AlN基荧光材料的合成及性质研究
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摘要
在20世纪末,日本的LED产业巨头开发出了应用高亮度GaN蓝色发光二极管(light emitting diode,简称LED)为基础,涂覆黄色荧光粉YAG:C(?)产生白光的照明器件。相比于白炽灯和荧光灯,固态LED光源具有很多优点,包括：安全性高(LED使用低压电源)、节能(消耗能量较同光效的白炽灯减少80%)、适用性很强(每个单元LED芯片可小至0.2mmm,也可大到正在发展的10cm以上)、寿命长(10万小时,光衰为初始的50%)、响应时间短(白炽灯的响应时间为毫秒级,LED灯的响应时间为纳秒级)、环保(无有害金属汞)等优点,因此,LED被称为第三代照明技术,在各个领域的应用越来越广泛,我国也出台了很多优惠政策加快LED产业的研发。
在普通照明领域,获得类似于太阳光的白光照明是人们的关注焦点。目前实现白光LED的主要方式有：(1)全芯片结构,即用红绿蓝三基色的LED芯片组合在一起,形成一个发光矩阵；(2)单芯片结构。利用蓝光LED和可被蓝光激发的黄色荧光粉或者红、绿荧光粉,这样形成了蓝光加黄光、蓝光加红绿光的白光产生形式。也可采用利用紫外LED和可被紫外LED激发的红绿蓝荧光粉,三基色组合成白光。多芯片发光不仅成本高,而且各个芯片的发光效率也很难相同,难以获得色温合适的日光器件。此外,多芯片集成的器件,热量的积聚会导致LED芯片的光衰,CIE色坐标和色温也会发生偏移。因此,现阶段主流是单芯片加荧光粉的白光实现方式。荧光粉在白光LED中起着举足轻重的作用,其发光效率、发光性质和稳定性直接决定着LED器件的性能。
传统的荧光粉主要是铝酸盐、硅酸盐、硫化物等。近年来,相继发现了发光离子掺杂氧氮化物基质的新型荧光材料,例如红色荧光粉M2Si5N8:Eu2+(M=Ca, Sr,Ba)、MAlSiN3:Eu2+(M=Ca,Sr),绿色荧光粉MSi2O2N2:Eu2+(M=Ca, Sr, Ba)和AlON:Mn2+, Mg2+、黄色荧光粉Ca-a-SiAlON:Eu2+,蓝色荧光粉AlN:Eu2+等。氧氮化物基质中,金属发光离子处在O/N离子组成的网络结构中,具有优异的化学和热稳定性,同时一般用于发光的稀土离子(Eu2+, Ce3+等)的5d能级裸露于离子外层,在晶格场的作用下会发生不同程度的分裂,N3-的电荷数高于O2-且N3-具有更强的共价性,从而富氮的晶体场环境能够引起较大的电子云重排效应(Nephelauxetic effect),导致发光离子(Eu2+, Ce3+等)的5d电子能级发生更大分裂,4f-5d跃迁能量向长波方向移动,荧光粉的激发和发射光谱发生红移,与蓝光LED匹配,产生黄光或红光。同时,可以调控基质晶格中的O/N比例,获
得不同发射波长的荧光粉。因此氧氮化物荧光粉是白光LED用的理想荧光转换材料,本文主要探讨了AlN基(AlN和AlON)荧光材料的结构和发光性质,研究制备条件、晶体结构、发光性能的关系,并进行了理论计算,阐述稀土离子的发光机理。
本文分为八章,第一章绪论部分介绍了照明发展历史和部分荧光粉,着重介绍了AlN基荧光材料的结构和发光性质。第二章为实验部分,介绍原料、设备、表征方法。
第三章报道了通过碳热还原法合成了纯AIN:Eu2+荧光粉。系统研究了反应温度、保温时间、Eu2+掺杂浓度和C含量对AIN:Eu2+荧光粉晶体结构和发光性质的影响,结果表明在较低的1750℃下保温8小时是获得高纯、高发光强度荧光粉的最优条件；证明了Eu2+在单独掺杂AlN时,也可以固溶进AlN晶格,这是因为利用碳热还原法却可以获得低氧含量的AIN:Eu2+粉体,没有条件形成铝酸盐,因此可以获得纯AIN:Eu2+荧光粉；AIN:Eu2+荧光粉在紫外光激发下,发射出470nm左右的蓝光,来自于Eu2+的5d-4f跃迁,并可通过改变起始粉料中的C含量,使发射峰从蓝光波段调控至绿光波段；研究了了不同种类的助溶剂对AIN:Eu2+荧光粉晶体结构和发光性质的影响,表明BaF2可以有效促进AlN的结晶和提高荧光粉的发光强度。
第四章介绍了利用气相还原法,可以获得极低氧含量、无C残留的高纯AlN：Eu2+荧光粉,在紫外光激发下发出540nm左右的绿光,相比于碳热还原法制备的荧光粉发射波长出现了明显红移。这是因为N的电子云膨胀效应,导致Eu2+的5d能级产生更大的劈裂。通过EDS、HRTEM、ED、EXAFS测试结果,证实了Eu取代了AlN中的Al格位。由于Eu2+和Al3+两者的半径相差太大,所以Eu的固溶度非常低,而且不可避免地会有Eu3+的存在。理论计算的结果与实验符合的非常好,进一步证实了Eu取代A1N晶格中的Al这一结论,从(P) DOS谱上可以看出,Eu的5d、Eu的6p以及Al的4s和4p态都对荧光粉的发光都有贡献。此外,初步探讨了AlN:Mn2+荧光粉的结构、发光性质和Mn在AlN晶格中的格位。
第五章介绍了固相反应法制备的AlON:Eu2+和AlON:Eu2+, Mg2+荧光粉的结构和发光性质,在紫外光激发下,AlON:Eu2+,Mg2+荧光粉发射出非常强烈的490nm左右的蓝绿光。在Eu单掺AlON时,Eu并不能掺入AlON晶格,在Eu, Mg共掺AlON时,Eu便可固溶进AlON晶格,这可能是因为Mg的掺杂导致AlON晶格扩大,利于Eu的掺入。
