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We demonstrate a bismuth (Bi) saturable absorber (SA) for generating ultrafast pulse. The Bi SA is fabricated by the Bi film deposited on the surface of microfibers through using magnetron sputtering. Its nonlinear optical properties are investigated. The as-prepared Bi SA has outstanding nonlinear absorption property demonstrated by the open aperture (OA) Z-scan system at 1500 nm and balanced twin-detector method at 1560 nm. The nonlinear optical property of Bi SA shows that the modulation depth, the nonsaturable losses, and the saturable intensity at 1.5 μm are 14% and 79%, and 0.9 MW/cm2, respectively. Besides, the closed aperture (CA) Z-scan measurement is also implemented to estimate the nonlinear refractive index of Bi film. The Bi film shows that the typical CA/OA curve possesses the feature of peak-valley profile, meaning that the sample with a negative nonlinear refractive index is self-defocusing. In our experiments, the parameters of the nonlinear absorption coefficient β and the nonlinear refractive index n2 are estimated at about 2.38 × 10–4 cm/W and –1.47 × 10–9 cm2/W according to the actual experimental data points, respectively. To further investigate its nonlinear optical property, the microfiber-based Bi SA is embedded into an erbium-doped fiber laser with a typical ring cavity structure. Based on the Bi SA device, the stable ultrafast pulses are generated at 1.5 μm with the pulse width of 357 fs, the output power of 45.4 mW, corresponding to the pulse energy of 2.39 nJ, and the signal-to-noise ratio is 84 dB. The stable soliton pulses emitting at 1563 nm are obtained with a 3-dB and 6-nm spectral bandwidth. The experimental results suggest that the microfiber-based Bi SA prepared by magnetron sputtering deposition (MSD) technique can be used as an excellent photonic device for ultrafast pulse generation in the 1.5 μm regime, and the MSD technique opens a promising way to produce high-performance SA with a large modulation depth, low saturable intensity, and high power tolerance, which are conducible to the generation of high power and ultrafast pulse with high stability.
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Keywords:
- saturable absorber /
- fiber laser /
- magnetron sputtering deposition /
- bismuth
1. 引 言
超快光纤激光器在激光医学、吸收光谱、激光大气通信、遥感和高分子材料加工等方面具有广阔的应用前景[1]. 可饱和吸收体(SA)作为谐振腔内脉冲的启动器和整形器, 可从腔内噪声序列中选择出能量最高的脉冲, 是实现被动锁模运转的关键光学元件. 目前唯一商用的SA是半导体饱和吸收镜(SESAM)[2,3], 然而, 受半导体带隙宽度和反射镜衬底的限制, SESAM的工作带宽通常只有几十纳米, 且SESAM的制备复杂, 价格昂贵. 近年来一些低维材料, 如石墨烯[4-6]、拓扑绝缘体[7,8]、过渡金属二硫化物[9-12]、黑磷[13-15]等, 被制作成SA并应用于超快脉冲产生, 推动了新型SA的研制. 其中, 石墨烯和拓扑绝缘体虽然具有超快的载流子响应, 但其Dirac点附近较低的电子态密度限制了其非线性吸收特性(调制深度低)[16-18]; 过渡金属二硫化物具有较大的带隙, 其光学响应波段主要位于可见光区域; 尽管不同层数黑磷的带隙在0.3—2.0 eV可调[15], 可实现从可见光到中红外波段的光学响应, 但黑磷的化学稳定性差. 近年来, 科研工作者致力于研制新型的高性能SA, 以弥补现有SA存在的缺点. 其中, 铋烯因其独特的性质引起了人们极大的兴趣. 根据第一性原理理论计算, 铋烯具有高载流子迁移率[19]、优异的热导率[20]、良好的自旋电子性质和应变诱导带跃迁[20-22]等卓越的光电特性. 另外, 块体铋属于半金属, 当层数减小到22层以下时将表现出拓扑绝缘体性质, 当层数小于8层时将表现出量子自旋霍尔相位, 最终在单层情况下表现出半导体性质, 其带隙为0.74 eV并拥有高载流子迁移率[19,20,23]. 已有报道采用机械剥离法[24]和外延生长法[25]制备铋烯, 通常将铋烯和聚合物做成薄膜来作为SA, 由于聚合物容易被激光损伤, 这种薄膜类SA不利于高能量超短脉冲产生[24]. 机械剥离法存在厚度不可控以及不均匀等问题, 随机性大, 不利于SA的精准制备, 直接影响SA的表现性能. 与常见的机械剥离法与外延生长法相比, 磁控溅射沉积(MSD)法可在目标衬底上批次性、可重复、可控地制备薄膜, 是一种精准制备SA的有效方法[12,26].
