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8~10 μm长波红外谱段处于自然环境温度下的红外辐射波段并覆盖了许多分子的特征振动“指纹谱段”，因此在军事、医疗以及环境监测等领域有着重要应用。红外材料是构建各种红外系统的物质基础，特别是红外光纤材料，由于具有柔软易弯曲的特点，可方便的将红外信号传输至目标区域，因此特别适合狭小空间、强磁强电等环境下的红外信号和图像传输[1-2]。比如，用长波红外光纤排制成传像束，结合红外热像仪，可以用于变压器内部绕组温度的实时在线监测，实现智能电网负载的智能调控[3]。在医疗上，利用癌变组织与正常组织的温度差异[4]，可以用基于长波红外传像束的内窥镜实现体内病变组织的微创诊断，并利用病变组织对高温敏感特性[5]，用特定波段的红外激光辐照进行光热治疗，定向杀灭病变组织，实现诊疗一体化。
能够实现长波红外谱段传输的光纤主要有晶体光纤[6]、空芯光纤[7]、光子晶体光纤[8]和Te-基硫系玻璃光纤[9-15]。2002年，以色列特拉维夫大学[6]采用卤化银晶体光纤制备出长波光纤传像束，但是该方法制备的像元数比较低，仅有30~100元，且串扰率高达30%。2004年，美国罗格斯大学[7]采用空芯光纤制备出像元900元的传像束，但由于损耗过高，传像束传输长度仅为2.5 cm。Te-基硫系玻璃光纤具有物化性能稳定、传输带宽宽、弯曲不敏感、制备相对简单等特点，是一种优秀的长波红外传输材料，尤其适用于大面阵光纤传像束的制备。江苏师范大学[10]采用复丝法制备出大面阵Ge-As-Se-Te玻璃光纤传像束，其包层材料选用在红外波段有强吸收的有机聚合物PEI，导致光纤损耗偏高。As-Se-Te玻璃组成元素的熔沸点低，易于提纯，是制备低损耗长波红外光纤的理想组分之一。美国无定型公司[11]制备出As-Se-Te光纤，并采用叠片法制备出4900 pixel传像束，从红外成像图来看，断丝仍然较多。与红外相机联用，温度分辨率为0.35 K，进一步提高温度分辨率需要降低光纤的损耗。北京玻璃研究院[12]亦开展了As-Se-Te光纤的研制，但制备的光纤损耗高，约为1 dB/m，制约了传像束的性能。为了降低光纤损耗、提高传像束性能，文中开展了As-Se-Te硫系玻璃提纯及低损耗光纤制备研究。采用棒管法，拉制出丝径100 μm、具有芯包结构的低损耗长波红外传输光纤。利用叠片法，排制出150×150大面阵光纤传像束，并对传像束的传像特性进行了表征。
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实验原料Te、As、Se均为99.9999%高纯原料，Al的纯度为99.9%。所购Te、As、Se原料需进一步提纯处理，其中Se、Te采用真空多级蒸馏方式提纯：将高纯原料Se或Te加入到四节石英管中（见图1），同时加入0.05 wt%的Al作为除氧剂，一端密封，另一端接真空泵抽真空至7×10−3 Pa 以下。四温区炉依次升温，将Se、Te逐级蒸馏至第四节管中，获得精提纯原料。As原料在300 ℃下真空热处理2 h，除去表面氧杂质。石英管为羟基含量小于5×10−4 wt%的低羟基石英管，使用前首先用浓度为25%的氢氟酸浸泡20 min，然后用去离子水清洗干净，接着放入干燥箱内在200 ℃下干燥10 h。原料称量在水、氧含量均小于1×10−4 wt%的惰性气氛手套箱中进行。
图 1 Se、Te原料多级蒸馏示意图
Figure 1. Schematic diagram of multistage distillation of Se and Te raw materials
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光纤采用传统的棒管法拉制。拉纤芯棒玻璃组分为As30Se50Te20（AST），玻璃的制备采用传统的熔融淬冷法，根据制备工艺的不同，分别命名为AST-1、AST-2、AST-3、AST-4。采用商品原料不经任何处理提纯制备的玻璃样品记为AST-1；根据1.1节所述提纯工艺处理后的原料制备的玻璃样品记为AST-2；采用提纯后的原料，同时引入0.1 wt%的Al作为除氧剂，一起封入石英管，先在一侧高温熔制，之后将玻璃熔液蒸馏至另一侧，淬冷退火后得到最终玻璃样品，记为AST-3；在AST-3工艺基础上，进一步引入0.3 wt%的除羟剂TeCl4，所有原料真空封入U型管，高温熔制，之后边抽真空边蒸馏玻璃，再经均化、淬冷、退火后得到玻璃样品，记为AST-4。玻璃的高温熔制温度均为750 ℃，制备的光纤预制棒最终尺寸为Φ14 mm×150 mm。
光纤包层皮管采用真空旋管法制备。包层玻璃组分为As30Se51Te19，芯玻璃和包层玻璃的折射率分别约为2.90、2.89（@9 μm），光纤数值孔径约为0.24。首先采用与上文芯棒玻璃对应的工艺制备出包层皮管玻璃熟料，然后根据皮管规格尺寸精确称量玻璃熟料，把料装入内径17.5 mm的石英管中抽真空后熔封，装入高速离心旋管炉中，升温至580 ℃，高速旋转至3000 r/min，在离心效果作用下，玻璃熔液均匀附着在石英管内壁，最后冷却退火后得到包层皮管，其内外径尺寸分别为14.5、17.5 mm，详细制备过程可参考文献[16]。