第六章报道了碳热还原法制备AlON:Eu2+, Mg2+荧光粉,相较于固相反应法,利用碳热还原法,可以在低温下制备得到AlON:Eu2+, Mg2+荧光粉。此外,碳热还原法制备的荧光粉颗粒小、杂相少、Eu2+含量多并且更多的Eu2+固溶进AlON晶格,这些因素导致荧光粉的发光强度远远大于固相反应法制备的荧光粉,且高于在365nm激发下的商业粉BAM。荧光粉的发光波长可通过改变起始粉料中的C含量,从蓝光调控至绿光区域。
第七章报道了利用高能球磨工艺首次制备纯相的AlON:Eu2+,Mg2+荧光粉。在高能球磨过程中,起始粉体不断非晶化以达到原子尺度上均匀混合,粉体的反应活性得到提高,在较低的反应温度下,即可得到纯AlON:Eu2+,Mg2+荧光粉。Eu2+的固溶度从碳热还原法中的0.2%扩大到0.5%,并且具有更好的发光强度。
第八章对Al2O3-AlN体系中存在的的多形体进行了展望,并以Al7O3N5为例,结果证明了可以在高温下合成Al7O3N5:Eu2+荧光粉,在紫外光激发下,发出高强度的460nm的蓝光,并对全文进行了总结。
In the end of20th centrury, LED industry leader of Japan developed a white luminescence device based on high bright GaN LED coated a yellow phosphor YAG: Ce3+. Compared with Incandescent bulb and fluorescent lamp, LED has many advantages, such as high safety (low voltage used), energy saving (reduced by80%compared with incandescent lamp), strong applicability (each LED size:0.2mm-10cm), long life (in100000hours, luminescence degration remains50%), short response time (LED:-ns, incandescent lamp:ms) and Environmental protection (Without harmful mercury). So LED is called the third generation luminescence technology, which is being applied in wide area. Besides, our country has introduced many preferential policies to speed up the development of LED industry. In genery lighting field, how to get white light similar to sunlight attracts people's attention. Nowdays, the ways to generate white light are:(1) full LED chips structure, which is the combination of red, green, blue three LED chip, forming a luminous matrix;(2) single LED chip. Blue LED is coated by yellow phosphor or red, green phosphor, which can be excited by blue light. Yellow and blue light or red, green, blue light can generate white light. Another way is the use of UV-LED coated by red, green and blue phosphor, which can be excited bu UV ray. Full chips cost too much and they have different luminous efficiency, leading to an improper colour temperature in lighting device. Full chips also make heat accumulation, which leads to a luminescence degration and a shift of CIE color coordinates and colour temperature. Therefore, the potential realization method is a single LED chip combined with phosphors.
