磁控共溅射制备无氢碳化锗薄膜的结构和性能研究
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摘要
第Ⅳ主族元素单质及其合金材料是目前材料科学领域研究开发的重点和热点之一。碳化锗(Ge_(1-x)C_x)薄膜以其特有的结构、光学和电学性能引起了人们广泛的关注，特别是其折射率随着薄膜中锗碳含量的变化可以在大范围内调节，这种优良的性能使其适合制成多层红外增透保护薄膜。另外，碳化锗薄膜的光学带隙也可以随成分的变化而改变，这使得其成为设计电子设备和太阳能电池的候选材料，是一种具有应用前景的新型半导体材料。但是对碳化锗薄膜的研究大多集中在含氢碳化锗薄膜上，而对于无氢碳化锗薄膜的研究却很少。因其成分和结构上的差异，含氢碳化锗薄膜的热稳定性相对无氢碳化锗薄膜要差，在性能上也会有改变。本文采用磁控共溅射方法制备了无氢碳化锗薄膜，系统地研究工艺参数对薄膜结构、力学性能、热稳定性、光学性能和电学性能的影响。
在磁控共溅射制备无氢碳化锗薄膜过程中发现，锗靶溅射功率和衬底温度是影响薄膜微观结构的重要参数。研究结果发现随着锗靶溅射功率的增加，薄膜的沉积速率和锗含量均增大，而衬底温度对薄膜的沉积速率和锗含量影响较小。XRD结果表明所制备的碳化锗薄膜均为非晶结构，在高锗靶溅射功率和低衬底温度下薄膜的表面粗糙度较大。FTIR谱中出现了610cm~(-1)左右的Ge-C键振动峰，表明薄膜中生成了碳化锗，升高锗靶溅射功率和衬底温度会使锗原子周围的电负性逐渐降低，导致Ge-C键的峰位向低波数偏移。Raman光谱结果表明碳化锗薄膜中存在锗团簇和碳团簇，当锗靶溅射功率从40W增加到160W时，碳原子能够更好的以sp~3杂化形式融入到锗网络中，碳的D带和G带的相对强度比（ID/IG）从1.17逐渐降至0.75，G带的位置从1572cm~(-1)下移到1563cm~(-1)，这些变化都一致表明了薄膜中sp~2碳的含量在逐渐减少。当衬底温度从室温升高到600℃时，Ge-TO模的半高峰宽随着衬底温度的增加逐渐降低，表明了薄膜中锗原子的有序性在增加，同时碳的D带和G带的相对强度比（ID/IG）从0.80逐渐升至1.31，G带的位置从1561cm~(-1)上移到1576cm~(-1)，表明了薄膜中的sp~2碳含量在逐渐增加。X射线光电子谱分析表明碳化锗薄膜中的碳原子存在sp~3C-C、sp~2C-C和Ge-C三种结合方式，当锗靶溅射功率从40W增加到160W时，薄膜中sp~3C-C和Ge-C相对含量逐渐增多，而sp~2C-C的相对含量大幅降低。当衬底温度从室温升高到600℃时，薄膜中Ge-C相对含量略微减少，sp~3C-C的相对含量减少较快，而sp~2C-C的相对含量大幅升高，这表明衬底温度的升高使碳化锗薄膜产生石墨化倾向。
利用XRR、表面轮廓仪和纳米压痕研究了碳化锗薄膜的密度、应力、硬度和杨氏模量。结果表明当锗靶溅射功率从40W增加到160W时，碳化锗薄膜的密度从3.67g/cm~3增大到4.65g/cm~3，硬度从5.6GPa上升到8.0GPa，杨氏模量从100GPa上升至123Gpa；当衬底温度从室温增加到700℃时，薄膜的密度从4.39g/cm~3增大到4.47g/cm~3，硬度从7.5GPa上升到9.2GPa，杨氏模量从121GPa上升至141Gpa。薄膜的内应力随着锗靶溅射功率的降低从70MPa下降为5Mpa，表明碳化锗薄膜的内应力处于一个相对较低的水平，当降低锗靶溅射功率到40W时，基本可以达到消除薄膜内应力；当衬底温度从室温增加到600℃时，薄膜的内应力从50MPa逐渐上升至330Mpa，这表明随着衬底温度逐渐升高，薄膜中的空洞逐渐减少，锗原子的配位数增加。
将在锗靶功率为140W，衬底温度为200℃条件下制备的碳化锗薄膜在400~900℃下真空保温1小时进行退火处理，分别采用XPS和Raman光谱对薄膜结构的热稳定性进行研究。试验表明，当退火温度从400℃上升至700℃时，碳化锗薄膜的Raman光谱中Ge-TO振动模向300cm~(-1)处移动，表明薄膜中可能出现微晶锗。同时碳的D带和G带的相对强度比（ID/IG）缓慢地从1.10逐渐升至1.20，G带的位置从1559cm~(-1)缓慢上移到1569cm~(-1)。另外，随着退火温度从400℃升高到700℃的过程中，碳化锗薄膜的XPS C1s分峰后的sp~3C-C、sp~2C-C和Ge-C键的相对积分强度基本不变，表明在700℃以下，碳化锗薄膜都具有良好的热稳定性。采用纳米压痕对退火后的薄膜硬度进行了分析，结果表明当退火温度从400℃上升至700℃时，碳化锗薄膜的硬度从8.3Gpa增加到11.8Gpa，当退火温度为800℃时，由于薄膜结构疏松使薄膜硬度突然降低到4.9Gpa。
