CN110727052A - A low-loss infrared high nonlinear optical waveguide preparation method - Google Patents
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Abstract
Description
技术领域technical field
本发明涉及微纳加工及非线性光学领域,更具体地,涉及一种低损耗红外高非线性光波导制备方法。The invention relates to the fields of micro-nano processing and nonlinear optics, and more particularly, to a method for preparing a low-loss infrared high nonlinear optical waveguide.
背景技术Background technique
红外波段包括近、中、远红外三个波段,其中近红外波段包括通讯波段,中远红外波段则包括许多生物分子、典型有毒气体和危险品分子的指纹区以及大气温室气体荧光光谱波段,因此,具有高度集成化的红外波导具有极其重要的研究意义。除此之外,红外波导在激光传输、热像素传送、红外光谱研究等领域也具有重要的应用背景。The infrared band includes three bands: near-infrared, mid-infrared and far-infrared. The near-infrared band includes the communication band, and the mid-to-far infrared band includes the fingerprints of many biomolecules, typical toxic gas and dangerous goods molecules, and the fluorescence spectrum band of atmospheric greenhouse gases. Therefore, The highly integrated infrared waveguide has extremely important research significance. In addition, infrared waveguides also have important application backgrounds in the fields of laser transmission, thermal pixel transmission, and infrared spectroscopy research.
目前片上红外波导主要使用的材料有锗、硅及硫系等材料:其中锗波导在红外波导不仅损耗大,而且传输波段主要在3μm以后,不包含通讯波段,而硅波导除了具有严重的双光子吸收,损耗大之外,还有传输波段限制,制备难度等问题。At present, the main materials used in on-chip infrared waveguides are germanium, silicon, and chalcogenide materials. Among them, germanium waveguides not only have large losses in infrared waveguides, but also the transmission band is mainly after 3 μm, excluding the communication band. In addition to the large absorption and loss, there are also problems such as the limitation of the transmission band and the difficulty of preparation.
硫系波导是由硫、硒、碲及一些其他金属与非金属材料以共价键形成的一种非晶体材料,其具有非常宽的传输波段(从可见光波段到20μm)、高非线性、以及极低的双光子吸收等优势,而且较容易通过热蒸镀、磁控溅射等方法制备成薄膜并加工成波导;但是硫系波导目前也存在损耗大等问题严重限制了其应用性能。主要原因是在硫系波导加工过程中由于刻蚀速率不均匀导致的侧壁粗糙,从而使硫系波导的侧壁具有非常大的散射导致硫系波导损耗大。Chalcogenide waveguide is an amorphous material formed by covalent bonds of sulfur, selenium, tellurium and some other metals and non-metallic materials, which has a very wide transmission band (from visible light band to 20μm), high nonlinearity, and It has the advantages of extremely low two-photon absorption, etc., and it is easier to prepare thin films by thermal evaporation, magnetron sputtering, etc. and process them into waveguides; however, chalcogenide waveguides also have problems such as large losses, which seriously limit their application performance. The main reason is that the sidewalls of the chalcogenide waveguides are rough due to the uneven etching rate during the processing of the chalcogenide waveguides, so that the sidewalls of the chalcogenide waveguides have very large scattering and lead to large losses of the chalcogenide waveguides.
发明内容SUMMARY OF THE INVENTION
本发明为克服上述现有技术中的缺陷,提供一种低损耗红外高非线性光波导制备方法。In order to overcome the above-mentioned defects in the prior art, the present invention provides a low-loss infrared high nonlinear optical waveguide preparation method.
