rest glow time can not meet the requirements for the luminescent material used on luminescent articles such as watches and the like, so that the luminescent material with long energy storage time is needed.
Disclosure of Invention
The invention aims to provide an energy-storage luminescent material, which aims to solve the problems that the energy storage time of the existing luminescent material in the background technology is short in the actual use process, and the rest glow time can not meet the requirements when the luminescent material is used on luminescent articles such as watches and the like.
An energy storage luminescent material is characterized by comprising the following raw materials in parts by weight: sr2O3 45-50 parts of Al2O315-20 parts of Si0215-20 parts of, Y2037-9 parts of Yb2035-7 parts of Er2031-3 parts.
The preparation method of the energy storage luminescent material is characterized by comprising the following steps of:
step 1, weighing 45-50 parts of Sr2O3 And 15-20 parts of Si02And 15-20 parts of Al2O3Putting the mixture into a reaction container, and adding 6-7 parts of boric acid into the reaction container;
step 2: weighing 7-9 parts of Y2037-9 parts of Yb203And 1-3 parts of Er203Adding into a reaction vessel;
and step 3: placing the reaction container on a magnetic stirrer, fully stirring, finally reacting to obtain a transparent solution, pouring the solution obtained by reaction into a plastic reaction container, adding 8-9 parts of hydrofluoric acid into the plastic reaction container, and stirring to uniformly mix the solution;
and 4, step 4: putting the substance obtained in the step 3 into a centrifugal barrel, pouring out supernatant liquor after centrifugation is finished, washing the supernatant liquor for 3 to 4 times by using 20 to 25 parts of distilled water, and putting the washed substance into a drying box for vacuum drying;
and 5: putting the dried raw materials into an agate mortar, fully grinding for 20-25min, uniformly mixing, putting into a crucible, compacting, adding carbon powder which is 5-15% of the same volume of the dried raw materials and covers the mixture, covering a container with a cover, sealing, and then putting the crucible into a quartz tube;
step 6: burning the quartz tube in a high-temperature furnace, and continuously introducing hydrogen into the quartz tube taken out until the temperature of the crucible is reduced to 18-20 ℃ to obtain a finished product.
As a further scheme of the invention: in step 4, the centrifugation speed in the centrifugal barrel is 4800r/min, and the centrifugation time is 2-3 min.
As a further scheme of the invention: in step 4, the temperature in the drying oven is 420-.
As a further scheme of the invention: in step 6, the pyrolysis temperature of the high-temperature furnace is 1200-1250 ℃.
As a further scheme of the invention: in step 6, the combustion time in the high-temperature furnace is 3 to 5 hours.
The invention has the technical effects and advantages that:
the luminescent material obtained by the method has longer afterglow time which can reach more than 700min under the same condition, belongs to ultra-long afterglow and has good energy storage effect,simultaneous Yb3+As sensitizer, Er3+As an activator, the Yb-Er system is relatively stable, the interaction among particles is increased, the mutual adsorption and agglomeration are increased, and the preparation difficulty can be greatly reduced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The invention provides an energy storage luminescent material, which comprises the following raw materials in parts by weight: sr2O3 45 parts of Al2O315 parts of Si0215 parts of, Y2037 parts of Yb2035 parts of Er2031 part;
a preparation method of an energy storage luminescent material comprises the following steps:
step 1, weighing 45 parts of Sr2O3 And 15 parts of Si02And 15 parts of Al2O3Putting the mixture into a reaction container, and adding 6-7 parts of boric acid into the reaction container;
step 2: weighing 7 parts of Y2035 parts of Yb203And 1 part of Er203Adding into a reaction vessel;
and step 3: placing the reaction container on a magnetic stirrer, fully stirring, finally reacting to obtain a transparent solution, pouring the solution obtained by reaction into a plastic reaction container, adding 8-9 parts of hydrofluoric acid into the plastic reaction container, and stirring to uniformly mix the solution;
and 4, step 4: putting the substance obtained in the step 3 into a centrifugal barrel, performing centrifugal separation at 4800r/min for 2-3min, pouring out supernatant after the centrifugation is finished, washing the supernatant for 3-4 times by using 20-25 parts of distilled water, and putting the washed substance into a drying box for vacuum drying at the temperature of 420-;
and 5: putting the dried raw materials into an agate mortar, fully grinding for 20-25min, uniformly mixing, putting into a crucible, compacting, adding 5-15% of carbon powder with the same volume as the dried raw materials to cover the mixture, covering a container with a cover, sealing, and then putting the crucible into a quartz tube;
step 6: burning the quartz tube in a 1200-1250 ℃ high-temperature furnace for 3-5 hours, and taking out the quartz tube and continuing introducing hydrogen until the temperature of the crucible is reduced to 18-20 ℃ to obtain a finished product.
Example 2
The invention provides an energy storage luminescent material, which comprises the following raw materials in parts by weight: sr2O3 47 parts of Al2O317 parts of Si0217 parts of, Y2038 parts of Yb2036 parts of Er2032 parts of (1);
a preparation method of an energy storage luminescent material comprises the following steps:
step 1, weighing 47 parts of Sr2O3 And 17 parts of Si02And 17 parts of Al2O3Putting the mixture into a reaction container, and adding 6-7 parts of boric acid into the reaction container;
step 2: weighing 8 parts of Y2036 parts of Yb203And 2 parts of Er203Adding into a reaction vessel;
and step 3: placing the reaction container on a magnetic stirrer, fully stirring, finally reacting to obtain a transparent solution, pouring the solution obtained by reaction into a plastic reaction container, adding 8-9 parts of hydrofluoric acid into the plastic reaction container, and stirring to uniformly mix the solution;
and 4, step 4: putting the substance obtained in the step 3 into a centrifugal barrel, performing centrifugal separation at 4800r/min for 2-3min, pouring out supernatant after the centrifugation is finished, washing the supernatant for 3-4 times by using 20-25 parts of distilled water, and putting the washed substance into a drying box for vacuum drying at the temperature of 420-;
and 5: putting the dried raw materials into an agate mortar, fully grinding for 20-25min, uniformly mixing, putting into a crucible, compacting, adding 5-15% of carbon powder with the same volume as the dried raw materials to cover the mixture, covering a container with a cover, sealing, and then putting the crucible into a quartz tube;
step 6: burning the quartz tube in a 1200-1250 ℃ high-temperature furnace for 3-5 hours, and taking out the quartz tube and continuing introducing hydrogen until the temperature of the crucible is reduced to 18-20 ℃ to obtain a finished product.
