CN103773367B - Fluorescent material for white light LED (Light Emitting Diode) and preparation method thereof - Google Patents
Fluorescent material for white light LED (Light Emitting Diode) and preparation method thereof Download PDFInfo
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Abstract
本发明公开了一种用于白光LED的荧光材料,其化学表达式为:AMⅠMⅡMⅢO6:cR,c表示R与AMⅠMⅡMⅢO6的物质的量之比为c:1,且0.001 ≤ c ≤ 0.75。A为Na,Li,K,Ag中的一种或其组合;M 为Ca,Mg,Sr,Ba,Zn,Pb中的一种或其组合;MⅡ为Ti,Zr,Si,Ge中的一种或其组合;MⅢ为Nb,Ta,V中的一种或其组合;R为Pr,Sm,Eu,Tb,Dy,Mn,Bi中的一种或其组合。该荧光材料激发带覆盖200~500 nm范围,发射带较窄即半高宽狭窄,并经紫外、近紫外和蓝光激发后可发射出可见光,与其他适当的各色荧光材料组合可制造白光发光装置。本发明原料廉价易得,制作工艺简单,是理想的白光LED用荧光候选材料。本发明还公开了一种用于白光LED的荧光材料的制备方法。
The invention discloses a fluorescent material for white light LED, the chemical expression of which is: AM Ⅰ M Ⅱ M Ⅲ O 6 : cR, c represents the ratio of the amount of R to AM Ⅰ M Ⅱ M Ⅲ O 6 is c: 1, and 0.001 ≤ c ≤ 0.75. A is one of Na, Li, K, Ag or a combination thereof; M One or a combination of Ca, Mg, Sr, Ba, Zn, Pb; M Ⅱ is one or a combination of Ti, Zr, Si, Ge; M Ⅲ is one of Nb, Ta, V Or a combination thereof; R is one of Pr, Sm, Eu, Tb, Dy, Mn, Bi or a combination thereof. The excitation band of the fluorescent material covers the range of 200-500 nm, the emission band is narrow, that is, the half maximum width is narrow, and it can emit visible light after being excited by ultraviolet, near ultraviolet and blue light. It can be combined with other appropriate fluorescent materials of various colors to manufacture white light emitting devices. . The invention has cheap and easy-to-obtain raw materials and simple manufacturing process, and is an ideal fluorescent candidate material for white LEDs. The invention also discloses a preparation method of the fluorescent material used for the white light LED.
Description
技术领域 technical field
本发明属于荧光材料科学的技术领域,具体涉及一种可被紫外、近紫外和蓝光有效激发的用于白光LED的荧光材料及制备方法。 The invention belongs to the technical field of fluorescent material science, and in particular relates to a fluorescent material for white LEDs that can be effectively excited by ultraviolet, near ultraviolet and blue light and a preparation method.
背景技术 Background technique
白光LED是发出的光色为白色的发光二极管,白光由多个波长的光构成。其具有效率高、使用耗能少、低压电源、适用性强、稳定性高、响应时间短、对环境无污染、多色发光等的优点。白光LED自1977年研发以后,经过几十年的发展白光LED在发光效率等诸多方面取得了长足的进展。如今其在我们生活中得到了广泛的应用,如车灯、照明、LCD显示和屏幕背光。然而,当前其还是主要用于屏幕显示,也由于其制造成本稍高,对温度要求敏感,所以想要替代现有光源仍需一定的改进。白光LED通常采用两种方法形成,一种是通过“蓝光技术”与荧光粉配合形成白光,根据人们对可见光的研究,人眼睛所能见的白光,至少需两种光的混合,即蓝色光和黄色光或者蓝色光、绿色光和红色光的模式。上述两种模式的白光,都需要蓝光,所以摄取蓝色光的方法已成为制造白光的关键,即所谓的蓝光技术;第二种是多种单色光混合方法,即通过不同的色彩的LED发光二极管,利用其驱动电压、发光输出、温度特性及寿命各不相同的特点来产生白光。目前普遍采用蓝光LED加YAG荧光粉的方式制作白光LED,虽然其制作工艺较为简单,技术成本较低,但其显色指数也相对较低。采用近紫外的LED加RGB三基色荧光粉理论上可以获得任意色温及较高显色指数的白光LED,但目前用于紫外LED荧光粉的技术尚未成熟。并且目前可应用于白光LED的荧光材料有的吸收波长范围窄导致转换效率低,有的稳定性差,如含N的掺Eu荧光材料虽然激发带宽但其发射带也宽,满足不了高性能器件的需要,所以研发一种用于背景光用途的新型高效荧光材料具有一定研究和实际应用价值。 White LED is a light-emitting diode that emits white light, and white light is composed of light of multiple wavelengths. It has the advantages of high efficiency, low energy consumption, low-voltage power supply, strong applicability, high stability, short response time, no pollution to the environment, and multi-color luminescence. Since the white LED was developed in 1977, after decades of development, the white LED has made great progress in many aspects such as luminous efficiency. Nowadays it has been widely used in our life, such as car lights, lighting, LCD display and screen backlight. However, it is still mainly used for screen display at present, and due to its slightly higher manufacturing cost and sensitivity to temperature requirements, certain improvements are still needed to replace existing light sources. White light LEDs are usually formed by two methods. One is to form white light through the combination of "blue light technology" and phosphor powder. According to people's research on visible light, white light that can be seen by human eyes requires at least a mixture of two kinds of light, that is, blue light. and yellow light or blue light, green light and red light mode. The above two modes of white light require blue light, so the method of absorbing blue light has become the key to making white light, the so-called blue light technology; the second is a method of mixing multiple monochromatic lights, that is, emitting light through LEDs of different colors Diodes generate white light by utilizing their different characteristics of driving voltage, luminous output, temperature characteristics, and lifetime. Currently, blue LEDs and YAG phosphors are generally used to produce white LEDs. Although the manufacturing process is relatively simple and the technical cost is low, its color rendering index is relatively low. Theoretically, white LEDs with any color temperature and higher color rendering index can be obtained by using near-ultraviolet LEDs plus RGB three-color phosphors, but the technology for ultraviolet LED phosphors is not yet mature. Moreover, some fluorescent materials that can be applied to white light LEDs currently have a narrow absorption wavelength range, resulting in low conversion efficiency, and some have poor stability. For example, although the excitation bandwidth of the Eu-doped fluorescent material containing N is wide, the emission band is also wide, which cannot meet the requirements of high-performance devices. Therefore, the development of a new type of high-efficiency fluorescent material for background light has certain research and practical application value.