为解决上述技术问题,本发明采用的技术方案是:一种低损耗红外高非线性光波导制备方法,包括以下步骤:In order to solve the above-mentioned technical problems, the technical solution adopted in the present invention is: a low-loss infrared high nonlinear optical waveguide preparation method, comprising the following steps:
S1.分析硫系光波导在红外波段光波的传输特性;S1. Analyze the transmission characteristics of chalcogenide optical waveguides in the infrared band;
S2.分析电子束曝光各个参数及电子束胶种类对硫系波导制备的影响,并通过等离子体反应刻蚀,实现波导的制备;S2. Analyze the influence of various parameters of electron beam exposure and the type of electron beam glue on the preparation of chalcogenide waveguides, and realize the preparation of waveguides by plasma reactive etching;
S3.通过旋涂法实现聚合物包层的生长;S3. The growth of the polymer cladding layer is realized by spin coating;
S4.结合包层热退火工艺,将波导器件放置于退火炉中加热到超过硫系材料的玻璃化转变温度,从而使波导处于熔融状态,并在表面张力的作用下使其侧壁变的相对光滑,并通过截断法进行损耗测试。S4. Combined with the thermal annealing process of the cladding, the waveguide device is placed in an annealing furnace and heated to a temperature exceeding the glass transition temperature of the chalcogenide material, so that the waveguide is in a molten state, and its sidewalls become relatively relatively under the action of surface tension. Smooth and tested for loss by the truncation method.
作为优选的,波导横截面结构为脊型或矩形,所选用的材料为硫系材料。Preferably, the cross-sectional structure of the waveguide is a ridge or a rectangle, and the selected material is a chalcogenide material.
作为优选的,在选定波导结构中,若结构为矩形波导,其截面宽度范围为1微米至10微米,高度范围为300纳米至5微米,若结构为脊型波导,则脊高根据传输波段要求设计。Preferably, in the selected waveguide structure, if the structure is a rectangular waveguide, its cross-sectional width ranges from 1 micron to 10 microns, and its height ranges from 300 nanometers to 5 microns. If the structure is a ridge waveguide, the ridge height depends on the transmission band. Design required.
作为优选的,所述的波导结构包括下部包层、纤芯、以及上部包层;所述纤芯的折射率高于上下部包层,且纤芯与包层的接触界面平滑。Preferably, the waveguide structure includes a lower cladding layer, a fiber core, and an upper cladding layer; the refractive index of the fiber core is higher than that of the upper and lower cladding layers, and the contact interface between the fiber core and the cladding layer is smooth.
作为优选的,通过等离子体反应刻蚀参数的调整实现低损耗红外硫系光波导的制备,该刻蚀过程包括化学刻蚀和物理刻蚀;化学刻蚀主要使用CHF3或CF4+H2气体;物理刻蚀则通过Ar或He气体实现。Preferably, the preparation of low-loss infrared chalcogenide optical waveguide is realized by adjusting the parameters of plasma reactive etching, and the etching process includes chemical etching and physical etching; chemical etching mainly uses CHF3 or CF4+H2 gas; physical Etching is achieved by Ar or He gas.
作为优选的,低损耗红外硫系波导的包层通过匀胶机通过旋涂法,即使用匀胶机在2000rpm的旋转速度下,旋转1分钟,使波导上方生长一层聚合物包层,并结合包层热退火工艺,将波导器件放置于退火炉中,在200℃~240℃条件下,具体温度根据具体材料决定,加热8-12小时。Preferably, the cladding layer of the low-loss infrared chalcogenide waveguide is passed through a spin coating method through a glue machine, that is, the glue machine is used for 1 minute at a rotation speed of 2000 rpm, so that a layer of polymer cladding layer is grown on the waveguide, and Combined with the cladding thermal annealing process, the waveguide device is placed in an annealing furnace, and heated for 8-12 hours at a temperature of 200°C to 240°C, depending on the specific material.
作为优选地,所述的截断法测试需要包括至少两根不同长度的波导结构。确保排除端面耦合及耦合误差的影响。Preferably, the truncation method test needs to include at least two waveguide structures with different lengths. Make sure to exclude the effects of end-face coupling and coupling errors.
作为优选地,所述的波导结构可测量波导传输的传输功率、损耗系数及工作频率。Preferably, the waveguide structure can measure the transmission power, loss coefficient and operating frequency of the waveguide transmission.
