CN101768441B - Rare earth borate luminescent material and preparation material thereof - Google Patents
Rare earth borate luminescent material and preparation material thereof Download PDFInfo
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- CN101768441B CN101768441B CN201010042740.3A CN201010042740A CN101768441B CN 101768441 B CN101768441 B CN 101768441B CN 201010042740 A CN201010042740 A CN 201010042740A CN 101768441 B CN101768441 B CN 101768441B
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Abstract
The invention provides a rare earth borate luminescent material and a preparation method thereof. The chemical formula of the luminescent material is M3N1-xLnxB2O6, wherein M is one of Na, K and Li, N is one or two of Y, Gd, Sc, Lu and La, Ln is one or two of Tm, Tb, Eu, Sm, Pr, Dy, Ce and Bi, and the value of x is more than 0 and less than or equal to 0.5. The preparation method comprises the following steps of: weighing each raw material according to a mol ratio, grinding the raw materials, mixing the raw materials uniformly, and then pre-calcining the mixture at a lower temperature; sintering the mixture for 1 to 20 hours at the temperature of between 800 and 1,000 DEG C; and cooling the sintered mixture to obtain the rare earth borate luminescent material. The preparation method has a simple process and a low cost; the obtained luminescent material has the advantages of high luminous efficiency, good stability, good color purity and the like; and the preparation method can be widely used for manufacturing luminescent materials.
Description
Technical field
The present invention relates to luminescent material technical field, relate in particular to a kind of fluorescent material and preparation method thereof, more particularly, relate to a kind of rare earth borate luminescent material and preparation method thereof.
Background technology
At present, rare earth luminescent material, as a kind of new and effective luminescent material, has developed into the important luminescent material of various fields such as being applied to information demonstration, lighting source, photoelectric device.By improving the luminous intensity of rare earth luminescent material, not only can effectively improve the luminescent properties of luminescent device, and can improve the luminous efficiency of luminescent device, and effectively energy-conservation.Therefore the luminescent material that, has a high-luminous-efficiency is the important research content in materials chemistry and materials physics field always.
Rare earth ion doped light emitting borate material has good photoluminescence performance, after being stimulated the purity of color of the fluorescence that sends and brightness all higher, can be used as the three primary colors fluorescent powder application of UV-LED.Yet the luminescent properties that how further to improve this kind of material is the target that researchist makes great efforts always.
Summary of the invention
The technical problem to be solved in the present invention is, for the above-mentioned defect of prior art, provides a kind of rare earth borate luminescent material of good luminous performance.
The technical problem that the present invention further will solve is, a kind of preparation method of rare earth borate luminescent material is also provided.
The technical solution adopted for the present invention to solve the technical problems is: a kind of rare earth borate luminescent material, its chemical formula is M
3n
1-xln
xb
2o
6, wherein, M is a kind of in Na, K, Li, and N is one or both in Y, Gd, Sc, Lu, La, and Ln is one or both in Tm, Tb, Eu, Sm, Pr, Dy, Ce, Bi, and the span of x is 0 < x≤0.5.
In rare earth borate luminescent material of the present invention, the span of described x is preferably 0.001≤x≤0.3.
A preparation method for rare earth borate luminescent material, comprises the following steps:
1. take containing M compound, containing N compound, containing Ln compound, boride alloy is raw material, by the molar ratio of each element in above-mentioned chemical formula, takes raw material, and makes boride alloy excessive 5%～30% by aforementioned molar ratio, and ground and mixed is even;
2. by step the compound in 1. prior to 600～800 ℃ of precalcinings, then in 800～1200 ℃ of sintering;
3. by step, the sintered product in is 2. cooled to room temperature, obtains rare earth borate luminescent material.
Wherein, preferably, the described carbonate or the oxalate that containing M compound, are M, the described oxide compound, muriate, nitrate, carbonate or the oxalate that containing N compound, are N, the described oxide compound, muriate, nitrate, carbonate or the oxalate that containing Ln compound, are Ln, described boride alloy is boric acid or boron oxide.