Traditional phosphors are majorly Sulfide, aluminate, Portland and so on. In recent years, some novel oxynitride based phosphors have been developed, such as red phosphors M2Si5N8:Eu2+(M=Ca, Sr, Ba) and MAISiN3:Eu2+(M=Ca,Sr), green phosphor MSi2O2N2:Eu2+(M=Ca, Sr, Ba)and AlON:Mn2+, Mg2+, yellow phosphor Ca-a-SiAlON:Eu2+and blue phosphor AlN:Eu2+.For oxynitrides, metal ions are located in the O/N network, which make phosphors excellent chemical and thermal stability.5d energy level of rare earth(Eu2+, Ce3+) is bare in the crystal field and will split to a different degree. The charge of N3-is more than O2-and N3-shows stronger covalence. An N-rich crystal environment will cause larger Nephelauxetic effect, which leads to a larger5d split.4f-5d transitions will shift to longer wavelength. The redshift of excitation and emission spectra can be observed. Matched with blue LED, phosphors will exibit yellow or red emission. Meanwhile, the emission wavlength can be adjusted by changing O/N ratio in the matrix. So oxynitride phosphors are ideal Fluorescence conversion materials used in white LED. This paper majorly talks about structure and luminescence of AlN based phosphors (AlN and AlON). The relationship of preparation conditions, crystal structure, and luminous property is researched. The theoretical calculation is adopted to explain the luminescence mechanism.
This paper includes8chapters. The introduction as the first chapter starts with a description of the lighting history, part phosphors and mainly focus on the structure and optical property of AlN based phosphors. Chapter2is the experimental procedure, including raw materials, synthesis equipments, and characterization methods.
In chapter3, single phase AlN:Eu2+phosphor is obtained by carbothermal reduction method. The effect of reaction temperature, holding time, Eu2+concentration and C content on the structure and optical property of AlN:Eu2+phosphor is systematically researched. The results indicate low synthesis temperature1750℃and holding time8h is the optimal condition for the syethesis of pure and high luminous phosphors, which proves Eu2+can be dissolved into AlN without other ions co-doping. AlN:Eu2+powders with low oxygen content are achived by carbothermal reduction. It seems easy to get pure AlN:Eu2+phosphor because Aluminate is impossible to generate in this process. Under UV excitation, AlN:Eu2+shows blue emission at470nm, which is ascribed to5d-4f transition of Eu2+. The result indicates1750℃for8h is the optimal condition for the synthesis of AlN:Eu2+with high purity and luminescence intensity. The emission can be adjusted from blue to green band by changing C content in the rew materials. The effect of different fluxes on the structure and optical property of AlN:Eu2+is researched, indicating BaF2can effectively promotes the crystallinity of AlN and increases the luminecnce intensity.
