稀土掺杂材料的光特性及其应用研究
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摘要
将光学高科技应用于防伪及激光防护领域一直是国际上的热点，基于稀土掺杂的特殊光吸收与频率变换材料就极具代表性。随着我国市场经济及各项技术的发展，各种假冒伪劣现象层出不穷，这对防伪技术的发展带来了机遇与挑战。稀土掺杂材料因其具有其他材料无法比拟的光学特性，在光学、工业加工、通信、传感等领域都已有广泛的应用，若能把此种材料与光学防伪相结合，制成特殊光谱防伪材料，并配套出一种新型的防伪检测仪器，将会对我国经济发展及稳定具有十分重要的意义。另一方面，随着现代化激光武器与激光侦测技术的普遍应用，信息战已是决定战场甚至战争胜负的关键。在现代和未来战场的发现、瞄准、锁定和摧毁四大环节中，信息战举足轻重。对前三个环节的应对即反发现、反瞄准、反锁定是防摧毁的先决条件。因此，掌握新型的激光防护材料已经迫在眉睫。稀土掺杂材料在其丰富的跃迁能级作用下，能吸收多种波长的激光能量，大幅度降低激光反射率，因而是一种十分具有发展潜力的激光防护材料。
本文首先介绍了稀土掺杂材料的主要合成方法，着重介绍了高温固相合成与微波合成新方法。根据微波与介质相互作用的关系，通过石墨与微波的良耦合性质，利用微波能量实现了小介电常数的稀土掺杂材料简便快捷地合成，克服了其他方法合成时间长、对设备要求高等缺点，并设计了一套具有混合加热、保温、隔热、改善加热均匀性等多重作用的微波耦合合成装置。
通过高温固相反应法分别合成了Er~(3+)/Yb~(3+)共掺和掺Nd~(3+)的频率下转换防伪涂料，分析了涂料的结构、发光原理并用自制的新型光谱防伪系统检验了其防伪特性。结果表明该涂料激发光和发射光均在人眼不可见的近红外区，比其它防伪涂料更具隐蔽性，而且具有多重防伪能力，使用方便，是十分实用的新型防伪产品。
在微波合成新方法中，将微波法应用于防伪材料的研究，首次用微波法合成了CaF_2：Er~(3+)/Yb~(3+)粉末，通过XRD测试证实Er~(3+)/Yb~(3+)已经进入基质晶体，并用有质动力理论解释了其形成原理。分析了材料的上转换发光谱以及红光发射较强的原因，最后讨论了该材料以及此种制备方法在防伪领域的应用潜力。
在微波合成新方法中，将微波法应用于激光防护材料的研究，首次用微波法合成了稀土掺杂的激光防护涂料，讨论了其反射率与热处理时间及掺杂浓度的关系，确定了最佳合成条件，并用反射光谱、温度、激光测距等实验证明该涂料能很好的对目标实现激光伪装防护。
The application of optical high-tech to security and laser protection fields hasalways being a hot topic. Frequency conversion and laser absorption materials dopedwith rare-earth ions are the most promising candidates for applications in such fields.With the development of our market economy, newly forgery techniques have beenproducing kinds of counterfeits. However, these situations bring opportunities andchallenges to the progress of anti-counterfeiting technology. Rare-earth dopedmaterials have more superior optical properties comparing with other materials. Itwould be very important to the stability and development of our economy, if we couldcombine these materials with optical anti-counterfeiting technologies and develop anew kind of detection equipment. Furthermore, with the universal application ofmodern laser weapons and laser detection technologies, information war is key to thediscovery, aim, lock and destruction areas of modern war. Anti-discovery, anti-aimand anti-lock are the preerquisites of anti-destruction. Consequently, the developmentof novel laser protection materials is a pressing issue. Rare-earth doped materials thatcan absorb lasers of various wavelengths and dramatically reduce reflectance with thehelp of their abundant energy levels would have great potential applications in laserprotection.
In this thesis, several synthesis methods of rare-earth ions doped material arefirstly introduced with an emphasis on the high-temperature solid-state reaction andnew microwave heating process methods. Based on the microwave heating theory andthe coupling effects between graphite and microwaves, the rare-earth doped materialswith low dielectric loss were synthesized. A microwave coupling insulation apparatusis designed to realize microwave-conventional hybrid heating. It can also improve theheating uniformity while keeping insulation.
By conventional high-temperature solid-state reaction, two anti-counterfeitcoatings doped with Nd~(3+)and co-doped with Er~(3+)/Yb~(3+), respectively, weresynthesized. Their structure and photoluminescence mechanisms were analyzed, andthe anti-counterfeiting features were also verified by a new security instrument madeby ourselves. The results indicated that these coatings were more covert than others,because their exciting and emitting lights were both in the near infrared (NIR) region,which were invisible to by human eyes. Besides, they were also a kind of multiple anti-forgery coatings very convenient for use as well. These make them a kind of veryuseful and novel anti-counterfeit product.
The new microwave heating method is applied to synthesize anti-counterfeitmaterials. Using the self-made instrument mentioned above, CaF2: Er~(3+)/Yb~(3+)wassynthesized for the first time in a microwave furnace. The X-ray diffraction (XRD)test results verified that RE~(3+)ions have been successfully doped into CaF2lattice. Theformation mechanism was explained by ponderomotive theory and the up-conversionemission spectrum was analyzed in detail as well. We found that its red emission ismuch stronger then the green and explained the reason of it. Afterwards, potentialapplications of the synthesis method and as-prepared material in anti-counterfeitingfield are discussed.