The preparation method of rare earth borate luminescent material of the present invention, step 2. in, the precalcining time is 0.5～2h, further, precalcining temperature is preferably 650～750 ℃, the precalcining time is preferably 0.5～1.5h; Sintering time is 1～20h, and further, sintering temperature is preferably 850～950 ℃, and sintering time is preferably 4～15h.
In the preparation method of rare earth borate luminescent material of the present invention, preferably, 2. described step is: the compound by step in is 1. prior to 600～800 ℃ of precalcinings, and precalcining product is cooled to room temperature, grinds, then in 800～1200 ℃ of sintering.
Rare earth borate luminescent material of the present invention is the N that adulterated
3+and Ln
3+light emitting borate material, not only luminous efficiency is high, and has the feature of good stability, high color purity, can launch ruddiness, green glow, blue light, UV-light etc.
Preparation method's technique of the present invention is simple, cost is low, and the luminescent material quality obtaining is high, can be widely used in the manufacture of luminescent material.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing:
Fig. 1 is the Na of the embodiment of the present invention 4 preparations
3y
0.90tb
0.10b
2o
6the luminescent spectrum figure of rare earth borate luminescent material;
Fig. 2 is the Na of the embodiment of the present invention 6 preparations
3y
0.99tm
0.01b
2o
6the luminescent spectrum figure of rare earth borate luminescent material;
Fig. 3 is the Na of the embodiment of the present invention 8 preparations
3y
0.915ce
0.005tb
0.08b
2o
6the luminescent spectrum figure of rare earth borate luminescent material;
Fig. 4 is the Na of the embodiment of the present invention 9 preparations
3y
0.997bi
0.003b
2o
6the luminescent spectrum figure of rare earth borate luminescent material;
Fig. 5 is the Na of the embodiment of the present invention 11 preparations
3y
0.97ce
0.03b
2o
6the luminescent spectrum figure of rare earth borate luminescent material.
Above-mentioned luminescent spectrum is to adopt Shimadzu RF-5301PC fluorescence spectrophotometer scanning analysis to obtain.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is described in further detail.But, should be appreciated that protection scope of the present invention is not subject to the restriction of these embodiment.
Raw materials usedly in following examples be common commercial goods, purity is analytical pure.When preparation rare earth borate luminescent material of the present invention, according to the molar ratio of each element in chemical formula, take each raw material, and make boride alloy by aforementioned molar ratio excessive 5%～30%, ground and mixed, prior to precalcining for some time under lesser temps, after being cooled to room temperature and grinding, then in 800～1000 ℃ of sintering 1～20h, obtain rare earth borate luminescent material of the present invention after cooling.
For convenient application, can be by rare earth borate luminescent material grind into powder of the present invention.In the sintering step of following part embodiment, used reducing atmosphere, but, in the preparation process of the luminescent material of these embodiment, reducing atmosphere is not must condition, when sintering, does not use reducing atmosphere can prepare the luminescent material of these embodiment equally.
Embodiment 1 high temperature solid-state method is prepared K
3y
0.999tm
0.001b
2o
6luminescent material
Take K
2cO
30.8292g, Y (NO
3)
31.0985g, Tm
2(CO
3)
30.0010g and H
3bO
30.5193g (excessive 5%) is raw material.All raw materials are placed in to agate mortar and are fully ground to and mix, the powder transfer then grinding being obtained, in corundum crucible, at 600 ℃ of precalcining 1h, is cooled to room temperature and again fully grinds.Will be again grinding product be placed in high temperature box furnace in 1000 ℃ of sintering 2h, grind after being cooled to room temperature, obtain launching the K of blue light
3y
0.999tm
0.001b
2o
6luminescent material.
Embodiment 2 high temperature solid-state methods are prepared Li
3sc
0.995sm
0.005b
2o
6luminescent material
Take Li
2cO
30.4432g, Sc
2o
30.2744g, SmCl
30.0051g and B
2o
30.3064g (excessive 10%) is raw material.All raw materials are placed in to agate mortar and are fully ground to and mix, the powder transfer then grinding being obtained, in corundum crucible, at 800 ℃ of precalcining 0.5h, is cooled to room temperature and again fully grinds.Will be again grinding product be placed in high temperature box furnace in 800 ℃ of sintering 10h, grind after being cooled to room temperature, obtain launching the Li of orange red light
3sc
0.995sm
0.005b
2o
6luminescent material.