发明内容 Contents of the invention
本发明的目的在于为了解决目前用于白光LED的荧光材料有的吸收波长范围窄导致转换效率低,有的稳定性差,如用于白光LED的含N的掺Eu荧光材料激发带宽但其发射带也宽,满足不了高性能器件的需要等问题,而提供一种激发带覆盖200~500 nm范围,发射带较窄即半高宽狭窄,并可被可被紫外、近紫外和蓝光有效激发的用于白光LED的荧光材料。 The purpose of the present invention is to solve the problem that some fluorescent materials currently used in white light LEDs have narrow absorption wavelength ranges resulting in low conversion efficiency and poor stability. It is also wide and cannot meet the needs of high-performance devices. Instead, it provides an excitation band covering the range of 200-500 nm, a narrow emission band, that is, a narrow half-maximum width, and can be effectively excited by ultraviolet, near-ultraviolet and blue light. Fluorescent materials for white LEDs.
本发明的目的还提供了一种用于白光LED的荧光材料的制备方法。 The object of the present invention is also to provide a method for preparing a fluorescent material for white LEDs.
为实现本发明目的,本发明采取以下技术方案, To realize the object of the present invention, the present invention takes the following technical solutions,
一种用于白光LED的荧光材料,其化学表达式为AMIMⅡMⅢO6:cR,其中,所述的A为Na,Li,K,Ag中的一种或其组合; A fluorescent material for white light LEDs, the chemical expression of which is AM I M Ⅱ M Ⅲ O 6 :cR, wherein said A is one of Na, Li, K, Ag or a combination thereof;
MI为Ca,M g,Sr,Ba,Zn,Pb中的一种或其组合; MI is one or a combination of Ca, Mg, Sr, Ba, Zn, Pb;
MⅡ为Ti,Zr,Si,Ge中的一种或其组合; M Ⅱ is one of Ti, Zr, Si, Ge or a combination thereof;
MⅢ为Nb,Ta,V中的一种或其组合; M Ⅲ is one or a combination of Nb, Ta, V;
O为氧元素; O is oxygen element;
c表示R与AMⅠMⅡMⅢO6的物质的量之比为c:1,且0.001 ≤ c ≤ 0.75; c means that the ratio of the amount of R to AM Ⅰ M Ⅱ M Ⅲ O 6 is c:1, and 0.001 ≤ c ≤ 0.75;
R为Pr,Sm,Eu,Tb,Dy,Mn,Bi中的一种或其组合。 R is one of Pr, Sm, Eu, Tb, Dy, Mn, Bi or a combination thereof.
所述的荧光材料进一步为Na1-xAxCaTiNbO6:cPr(A=Li、K或Ag,0 ≤ x ≤ 1)、 The fluorescent material is further Na 1-x A x CaTiNbO 6 :cPr (A=Li, K or Ag, 0 ≤ x ≤ 1),
NaCa1-x MI xTiNbO6:cPr(M =Mg、Sr、Ba、Zn或Pb,0 ≤ x ≤ 1)、 NaCa 1-x M I x TiNbO 6 :cPr(M =Mg, Sr, Ba, Zn or Pb, 0 ≤ x ≤ 1),
NaCaTi1-x MⅡ xNbO6:cPr(MⅡ=Zr、Si或Ge,0 ≤ x ≤ 1)、 NaCaTi 1-x M Ⅱ x NbO 6 :cPr (M Ⅱ =Zr, Si or Ge, 0 ≤ x ≤ 1),
NaCaTiNb1-x MⅢ xO6:cPr(MⅢ=Ta、或V,0 ≤ x ≤ 1)、 NaCaTiNb 1-x M Ⅲ x O 6 :cPr (M Ⅲ =Ta, or V, 0 ≤ x ≤ 1),
或NaCaTiNbO6:cR1、cR2(R1,R2=Pr、Sm、Eu、Tb、Dy、Mn或Bi) 。 Or NaCaTiNbO 6 : cR 1 , cR 2 (R 1 , R 2 =Pr, Sm, Eu, Tb, Dy, Mn or Bi).