采用椭偏仪、傅里叶变换红外光谱仪和高温电阻测试系统对碳化锗薄膜的光学性能和电学性能进行了研究。结果显示随着锗靶溅射功率升高，碳化锗薄膜在可见光623.8nm处的折射率从3.0升至4.5，消光系数从0.12增加到1.15，对应的红外9μm处的折射率为2.8升至4.1，而光学带隙从1.55eV降低到1.05eV，碳化锗薄膜/硫化锌衬底组成系统在8~12μm范围内的平均红外透过率从49.5%降低到42.5%。当衬底温度改变时，薄膜的折射率、消光系数、光学带隙和红外透过率变化都不是很大。变温电导率结果表明碳化锗薄膜在室温到500K的温度范围内存在两种导电机制。在室温到400K的温度范围内载流子很容易被激发到导带的定域态，通过跳跃的传导极大增加了薄膜的电导率。随着温度的进一步增加，载流子被热激发到扩展态，并且通过热激活传导增加薄膜的导电能力。增大锗靶溅射功率和升高衬底温度，都能使薄膜的电导率增大，激活能减小。
Ge_(1-x)C_x薄膜与a-Si:H相比对太阳光的吸收范围要宽，吸收系数要大，特别是碳含量较低的Ge_(1-x)C_x薄膜在光伏应用上更有优势。根据光学薄膜增透原理，在ZnS红外窗口上单面镀制了Ge_(1-x)C_x双层增透保护膜系，测试结果表明在9.6μm处透过率增加8%，硬度增加到13.1Gpa，能够对ZnS衬底起到增透保护作用，并且经过500℃退火后膜系的红外透过率基本没有变化。
最后，以实际应用为目的，设计了一种衬底自转-磁控溅射靶步进运动的复合运动方式，实现了小尺寸磁控溅射靶材镀制大平面/半球面均匀薄膜，当满足以下两个条件：(1)靶在所停留位置驻停时间与在该位置的面积成正比，(2)移动的步长不大于5，那么用这种方式制备的薄膜膜厚相对偏差小于5%，能够满足实际应用要求。
Great attention has been given to the development of Group Ⅳ materials inthe field of material science. The amorphous germanium carbide (a-Ge1xCx:H),which have received considerable attention and experimental study, reflecting thehigh interest in these materials because of their exciting structural, optical, andelectrical properties. In particular, the refractive index values of a-Ge1xCx:H maybe adjusted by x in a wide range, this excellent performance makes the a-Ge_(1-x)C_x:Hfilms applicable for design and preparation of multilayer anti-reflection andprotection coatings of IR windows. In addition, the band gap of a-Ge_(1-x)C_x:H filmscan be changed with x in a very wide range, this makes a-Ge_(1-x)C_x:H films goodcandidates in the design of electronic devices and photovoltaic cells. Therefore, a-Ge_(1-x)C_x:H is a new semiconducting material with great potential application.However, a great deal of hydrogen content from the precursors has been remainedin the films. If the service temperature is raised up to350oC, the properties of a-Ge_(1-x)C_x:H films will gradually deteriorate because of the broken C–H and Ge–Hbonds in the films. Therefore, the amorphous non-hydrogenated germanium carbide(a-Ge_(1-x)C_x) films with a better stability are urgently demanded for the harshapplications. However, so far, there are very few reports on a-Ge_(1-x)C_xfilms. In thispaper, the a-Ge1xCxfilms were prepared using magnetron co-sp~uttering technique.The structural, mechanical, optical and electrical properties were focused on anddiscussed.