In chapter4, high pure AlN:Eu2+phosphor with extreamly low oxygen content and no residual carbon is obtained by a novel gas reduction route. Under UV excitation, a green emission at540nm is observed. Compared with the emission in AlN:Eu2+phosphor prepared by carbothermal reduction, it shows a redshift here, which is due to larger5d split caused by nephelauxetic effect of N3-. EDS, HRTEM, ED and EXAFS results proves Eu substitution for Al sites in AlN crystal llatice. Because of the large different radius between Eu2+and Al3+, the solid solubility must be very low and Eu3+unavoidabley coexist in the products. The theoretical calculation result agrees well with the experimental, further proving that Eu2+ions occupy A13+sites.(P)DOS spectra show Eu5d, Eu6p, Al4s and Al4p all contribute to the luminescence of AlN:Eu2+phosphor. Besides, The structure and optical property and Mn location in AlN:Mn2+phosphor are also simply discussed.
Chapter5reports the structure and optical property of AlON:Eu2+and AlON:Eu2+, Mg2+phosphors synthesized by solid-state reaction. Under UV excitation, AlON: Eu2+, Mg2+phosphor show very strong blue-green emission at490nm. In single Eu doped AlON. It is found Eu can't dissolve into AlON crystal lattice. But with the favor of Mg co-doping, the result is inverse, which is possiblely dute to expanded crstal lattice afer Mg doping.
In chapter6, AlON:Eu2+, Mg2+phosphor is synthesized by carbothermal reduction method, which shows a character of low synthesis temperature compared with solid-state reaction. Besides, the phosphor synthesized by carbothermal reduction show much higher luminescence intensity than that by solid-state reaction due to the smaller particle size, better purity, laiger Eu2+ratio and more Eu2+content dissolved into AlON crystal lattice. Under the some365nm excitation, AlON:Eu2+, Mg2+phosphor shows better optical property, compared with famous commercial BAM phosphor.
In chapter7, single phase AlON:Eu2+, Mg2+phosphor is firstly obtained by high-energy ball mill route. In the process of mechachemical acticvation, decrystallizatoin and homogeneous mixing at an atom scale is gradualy achived in the starting materials. The reaction activation of the powders is greatly improved, resulting pure AlON:Eu2+, Mg2+phosphor under a low synthesis temperature. The solid solubility of Eu2+in Mg-AION increases from0.2%in products prepared by carbothermal reduction to0.5%here, also leading a better luminescence intensity.
Chapter8gives an outlook related polyroid in Al2O3-AIN system. Taken Al7O3N5as an example, the result proves Al7O3N5:Eu2+phosphor can be synthesized under high temperature, which is a blue phosphor with a emission460nm under UVexcitation. Furthermore, it is summarized through the full text.