此类荧光粉可实现包括红光、黄白光等可见光在内的可见光发射,如NaCaTiTaO6:0.005Pr具有红光发射,NaCaTiNbO6:0.01Dy具有黄白光发射等,此类荧光粉包括但不限于,下列所述的优选荧光材料:LiCaTiNbO6:0.005Pr、NaCaTiNbO6:0.005Pr、KCaTiNbO6:0.005Pr 、Na0.99Li0.01CaTiNbO6:0.005Pr、Na0.9Ag0.1CaTiNbO6:0.005Pr、NaMgTiNbO6:0.005Pr、NaSrTiNbO6:0.005Pr、NaBaTiNbO6:0.005Pr、NaZnTiNbO6:0.005Pr、NaCa0.99Mg0.01TiNbO6:0.005Pr、NaCa0.99Ba0.01TiNbO6:0.005Pr、NaCa0.99Sr0.01TiNbO6:0.005Pr、NaCa0.99Zn0.01TiNbO6:0.005Pr、NaCa0.99Pb0.01TiNbO6:0.005Pr 、NaCaZrNbO6:0.005Pr、NaCaGeNbO6:0.005Pr、NaCaSiNbO6:0.005Pr、NaCaTiTaO6:0.005Pr、NaCaTiNbO6:0.02Sm、NaCaTiNbO6:0.07Eu、NaCaTiNbO6:0.01Dy、NaCaTiNbO6:0.1Bi、NaCaTiNbO6:0.01Pr,0.01Bi、NaCaTiNbO6:0.005Pr,0.005Sm、NaCaTiNbO6:0.005Pr,0.005Mn。 This type of phosphor can realize visible light emission including red light, yellow and white light and other visible light, such as NaCaTiTaO 6 : 0.005Pr has red light emission, NaCaTiNbO 6 : 0.01Dy has yellow and white light emission, etc. Such phosphors include but are not limited to , the following preferred fluorescent materials: LiCaTiNbO 6 : 0.005Pr, NaCaTiNbO 6 : 0.005Pr, KCaTiNbO 6 : 0.005Pr, Na 0.99 Li 0.01 CaTiNbO 6 : 0.005Pr, Na 0.9 Ag 0.1 CaTiNbO 6 Ti : 0.005Pr, NaM6 0.005pr, NASRTININ: 0.005PR, Nabatinbo 6 : 0.005pr, Nazntinbo 6 : 0.005pr, NACA 0.99 MG 0.01 Tinbo 6 : 0.005pr, NACA 0.99 BA 0.01 Tinbo 6 : 0.99 SR 0.01 Tinbo 6 : 0.01 Tinbo , NACA 0.99 ZN 01 Tinbo 6 : 0.005pr, NACA 0.99 PB 0.01 Tinbo 6 : 0.005pr, NacazRNBO 6: 0.005pr, NacAgenbo 6 : 0.005pr 6: 0.005pr 6: 0.005PR, NACATINBO 6 : 0.005PR, NACATINBO 6 : 0.005PR, NACatinbo . _ _ _ _ _
一种如上述的用于白光LED的荧光材料的制备方法,包括以下步骤: A method for preparing a fluorescent material for a white light LED as described above, comprising the following steps:
a、依基质材料和使用的激活剂R按所述的荧光材料组成化学表达式中的任意一种进行配料; a. Dosing according to any one of the chemical expressions of the fluorescent material composition according to the matrix material and the activator R used;
b、将步骤a中所配原料经30分钟精细研磨后装入带盖刚玉坩埚中,置于煅烧炉中煅烧,煅烧温度为1100 ~1300°C,烧制时间为7 ~10小时,后经冷却,破碎,再次研磨得到该荧光材料。 b. Put the raw materials prepared in step a into a corundum crucible with a cover after being finely ground for 30 minutes, place them in a calciner for calcination, the calcination temperature is 1100 ~ 1300 ° C, and the firing time is 7 ~ 10 hours, after Cool, crush and grind again to obtain the fluorescent material.
一种用于白光LED的荧光材料的制备方法,进一步具体包括以下步骤: A method for preparing a fluorescent material for white light LEDs, further specifically comprising the following steps:
a、将含A的氧化物或碳酸盐,含M的氧化物或碳酸盐,含MⅡ的氧化物或碳酸盐,含MⅢ的氧化物或碳酸盐,含R的氧化物或碳酸盐按照所述的荧光材料组成化学表达式中的任意一种进行混合配料; a, the oxide or carbonate containing A, containing M Oxides or carbonates, oxides or carbonates containing M Ⅱ , oxides or carbonates containing M Ⅲ , oxides or carbonates containing R, according to the composition of the fluorescent material in the chemical expression Any one of the mixed ingredients;
b、将上述a步骤中的混合配料研细、混匀,装入带盖刚玉坩埚中,置于煅烧炉中煅烧,煅烧温度为1100 ~1300°C,烧制时间为7 ~10小时,后经冷却,破碎,再次研磨得到该荧光材料。 b. Grind and mix the mixed ingredients in the above step a, put them into a corundum crucible with a cover, place them in a calciner for calcining, the calcining temperature is 1100 ~ 1300 ° C, and the firing time is 7 ~ 10 hours. After cooling, crushing and grinding again, the fluorescent material is obtained.