The germanium target sp~uttering power and substrate temperature areimportant parameters affectting the film microstructure. As the germanium targetpower increases, the deposition rate and Ge content increase. The deposition rateand germanium content scarcely depond on the substrate temperature. XRD resultsshowed that the films are amorphous, and AFM results demonstrate that the largersurface roughness of the film with high germanium target sp~uttering power and lowsubstrate temperature. FTIR sp~ectra show that Ge-C bond vibration peak positionsare at about610cm~(-1), and Ge target power and substrate temperature graduallyincrease, resulting in the Ge-C peak position shifted to lower wave number. Ramansp~ectroscopy results show that germanium clusters and carbon clusters are in thefilms. As the germanium target power increases from40W to160W, the ratio ofRaman I(D)/I(G) reduces from1.17to0.75, the G peak position reduces from1572cm~(-1)to1563cm~(-1), which implies that the sp~2carbon content gradually reduced in the film. As the substrate temperature increases from room temperature to600°C,the ratio of Raman I(D)/I(G) rises up from0.80to1.31, the G peak positionincreases from1561cm~(-1)to1576cm~(-1), which implies that the sp~2carbon contentgradually increases in the film. XPS results show that the carbon atoms form sp~3C-C, sp~2C-C and Ge-C in the film. As the germanium target power increases from40W to160W, the relative content of sp~3C-C and Ge-C increases, while the relativecontent of sp~2C-C significantly reduces. As the substrate temperature rises up fromroom temperature to600°C, the relative content of the Ge-C reduces slightly, therelative content of sp~3C-C decreased rapidly, while the relative content of sp~2C-Csignificantly increases, suggesting that a progressive inecrease in the size ofgraphitic clusters.
The density, hardness,Young’s modulus and compressive stress of the a-Ge_(1-x)C_xfilms were resp~ectively measured using X-ray reflectivity, surface profilemeter andnano-indenter. It was identified that the density increases from3.67g/cm~3to4.65g/cm~3, the hardness increases from5.6GPa to8.0GPa and Young’s modulusincreases from100GPa to123Gpa, as the germanium target power increases from40W to160W; the density increases from4.39g/cm~3to4.47g/cm~3, the hardnessincreases from7.5GPa to9.2GPa and Young’s modulus increases from121GPa to141Gpa, as the substrate temperature rises up from room temperature to600°C. Thecompressive stress decreases gradually from70MPa to5Mpa, as the germanium targetpower decreases. The compressive stress inecreases from50MPa to330Mpa, as thesubstrate temperature inecreases room temperature to600°C, hinting that the defectsreduce and coordination number of germanium atoms increases.