本文采用MSD方法在微纳光纤表面沉积纳米级厚度铋膜制备铋SA. 将其应用到掺铒光纤激光器中, 获得稳定的锁模脉冲输出. 脉冲中心波长为1563 nm, 输出功率为45.4 mW, 脉冲宽度为357 fs, 重复频率为19 MHz. 实验表明, 微纳光纤-铋结构可以作为一种有效的倏逝波耦合型SA器件.
2. 微纳光纤-铋SA的制备与表征
在光纤拉锥机上对单模光纤(SMF-28e)进行熔融拉锥处理, 制备出锥区束腰直径约为13 μm的微纳光纤. 将铋靶材、石英片和微纳光纤置于磁控溅射仪的真空室中, 将真空度降至9 × 10–4 Pa, 再将氩气注入到腔内. 由于铋为单质半金属材料, 使用直流驱动的方式镀膜, 参数为: 氩气流量为15 sccm (1 sccm = 1 mL/min), 电流为0.2 A, 持续时间为2 min, 通过控制时间来控制薄膜厚度.
图1(a)是在扫描电子显微镜下观察到的微纳光纤-铋SA的锥区位置, 锥区直径为13 μm, 插图为镀在锥区表面铋薄膜的表面形态, 可见薄膜十分致密地覆盖在微纳光纤的表面上. 图1(b)为镀膜光纤端面, 图1(c)是图1(b)中红色框内的放大结果, 可以看出铋薄膜在光纤表面沉积的厚度约为39.7 nm. 由514 nm激光激发的50—500 cm–1范围内铋的拉曼光谱如图1(d)所示, 铋薄膜在约72 cm–1处显示出面内Eg模的显著峰, 在约97 cm–1处显示出面外A1g模的相对弱峰, 此结果与先前的工作[27]中报道的值一致, 证实了我们所制备的铋薄膜的高质量. 为了进一步评价铋薄膜的质量, 对所制备的铋薄膜进行了X射线衍射(XRD)分析, 图1(e)是石英片上铋膜的XRD图谱, 将其与铋的XRD标准PDF卡片(PDF#97-005-3796)比对, 表明铋膜的XRD图谱中仅有纯铋元素的峰, 进一步证实通过磁控溅射法制备了高质量薄膜. 图1(f)为石英片上铋膜在1400—1800 nm之间的线性透过率, 在1563 nm处的平均透过率为22.2%.
图 1 铋薄膜表征结果 (a)覆盖铋薄膜拉锥光纤的锥区扫描电子显微镜图像, 插图为铋薄膜的表面形貌; (b)镀铋膜的光纤端面; (c)铋薄膜沉积在光纤上的厚度; (d)铋薄膜的拉曼光谱; (e)铋薄膜的XRD图; (f)铋薄膜的线性透过率Fig. 1. Bi film characterization results: (a) Scanning electron microscope images for the taper region of the microfiber coated with the bismuth film (the inset shows the surface morphology of the bismuth film); (b) optical fiber end face with bismuth coating; (c) thickness of bismuth thin film deposited on optical fiber; (d) Raman spectrum of bismuth film; (e) XRD diagram of the bismuth film; (f) linear transmittance of bismuth thin film.为了确认光与覆盖在锥区表面铋膜的渐逝波相互作用, 将波长为650 nm的红光导入镀膜锥区, 图2(a)所示为未通光前的光学图像, 图2(b)显示了通光后的锥区图像, 通过泄漏的红光可以明显地看出光与物质的相互作用. 采用自制的锁模光纤激光器, 在中心波长为1550 nm、脉冲宽度为270 fs、基频为40.5 MHz的条件下, 测量了基于铋SA的非线性光学吸收特性. 非线性饱和吸收曲线如图2(c)所示, 测得调制深度(αs)、非线性饱和损耗(αns)和饱和强度(Isat)分别约为14%, 79%和0.9 MW/cm2.