本发明的实验方案简述如下: Experimental scheme of the present invention is briefly described as follows:
1. 材料的制备 1. Preparation of Materials
所述的荧光材料的原料为各元素的无机盐,包括但不限于氧化物、碳酸盐硝酸盐,并均采用高温固相法获得。通过该荧光材料的化学式计算出具体剂量,依据荧光粉基本材料和激活剂的不同,我们选择在各种原材料其熔点处煅烧10分钟,烧温度为1100 ~1300°C,制备时间为7~10小时,过程包括称量,煅烧,而后形成的晶体冷却经过破碎处理后仔细研磨得到本发明的荧光材料。 The raw materials of the fluorescent material are inorganic salts of various elements, including but not limited to oxides, carbonates and nitrates, all of which are obtained by high-temperature solid-phase method. The specific dose is calculated by the chemical formula of the fluorescent material. According to the difference of the basic material of the fluorescent powder and the activator, we choose to calcinate at the melting point of various raw materials for 10 minutes, the firing temperature is 1100 ~ 1300 ° C, and the preparation time is 7 ~ 10 minutes. Hours, the process includes weighing, calcining, and then the formed crystals are cooled, crushed and then carefully ground to obtain the fluorescent material of the present invention.
2. 性能评价 2. Performance evaluation
光学吸收发射性质:对本发明所得的荧光粉样品在日本日立公司的F-7000 FL Spectrophotometer测试其紫外-可见吸收发射光谱。总之本发明涉及将紫外光、近紫外光和蓝光转换为亮度较高的可见光、可用于白光LED荧光材料。本发明的荧光的材料可用于白光LED及相关显示、照明器件。本发明原材料简单易得,制作工艺简单,是理想的白光LED荧光粉候选材料。 Optical absorption and emission properties: the fluorescent powder sample obtained in the present invention tests its ultraviolet-visible absorption and emission spectrum on the F-7000 FL Spectrophotometer of Hitachi, Japan. In a word, the present invention relates to converting ultraviolet light, near ultraviolet light and blue light into visible light with higher brightness, which can be used in white LED fluorescent materials. The fluorescent material of the present invention can be used for white light LEDs and related display and lighting devices. The raw material of the invention is simple and easy to obtain, and the manufacturing process is simple, so it is an ideal candidate material for white light LED phosphor powder.
附图说明 Description of drawings
图1为本发明实施例1中NaCaTiNbO6:0.01Pr、NaCaTiNbO6:0.01Pr,0.01Bi材料的激发光谱(λem=615 nm)和发射光谱(λex=357 nm)。 Figure 1 shows the excitation spectrum (λ em =615 nm) and emission spectrum (λ ex =357 nm) of NaCaTiNbO 6 :0.01Pr, NaCaTiNbO 6 :0.01Pr,0.01Bi materials in Example 1 of the present invention.
图2为本发明实施例5中NaCaTiNbO6:0.02Sm材料的激发光谱(λem=567 nm;λem=602 nm)和发射光谱(λex=408 nm)。 Fig. 2 is the excitation spectrum (λ em =567 nm ; λ em =602 nm) and emission spectrum (λ ex =408 nm) of the NaCaTiNbO 6 :0.02Sm material in Example 5 of the present invention.
图3为本发明实施例6中NaCaTiNbO6:0.07Eu材料的激发光谱(λem=617 nm)和发射光谱(λex=398 nm)。 Fig. 3 is the excitation spectrum (λ em =617 nm) and emission spectrum (λ ex =398 nm) of the NaCaTiNbO 6 :0.07Eu material in Example 6 of the present invention.
图4为本发明实施例7中NaCaTiNbO6:0.01Dy材料的激发光谱(λem=485 nm;λem=576 nm)和发射光谱(λex=390 nm)。 Fig. 4 is the excitation spectrum (λ em =485 nm ; λ em =576 nm) and emission spectrum (λ ex =390 nm) of the NaCaTiNbO 6 :0.01Dy material in Example 7 of the present invention.
图5为本发明实施例15中Li0.01Na0.99CaTiNbO6:0.005Pr材料的激发光谱(λem = 615 nm)和发射光谱(λex = 357 nm)。 Fig. 5 shows the excitation spectrum (λ em = 615 nm) and emission spectrum (λ ex = 357 nm) of Li 0.01 Na 0.99 CaTiNbO 6 :0.005Pr material in Example 15 of the present invention.
图6为本发明实施例16中NaCa0.495Mg0.5TiNbO6:0.005Pr材料的激发光谱(λem = 613 nm)和发射光谱(λex = 343 nm)。 Fig. 6 is the excitation spectrum (λ em = 613 nm) and emission spectrum (λ ex = 343 nm) of NaCa 0.495 Mg 0.5 TiNbO 6 :0.005Pr material in Example 16 of the present invention.
图7为本发明实施例17中NaCa0.495Ba0.5TiNbO6:0.005Pr材料的激发光谱(λem = 613 nm)和发射光谱(λex = 276 nm)。 Fig. 7 shows the excitation spectrum (λ em = 613 nm) and emission spectrum (λ ex = 276 nm) of NaCa 0.495 Ba 0.5 TiNbO 6 :0.005Pr material in Example 17 of the present invention.
图8为本发明实施例18中NaCaTi0.9Zr0.1NbO6:0.005Pr材料的激发光谱(λem = 615 nm)和发射光谱(λex = 344 nm)。 Fig. 8 shows the excitation spectrum (λ em = 615 nm) and emission spectrum (λ ex = 344 nm) of NaCaTi 0.9 Zr 0.1 NbO 6 :0.005Pr material in Example 18 of the present invention.
图9为本发明实施例19中NaCaTiNb0.8Ta0.2O6:0.005Pr材料的激发光谱(λem = 615 nm)和发射光谱(λex = 358 nm)。 Fig. 9 shows the excitation spectrum (λ em = 615 nm) and emission spectrum (λ ex = 358 nm) of NaCaTiNb 0.8 Ta 0.2 O 6 :0.005Pr material in Example 19 of the present invention.