Embodiment 3 high temperature solid-state methods are prepared Na
3y
0.946sc
0.05pr
0.004b
2o
6luminescent material
Take Na
2c
2o
40.8040g, YCl
30.7388g, Sc
2o
30.0137g, Pr
6o
110.0027g and H
3bO
30.5442g (excessive 10%) is raw material.All raw materials are placed in to agate mortar and are fully ground to and mix, the powder transfer then grinding being obtained, in corundum crucible, at 700 ℃ of precalcining 0.5h, is cooled to room temperature and again fully grinds.Grinding product is placed in high temperature process furnances again, at the N that is 95: 5 by volume ratio
2and H
2under the reducing atmosphere that mixed gas forms, in 1000 ℃ of sintering 6h, grind after being cooled to room temperature, obtain launching the Na of ruddiness
3y
0.946sc
0.05pr
0.004b
2o
6luminescent material.
Embodiment 4 high temperature solid-state methods are prepared Na
3y
0.90tb
0.10b
2o
6luminescent material
Take Na
2cO
30.6360g, Y
2o
30.4064g, Tb
4o
70.0748g and H
3bO
30.5193g (excessive 5%) is raw material.All raw materials are placed in to agate mortar and are fully ground to and mix, the powder transfer then grinding being obtained, in corundum crucible, at 700 ℃ of precalcining 1h, is cooled to room temperature and again fully grinds.Grinding product is placed in high temperature process furnances again, at the N that is 95: 5 by volume ratio
2and H
2under the reducing atmosphere that mixed gas forms, in 900 ℃ of sintering 4h, grind after being cooled to room temperature, obtain launching the Na of green glow
3y
0.90tb
0.10b
2o
6luminescent material.
Fig. 1 is Na prepared by the present embodiment
3y
0.90tb
0.10b
2o
6the luminescent spectrum of luminescent material.As shown in Figure 1, the luminescent material that prepared by the present embodiment is that 544nm place launches arrowband green spectral at wavelength.
Embodiment 5 high temperature solid-state methods are prepared Li
3y
0.9gd
0.08sm
0.02b
2o
6luminescent material
Take Li
2c
2o
40.6114g, Y
2(CO
3)
30.6440g, Gd
2o
30.0580g, Sm
2(CO
3)
30.0192g and B
2o
30.3203g (excessive 15%) is raw material.All raw materials are placed in to agate mortar to be fully ground to and to mix, then powder transfer grinding being obtained in corundum crucible, at 800 ℃ of precalcining 1h, then in high temperature box furnace in 900 ℃ of sintering 16h, after being cooled to room temperature, grind, obtain launching the Li of orange-red light
3y
0.9gd
0.08sm
0.02b
2o
6luminescent material.
Embodiment 6 high temperature solid-state methods are prepared Na
3y
0.99tm
0.01b
2o
6luminescent material
Take Na
2cO
30.6360g, Y
2o
30.4471g, Tm
2o
30.0077g and H
3bO
30.5193g (excessive 5%) is raw material.All raw materials are placed in to agate mortar and are fully ground to and mix, the powder transfer then grinding being obtained, in corundum crucible, at 700 ℃ of precalcining 1h, is cooled to room temperature and again grinds.Will be again grinding product be placed in high temperature box furnace in 900 ℃ of sintering 4h, grind after being cooled to room temperature, obtain launching the Na of blue light
3y
0.99tm
0.01b
2o
6luminescent material.
Fig. 2 is Na prepared by the present embodiment
3y
0.99tm
0.01b
2o
6the luminescent spectrum of luminescent material.As shown in Figure 2, the luminescent material that prepared by the present embodiment is that 460nm place launches arrowband blue color spectrum at wavelength.