在普通照明领域,获得类似于太阳光的白光照明是人们的关注焦点。目前实现白光LED的主要方式有：(1)全芯片结构,即用红绿蓝三基色的LED芯片组合在一起,形成一个发光矩阵；(2)单芯片结构。利用蓝光LED和可被蓝光激发的黄色荧光粉或者红、绿荧光粉,这样形成了蓝光加黄光、蓝光加红绿光的白光产生形式。也可采用利用紫外LED和可被紫外LED激发的红绿蓝荧光粉,三基色组合成白光。多芯片发光不仅成本高,而且各个芯片的发光效率也很难相同,难以获得色温合适的日光器件。此外,多芯片集成的器件,热量的积聚会导致LED芯片的光衰,CIE色坐标和色温也会发生偏移。因此,现阶段主流是单芯片加荧光粉的白光实现方式。荧光粉在白光LED中起着举足轻重的作用,其发光效率、发光性质和稳定性直接决定着LED器件的性能。
传统的荧光粉主要是铝酸盐、硅酸盐、硫化物等。近年来,相继发现了发光离子掺杂氧氮化物基质的新型荧光材料,例如红色荧光粉M2Si5N8:Eu2+(M=Ca, Sr,Ba)、MAlSiN3:Eu2+(M=Ca,Sr),绿色荧光粉MSi2O2N2:Eu2+(M=Ca, Sr, Ba)和AlON:Mn2+, Mg2+、黄色荧光粉Ca-a-SiAlON:Eu2+,蓝色荧光粉AlN:Eu2+等。氧氮化物基质中,金属发光离子处在O/N离子组成的网络结构中,具有优异的化学和热稳定性,同时一般用于发光的稀土离子(Eu2+, Ce3+等)的5d能级裸露于离子外层,在晶格场的作用下会发生不同程度的分裂,N3-的电荷数高于O2-且N3-具有更强的共价性,从而富氮的晶体场环境能够引起较大的电子云重排效应(Nephelauxetic effect),导致发光离子(Eu2+, Ce3+等)的5d电子能级发生更大分裂,4f-5d跃迁能量向长波方向移动,荧光粉的激发和发射光谱发生红移,与蓝光LED匹配,产生黄光或红光。同时,可以调控基质晶格中的O/N比例,获
得不同发射波长的荧光粉。因此氧氮化物荧光粉是白光LED用的理想荧光转换材料,本文主要探讨了AlN基(AlN和AlON)荧光材料的结构和发光性质,研究制备条件、晶体结构、发光性能的关系,并进行了理论计算,阐述稀土离子的发光机理。
本文分为八章,第一章绪论部分介绍了照明发展历史和部分荧光粉,着重介绍了AlN基荧光材料的结构和发光性质。第二章为实验部分,介绍原料、设备、表征方法。
第三章报道了通过碳热还原法合成了纯AIN:Eu2+荧光粉。系统研究了反应温度、保温时间、Eu2+掺杂浓度和C含量对AIN:Eu2+荧光粉晶体结构和发光性质的影响,结果表明在较低的1750℃下保温8小时是获得高纯、高发光强度荧光粉的最优条件；证明了Eu2+在单独掺杂AlN时,也可以固溶进AlN晶格,这是因为利用碳热还原法却可以获得低氧含量的AIN:Eu2+粉体,没有条件形成铝酸盐,因此可以获得纯AIN:Eu2+荧光粉；AIN:Eu2+荧光粉在紫外光激发下,发射出470nm左右的蓝光,来自于Eu2+的5d-4f跃迁,并可通过改变起始粉料中的C含量,使发射峰从蓝光波段调控至绿光波段；研究了了不同种类的助溶剂对AIN:Eu2+荧光粉晶体结构和发光性质的影响,表明BaF2可以有效促进AlN的结晶和提高荧光粉的发光强度。
第四章介绍了利用气相还原法,可以获得极低氧含量、无C残留的高纯AlN：Eu2+荧光粉,在紫外光激发下发出540nm左右的绿光,相比于碳热还原法制备的荧光粉发射波长出现了明显红移。这是因为N的电子云膨胀效应,导致Eu2+的5d能级产生更大的劈裂。通过EDS、HRTEM、ED、EXAFS测试结果,证实了Eu取代了AlN中的Al格位。由于Eu2+和Al3+两者的半径相差太大,所以Eu的固溶度非常低,而且不可避免地会有Eu3+的存在。理论计算的结果与实验符合的非常好,进一步证实了Eu取代A1N晶格中的Al这一结论,从(P) DOS谱上可以看出,Eu的5d、Eu的6p以及Al的4s和4p态都对荧光粉的发光都有贡献。此外,初步探讨了AlN:Mn2+荧光粉的结构、发光性质和Mn在AlN晶格中的格位。
第五章介绍了固相反应法制备的AlON:Eu2+和AlON:Eu2+, Mg2+荧光粉的结构和发光性质,在紫外光激发下,AlON:Eu2+,Mg2+荧光粉发射出非常强烈的490nm左右的蓝绿光。在Eu单掺AlON时,Eu并不能掺入AlON晶格,在Eu, Mg共掺AlON时,Eu便可固溶进AlON晶格,这可能是因为Mg的掺杂导致AlON晶格扩大,利于Eu的掺入。
第六章报道了碳热还原法制备AlON:Eu2+, Mg2+荧光粉,相较于固相反应法,利用碳热还原法,可以在低温下制备得到AlON:Eu2+, Mg2+荧光粉。此外,碳热还原法制备的荧光粉颗粒小、杂相少、Eu2+含量多并且更多的Eu2+固溶进AlON晶格,这些因素导致荧光粉的发光强度远远大于固相反应法制备的荧光粉,且高于在365nm激发下的商业粉BAM。荧光粉的发光波长可通过改变起始粉料中的C含量,从蓝光调控至绿光区域。
第七章报道了利用高能球磨工艺首次制备纯相的AlON:Eu2+,Mg2+荧光粉。在高能球磨过程中,起始粉体不断非晶化以达到原子尺度上均匀混合,粉体的反应活性得到提高,在较低的反应温度下,即可得到纯AlON:Eu2+,Mg2+荧光粉。Eu2+的固溶度从碳热还原法中的0.2%扩大到0.5%,并且具有更好的发光强度。
第八章对Al2O3-AlN体系中存在的的多形体进行了展望,并以Al7O3N5为例,结果证明了可以在高温下合成Al7O3N5:Eu2+荧光粉,在紫外光激发下,发出高强度的460nm的蓝光,并对全文进行了总结。