具体实施方式 Detailed ways
下面介绍本发明的实施方案,但本发明绝非仅限于实施方案 Embodiments of the present invention are described below, but the present invention is by no means limited to the embodiments
实施例1: Example 1:
将原料Na2CO3、CaCO3、TiO2、Nb2O5、Pr2O3按NaCaTiNbO6:0.01Pr化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,在825°C(CaCO3熔点)、851°C(Na2CO3熔点)分别煅烧10分钟,在1300°C煅烧2小时。经过冷却,精细研磨得到NaCaTiNbO6:0.01Pr荧光材料。测试结果见图1。 Weigh the raw materials Na 2 CO 3 , CaCO 3 , TiO 2 , Nb 2 O 5 , and Pr 2 O 3 according to the stoichiometric ratio of NaCaTiNbO 6 :0.01Pr, and mix them uniformly in a mortar for 30 minutes. The body was put into a corundum crucible with a cover and then put into a calcination furnace for calcination at 825°C (melting point of CaCO 3 ) and 851°C (melting point of Na 2 CO 3 ) for 10 minutes respectively, and at 1300°C for 2 hours. After cooling and fine grinding, NaCaTiNbO 6 :0.01Pr fluorescent material is obtained. The test results are shown in Figure 1.
实施例2: Example 2:
将原料Na2CO3、CaCO3、TiO2、Nb2O5、Pr2O3、Bi2O3按NaCaTiNbO6:0.01Pr,0.01Bi化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,851°C(Na2CO3熔点),在825°C(CaCO3熔点)煅烧10分钟,在1300°C煅烧2小时。经过冷却,精细研磨得到NaBaTiNbO6:0.01Pr,0.01Bi荧光材料。测试结果见图1。 Weigh the raw materials Na 2 CO 3 , CaCO 3 , TiO 2 , Nb 2 O 5 , Pr 2 O 3 , and Bi 2 O 3 according to the stoichiometric ratio of NaCaTiNbO 6 : 0.01Pr, 0.01Bi, and mix them uniformly in a mortar , with a duration of 30 minutes, the resulting fragments were put into a corundum crucible with a lid and then put into a calciner for calcination, at 851°C (Na 2 CO 3 melting point), at 825°C (CaCO 3 melting point) for 10 minutes, at 1300°C C calcined for 2 hours. After cooling and fine grinding, NaBaTiNbO 6 : 0.01Pr, 0.01Bi fluorescent material is obtained. The test results are shown in Figure 1.
实施例3: Example 3:
将原料Li2CO3、CaCO3、TiO2、Nb2O5、Pr2O3按LiCaTiNbO6:0.005Pr化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,618°C(Li2CO3熔点)、在825°C(CaCO3熔点)分别煅烧10分钟,在1200°C煅烧2小时。经过冷却,精细研磨得到LiCaTiNbO6:0.005Pr荧光材料。其在紫外激发下可有效发出红光。 Weigh the raw materials Li 2 CO 3 , CaCO 3 , TiO 2 , Nb 2 O 5 , and Pr 2 O 3 according to the stoichiometric ratio of LiCaTiNbO 6 :0.005Pr, and mix them uniformly in a mortar for 30 minutes. The body was put into a corundum crucible with a cover and then put into a calcination furnace for calcination, calcination at 618°C (melting point of Li 2 CO 3 ), calcination at 825°C (melting point of CaCO 3 ) for 10 minutes, and calcination at 1200°C for 2 hours. After cooling and fine grinding, LiCaTiNbO 6 :0.005Pr fluorescent material is obtained. It efficiently emits red light under ultraviolet excitation.
实施例4: Example 4:
将原料K2CO3、CaCO3、TiO2、Nb2O5、Pr2O3按KCaTiNbO6:0.005Pr化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,在825°C(CaCO3熔点)、891°C(K2CO3熔点)分别煅烧10分钟,在1300°C煅烧2小时。经过冷却,精细研磨得到KCaTiNbO6:0.005Pr荧光材料。其在紫外激发下可有效发出红光。 Weigh the raw materials K 2 CO 3 , CaCO 3 , TiO 2 , Nb 2 O 5 , and Pr 2 O 3 according to the stoichiometric ratio of KCaTiNbO 6 :0.005Pr, and mix them uniformly in a mortar for 30 minutes. The body was put into a corundum crucible with a cover and then put into a calcination furnace for calcination at 825°C (melting point of CaCO 3 ) and 891°C (melting point of K 2 CO 3 ) for 10 minutes respectively, and at 1300°C for 2 hours. After cooling and fine grinding, KCaTiNbO 6 :0.005Pr fluorescent material is obtained. It efficiently emits red light under ultraviolet excitation.
实施例5: Example 5:
将原料Na2CO3、CaCO3、TiO2、Nb2O5、Sm2O3按NaCaTiNbO6:0.02Sm化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,在825°C(CaCO3熔点)、851°C(Na2CO3熔点)分别煅烧10分钟,在1300°C煅烧2小时。经过冷却,精细研磨得到NaCaTiNbO6:0.02Sm荧光材料。测试结果见图2。 Weigh the raw materials Na 2 CO 3 , CaCO 3 , TiO 2 , Nb 2 O 5 , and Sm 2 O 3 according to the stoichiometric ratio of NaCaTiNbO 6 :0.02Sm, and mix them uniformly in a mortar for 30 minutes. The body was put into a corundum crucible with a cover and then put into a calcination furnace for calcination at 825°C (melting point of CaCO 3 ) and 851°C (melting point of Na 2 CO 3 ) for 10 minutes respectively, and at 1300°C for 2 hours. After cooling and fine grinding, NaCaTiNbO 6 :0.02Sm fluorescent material is obtained. The test results are shown in Figure 2.