Embodiment 7 high temperature solid-state methods are prepared K
3y
0.79gd
0.2dy
0.01b
2o
6luminescent material
Take K
2c
2o
40.9974g, YCl
30.6170g, Gd
2o
30.1450g, Dy
2o
30.0074g and H
3bO
30.6431g (excessive 30%) is raw material.All raw materials are placed in to agate mortar and are fully ground to and mix, the powder transfer then grinding being obtained, in corundum crucible, at 600 ℃ of precalcining 2h, is cooled to room temperature and again fully grinds.Will be again grinding product be placed in high temperature box furnace in 1000 ℃ of sintering 15h, grind the K that obtains launching inclined to one side white light after being cooled to room temperature
3y
0.79gd
0.2dy
0.01b
2o
6luminescent material.
Embodiment 8 high temperature solid-state methods are prepared Na
3y
0.915ce
0.005tb
0.08b
2o
6luminescent material
Take Na
2cO
30.6360g, Y
2o
30.4132g, CeO
20.0034, Tb
4o
70.0597g and H
3bO
30.5193g (excessive 5%) is raw material.All raw materials are placed in to agate mortar and are fully ground to and mix, the powder transfer then grinding being obtained, in corundum crucible, at 700 ℃ of precalcining 1h, is cooled to room temperature and again fully grinds.Grinding product is placed in high temperature process furnances again, at the N that is 95: 5 by volume ratio
2and H
2under the reducing atmosphere that mixed gas forms, in 900 ℃ of sintering 4h, grind after being cooled to room temperature, obtain launching the Na of green glow
3y
0.915ce
0.005tb
0.08b
2o
6luminescent material.
Fig. 3 is Na prepared by the present embodiment
3y
0.915ce
0.005tb
0.08b
2o
6the luminescent spectrum of luminescent material.As shown in Figure 3, the luminescent material that prepared by the present embodiment is that 544nm place launches arrowband green spectral at wavelength.
Embodiment 9 high temperature solid-state methods are prepared Na
3y
0.997bi
0.003b
2o
6luminescent material
Take Na
2cO
30.6360g, Y
2o
30.4502g, Bi
2o
30.0027g and H
3bO
30.5193g (excessive 5%) is raw material.All raw materials are placed in to agate mortar and are fully ground to and mix, the powder transfer then grinding being obtained, in corundum crucible, at 700 ℃ of precalcining 1h, is cooled to room temperature and again fully grinds.Will be again grinding product be placed in high temperature box furnace in 900 ℃ of sintering 4h, grind after being cooled to room temperature, obtain launching the Na of UV-light
3y
0.997bi
0.003b
2o
6luminescent material.
Fig. 4 is Na prepared by the present embodiment
3y
0.997bi
0.003b
2o
6the luminescent spectrum of luminescent material.As shown in Figure 4, the luminescent material that prepared by the present embodiment is that 360nm place launches broadband UV-light at wavelength.
Embodiment 10 high temperature solid-state methods are prepared Na
3y
0.3lu
0.5tb
0.2b
2o
6luminescent material
Take Na
2c
2o
40.8040g, YCl
30.2343g, LuCl
30.5627g, TbCl
30.2122g and B
2o
30.3064g (excessive 10%) is raw material.All raw materials are placed in to agate mortar and are fully ground to and mix, the powder transfer then grinding being obtained, in corundum crucible, at 700 ℃ of precalcining 0.5h, is cooled to room temperature and again fully grinds.Grinding product is placed in high temperature process furnances again, at the N that is 95: 5 by volume ratio
2and H
2under the reducing atmosphere that mixed gas forms, in 950 ℃ of sintering 10h, grind after being cooled to room temperature, obtain launching the Na of green glow
3y
0.3lu
0.5tb
0.2b
2o
6luminescent material.