Example 3
The invention provides an energy storage luminescent material, which comprises the following raw materials in parts by weight: sr2O3 50 parts of Al2O320 parts of Si0220 parts of, Y2039 parts of Yb2037 parts of Er2033 parts of a mixture;
a preparation method of an energy storage luminescent material comprises the following steps:
step 1, weighing 50 parts of Sr2O3 And 20 parts of Si02And 20 parts of Al2O3Putting the mixture into a reaction container, and adding 6-7 parts of boric acid into the reaction container;
step 2: weighing 9 parts of Y2037 parts of Yb203And 3 parts of Er203Adding into a reaction vessel;
and step 3: placing the reaction container on a magnetic stirrer, fully stirring, finally reacting to obtain a transparent solution, pouring the solution obtained by reaction into a plastic reaction container, adding 8-9 parts of hydrofluoric acid into the plastic reaction container, and stirring to uniformly mix the solution;
and 4, step 4: putting the substance obtained in the step 3 into a centrifugal barrel, performing centrifugal separation at 4800r/min for 2-3min, pouring out supernatant after the centrifugation is finished, washing the supernatant for 3-4 times by using 20-25 parts of distilled water, and putting the washed substance into a drying box for vacuum drying at the temperature of 420-;
and 5: putting the dried raw materials into an agate mortar, fully grinding for 20-25min, uniformly mixing, putting into a crucible, compacting, adding 5-15% of carbon powder with the same volume as the dried raw materials to cover the mixture, covering a container with a cover, sealing, and then putting the crucible into a quartz tube;
step 6: burning the quartz tube in a 1200-1250 ℃ high-temperature furnace for 3-5 hours, and taking out the quartz tube and continuing introducing hydrogen until the temperature of the crucible is reduced to 18-20 ℃ to obtain a finished product.
And (3) experimental comparison:
after 20 minutes of irradiation of the above-mentioned finished products of examples 1 to 3 in daylight or sunlight, the afterglow time is recorded in the dark:
| group of | Time of light emission |
| Example 1 | 731min |
| Example 2 | 726min |
| Example 3 | 716min |
| Existing luminescent materials | 503min |
The experiment shows that the phosphor prepared by the method has longer afterglow time which can reach more than 700min under the same condition, belongs to ultra-long afterglow, has good energy storage effect, and Yb3+As sensitizer, Er3+As an activator, the Yb-Er system is relatively stable, the interaction among particles is increased, the mutual adsorption and agglomeration are increased, and the preparation difficulty can be greatly reduced.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (6)
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06337303A (en) * | 1993-05-31 | 1994-12-06 | Toray Ind Inc | Antireflection plastic optical parts |
| CN1377934A (en) * | 2002-04-19 | 2002-11-06 | 何清 | Environment protection energy accumulating luminous material without radioactivity and its preparing method |
| US20100164367A1 (en) * | 2007-05-22 | 2010-07-01 | Kousuke Shioi | Fluorescent substance, method for producing the same, and light-emitting device using the same |
| CN101935204A (en) * | 2009-10-23 | 2011-01-05 | 郑子山 | A kind of ultra-long afterglow blue light-storing ceramic material and its preparation method |
| CN103374350A (en) * | 2012-04-17 | 2013-10-30 | 梁清源 | Ultrafine particle energy-storage type long-lasting phosphor material and preparation method thereof |
| CN105733581A (en) * | 2016-03-16 | 2016-07-06 | 安徽中益新材料科技有限公司 | Novel energy accumulation luminescent powder and preparation method thereof |
| CN108250882A (en) * | 2018-01-22 | 2018-07-06 | 东南大学 | A kind of energy-storing type long-afterglow self-luminescent road marking coating and preparation method thereof |
-
2020
- 2020-11-03 CN CN202011208865.9A patent/CN112662400B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06337303A (en) * | 1993-05-31 | 1994-12-06 | Toray Ind Inc | Antireflection plastic optical parts |
| CN1377934A (en) * | 2002-04-19 | 2002-11-06 | 何清 | Environment protection energy accumulating luminous material without radioactivity and its preparing method |
| US20100164367A1 (en) * | 2007-05-22 | 2010-07-01 | Kousuke Shioi | Fluorescent substance, method for producing the same, and light-emitting device using the same |
| CN101935204A (en) * | 2009-10-23 | 2011-01-05 | 郑子山 | A kind of ultra-long afterglow blue light-storing ceramic material and its preparation method |
| CN103374350A (en) * | 2012-04-17 | 2013-10-30 | 梁清源 | Ultrafine particle energy-storage type long-lasting phosphor material and preparation method thereof |
| CN105733581A (en) * | 2016-03-16 | 2016-07-06 | 安徽中益新材料科技有限公司 | Novel energy accumulation luminescent powder and preparation method thereof |
| CN108250882A (en) * | 2018-01-22 | 2018-07-06 | 东南大学 | A kind of energy-storing type long-afterglow self-luminescent road marking coating and preparation method thereof |
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