实施例6: Embodiment 6:
将原料Na2CO3、CaCO3、TiO2、Nb2O5、Eu2O3按NaCaTiNbO6:0.07Eu化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,851°C(Na2CO3熔点)、在825°C(CaCO3熔点)分别煅烧10分钟,在1300°C煅烧2小时。经过冷却,精细研磨得到NaCaTiNbO6:0.07Eu荧光材料。测试结果见图3。 Weigh the raw materials Na 2 CO 3 , CaCO 3 , TiO 2 , Nb 2 O 5 , and Eu 2 O 3 according to the stoichiometric ratio of NaCaTiNbO 6 :0.07Eu, and mix them uniformly in a mortar for 30 minutes. The body was put into a corundum crucible with a cover and then put into a calciner for calcination at 851°C (melting point of Na 2 CO 3 ), calcination at 825°C (melting point of CaCO 3 ) for 10 minutes, and calcination at 1300°C for 2 hours. After cooling and fine grinding, NaCaTiNbO 6 :0.07Eu fluorescent material is obtained. The test results are shown in Figure 3.
实施例7: Embodiment 7:
将原料Na2CO3、CaCO3、TiO2、Nb2O5、Dy2O3按NaCaTiNbO6:0.01Dy化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,851°C(Na2CO3熔点)、在825°C(CaCO3熔点)分别煅烧10分钟,在1300°C煅烧2小时。经过冷却,精细研磨得到NaCaTiNbO6:0.01Dy荧光材料。测试结果见图4。 Weigh the raw materials Na 2 CO 3 , CaCO 3 , TiO 2 , Nb 2 O 5 , and Dy 2 O 3 according to the stoichiometric ratio of NaCaTiNbO 6 : 0.01Dy, and mix them uniformly in a mortar for 30 minutes. The body was put into a corundum crucible with a cover and then put into a calciner for calcination at 851°C (melting point of Na 2 CO 3 ), calcination at 825°C (melting point of CaCO 3 ) for 10 minutes, and calcination at 1300°C for 2 hours. After cooling and fine grinding, NaCaTiNbO 6 :0.01Dy fluorescent material is obtained. The test results are shown in Figure 4.
实施例8: Embodiment 8:
将原料Na2CO3、CaCO3、ZrO2、Nb2O5、Pr2O3按NaCaZrNbO6:0.005Pr化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,851°C(Na2CO3熔点)、在825°C(CaCO3熔点)分别煅烧10分钟,在1300°C煅烧2小时。经过冷却,精细研磨得到NaCaZrNbO6:0.005Pr荧光材料。其在紫外激发下可有效发出红光。 Weigh the raw materials Na 2 CO 3 , CaCO 3 , ZrO 2 , Nb 2 O 5 , and Pr 2 O 3 according to the stoichiometric ratio of NaCaZrNbO 6 :0.005Pr, and mix them uniformly in a mortar for 30 minutes. The body was put into a corundum crucible with a cover and then put into a calciner for calcination at 851°C (melting point of Na 2 CO 3 ), calcination at 825°C (melting point of CaCO 3 ) for 10 minutes, and calcination at 1300°C for 2 hours. After cooling and fine grinding, NaCaZrNbO 6 :0.005Pr fluorescent material is obtained. It efficiently emits red light under ultraviolet excitation.
实施例9: Embodiment 9:
将原料Na2CO3、MgO、TiO2、Nb2O5、Pr2O3按NaMgTiNbO6:0.005Pr化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,851°C(Na2CO3熔点)分别煅烧10分钟,在1100°C煅烧2小时。经过冷却,精细研磨得到NaMgTiNbO6:0.005Pr荧光材料。其在紫外激发下可有效发出红光。 Weigh the raw materials Na 2 CO 3 , MgO, TiO2, Nb 2 O 5 , and Pr 2 O 3 according to the stoichiometric ratio of NaMgTiNbO 6 :0.005Pr, and mix them uniformly in a mortar for 30 minutes. Put it into a corundum crucible with a cover and put it into a calcination furnace for calcination at 851°C (Na 2 CO 3 melting point) for 10 minutes and 1100°C for 2 hours. After cooling and fine grinding, NaMgTiNbO 6 :0.005Pr fluorescent material is obtained. It efficiently emits red light under ultraviolet excitation.
实施例10: Example 10:
将原料Na2CO3、ZnO、TiO2、Nb2O5、Pr2O3按NaZnTiNbO6:0.005Pr化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,851°C(Na2CO3熔点)煅烧10分钟,在1100°C煅烧2小时。经过冷却,精细研磨得到NaZnTiNbO6:0.005Pr荧光材料。其在紫外激发下可有效发出红光。 Weigh the raw materials Na 2 CO 3 , ZnO, TiO 2 , Nb 2 O 5 , and Pr 2 O 3 according to the NaZnTiNbO 6 :0.005Pr stoichiometric ratio, and mix them uniformly in a mortar for 30 minutes. Put it into a corundum crucible with a cover and put it into a calciner for calcination at 851°C (Na 2 CO 3 melting point) for 10 minutes, and at 1100°C for 2 hours. After cooling and fine grinding, NaZnTiNbO 6 :0.005Pr fluorescent material is obtained. It efficiently emits red light under ultraviolet excitation.