与现有技术相比,有益效果是:本发明通过电子束曝光及调整等离子体反应的刻蚀参数,并结合热退火工艺,实现一种高精度、侧壁低粗糙度的高非线性波导制备,并与传统的光刻作比较,提供了一种低损耗红外硫系波导的制备方法,实现了对红外波段光波低损耗的传输。Compared with the prior art, the beneficial effects are as follows: the present invention realizes the preparation of a highly nonlinear waveguide with high precision and low sidewall roughness through electron beam exposure and adjusting the etching parameters of the plasma reaction, combined with the thermal annealing process , and compared with the traditional lithography, a preparation method of a low-loss infrared chalcogenide waveguide is provided, which realizes the low-loss transmission of light waves in the infrared band.
附图说明Description of drawings
图1是本发明波导横截面结构图。FIG. 1 is a cross-sectional structural diagram of the waveguide of the present invention.
图2是本发明脊型波导SEM表征图。FIG. 2 is a SEM characterization diagram of the ridge waveguide of the present invention.
图3是本发明脊型波导仿真电场模图。FIG. 3 is a simulated electric field model diagram of the ridge waveguide of the present invention.
图4是本发明制备流程图。Fig. 4 is the preparation flow chart of the present invention.
图5为本发明测试系统结构示意图。FIG. 5 is a schematic structural diagram of the testing system of the present invention.
具体实施方式Detailed ways
附图仅用于示例性说明,不能理解为对本发明的限制;为了更好说明本实施例,附图某些部件会有省略、放大或缩小,并不代表实际产品的尺寸;对于本领域技术人员来说,附图中某些公知结构及其说明可能省略是可以理解的。附图中描述位置关系仅用于示例性说明,不能理解为对本发明的限制。The accompanying drawings are for illustrative purposes only, and should not be construed as limiting the present invention; in order to better illustrate the present embodiment, some parts of the accompanying drawings may be omitted, enlarged or reduced, and do not represent the size of the actual product; for those skilled in the art It is understandable to the artisan that certain well-known structures and descriptions thereof may be omitted from the drawings. The positional relationships described in the drawings are only for exemplary illustration, and should not be construed as limiting the present invention.
实施例1:Example 1:
如图4所示,结合图1至5说明本实施方式,如图1所示,低损耗红外硫系光波导,包括:自下至上依次是衬底硅201、下部包层202、纤芯203、上部包层204;下部包层202为二氧化硅;设于该下部包层202覆层上且具有入射面和出射面的纤芯203为红外硫系;及至少埋入这些纤芯203的上部包层204为空气;纤芯203的折射率比上下部包层大,且纤芯203与上部包层204、下部包层202的界面平滑。As shown in FIG. 4 , the present embodiment will be described with reference to FIGS. 1 to 5 . As shown in FIG. 1 , the low-loss infrared chalcogenide optical waveguide includes:
本实施方式提供了一种低损耗红外硫系波导的制备方法,涉及微纳加工及非线性光学领域,尤其涉及波导中低损耗光波传输,具体步骤包括步骤一:分析硫系光波导红外波段光波的传输特性;步骤二:分析电子束曝光各个参数及电子束胶对硫系波导制备的影响,选择合适的曝光参数及电子束胶进行掩膜版制备,并通过等离子体反应刻蚀,实现波导的制备;步骤三:通过旋涂法实现聚合物包层的生长;步骤四:结合包层热退火工艺,将器件放置于退火炉中加热到超过硫系波导的玻璃化转变温度,从而使波导处于熔融状态,并在表面张力的作用下使侧壁变的相对光滑,从而降低波导的传输损耗,并通过截断法进行损耗测试。This embodiment provides a method for preparing a low-loss infrared chalcogenide waveguide, which relates to the fields of micro-nano processing and nonlinear optics, and in particular to low-loss optical wave transmission in waveguides. Step 2: Analyze the influence of various parameters of electron beam exposure and electron beam glue on the preparation of chalcogenide waveguide, select appropriate exposure parameters and electron beam glue for mask preparation, and realize the waveguide through plasma reactive etching Step 3: realize the growth of the polymer cladding by spin coating method; Step 4: combine the thermal annealing process of the cladding layer, place the device in an annealing furnace and heat the device to exceed the glass transition temperature of the chalcogenide waveguide, so that the waveguide It is in a molten state, and the sidewall becomes relatively smooth under the action of surface tension, thereby reducing the transmission loss of the waveguide, and the loss test is performed by the truncation method.