Embodiment 11 high temperature solid-state methods are prepared Na
3y
0.97ce
0.03b
2o
6luminescent material
Take Na
2cO
30.6360g, Y
2o
30.4380g, CeO
20.0206g and H
3bO
30.5193g (excessive 5%) is raw material.All raw materials are placed in to agate mortar and are fully ground to and mix, the powder transfer then grinding being obtained, in corundum crucible, at 700 ℃ of precalcining 1h, is cooled to room temperature and again fully grinds.Grinding product is placed in high temperature process furnances again, at the N that is 95: 5 by volume ratio
2and H
2under the reducing atmosphere that mixed gas forms, in 900 ℃ of sintering 4h, grind after being cooled to room temperature, obtain launching the Na of blue light
3y
0.97ce
0.03b
2o
6luminescent material.
Fig. 5 is Na prepared by the present embodiment
3y
0.97ce
0.03b
2o
6the luminescent spectrum of luminescent material.As shown in Figure 5, the luminescent material that prepared by the present embodiment is that 415nm place launches broadband blue light at wavelength.
Embodiment 12 high temperature solid-state methods are prepared Li
3y
0.4la
0.3eu
0.3b
2o
6luminescent material
Take Li
2cO
30.2217g, Y
2(CO
3)
30.1431g, LaCl
30.1471g, Eu
2o
30.1056g and B
2o
30.1740g (excessive 25%) is raw material.All raw materials are placed in to agate mortar and are fully ground to and mix, the powder transfer then grinding being obtained, in corundum crucible, at 800 ℃ of precalcining 1h, is cooled to room temperature and again fully grinds.Will be again grinding product be placed in 800 ℃ of sintering 20h of high temperature box furnace, grind after being cooled to room temperature, obtain launching the Li of ruddiness
3y
0.4la
0.3eu
0.3b
2o
6luminescent material.
Embodiment 13 high temperature solid-state methods are prepared Na
3gd
0.8tb
0.2b
2o
6luminescent material
Take Na
2cO
30.6360g, Gd
2(C
2o
4)
30.9256g, Tb
4o
70.1494g and H
3bO
30.5442g (excessive 10%) is raw material.All raw materials are placed in to agate mortar and are fully ground to and mix, the powder transfer then grinding being obtained, in corundum crucible, at 800 ℃ of precalcining 1h, is cooled to room temperature and again fully grinds.Grinding product is placed in high temperature process furnances again, at the N that is 95: 5 by volume ratio
2and H
2under the reducing atmosphere that mixed gas forms, in 800 ℃ of sintering 10h, grind after being cooled to room temperature, obtain launching the Na of green glow
3gd
0.8tb
0.2b
2o
6luminescent material.
Embodiment 14 high temperature solid-state methods are prepared Na
3y
0.5tb
0.5b
2o
6luminescent material
Take Na
2cO
30.6360g, Y
2o
30.2258g, Tb
4o
70.3736g and H
3bO
30.5689g (excessive 15%) is raw material.All raw materials are placed in to agate mortar and are fully ground to and mix, the powder transfer then grinding being obtained, in corundum crucible, at 700 ℃ of precalcining 1h, is cooled to room temperature and again fully grinds.Grinding product is placed in high temperature process furnances again, at the N that is 95: 5 by volume ratio
2and H
2under the reducing atmosphere that mixed gas forms, in 850 ℃ of sintering 12h, grind after being cooled to room temperature, obtain launching green Na
3y
0.5tb
0.5b
2o
6luminescent material.
Embodiment 15 high temperature solid-state methods are prepared Na
3y
0.947ce
0.003tb
0.05b
2o
6luminescent material
Take Na
2cO
30.6360g, Y
2o
30.4276g, CeO
20.0020g, Tb
4o
70.0373g and H
3bO
30.5442g (excessive 10%) is raw material.All raw materials are placed in to agate mortar and are fully ground to and mix, the powder transfer then grinding being obtained, in corundum crucible, at 700 ℃ of precalcining 1h, is cooled to room temperature and again fully grinds.Grinding product is placed in high temperature process furnances again, at the N that is 95: 5 by volume ratio
2and H
2under the reducing atmosphere that mixed gas forms, in 900 ℃ of sintering 10h, grind after being cooled to room temperature, obtain launching the Na of green glow
3y
0.947ce
0.003tb
0.05b
2o
6luminescent material.