实施例11: Example 11:
将原料Na2CO3、SrCO3、TiO2、Nb2O5、Pr2O3按NaSrTiNbO6:0.005Pr化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,851°C(Na2CO3熔点)、在1100°C(SrCO3熔点)分别煅烧10分钟,在1300°C煅烧2小时。经过冷却,精细研磨得到NaSrTiNbO6:0.005Pr荧光材料。其在紫外激发下可有效发出红光。 Weigh the raw materials Na 2 CO 3 , SrCO 3 , TiO 2 , Nb 2 O 5 , and Pr 2 O 3 according to the stoichiometric ratio of NaSrTiNbO 6 :0.005Pr, and mix them uniformly in a mortar for 30 minutes. The body was put into a corundum crucible with a cover and then put into a calcination furnace for calcination at 851°C (Na 2 CO 3 melting point), at 1100°C (SrCO 3 melting point) for 10 minutes, and at 1300°C for 2 hours. After cooling and fine grinding, NaSrTiNbO 6 :0.005Pr fluorescent material is obtained. It efficiently emits red light under ultraviolet excitation.
实施例12: Example 12:
将原料Na2CO3、CaCO3、SiO2、Nb2O5、Pr2O3按NaCaSiNbO6:0.005Pr化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,851°C(Na2CO3熔点)、在825°C(CaCO3熔点)分别煅烧10分钟,在1100°C煅烧2小时。经过冷却,精细研磨得到NaCaSiNbO6:0.005Pr荧光材料。其在紫外激发下可有效发出红光。 Weigh the raw materials Na 2 CO 3 , CaCO 3 , SiO 2 , Nb 2 O 5 , and Pr 2 O 3 according to the stoichiometric ratio of NaCaSiNbO 6 :0.005Pr, and mix them uniformly in a mortar for 30 minutes. The body was put into a corundum crucible with a cover and then put into a calciner for calcination at 851°C (Na 2 CO 3 melting point), at 825°C (CaCO 3 melting point) for 10 minutes, and at 1100°C for 2 hours. After cooling and fine grinding, NaCaSiNbO 6 :0.005Pr fluorescent material is obtained. It efficiently emits red light under ultraviolet excitation.
实施例13: Example 13:
将原料Na2CO3、CaCO3、 GeO2、Nb2O5、Pr2O3按NaCa GeNbO6:0.005Pr化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,851°C(Na2CO3熔点)、在825°C(CaCO3熔点)分别煅烧10分钟,在1100°C煅烧2小时。经过冷却,精细研磨得到NaCa GeNbO6:0.005Pr荧光材料。其在紫外激发下可有效发出红光。 The raw materials Na 2 CO 3 , CaCO 3 , GeO 2 , Nb 2 O 5 , and Pr 2 O 3 were weighed according to the stoichiometric ratio of NaCa GeNbO 6 :0.005Pr, and uniformly mixed in a mortar for 30 minutes, and the obtained Separately put into a corundum crucible with a cover and then put into a calciner for calcination, calcination at 851°C (Na 2 CO 3 melting point), 825°C (CaCO 3 melting point) for 10 minutes, and 1100°C for 2 hours. After cooling and fine grinding, NaCa GeNbO 6 :0.005Pr fluorescent material is obtained. It efficiently emits red light under ultraviolet excitation.
实施例14: Example 14:
将原料Na2CO3、CaCO3、TiO2、Ta2O5、Pr2O3按NaCaTiTaO6:0.005Pr化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,851°C(Na2CO3熔点)、在825°C(CaCO3熔点)、1115°C (GeO2熔点)分别煅烧10分钟,在1300°C煅烧2小时。经过冷却,精细研磨得到NaCaTiTaO6:0.005Pr荧光材料。其在紫外激发下可有效发出红光。 Weigh the raw materials Na 2 CO 3 , CaCO 3 , TiO 2 , Ta 2 O 5 , and Pr 2 O 3 according to the stoichiometric ratio of NaCaTiTaO 6 :0.005Pr, and mix them uniformly in a mortar for 30 minutes. The body was put into a corundum crucible with a cover and then put into a calciner for calcination. Calcined at 851°C (melting point of Na 2 CO 3 ), calcination at 825°C (melting point of CaCO 3 ), and 1115°C (melting point of GeO 2 ) for 10 minutes respectively. Calcined at 1300°C for 2 hours. After cooling and fine grinding, NaCaTiTaO 6 :0.005Pr fluorescent material is obtained. It efficiently emits red light under ultraviolet excitation.
实施例15: Example 15:
将原料Li2CO3、Na2CO3、CaCO3、TiO2、Nb2O5、Pr2O3按Li0.01Na0.99CaTiNbO6:0.005Pr化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,在618°C(Li2CO3熔点)、825°C(CaCO3熔点)、851°C(Na2CO3熔点)分别煅烧10分钟,在1300°C煅烧2小时。经过冷却,精细研磨得到Li0.01Na0.99CaTiNbO6:0.005Pr荧光材料。测试结果见图5。 Weigh the raw materials Li 2 CO 3 , Na 2 CO 3 , CaCO 3 , TiO 2 , Nb 2 O 5 , and Pr 2 O 3 according to the stoichiometric ratio of Li 0.01 Na 0.99 CaTiNbO 6 : 0.005Pr, and carry out uniform Mixed for 30 minutes, the resulting fraction was put into a corundum crucible with a lid and then put into a calciner for calcination at 618°C (Li 2 CO 3 melting point), 825°C (CaCO 3 melting point), 851°C (Na 2 CO 3 melting point) were calcined for 10 minutes at 1300 °C for 2 hours, respectively. After cooling and fine grinding, Li 0.01 Na 0.99 CaTiNbO 6 :0.005Pr fluorescent material is obtained. The test results are shown in Figure 5.