In order to strudy the properties of thermal stability, the a-Ge_(1-x)C_xfilms depositedat140W and200°C were resp~ectively annealed at400~900°C for1h under vacuumconditions. The structural variations of the as-annealed a-Ge_(1-x)C_xfilms were studied byXPS and Raman sp~ectroscopy. Raman analysis shows that the Ge-TO peak position risesup300cm~(-1), the I(D)/I(G) ratio rises up from1.10to1.20, the G peak positionincreases from1559cm~(-1)to1569cm~(-1), as the annealing temperature rises up from400to700°C. Furthermore, the relative content of sp~3C-C, sp~3C-C and Ge-C almostremain below700°C, indicating very good thermal stabilities below this temperature.The hardness of the as-annealed a-Ge_(1-x)C_xfilms were disscussed. The results showthat the hardness increases from5.6GPa to8.0Gpa. It was identified that the hardnessincreases gradually from8.3GPa to11.8GPa with the annealed temperature from400to700°C, and then reduces sharply to4.9GPa at800°C
The optical and electrical properties of the a-Ge_(1-x)C_xfilms were repectively studied by ellipsometry, FTIR, and temperature dependence resistance measuringsystem. As the germanium target power increases, the refractive index increasesfrom3.0to4.5and the extinction coefficient increases from0.12to1.15at623.8nm, the refractive index increases from2.8to4.1at9μm, while the opticalgap reduces from1.55to1.05eV, and the average transmittance of a-Ge_(1-x)C_x/ZnSsysterm reduces from49.5%to42.5%in range of8~12μm. The refractive index,the extinction coefficient, the optical gap and the average transmittance of the a-Ge_(1-x)C_xfilms scarcely change as the substrate temperature increases. Thetemperature dependence of conductivity indicates the thermally activatedconduction of carriers in extended states and hopping conduction in localized bandtail states near conduction band edges at above and below400K, resp~ectively. Asgermanium target power and substrate temperature increase, the room-temperatureconductivity increases and activation energy decreases.
The absorption coefficient and resp~onse range of Ge_(1-x)C_xfilms are larger thanthat of a-Si:H films, and the esp~ecially Ge_(1-x)C_xfilm with low carbon content havemore advantage in the field of pv-tech application. According to the optical principle,a double-layer antireflection and protection coating was deposited on the single sidepolished polycrystalline ZnS. The value of the IR transmittance of ZnS wafer withthe double-layer coating is increased by8%at9.6μm, and the hardness is up to13.1GPa, which implies that a-Ge_(1-x)C_xfilms can be used as an effective antireflectionand protection coating for the ZnS IR window. The excellent optical transmission foran antireflection a-Ge_(1-x)C_xdouble-layer film on ZnS substrate is still maintainedafter annealing at400oC.