In the end of20th centrury, LED industry leader of Japan developed a white luminescence device based on high bright GaN LED coated a yellow phosphor YAG: Ce3+. Compared with Incandescent bulb and fluorescent lamp, LED has many advantages, such as high safety (low voltage used), energy saving (reduced by80%compared with incandescent lamp), strong applicability (each LED size:0.2mm-10cm), long life (in100000hours, luminescence degration remains50%), short response time (LED:-ns, incandescent lamp:ms) and Environmental protection (Without harmful mercury). So LED is called the third generation luminescence technology, which is being applied in wide area. Besides, our country has introduced many preferential policies to speed up the development of LED industry. In genery lighting field, how to get white light similar to sunlight attracts people's attention. Nowdays, the ways to generate white light are:(1) full LED chips structure, which is the combination of red, green, blue three LED chip, forming a luminous matrix;(2) single LED chip. Blue LED is coated by yellow phosphor or red, green phosphor, which can be excited by blue light. Yellow and blue light or red, green, blue light can generate white light. Another way is the use of UV-LED coated by red, green and blue phosphor, which can be excited bu UV ray. Full chips cost too much and they have different luminous efficiency, leading to an improper colour temperature in lighting device. Full chips also make heat accumulation, which leads to a luminescence degration and a shift of CIE color coordinates and colour temperature. Therefore, the potential realization method is a single LED chip combined with phosphors.
Traditional phosphors are majorly Sulfide, aluminate, Portland and so on. In recent years, some novel oxynitride based phosphors have been developed, such as red phosphors M2Si5N8:Eu2+(M=Ca, Sr, Ba) and MAISiN3:Eu2+(M=Ca,Sr), green phosphor MSi2O2N2:Eu2+(M=Ca, Sr, Ba)and AlON:Mn2+, Mg2+, yellow phosphor Ca-a-SiAlON:Eu2+and blue phosphor AlN:Eu2+.For oxynitrides, metal ions are located in the O/N network, which make phosphors excellent chemical and thermal stability.5d energy level of rare earth(Eu2+, Ce3+) is bare in the crystal field and will split to a different degree. The charge of N3-is more than O2-and N3-shows stronger covalence. An N-rich crystal environment will cause larger Nephelauxetic effect, which leads to a larger5d split.4f-5d transitions will shift to longer wavelength. The redshift of excitation and emission spectra can be observed. Matched with blue LED, phosphors will exibit yellow or red emission. Meanwhile, the emission wavlength can be adjusted by changing O/N ratio in the matrix. So oxynitride phosphors are ideal Fluorescence conversion materials used in white LED. This paper majorly talks about structure and luminescence of AlN based phosphors (AlN and AlON). The relationship of preparation conditions, crystal structure, and luminous property is researched. The theoretical calculation is adopted to explain the luminescence mechanism.