Embodiment 16 high temperature solid-state methods are prepared K
3lu
0.98tm
0.01pr
0.01b
2o
6luminescent material
Take K
2cO
30.4146g, Lu (NO
3)
30.7075g, Tm (NO
3)
30.0071g, Pr
6o
110.0034g and H
3bO
30.2597g (excessive 5%) is raw material.All raw materials are placed in to agate mortar and are fully ground to and mix, the powder transfer then grinding being obtained, in corundum crucible, at 650 ℃ of precalcining 1.5h, is cooled to room temperature and again fully grinds.Will be again grinding product be placed in high temperature box furnace in 950 ℃ of sintering 4h, grind after being cooled to room temperature, obtain launching the K of blue light
3lu
0.98tm
0.01pr
0.01b
2o
6luminescent material.
Embodiment 17 high temperature solid-state methods are prepared Li
3la
0.9995sm
0.0005b
2o
6luminescent material
Take Li
2cO
30.2217g, La
2o
30.3256g, Sm
2(C
2o
4)
30.0003g and B
2o
30.1601g (excessive 15%) is raw material.All raw materials are placed in to agate mortar to be fully ground to and to mix, then powder transfer grinding being obtained in corundum crucible, at 750 ℃ of precalcining 0.5h, then in high temperature box furnace in 850 ℃ of sintering 15h, after being cooled to room temperature, grind, obtain launching the Li of orange red light
3la
0.9995sm
0.0005b
2o
6luminescent material.
Embodiment 18 high temperature solid-state methods are prepared Na
3gd
0.90sc
0.06pr
0.04b
2o
6luminescent material
Take Na
2c
2o
40.402g, GdCl
30.4745g, Sc
2o
30.0083g, Pr
6o
110.0136g and H
3bO
30.2721g (excessive 10%) is raw material.All raw materials are placed in to agate mortar and are fully ground to and mix, the powder transfer then grinding being obtained, in corundum crucible, at 700 ℃ of precalcining 0.5h, is cooled to room temperature and again fully grinds.Grinding product is placed in high temperature process furnances again, at the N that is 95: 5 by volume ratio
2and H
2under the reducing atmosphere that mixed gas forms, in 1000 ℃ of sintering 6h, grind after being cooled to room temperature, obtain launching the Na of ruddiness
3gd
0.90sc
0.06pr
0.04b
2o
6luminescent material.
Claims (1)
1. a preparation method for rare earth borate luminescent material, is characterized in that, comprises the following steps:
1. with K
2cO
3, Lu (NO
3)
3, Tm (NO
3)
3, Pr
6o
11and H
3bO
3for raw material, by K
3lu
0.98tm
0.01pr
0.01b
2o
6in the molar ratio of each element take raw material, and make H
3bO
3excessive 5% by aforementioned molar ratio, ground and mixed is even;
2. by step, the compound in 1., prior to 650 ℃ of precalcining 1.5h, is cooled to room temperature by precalcining product, grinds, then in 950 ℃ of sintering 4h;
3. by step, the sintered product in is 2. cooled to room temperature, obtains launching the rare earth borate luminescent material of blue light.
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| CN201010042740.3A CN101768441B (en) | 2010-01-11 | 2010-01-11 | Rare earth borate luminescent material and preparation material thereof |
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|---|---|---|---|
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| CN101768441B true CN101768441B (en) | 2014-07-23 |
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| CN112552910A (en) * | 2020-12-10 | 2021-03-26 | 广东工业大学 | Borate fluorescent powder with beta-potassium carbonate configuration and preparation method thereof |
| CN115367767B (en) * | 2022-08-05 | 2023-06-13 | 广东省科学院资源利用与稀土开发研究所 | Lithium sodium yttrium borate and cerium doped compound and crystal thereof, and preparation methods and application thereof |
| CN115571911B (en) * | 2022-09-28 | 2023-10-27 | 江苏迪飞达电子有限公司 | Praseodymium ion activated near infrared emission material and preparation method thereof |
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2010
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