实施例16: Example 16:
将原料Na2CO3、CaCO3、MgO、TiO2、Nb2O5、Pr2O3按NaCa0.495Mg0.5TiNbO6:0.005Pr化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,在825°C(CaCO3熔点)、851°C(Na2CO3熔点)分别煅烧10分钟,在1300°C煅烧2小时。经过冷却,精细研磨得到NaCa0.495Mg0.5TiNbO6:0.005Pr荧光材料。测试结果见图6。 Weigh the raw materials Na 2 CO 3 , CaCO 3 , MgO, TiO 2 , Nb 2 O 5 , and Pr 2 O 3 according to the stoichiometric ratio of NaCa 0.495 Mg 0.5 TiNbO 6 : 0.005Pr, and mix them uniformly in a mortar. For 30 minutes, the obtained fractions were put into a corundum crucible with a cover and then put into a calciner for calcination. Calcined at 825°C (melting point of CaCO 3 ) and 851°C (melting point of Na 2 CO 3 ) for 10 minutes respectively, and at 1300°C Calcined for 2 hours. After cooling and fine grinding, NaCa 0.495 Mg 0.5 TiNbO 6 :0.005Pr fluorescent material is obtained. The test results are shown in Figure 6.
实施例17: Example 17:
将原料Na2CO3、CaCO3、BaCO3、TiO2、Nb2O5、Pr2O3按NaCa0.495Ba0.5TiNbO6:0.005Pr化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,在825°C(CaCO3熔点)、851°C(Na2CO3熔点)分别煅烧10分钟,在1300°C煅烧2小时。经过冷却,精细研磨得到NaCa0.495Ba0.5TiNbO6:0.005Pr荧光材料。测试结果见图7。 Weigh the raw materials Na 2 CO 3 , CaCO 3 , BaCO 3 , TiO 2 , Nb 2 O 5 , and Pr 2 O 3 according to the stoichiometric ratio of NaCa 0.495 Ba 0.5 TiNbO 6 :0.005Pr, and mix them uniformly in a mortar. The duration is 30 minutes, and the obtained fractions are put into a corundum crucible with a cover and then put into a calciner for calcination, and calcined at 825°C (melting point of CaCO 3 ) and 851°C (melting point of Na 2 CO 3 ) for 10 minutes respectively, and at 1300°C C calcined for 2 hours. After cooling and fine grinding, NaCa 0.495 Ba 0.5 TiNbO 6 :0.005Pr fluorescent material is obtained. The test results are shown in Figure 7.
实施例18: Example 18:
将原料Na2CO3、CaCO3、TiO2、ZrO2、Nb2O5、Pr2O3按NaCaTi0.9Zr0.1NbO6:0.005Pr化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,在825°C(CaCO3熔点)、851°C(Na2CO3熔点)分别煅烧10分钟,在1300°C煅烧2小时。经过冷却,精细研磨得到NaCaTi0.9Zr0.1NbO6:0.005Pr荧光材料。测试结果见图8。 Weigh the raw materials Na 2 CO 3 , CaCO 3 , TiO 2 , ZrO 2 , Nb 2 O 5 , and Pr 2 O 3 according to the stoichiometric ratio of NaCaTi 0.9 Zr 0.1 NbO 6 :0.005Pr, and mix them uniformly in a mortar. The duration is 30 minutes, and the obtained fractions are put into a corundum crucible with a cover and then put into a calciner for calcination, and calcined at 825°C (melting point of CaCO 3 ) and 851°C (melting point of Na 2 CO 3 ) for 10 minutes respectively, and at 1300°C C calcined for 2 hours. After cooling and fine grinding, NaCaTi 0.9 Zr 0.1 NbO 6 :0.005Pr fluorescent material is obtained. The test results are shown in Figure 8.
实施例19: Example 19:
将原料Na2CO3、CaCO3、TiO2、Nb2O5、Ta2O5、Pr2O3按NaCaTiNb0.8Ta0.2O6:0.005Pr化学计量比进行称量,在研钵中进行均匀混合,时长为30分钟,所得分体装入带盖刚玉坩埚然后放入煅烧炉中煅烧,在825°C(CaCO3熔点)、851°C(Na2CO3熔点)分别煅烧10分钟,在1300°C煅烧2小时。经过冷却,精细研磨得到NaCaTiNb0.8Ta0.2O6:0.005Pr荧光材料。测试结果见图9。 Weigh the raw materials Na 2 CO 3 , CaCO 3 , TiO 2 , Nb 2 O 5 , Ta 2 O 5 , and Pr 2 O 3 according to the stoichiometric ratio of NaCaTiNb 0.8 Ta 0.2 O 6 : 0.005Pr, and uniformly Mixed for 30 minutes, the obtained fraction was put into a corundum crucible with a cover and then put into a calciner for calcination, and calcined at 825°C (CaCO 3 melting point) and 851°C (Na 2 CO 3 melting point) for 10 minutes, respectively. Calcined at 1300°C for 2 hours. After cooling and fine grinding, NaCaTiNb 0.8 Ta 0.2 O 6 :0.005Pr fluorescent material is obtained. The test results are shown in Figure 9.
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