To grow uniform films on a large substrate by magnetron sp~uttering with a smalltarget, a new theoretical model has been proposed, implemented and confirmed. Themodel was based on a magnetron sp~uttering system containing a rotation substrateholder and a step-moving target. A magnetron sp~uttering system containing a rotationsubstrate holder and an Φ50mm step-moving target has been established by us. Whentarget stay time was proportional to the target scanning area at the rotating substrateand target moving step was5mm, the relative deviation of film thickness distributionwas less than5%within a diameter of Φ300mm. The numerical results agreed wellwith measurements, which demonstrated that our model was applicable to depositinglarge uniform film.
在磁控共溅射制备无氢碳化锗薄膜过程中发现，锗靶溅射功率和衬底温度是影响薄膜微观结构的重要参数。研究结果发现随着锗靶溅射功率的增加，薄膜的沉积速率和锗含量均增大，而衬底温度对薄膜的沉积速率和锗含量影响较小。XRD结果表明所制备的碳化锗薄膜均为非晶结构，在高锗靶溅射功率和低衬底温度下薄膜的表面粗糙度较大。FTIR谱中出现了610cm~(-1)左右的Ge-C键振动峰，表明薄膜中生成了碳化锗，升高锗靶溅射功率和衬底温度会使锗原子周围的电负性逐渐降低，导致Ge-C键的峰位向低波数偏移。Raman光谱结果表明碳化锗薄膜中存在锗团簇和碳团簇，当锗靶溅射功率从40W增加到160W时，碳原子能够更好的以sp~3杂化形式融入到锗网络中，碳的D带和G带的相对强度比（ID/IG）从1.17逐渐降至0.75，G带的位置从1572cm~(-1)下移到1563cm~(-1)，这些变化都一致表明了薄膜中sp~2碳的含量在逐渐减少。当衬底温度从室温升高到600℃时，Ge-TO模的半高峰宽随着衬底温度的增加逐渐降低，表明了薄膜中锗原子的有序性在增加，同时碳的D带和G带的相对强度比（ID/IG）从0.80逐渐升至1.31，G带的位置从1561cm~(-1)上移到1576cm~(-1)，表明了薄膜中的sp~2碳含量在逐渐增加。X射线光电子谱分析表明碳化锗薄膜中的碳原子存在sp~3C-C、sp~2C-C和Ge-C三种结合方式，当锗靶溅射功率从40W增加到160W时，薄膜中sp~3C-C和Ge-C相对含量逐渐增多，而sp~2C-C的相对含量大幅降低。当衬底温度从室温升高到600℃时，薄膜中Ge-C相对含量略微减少，sp~3C-C的相对含量减少较快，而sp~2C-C的相对含量大幅升高，这表明衬底温度的升高使碳化锗薄膜产生石墨化倾向。
利用XRR、表面轮廓仪和纳米压痕研究了碳化锗薄膜的密度、应力、硬度和杨氏模量。结果表明当锗靶溅射功率从40W增加到160W时，碳化锗薄膜的密度从3.67g/cm~3增大到4.65g/cm~3，硬度从5.6GPa上升到8.0GPa，杨氏模量从100GPa上升至123Gpa；当衬底温度从室温增加到700℃时，薄膜的密度从4.39g/cm~3增大到4.47g/cm~3，硬度从7.5GPa上升到9.2GPa，杨氏模量从121GPa上升至141Gpa。薄膜的内应力随着锗靶溅射功率的降低从70MPa下降为5Mpa，表明碳化锗薄膜的内应力处于一个相对较低的水平，当降低锗靶溅射功率到40W时，基本可以达到消除薄膜内应力；当衬底温度从室温增加到600℃时，薄膜的内应力从50MPa逐渐上升至330Mpa，这表明随着衬底温度逐渐升高，薄膜中的空洞逐渐减少，锗原子的配位数增加。
将在锗靶功率为140W，衬底温度为200℃条件下制备的碳化锗薄膜在400~900℃下真空保温1小时进行退火处理，分别采用XPS和Raman光谱对薄膜结构的热稳定性进行研究。试验表明，当退火温度从400℃上升至700℃时，碳化锗薄膜的Raman光谱中Ge-TO振动模向300cm~(-1)处移动，表明薄膜中可能出现微晶锗。同时碳的D带和G带的相对强度比（ID/IG）缓慢地从1.10逐渐升至1.20，G带的位置从1559cm~(-1)缓慢上移到1569cm~(-1)。另外，随着退火温度从400℃升高到700℃的过程中，碳化锗薄膜的XPS C1s分峰后的sp~3C-C、sp~2C-C和Ge-C键的相对积分强度基本不变，表明在700℃以下，碳化锗薄膜都具有良好的热稳定性。采用纳米压痕对退火后的薄膜硬度进行了分析，结果表明当退火温度从400℃上升至700℃时，碳化锗薄膜的硬度从8.3Gpa增加到11.8Gpa，当退火温度为800℃时，由于薄膜结构疏松使薄膜硬度突然降低到4.9Gpa。
采用椭偏仪、傅里叶变换红外光谱仪和高温电阻测试系统对碳化锗薄膜的光学性能和电学性能进行了研究。结果显示随着锗靶溅射功率升高，碳化锗薄膜在可见光623.8nm处的折射率从3.0升至4.5，消光系数从0.12增加到1.15，对应的红外9μm处的折射率为2.8升至4.1，而光学带隙从1.55eV降低到1.05eV，碳化锗薄膜/硫化锌衬底组成系统在8~12μm范围内的平均红外透过率从49.5%降低到42.5%。当衬底温度改变时，薄膜的折射率、消光系数、光学带隙和红外透过率变化都不是很大。变温电导率结果表明碳化锗薄膜在室温到500K的温度范围内存在两种导电机制。在室温到400K的温度范围内载流子很容易被激发到导带的定域态，通过跳跃的传导极大增加了薄膜的电导率。随着温度的进一步增加，载流子被热激发到扩展态，并且通过热激活传导增加薄膜的导电能力。增大锗靶溅射功率和升高衬底温度，都能使薄膜的电导率增大，激活能减小。
Ge_(1-x)C_x薄膜与a-Si:H相比对太阳光的吸收范围要宽，吸收系数要大，特别是碳含量较低的Ge_(1-x)C_x薄膜在光伏应用上更有优势。根据光学薄膜增透原理，在ZnS红外窗口上单面镀制了Ge_(1-x)C_x双层增透保护膜系，测试结果表明在9.6μm处透过率增加8%，硬度增加到13.1Gpa，能够对ZnS衬底起到增透保护作用，并且经过500℃退火后膜系的红外透过率基本没有变化。
最后，以实际应用为目的，设计了一种衬底自转-磁控溅射靶步进运动的复合运动方式，实现了小尺寸磁控溅射靶材镀制大平面/半球面均匀薄膜，当满足以下两个条件：(1)靶在所停留位置驻停时间与在该位置的面积成正比，(2)移动的步长不大于5，那么用这种方式制备的薄膜膜厚相对偏差小于5%，能够满足实际应用要求。