The new microwave heating meathod is applied to synthesize laser protectionmaterials. Rare-earth doped ultra-fine powders with low reflectance at several wavenumbers were synthesized in our microwave heating apparatus. Relationships amongreflectance, RE~(3+)concentration and hearting time were discussed. By mixing thepowders with coatings, the property of strong absorption could be transplanted tothem. Experiments of spectral reflectance, temperature and laser ranging wereperformed. The results verifed that these coatings could achieve excellent laserprotection. These findings may have potential applications in the fields of laserprotection and camouflage.
本文首先介绍了稀土掺杂材料的主要合成方法，着重介绍了高温固相合成与微波合成新方法。根据微波与介质相互作用的关系，通过石墨与微波的良耦合性质，利用微波能量实现了小介电常数的稀土掺杂材料简便快捷地合成，克服了其他方法合成时间长、对设备要求高等缺点，并设计了一套具有混合加热、保温、隔热、改善加热均匀性等多重作用的微波耦合合成装置。
通过高温固相反应法分别合成了Er~(3+)/Yb~(3+)共掺和掺Nd~(3+)的频率下转换防伪涂料，分析了涂料的结构、发光原理并用自制的新型光谱防伪系统检验了其防伪特性。结果表明该涂料激发光和发射光均在人眼不可见的近红外区，比其它防伪涂料更具隐蔽性，而且具有多重防伪能力，使用方便，是十分实用的新型防伪产品。
在微波合成新方法中，将微波法应用于防伪材料的研究，首次用微波法合成了CaF_2：Er~(3+)/Yb~(3+)粉末，通过XRD测试证实Er~(3+)/Yb~(3+)已经进入基质晶体，并用有质动力理论解释了其形成原理。分析了材料的上转换发光谱以及红光发射较强的原因，最后讨论了该材料以及此种制备方法在防伪领域的应用潜力。
在微波合成新方法中，将微波法应用于激光防护材料的研究，首次用微波法合成了稀土掺杂的激光防护涂料，讨论了其反射率与热处理时间及掺杂浓度的关系，确定了最佳合成条件，并用反射光谱、温度、激光测距等实验证明该涂料能很好的对目标实现激光伪装防护。
The application of optical high-tech to security and laser protection fields hasalways being a hot topic. Frequency conversion and laser absorption materials dopedwith rare-earth ions are the most promising candidates for applications in such fields.With the development of our market economy, newly forgery techniques have beenproducing kinds of counterfeits. However, these situations bring opportunities andchallenges to the progress of anti-counterfeiting technology. Rare-earth dopedmaterials have more superior optical properties comparing with other materials. Itwould be very important to the stability and development of our economy, if we couldcombine these materials with optical anti-counterfeiting technologies and develop anew kind of detection equipment. Furthermore, with the universal application ofmodern laser weapons and laser detection technologies, information war is key to thediscovery, aim, lock and destruction areas of modern war. Anti-discovery, anti-aimand anti-lock are the preerquisites of anti-destruction. Consequently, the developmentof novel laser protection materials is a pressing issue. Rare-earth doped materials thatcan absorb lasers of various wavelengths and dramatically reduce reflectance with thehelp of their abundant energy levels would have great potential applications in laserprotection.
In this thesis, several synthesis methods of rare-earth ions doped material arefirstly introduced with an emphasis on the high-temperature solid-state reaction andnew microwave heating process methods. Based on the microwave heating theory andthe coupling effects between graphite and microwaves, the rare-earth doped materialswith low dielectric loss were synthesized. A microwave coupling insulation apparatusis designed to realize microwave-conventional hybrid heating. It can also improve theheating uniformity while keeping insulation.
By conventional high-temperature solid-state reaction, two anti-counterfeitcoatings doped with Nd~(3+)and co-doped with Er~(3+)/Yb~(3+), respectively, weresynthesized. Their structure and photoluminescence mechanisms were analyzed, andthe anti-counterfeiting features were also verified by a new security instrument madeby ourselves. The results indicated that these coatings were more covert than others,because their exciting and emitting lights were both in the near infrared (NIR) region,which were invisible to by human eyes. Besides, they were also a kind of multiple anti-forgery coatings very convenient for use as well. These make them a kind of veryuseful and novel anti-counterfeit product.
The new microwave heating method is applied to synthesize anti-counterfeitmaterials. Using the self-made instrument mentioned above, CaF2: Er~(3+)/Yb~(3+)wassynthesized for the first time in a microwave furnace. The X-ray diffraction (XRD)test results verified that RE~(3+)ions have been successfully doped into CaF2lattice. Theformation mechanism was explained by ponderomotive theory and the up-conversionemission spectrum was analyzed in detail as well. We found that its red emission ismuch stronger then the green and explained the reason of it. Afterwards, potentialapplications of the synthesis method and as-prepared material in anti-counterfeitingfield are discussed.
The new microwave heating meathod is applied to synthesize laser protectionmaterials. Rare-earth doped ultra-fine powders with low reflectance at several wavenumbers were synthesized in our microwave heating apparatus. Relationships amongreflectance, RE~(3+)concentration and hearting time were discussed. By mixing thepowders with coatings, the property of strong absorption could be transplanted tothem. Experiments of spectral reflectance, temperature and laser ranging wereperformed. The results verifed that these coatings could achieve excellent laserprotection. These findings may have potential applications in the fields of laserprotection and camouflage.
引文
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