This paper includes8chapters. The introduction as the first chapter starts with a description of the lighting history, part phosphors and mainly focus on the structure and optical property of AlN based phosphors. Chapter2is the experimental procedure, including raw materials, synthesis equipments, and characterization methods.
In chapter3, single phase AlN:Eu2+phosphor is obtained by carbothermal reduction method. The effect of reaction temperature, holding time, Eu2+concentration and C content on the structure and optical property of AlN:Eu2+phosphor is systematically researched. The results indicate low synthesis temperature1750℃and holding time8h is the optimal condition for the syethesis of pure and high luminous phosphors, which proves Eu2+can be dissolved into AlN without other ions co-doping. AlN:Eu2+powders with low oxygen content are achived by carbothermal reduction. It seems easy to get pure AlN:Eu2+phosphor because Aluminate is impossible to generate in this process. Under UV excitation, AlN:Eu2+shows blue emission at470nm, which is ascribed to5d-4f transition of Eu2+. The result indicates1750℃for8h is the optimal condition for the synthesis of AlN:Eu2+with high purity and luminescence intensity. The emission can be adjusted from blue to green band by changing C content in the rew materials. The effect of different fluxes on the structure and optical property of AlN:Eu2+is researched, indicating BaF2can effectively promotes the crystallinity of AlN and increases the luminecnce intensity.
In chapter4, high pure AlN:Eu2+phosphor with extreamly low oxygen content and no residual carbon is obtained by a novel gas reduction route. Under UV excitation, a green emission at540nm is observed. Compared with the emission in AlN:Eu2+phosphor prepared by carbothermal reduction, it shows a redshift here, which is due to larger5d split caused by nephelauxetic effect of N3-. EDS, HRTEM, ED and EXAFS results proves Eu substitution for Al sites in AlN crystal llatice. Because of the large different radius between Eu2+and Al3+, the solid solubility must be very low and Eu3+unavoidabley coexist in the products. The theoretical calculation result agrees well with the experimental, further proving that Eu2+ions occupy A13+sites.(P)DOS spectra show Eu5d, Eu6p, Al4s and Al4p all contribute to the luminescence of AlN:Eu2+phosphor. Besides, The structure and optical property and Mn location in AlN:Mn2+phosphor are also simply discussed.
Chapter5reports the structure and optical property of AlON:Eu2+and AlON:Eu2+, Mg2+phosphors synthesized by solid-state reaction. Under UV excitation, AlON: Eu2+, Mg2+phosphor show very strong blue-green emission at490nm. In single Eu doped AlON. It is found Eu can't dissolve into AlON crystal lattice. But with the favor of Mg co-doping, the result is inverse, which is possiblely dute to expanded crstal lattice afer Mg doping.
In chapter6, AlON:Eu2+, Mg2+phosphor is synthesized by carbothermal reduction method, which shows a character of low synthesis temperature compared with solid-state reaction. Besides, the phosphor synthesized by carbothermal reduction show much higher luminescence intensity than that by solid-state reaction due to the smaller particle size, better purity, laiger Eu2+ratio and more Eu2+content dissolved into AlON crystal lattice. Under the some365nm excitation, AlON:Eu2+, Mg2+phosphor shows better optical property, compared with famous commercial BAM phosphor.
In chapter7, single phase AlON:Eu2+, Mg2+phosphor is firstly obtained by high-energy ball mill route. In the process of mechachemical acticvation, decrystallizatoin and homogeneous mixing at an atom scale is gradualy achived in the starting materials. The reaction activation of the powders is greatly improved, resulting pure AlON:Eu2+, Mg2+phosphor under a low synthesis temperature. The solid solubility of Eu2+in Mg-AION increases from0.2%in products prepared by carbothermal reduction to0.5%here, also leading a better luminescence intensity.
Chapter8gives an outlook related polyroid in Al2O3-AIN system. Taken Al7O3N5as an example, the result proves Al7O3N5:Eu2+phosphor can be synthesized under high temperature, which is a blue phosphor with a emission460nm under UVexcitation. Furthermore, it is summarized through the full text.
引文
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