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拉丝塔为英国SG Control公司生产，拉丝炉为窄温区拉丝炉，拉丝工作温度240 ℃，控温精度±0.2 ℃，拉丝速度约为10 m/min，光纤单丝直径100 μm。传像束采用叠片法制备，首先用排丝机排制光纤单片，采用光栅尺精确定位光纤的位置，然后用环氧树脂对光纤进行固定。再将光纤片涂胶，层叠压紧，固化后得光纤传像阵列。最后用金属管铠装，两端面研磨抛光。制备的传像束端面像元规格为150 pixel×150 pixel，呈六边形紧密排列，长度约350 mm。
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玻璃的热学性能采用耐驰公司（型号NetzschSTA 449C）差示扫描量热仪测试，升温速率为10 ℃/min，温度范围为室温至300 ℃，精度±1 ℃。玻璃红外透过光谱测试采用BRUKER VERTEX70型红外傅里叶变换光谱仪（测试精度为2 cm−1），样品双面抛光，厚度5 mm。成分测试采用电子探针成分分析仪（日本电子公司，型号JEOLJXA-8230）测试，测试电压15 kV，电流10 nA，光斑直径10 µm。光纤损耗光谱采用传统的截断法测试，分别采用红外傅里叶变换光谱仪和4.3 µm可调谐量子级联激光器（美国DAYLIGHT公司，型号TLS-SK-41043-MHF）进行测试，测试在室温下进行。光纤和传像束端面采用OLYMPUS-BX51M显微镜观测。红外光纤传像束成像测试利用自行搭建的光学系统，如图2所示，探测器为法国SOFRADIR公司生产的碲镉汞探测器，像元为320×256。
图 2 传像束成像测试系统示意图
Figure 2. Schematic diagram of bundles imaging test system
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表1列出了高纯原料提纯处理前后表面氧杂质含量，通过对比可以看出，由于单质原料的表面活性，直接采购的Te、As、Se原料表面均有一层氧化物，氧含量分别为1.3 at%、0.46 at%、0.48 at%。经提纯处理后，表面的氧含量分别降至0 at% （未检出）、0.06 at%、0.15 at%，说明适当的真空多级蒸馏或热处理的除氧效果显著。Te、As、Se单质的沸点分别为988、613.8、685 ℃，而其氧化物TeO2、As2O3、SeO2的沸点分别为450（升华）、457.2、315 ℃，均低于各自的单质材料。因此在多级蒸馏过程或真空热处理过程中，原料表面的氧化物率先气化并被真空泵抽走，达到除去氧杂质的目的。Te、Se原料还是C杂质的一个引入途径[17]，采用多级蒸馏工艺进行提纯时，不易挥发的碳杂质会残留在石英管中，从而也可同时达到除碳的效果。图3为As30Se50Te20芯棒玻璃和As30Se51Te19皮管玻璃的DSC曲线，其玻璃的转变温度Tg分别为137.5 ℃和139.1 ℃，非常接近，热学性能匹配。在测试温度范围内没有观察到明显的析晶峰，说明析晶起始温度与转变温度之差远大于100 ℃，表明该芯、包玻璃均具有优异的热学稳定性，适宜拉制光纤。
表 1 As、Se 、Te原料除杂前后表面氧含量
Table 1. O content of raw materials (As, Se, Te) before and after purification
O content/at% As Se Te Before purification 0.46 0.48 1.3 After purification 0.06 0.15 0 (undetected) 
图 3 As30Se50Te20和As30Se51Te19玻璃的DSC曲线
Figure 3. DSC curves of As30Se50Te20 and As30Se51Te19 glasses
图4所示为采用不同制备工艺所制备的As30Se50Te20玻璃样品的红外吸收光谱，内插图为样品的透过光谱，由于样品加工的表面质量和平行度的不同，使得透过率基线差异明显。但是通过吸收谱线，仍可以看到一系列吸收峰及其吸收强度的相对变化规律。采用商品化原料直接制备的AST-1玻璃，在2~16 µm波段存在一系列的杂质吸收峰，分别为2.9 µm处O-H键伸缩振动吸收、6.3 µm处H-O-H弯曲振动吸收、9.6 µm处As-O吸收、以及12~16 µm波段内由As-O/Te-O引起的吸收等。采用提纯后原料制备的AST-2玻璃，在上述波段的杂质吸收均得到显著降低，归因于原料经提纯处理后，表面的氧杂质得到了有效的消除，从而降低了玻璃中的氧杂质含量，改善了玻璃的氧杂质吸收。在AST-3玻璃的红外光谱中，2.9、6.3、9.6 µm处的吸收基本得到消除，12 μm后的吸收也得到进一步降低，但是同时出现了4.5 μm处的H-Se杂质吸收。与AST-2相比，AST-3引入了0.1 wt%的铝作为除氧剂，铝单质与玻璃中的氧杂质充分反应生成Al2O3，Al2O3具有高的熔沸点和低的饱和蒸气压，通过蒸馏工艺被排出玻璃之外，因此进一步降低了玻璃中的氧杂质吸收。同时，随着氧含量的降低，玻璃中的氢杂质由O-H键逐渐趋向与Se元素结合形成H-Se键，因此导致了玻璃中4.5 μm处H-Se杂质吸收的增大，反应方程式为：