其中,所述的波导结构中,其截面长为2μm,脊高0.5μm,总高0.8μm,能够实现与光纤高斯模式较好的尺寸匹配,降低耦合损耗。Wherein, in the waveguide structure, the section length is 2 μm, the ridge height is 0.5 μm, and the total height is 0.8 μm, which can achieve better size matching with the Gaussian mode of the optical fiber and reduce coupling loss.
另外,所述的波导结构包括下部包层、纤芯、以及上部包层。所述纤芯的折射率高于上下部包层,且纤芯与包层接触界面平滑。Additionally, the waveguide structure includes a lower cladding, a core, and an upper cladding. The refractive index of the core is higher than that of the upper and lower cladding layers, and the contact interface between the core and the cladding layers is smooth.
在本实施例中,所述的低损耗红外硫系波导的制备方法通过调整反应等离子体反应刻蚀参数的调整实现,该刻蚀过程主要使用Ar和CHF3两种反应物质。In this embodiment, the preparation method of the low-loss infrared chalcogenide waveguide is realized by adjusting the parameters of reactive plasma reactive etching, and the etching process mainly uses two reactive substances, Ar and CHF 3 .
具体包括以下步骤:Specifically include the following steps:
步骤一:清洗:即通过一定的手段将需要进行制备结构的衬底进行清洁,使其涂胶过程中能使胶厚度更均匀。目前,主流的清洗方法为三步清洗法,即分别通过超声清洗机分别在丙酮、异丙醇和去离子水中进行超声10分钟。然后,通过软烘除去薄膜表面的水分,增强薄膜与电子束胶之间的黏附性。Step 1: Cleaning: that is, cleaning the substrate that needs to be structured by certain means, so that the thickness of the glue can be more uniform during the gluing process. At present, the mainstream cleaning method is a three-step cleaning method, that is, ultrasonication is carried out in acetone, isopropanol and deionized water for 10 minutes by an ultrasonic cleaning machine respectively. Then, the moisture on the surface of the film is removed by soft baking to enhance the adhesion between the film and the electron beam glue.
步骤二:涂胶:将衬底放到匀胶机上,并通过真空泵将衬底吸附住。然后,通过移液枪将选好的正电子束胶滴到衬底上面直到整个衬底覆盖满该电子束胶。最后,运行设计好的旋涂程序。旋涂完成后,将衬底放置于加热台上,温度为150℃进行前烘。Step 2: Gluing: put the substrate on the glue spinner, and suck the substrate by a vacuum pump. Then, the selected positron beam glue was dropped onto the substrate by a pipette until the entire substrate was covered with the electron beam glue. Finally, run the designed spin coating program. After the spin coating was completed, the substrate was placed on a heating table, and the temperature was 150°C for pre-baking.
步骤三:进样:将之前制备好的样品通过样品台运输到曝光室。Step 3: Sample injection: Transport the previously prepared sample to the exposure chamber through the sample stage.
步骤四:曝光:通过“电子束”将设计好的版图曝光到电子束胶上,使曝光部位发生变性。Step 4: Exposure: Expose the designed layout to the electron beam glue through "electron beam" to denature the exposed part.
步骤五:显影:通过对应的显影液将曝光部位的电子束胶除去,其他多余的电子束胶保留下来。Step 5: Development: The electron beam glue in the exposed part is removed by the corresponding developer, and the other excess electron beam glue is retained.