Great attention has been given to the development of Group Ⅳ materials inthe field of material science. The amorphous germanium carbide (a-Ge1xCx:H),which have received considerable attention and experimental study, reflecting thehigh interest in these materials because of their exciting structural, optical, andelectrical properties. In particular, the refractive index values of a-Ge1xCx:H maybe adjusted by x in a wide range, this excellent performance makes the a-Ge_(1-x)C_x:Hfilms applicable for design and preparation of multilayer anti-reflection andprotection coatings of IR windows. In addition, the band gap of a-Ge_(1-x)C_x:H filmscan be changed with x in a very wide range, this makes a-Ge_(1-x)C_x:H films goodcandidates in the design of electronic devices and photovoltaic cells. Therefore, a-Ge_(1-x)C_x:H is a new semiconducting material with great potential application.However, a great deal of hydrogen content from the precursors has been remainedin the films. If the service temperature is raised up to350oC, the properties of a-Ge_(1-x)C_x:H films will gradually deteriorate because of the broken C–H and Ge–Hbonds in the films. Therefore, the amorphous non-hydrogenated germanium carbide(a-Ge_(1-x)C_x) films with a better stability are urgently demanded for the harshapplications. However, so far, there are very few reports on a-Ge_(1-x)C_xfilms. In thispaper, the a-Ge1xCxfilms were prepared using magnetron co-sp~uttering technique.The structural, mechanical, optical and electrical properties were focused on anddiscussed.
The germanium target sp~uttering power and substrate temperature areimportant parameters affectting the film microstructure. As the germanium targetpower increases, the deposition rate and Ge content increase. The deposition rateand germanium content scarcely depond on the substrate temperature. XRD resultsshowed that the films are amorphous, and AFM results demonstrate that the largersurface roughness of the film with high germanium target sp~uttering power and lowsubstrate temperature. FTIR sp~ectra show that Ge-C bond vibration peak positionsare at about610cm~(-1), and Ge target power and substrate temperature graduallyincrease, resulting in the Ge-C peak position shifted to lower wave number. Ramansp~ectroscopy results show that germanium clusters and carbon clusters are in thefilms. As the germanium target power increases from40W to160W, the ratio ofRaman I(D)/I(G) reduces from1.17to0.75, the G peak position reduces from1572cm~(-1)to1563cm~(-1), which implies that the sp~2carbon content gradually reduced in the film. As the substrate temperature increases from room temperature to600°C,the ratio of Raman I(D)/I(G) rises up from0.80to1.31, the G peak positionincreases from1561cm~(-1)to1576cm~(-1), which implies that the sp~2carbon contentgradually increases in the film. XPS results show that the carbon atoms form sp~3C-C, sp~2C-C and Ge-C in the film. As the germanium target power increases from40W to160W, the relative content of sp~3C-C and Ge-C increases, while the relativecontent of sp~2C-C significantly reduces. As the substrate temperature rises up fromroom temperature to600°C, the relative content of the Ge-C reduces slightly, therelative content of sp~3C-C decreased rapidly, while the relative content of sp~2C-Csignificantly increases, suggesting that a progressive inecrease in the size ofgraphitic clusters.