图 4 不同工艺制备的AST玻璃样品的红外吸收光谱（内插图为玻璃样品的红外透过光谱）
Figure 4. Infrared absorption spectra of AST glass samples prepared by different processes (The inset shows the infrared transmission spectra of all samples)
$$ 2{\rm{Al}}{_{solid}} + 3{\rm{O}} - {{\rm{H}}_{liquid}} \to {\rm{Al}}{_2}{{\rm{O}}_{3solid}} + 3{{\rm{H}}_{liquid}} $$ (1) $$ - {{\rm{H}}_{liquid}} + {\rm{As}} - {\rm{Se}}{_{liquid}} \to {\rm{H}} - {{\rm{Se}}_{liquid}} + - {{\rm{As}}_{liquid}} $$ (2) AST-4的红外吸收光谱与AST-3相比，4.5 μm处的H-Se杂质吸收得到消除，但12 μm后的吸收反而升高。AST-4玻璃制备过程进一步引入了除羟剂TeCl4，玻璃熔制过程中，其与羟基反应生成HCl，随后在抽真空蒸馏过程中将H杂质排出玻璃外，反应方程式为：
$$ {\rm{TeCl}}{_4} + 4{\rm{H}} - {{\rm{Se}}_{liquid}} \to 4 - {{\rm{Se}}_{liquid}} + - {{\rm{Te}}_{liquid}} + 4{\rm{HCl}}{_{gas}} \uparrow $$ (3) 因此AST-4样品的4.5 μm处的H-Se杂质吸收得到消除。但是TeCl4作为一种氯化物极易吸潮，使得玻璃中的氧杂质含量升高，因此导致了12 μm后的氧杂质吸收抬升。考虑到AST玻璃主要是用于8~10 μm长波红外传输，因此选择了AST-3玻璃工艺制备后续光纤。
图5（a）所示为制备的拉纤预制棒棒管组合照片；图5（b）所示为预制棒组合在红外拉丝塔上拉制成丝径100 μm的光纤；拉丝时，预制棒组合外加一层聚醚酰亚胺涂覆层，使得该光纤机械性能良好，弯曲半径不大于5 mm，见图5（c），该光纤纤芯直径78 μm、包层直径95 μm、涂覆层厚度约2.5 μm；图5（d）所示为采用AST-3工艺所制备光纤的损耗谱，为便于耦合，损耗测试所用光纤的丝径为280 μm。通过光纤的损耗光谱可以看出，该光纤低损耗区域位于7~9 μm波段，吸收基线约为0.2 dB/m，光纤在4.5 μm和6.3 μm处存在两处吸收峰，吸收强度分别为3.8 dB/m和10.6 dB/m。与玻璃红外光谱相比，光纤中出现了6.3 μm处的H2O分子吸收，产生的原因可能是由于拉丝时通入的惰性保护气中含有微量的水蒸汽杂质，水蒸汽吸附在芯棒和皮管界面，经高温拉丝后，产生了水分子的杂质吸收。水在6.3 μm处引起的吸收系数约为34 dB/(m·ppm)[18]（1 ppm=1×10−4 wt%），由此计算可得光纤中水分子的含量约为0.3 ppm。采用红外成像测试系统对单根光纤的传输性能进行了测试，光纤端面输出光斑的能量分布见图5（e），由此可以看出，在非相干连续光耦合下，光场基本呈均匀分布，表现出典型的大芯径多模光纤能量分布。
图 5 (a)拉纤预制棒；(b)拉制的AST光纤；(c) AST光纤的弯曲性能测试；(d) AST光纤的损耗光谱；(e)光纤端面能量分布
Figure 5. (a) Optical fiber preform; (b) The prepared AST glass fiber; (c) Bending test of the AST fiber; (d) Loss spectrum of AST glass fiber; (e) Energy distribution at the fiber end face
采用叠片法制备出长约350 mm，像元为150 pixel×150 pixel，面阵呈紧密排列的长波红外光纤传像束。抛光加工后的端面光学显微成像照片如图6（a）所示，像元单丝排列基本规整，端面光洁，无划痕、斑裂等缺陷。光纤填充系数K可表示为：
图 6 (a)传像束端面显微照片；(b)传像束对黑体面光源成像；(c)传像束对红外目标成像
Figure 6. (a) Micrograph of the coherent fiber bundle; (b) Infrared thermal imaging of the bundle for the planar array black body; (c) Infrared thermal imaging of the bundle for the infrared target
$$ K = \frac{\pi }{{2\sqrt 3 }}{\left( {\frac{d}{D}} \right)^2} $$ (4) 式中：d为光纤纤芯直径；D为光纤单丝外径。文中制备的光纤外径100 μm，纤芯直径78 μm，由公式（4）计算可得传像束的理论填充系数约为55%。100 μm像元直径在六边形紧密排列时的理论分辨率约为6 lp/mm。