步骤六:刻蚀及去胶:将样品贴到反应离子刻蚀机的载盘上。然后,抽真空,并将样品送入反应腔体内,运行设置好的程序。关键在于设置好Ar和CHF3两种反应物质的参数及反应过程中的工作功率。刻蚀完之后,将样品放入反应离子刻蚀机内再次运行去胶程序,将残留的电子束胶去除。Step 6: Etching and degumming: Attach the sample to the carrier plate of the reactive ion etching machine. Then, a vacuum is drawn, the sample is fed into the reaction chamber, and the programmed program is run. The key lies in setting the parameters of Ar and CHF 3 reactive species and the working power during the reaction. After etching, put the sample into the reactive ion etching machine and run the degumming procedure again to remove the residual electron beam glue.
步骤七:包层生长及热退火:通过旋涂法将聚合物包层覆盖满整个波导结构。最后,将样品放置于退火炉中,在220℃条件下,具体温度根据具体材料决定,加热12小时。Step 7: cladding growth and thermal annealing: the polymer cladding is applied to the entire waveguide structure by spin coating. Finally, the sample was placed in an annealing furnace and heated for 12 hours at a temperature of 220°C, depending on the specific material.
实施例2Example 2
结合图5说明本实施方式,本实施方式通过对不同长度的波导输入输出功率进行对比,然后利用两个不同长度的波导输出功率进行作差,求得波导损耗系数。This embodiment is described with reference to FIG. 5 . In this embodiment, the input and output powers of waveguides with different lengths are compared, and then the output powers of two waveguides with different lengths are used to make a difference to obtain the waveguide loss coefficient.
测试系统为波导损耗因子的测试方案包括以下步骤:The test system for the waveguide loss factor test scheme includes the following steps:
步骤一:首先将制备好的波导结构放在一个吸附台上,保证测试过程中结构不会出现抖动。Step 1: First, place the prepared waveguide structure on an adsorption table to ensure that the structure will not shake during the test.
步骤二:将透镜光纤通过三维调节架,粗调对准波导的输入输出两端,通过CCD进行观察,再在输入端输入一束红外波段、10dBm的光源,在输出端接入一个功率计,并通过细调三维调节架使透镜光纤恰好对准波导输入输出端口,可以通过功率计进行观察,得到最大输出即为一束光经过耦合进入波导后的输出。同理测得其他不同长度波导的输出功率。本实施过程中,所测长波导长L2=8.28cm,输入光束经过该长度波导之后输出功率为-0.84dBm,短波导长L1=0.7cm,输入光束经过该长度波导之后输出功率为1.10dBm。根据截断法计算波导损耗因子的公式α=(P2-P1)/(L2-L1)可算,波导损耗因子α=0.26dB/cm。此损耗因子,目前在红外硫系波导中相同波导尺寸下,已经属于低损耗行列。Step 2: Pass the lens fiber through the three-dimensional adjustment frame, roughly adjust the input and output ends of the waveguide, observe through the CCD, and then input a beam of infrared band, 10dBm light source at the input end, and connect a power meter at the output end. And through fine adjustment of the three-dimensional adjustment frame, the lens fiber is just aligned with the input and output ports of the waveguide, which can be observed by a power meter, and the maximum output is obtained after a beam of light is coupled into the waveguide. Similarly, the output powers of other waveguides with different lengths are measured. In this implementation process, the measured long waveguide length L 2 =8.28cm, the output power of the input beam after passing through the length of the waveguide is -0.84dBm, the short waveguide length L 1 =0.7cm, the output power of the input beam after passing through the length of the waveguide is 1.10 dBm dBm. The formula α=(P 2 -P 1 )/(L 2 -L 1 ) for calculating the waveguide loss factor can be calculated according to the truncation method, and the waveguide loss factor α=0.26dB/cm. This loss factor, currently in the infrared chalcogenide waveguide with the same waveguide size, already belongs to the ranks of low loss.
显然,本发明的上述实施例仅仅是为清楚地说明本发明所作的举例,而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明权利要求的保护范围之内。Obviously, the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, rather than limiting the embodiments of the present invention. For those of ordinary skill in the art, changes or modifications in other different forms can also be made on the basis of the above description. There is no need and cannot be exhaustive of all implementations here. Any modifications, equivalent replacements and improvements made within the spirit and principle of the present invention shall be included within the protection scope of the claims of the present invention.
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