图 2 微纳光纤-铋SA的非线性表征 (a)没有和(b)具有650 nm引导光时样品腰部区域的光学显微镜图像; (c) SA的饱和吸收特性Fig. 2. Nonlinear characterization of micro-nano fiber-bismuth SA: Optical microscope images of the waist region of the sample (a) without and (b) with the guiding 650 nm light; (c) saturable absorption property of SA.此外, 利用开孔Z扫描技术在1500 nm波长处测试了铋膜在10, 30, 50, 70 mW激发功率下的可饱和吸收特性, 结果如图3(a)所示, 可以看出微纳光纤-铋膜结构的SA在1500 nm处呈现出明显的饱和吸收特性. 图3(b)所示的标准化的闭孔/开孔Z扫描曲线, 展现出典型的先峰后谷特性, 表明铋膜的非线性折射率为负, 具有自散焦特性. 根据数值分析可得铋膜的非线性吸收系数β与非线性折射率n2分别为2.38 × 10–4 cm/W和–1.47 × 10–9 cm2/W.
图 3 (a)不同激发功率下的标准开孔Z扫描曲线; (b)标准化的闭孔/开孔Z扫描曲线Fig. 3. (a) Normalized open-aperture Z-scan traces with different excitation powers; (b) normalized close-aperture/ open-aperture Z-scan trace.3. 实验装置
实验装置如图4所示, 在掺铒光纤激光器中, 增益介质为120 cm的掺铒(OFS/EDF-80)光纤, 采用980 nm半导体激光器作为抽运源. 使用波长为980/1550 nm的波分复用(WDM)耦合器将抽运光耦合到腔内. 采用偏振不敏感隔离器(PI-ISO)以保证激光在腔内的单向传输, 中心波长为1550 nm. 加入偏振控制器(PC)调节激光腔内光束的偏振特性状态. 采用10∶90光耦合器(OC)将10%的光输出, 用以测试激光输出特性, 谐振腔内的光纤器件都是偏振不敏感的. 激光腔长度为11.2 m. 单模光纤的参数约为–23.9 ps2/km, 掺铒光纤的净腔色散值约为40 ps2/km[9], 计算得到腔内净色散约为–0.191 ps2. 为分析输出激光特性, 使用了数字示波器(Rohde&Schwarzr RTO2024)、射频频谱分析仪(Rohde&Schwarzr FSV13)、光电探测器(EOT ET-3500F)、光学频谱分析仪(Yokogawa AQ6370)、自相关仪(APE Pulsecheck).