光纤断丝率R定义为：
$$ R = {Q_b}/{Q_t} $$ (5) 式中：Qb为光纤束断丝的根数；Qt为光纤束总的像元数量。利用图2所示成像系统对传像束进行断丝率测试，成像目标物为红外大面阵热源，红外成像图见图6（b）。可以看出，光纤的断丝集中在四周边界部位，主要系铠装过程中受力所致，内部有效区域透过均匀，无黑丝、暗丝，传像束的整体断丝率小于3‰。
利用图2的光纤传像束成像测试系统，对红外目标物电烙铁进行成像，见图6（c）。可以看出，目标物成像清晰，不同温区成像对比明显、层次分明，温度分辨良好。成像无明显畸变，表明传像束两端阵列对应规整，传像束综合成像质量良好。
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采用多级蒸馏工艺和真空热处理工艺对Te、As、Se高纯原料开展了提纯研究， 原料表面氧杂质含量分别由1.3 at%、0.46 at%、0.48 at%降至0 at% （未检出）、0.06 at%、0.15 at%，除氧效果显著。
研究了As-Se-Te玻璃的提纯除杂工艺，结果表明，采用Al做除氧剂结合蒸馏提纯工艺制备的样品具有良好的长波红外透过性能。制备的光纤在长波红外波段损耗基线约为0.2 dB/m，弯曲半径小于5 mm。
制备出像元2.25万、单丝呈紧密排列的长波光纤传像束，传像束有效区域透过均匀，无黑丝、暗丝，整体断丝率小于3 ‰。对红外目标进行成像，成像清晰、对比度层次分明、无明显畸变，综合成像质量良好。
Preparation and imaging properties of coherent chalcogenide glass fiber bundles with large planar array for far-infrared transmission (invited)
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摘要: 长波红外光纤传像束在军事、医疗以及环境监测等领域有着重要应用。当前，长波红外光纤高的光学损耗制约了红外光纤传像束的性能和应用。为了制备低损耗长波红外光纤，选择As-Se-Te硫系玻璃组分，首先对As、Se、Te高纯原料进行了提纯工艺研究，原料表面氧杂质含量分别由1.3 at%、0.46 at%、0.48 at%降至0 at% （未检出）、0.06 at%、0.15 at%，除氧效果显著。以As-Se-Te玻璃为基质组分，对比研究了制备工艺对玻璃红外透过谱段的影响，采用Al作为除氧剂结合蒸馏提纯工艺，制备出热学性能优异、长波红外谱段良好的红外硫系玻璃。采用棒管法拉制出丝径100 μm的光纤，弯曲半径小于5 mm，在长波红外波段损耗基线约为0.2 dB/m。采用叠片法制备出像元2.25万，单丝呈紧密排列的光纤传像束，断丝率小于3‰，传像束有效区域透过均匀，无黑丝、暗丝，对红外目标成像清晰，无明显畸变，综合成像质量良好。Abstract:
Objective The 8-10 μm far-infrared spectrum is in the infrared radiation band at natural temperatures and covers the characteristic "fingerprint spectrum" of many molecules, so it has important applications in the military, medical and environmental monitoring fields. Infrared coherent fiber bundles which can realize the flexible transmission of infrared image are the basic components for assembling various infrared optical systems, and they can be used in the narrow space, high-intensity electric or magnetic field in particular. The main types of far infrared fibers mainly include crystal fiber, hollow fiber, photonic crystal fiber and Te- based chalcogenide glass fiber. Among them, Te-based fiber is an excellent far-infrared transmission material due to its wide transmission band, stable thermal, chemical properties, which means it is especially suitable for the preparation of coherent optical fiber bundles with large array. Until now, a series of components such as