The density, hardness,Young’s modulus and compressive stress of the a-Ge_(1-x)C_xfilms were resp~ectively measured using X-ray reflectivity, surface profilemeter andnano-indenter. It was identified that the density increases from3.67g/cm~3to4.65g/cm~3, the hardness increases from5.6GPa to8.0GPa and Young’s modulusincreases from100GPa to123Gpa, as the germanium target power increases from40W to160W; the density increases from4.39g/cm~3to4.47g/cm~3, the hardnessincreases from7.5GPa to9.2GPa and Young’s modulus increases from121GPa to141Gpa, as the substrate temperature rises up from room temperature to600°C. Thecompressive stress decreases gradually from70MPa to5Mpa, as the germanium targetpower decreases. The compressive stress inecreases from50MPa to330Mpa, as thesubstrate temperature inecreases room temperature to600°C, hinting that the defectsreduce and coordination number of germanium atoms increases.
In order to strudy the properties of thermal stability, the a-Ge_(1-x)C_xfilms depositedat140W and200°C were resp~ectively annealed at400~900°C for1h under vacuumconditions. The structural variations of the as-annealed a-Ge_(1-x)C_xfilms were studied byXPS and Raman sp~ectroscopy. Raman analysis shows that the Ge-TO peak position risesup300cm~(-1), the I(D)/I(G) ratio rises up from1.10to1.20, the G peak positionincreases from1559cm~(-1)to1569cm~(-1), as the annealing temperature rises up from400to700°C. Furthermore, the relative content of sp~3C-C, sp~3C-C and Ge-C almostremain below700°C, indicating very good thermal stabilities below this temperature.The hardness of the as-annealed a-Ge_(1-x)C_xfilms were disscussed. The results showthat the hardness increases from5.6GPa to8.0Gpa. It was identified that the hardnessincreases gradually from8.3GPa to11.8GPa with the annealed temperature from400to700°C, and then reduces sharply to4.9GPa at800°C
The optical and electrical properties of the a-Ge_(1-x)C_xfilms were repectively studied by ellipsometry, FTIR, and temperature dependence resistance measuringsystem. As the germanium target power increases, the refractive index increasesfrom3.0to4.5and the extinction coefficient increases from0.12to1.15at623.8nm, the refractive index increases from2.8to4.1at9μm, while the opticalgap reduces from1.55to1.05eV, and the average transmittance of a-Ge_(1-x)C_x/ZnSsysterm reduces from49.5%to42.5%in range of8~12μm. The refractive index,the extinction coefficient, the optical gap and the average transmittance of the a-Ge_(1-x)C_xfilms scarcely change as the substrate temperature increases. Thetemperature dependence of conductivity indicates the thermally activatedconduction of carriers in extended states and hopping conduction in localized bandtail states near conduction band edges at above and below400K, resp~ectively. Asgermanium target power and substrate temperature increase, the room-temperatureconductivity increases and activation energy decreases.
The absorption coefficient and resp~onse range of Ge_(1-x)C_xfilms are larger thanthat of a-Si:H films, and the esp~ecially Ge_(1-x)C_xfilm with low carbon content havemore advantage in the field of pv-tech application. According to the optical principle,a double-layer antireflection and protection coating was deposited on the single sidepolished polycrystalline ZnS. The value of the IR transmittance of ZnS wafer withthe double-layer coating is increased by8%at9.6μm, and the hardness is up to13.1GPa, which implies that a-Ge_(1-x)C_xfilms can be used as an effective antireflectionand protection coating for the ZnS IR window. The excellent optical transmission foran antireflection a-Ge_(1-x)C_xdouble-layer film on ZnS substrate is still maintainedafter annealing at400oC.
To grow uniform films on a large substrate by magnetron sp~uttering with a smalltarget, a new theoretical model has been proposed, implemented and confirmed. Themodel was based on a magnetron sp~uttering system containing a rotation substrateholder and a step-moving target. A magnetron sp~uttering system containing a rotationsubstrate holder and an Φ50mm step-moving target has been established by us. Whentarget stay time was proportional to the target scanning area at the rotating substrateand target moving step was5mm, the relative deviation of film thickness distributionwas less than5%within a diameter of Φ300mm. The numerical results agreed wellwith measurements, which demonstrated that our model was applicable to depositinglarge uniform film.
引文
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