4. 实验结果
在激光腔中, 没有加入SA前, 无论怎么调节抽运功率和偏振控制器, 都无法产生脉冲序列. 然后在WDM和PC之间, 将制备的SA集成到光纤激光器中. 当抽运功率增加到30 mW时, 振荡器开始工作在锁模状态. 图5(a)显示了以1563 nm为中心的典型锁模光谱, 其3 dB光谱带宽为6 nm. 谱线上Kelly边带的存在证实了锁模激光器运行在孤子区域内. 图5(b)为RF频谱, 基频为19.0 MHz, 信噪比为84 dB, 与腔长11.2 m相匹配. 图5(b)中的插图是在2 GHz大范围下的射频(RF)频谱, 连续平坦的频谱图表明锁模脉冲具有高的稳定性. 图5(c)为自相关测量得到的脉冲轨迹, 结果很好地符合sech2函数曲线, 脉宽为357 fs. 时间-带宽乘积为0.323, 表明输出脉冲含有轻微的啁啾. 图5(c)内插图为出脉冲的时间序列图, 可知激光器具有很好的稳定性. 图5(d)给出了输出功率/脉冲能量随着输入功率的变化, 当输入功率为280 mW时, 输出功率为45.4 mW, 相应的单脉冲能量为2.39 nJ. 此时输出功率仍然保持很好的线性增长关系, 斜率效率为17%. 相信通过增加抽运功率与优化谐振腔结构, 可以得到更高的输出功率与脉冲能量.
图 5 1.5 μm锁模特性 (a)锁模光谱; (b)基频为19.0 MHz、分辨率为10 Hz的射频频谱, 插图显示了2 GHz跨度的射频频谱; (c)具有sech2拟合的脉冲持续时间为357 fs输出脉冲的自相关轨迹, 插图是输出脉冲的时间序列图; (d)输出功率/脉冲能量随着输入功率的变化Fig. 5. Mode-locking characteristics at 1.5 μm: (a) Mode-locking optical spectrum; (b) RF spectrum at a fundamental frequency of 19.0 MHz with 10 Hz resolution; the inset shows the RF spectrum of 100 MHz span; (c) autocorrelation trace for an output pulse with a pulse duration of 357 fs with sech2 fit; the inset is the oscilloscope trace of the output pulse train; (d) relationship between the input power and laser output power/pulse energy.表1中比较了铋作为SA锁模的几种超快激光器的实验结果[28-33], 其中λc为中心波长, SNR为信噪比, Ppump为抽运功率, Pave为平均输出功率, E为脉冲能量, τ为脉冲持续时间, αs为调制深度. 在本文实验方案中, 基于微纳光纤-铋的SA可以有效避免激光直接透过SA材料, 防止材料与激光脉冲能量的直接相互作用. 因此, 这种类型的SA具有较高的损伤阈值. 基于液相剥离(LPE)法制备的微纳光纤-铋SA的平均输出功率和脉冲能量都相对较小, 而使用MSD法可以有效地提升输出功率和脉冲能量. 另外, 更高的信噪比说明输出脉冲有更高的稳定性. 此外, 二维材料可以通过MSD方法直接沉积在微纳光纤的整个区域上, 充分确保了调制效果, 这也很好地说明了表1中MSD法制备SA调制深度更高. 因此, 与通过其他方法制备的SA相比, 利用磁控溅射法制备的集成式微纳光纤-铋SA具有相对较大的调制深度, 可产生高能量锁模脉冲.
表 1 基于铋SA不同锁模激光器的比较Table 1. Comparison of different mode-locked lasers based on Bi saturable absorbers.Fabrication Integration method λc/nm SNR/dB Ppump/Pave/mW E/nJ τ/fs αs/% 来源 LPE Microfiber 1559.18 55 542/1.15 0.13 652 2.03 Ref. [28] LPE Microfiber 1034.4 45 238/8.35 — 30250 2.2 Ref. [29] LPE Microfiber 1561 55 350/5.6 — 193 5.6 Ref. [30] LPE Gold mirror 2030 — 2000/110 6.6 978 — Ref. [31] LPE Microfiber 1557.5 25 —/122.1 — 621.5 2.4 Ref. [32] LPE Microfiber 1531 56.54 314/1.3 0.35 1300 2.5 Ref. [33] MSD Microfiber 1563 84 280/45.4 2.39 357 14 This work 5. 结 论
利用MSD技术制备了一种微纳光纤-铋SA器件, 将其应用到掺铒光纤激光器中, 获得高稳定性的被动锁模脉冲, 其中心波长为1563 nm, 3 dB带宽为6 nm, 脉冲宽度357 fs, 重复频率为19 MHz, 信噪比为84 dB. 实现了大能量锁模激光输出, 最高单脉冲能量高达2.39 nJ. 本文提出了一种利用磁控溅射法制备SA的新方案, 将二维材料直接沉积在微纳光纤表面上并覆盖整个锥区, 充分实现对光的调制; 采用倏逝波-材料相互作用方式, 避免了材料被高能量脉冲的损伤, 大幅提高SA的损伤阈值, 有利于获得高能量超短脉冲产生.