Ge-As-Se-Te, GeTe-AgI, Ga-Ge-Te, Ge-Te-I and As-Se-Te have been studied. However, the optical loss of Te-base fiber is still higher at present, which limits the transmission distance of infrared signal and the resolution of the infrared bundles. Therefore, it is necessary to study the purification technology for optimizing the optical loss. Methods High purity raw materials of As, Se and Te were purified by multi-distillation purification technique and the content of O element was examined by EPMA. As-Se-Te chalcogenide glass was chosen and melted by different preparation process and their infrared transmission spectra were measured by FTIR. The optical fiber was drawn by the rod-in-tube method. The drawing temperature was 240 ℃ with the accuracy of ±0.2 ℃, and the drawing speed was about 10 m/min. The coherent fiber bundle was prepared by ribbon-stacking technique. The end face was observed by microscope. Infrared image was detected by home-made optical system and mercury cadmium telluride detector was used (Fig.2). Results and Discussions The oxygen content of As, Se, Te raw materials decreased from 1.3 at%, 0.46 at% and 0.48 at% in raw materials to 0 at% (undetected), 0.06 at% and 0.15 at% in purified materials respectively, indicating that the distillation process was effective (Tab.1). The transition temperature Tg is 137.5 ℃ for core material and 139.1 ℃ for clad material (Fig.3), which are very close and match well. No obvious crystallization peak was observed in the test temperature range, indicating that the core and clad glass are suitable for fiber drawing. Smooth spectrum was obtained in the sample of aluminum as a deaerator (Fig.4). The optical fiber with an outer diameter of 100 μm was obtained. Its bending radius is less than 5 mm, and the baseline of the optical loss is about 0.2 dB/m in the far infrared range (Fig.5). Finally, the coherent fiber bundle with 22.5 thousand pixels and close-packed arrangement was prepared. The total fracture rate is less than 3‰ and there are none black or dark pixels in the center region of the bundle. The bundle transmits infrared beam uniformly and the image of the infrared target is clear and distortionless, which indicates that the comprehensive properties of the bundle are satisfactory (Fig.6). Conclusions Far-infrared fiber bundles was prepared and measured. In order to eliminate impurities, As-Se-Te chalcogenide glass was chosen and the high purity raw materials of As, Se and Te were purified. As-Se-Te glasses were melting by different preparation process and their infrared transmission spectra were measured and analyzed. The results show that excellent thermal and far-infrared transmitting performance can be obtained in the sample of Al as deoxidizer process. The optical fiber was drawn with an outer diameter of 100 μm, bending radius of less than 5 mm, optical loss of 0.2 dB/m. The coherent fiber bundle was prepared by ribbon-stacking technique. It has 22.5 thousand pixels and the total fracture rate is less than 3‰. The infrared target imaging was distortionless and showed fine temperature resolution, demonstrating that the bundles can be widely used in infrared imaging systems. -
Key words:
- chalcogenide glasses /
- far-infrared fiber /
- low optical attenuation /
- image bundles /
- infrared imaging
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图 1 Se、Te原料多级蒸馏示意图
Figure 1. Schematic diagram of multistage distillation of Se and Te raw materials
图 3 As30Se50Te20和As30Se51Te19玻璃的DSC曲线
Figure 3. DSC curves of As30Se50Te20 and As30Se51Te19 glasses
图 4 不同工艺制备的AST玻璃样品的红外吸收光谱（内插图为玻璃样品的红外透过光谱）
Figure 4. Infrared absorption spectra of AST glass samples prepared by different processes (The inset shows the infrared transmission spectra of all samples)
图 5 (a)拉纤预制棒；(b)拉制的AST光纤；(c) AST光纤的弯曲性能测试；(d) AST光纤的损耗光谱；(e)光纤端面能量分布
Figure 5. (a) Optical fiber preform; (b) The prepared AST glass fiber; (c) Bending test of the AST fiber; (d) Loss spectrum of AST glass fiber; (e) Energy distribution at the fiber end face
图 6 (a)传像束端面显微照片；(b)传像束对黑体面光源成像；(c)传像束对红外目标成像
Figure 6. (a) Micrograph of the coherent fiber bundle; (b) Infrared thermal imaging of the bundle for the planar array black body; (c) Infrared thermal imaging of the bundle for the infrared target
表 1 As、Se 、Te原料除杂前后表面氧含量
Table 1. O content of raw materials (As, Se, Te) before and after purification
O content/at% As Se Te Before purification 0.46 0.48 1.3 After purification 0.06 0.15 0 (undetected) 
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