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图 1 铋薄膜表征结果 (a)覆盖铋薄膜拉锥光纤的锥区扫描电子显微镜图像, 插图为铋薄膜的表面形貌; (b)镀铋膜的光纤端面; (c)铋薄膜沉积在光纤上的厚度; (d)铋薄膜的拉曼光谱; (e)铋薄膜的XRD图; (f)铋薄膜的线性透过率
Figure 1. Bi film characterization results: (a) Scanning electron microscope images for the taper region of the microfiber coated with the bismuth film (the inset shows the surface morphology of the bismuth film); (b) optical fiber end face with bismuth coating; (c) thickness of bismuth thin film deposited on optical fiber; (d) Raman spectrum of bismuth film; (e) XRD diagram of the bismuth film; (f) linear transmittance of bismuth thin film.
图 2 微纳光纤-铋SA的非线性表征 (a)没有和(b)具有650 nm引导光时样品腰部区域的光学显微镜图像; (c) SA的饱和吸收特性
Figure 2. Nonlinear characterization of micro-nano fiber-bismuth SA: Optical microscope images of the waist region of the sample (a) without and (b) with the guiding 650 nm light; (c) saturable absorption property of SA.
图 3 (a)不同激发功率下的标准开孔Z扫描曲线; (b)标准化的闭孔/开孔Z扫描曲线
Figure 3. (a) Normalized open-aperture Z-scan traces with different excitation powers; (b) normalized close-aperture/ open-aperture Z-scan trace.
图 4 实验装置图
Figure 4. Experimental device diagram.
图 5 1.5 μm锁模特性 (a)锁模光谱; (b)基频为19.0 MHz、分辨率为10 Hz的射频频谱, 插图显示了2 GHz跨度的射频频谱; (c)具有sech2拟合的脉冲持续时间为357 fs输出脉冲的自相关轨迹, 插图是输出脉冲的时间序列图; (d)输出功率/脉冲能量随着输入功率的变化
Figure 5. Mode-locking characteristics at 1.5 μm: (a) Mode-locking optical spectrum; (b) RF spectrum at a fundamental frequency of 19.0 MHz with 10 Hz resolution; the inset shows the RF spectrum of 100 MHz span; (c) autocorrelation trace for an output pulse with a pulse duration of 357 fs with sech2 fit; the inset is the oscilloscope trace of the output pulse train; (d) relationship between the input power and laser output power/pulse energy.
表 1 基于铋SA不同锁模激光器的比较
Table 1. Comparison of different mode-locked lasers based on Bi saturable absorbers.
Fabrication Integration method λc/nm SNR/dB Ppump/Pave/mW E/nJ τ/fs αs/% 来源 LPE Microfiber 1559.18 55 542/1.15 0.13 652 2.03 Ref. [28] LPE Microfiber 1034.4 45 238/8.35 — 30250 2.2 Ref. [29] LPE Microfiber 1561 55 350/5.6 — 193 5.6 Ref. [30] LPE Gold mirror 2030 — 2000/110 6.6 978 — Ref. [31] LPE Microfiber 1557.5 25 —/122.1 — 621.5 2.4 Ref. [32] LPE Microfiber 1531 56.54 314/1.3 0.35 1300 2.5 Ref. [33] MSD Microfiber 1563 84 280/45.4 2.39 357 14 This work 
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1. 叶传香，李珺子，王金涛. 基于WTe_2可饱和吸收体的超快掺铒光纤激光器. 光学学报. 2024(20): 174-180 . 
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