CN103245995B - 10.3 mu m-11.3 mu m transmissive long-wave infrared optical filter and preparation method - Google Patents
10.3 mu m-11.3 mu m transmissive long-wave infrared optical filter and preparation method Download PDFInfo
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- 230000003287 optical effect Effects 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 36
- OCGWQDWYSQAFTO-UHFFFAOYSA-N tellanylidenelead Chemical compound [Pb]=[Te] OCGWQDWYSQAFTO-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000005083 Zinc sulfide Substances 0.000 claims abstract description 28
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 14
- 229910052732 germanium Inorganic materials 0.000 claims abstract description 9
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims abstract description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052786 argon Inorganic materials 0.000 claims abstract description 4
- 238000001704 evaporation Methods 0.000 claims abstract 2
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 27
- 238000012544 monitoring process Methods 0.000 claims description 9
- 230000008021 deposition Effects 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims 2
- 239000010408 film Substances 0.000 abstract description 92
- 238000002834 transmittance Methods 0.000 abstract description 9
- 239000010409 thin film Substances 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 230000008020 evaporation Effects 0.000 abstract 1
- 238000010884 ion-beam technique Methods 0.000 abstract 1
- 230000003595 spectral effect Effects 0.000 description 9
- 238000001228 spectrum Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000000411 transmission spectrum Methods 0.000 description 2
- 229910002665 PbTe Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
Description
技术领域technical field
本发明涉及一种10.3~11.3μm透过长波红外滤光片及制备方法,具体地说,涉及一种在10.3~11.3μm谱段具有高透过率,同时在0.9~10.15μm和11.45~20μm谱段宽截止的长波红外滤光片;属于光学薄膜技术领域。The invention relates to a 10.3-11.3 μm long-wave infrared filter and a preparation method thereof, in particular to a filter with high transmittance in the 10.3-11.3 μm spectral band and at the same time at 0.9-10.15 μm and 11.45-20 μm The invention relates to a long-wave infrared filter with a wide cut-off spectrum; it belongs to the technical field of optical thin films.
背景技术Background technique
在10.3~11.3μm谱段具有高透过率的滤光片是目前遥感探测系统中一个关键的滤光片。为了减少信号噪声的影响,遥感探测系统中需要对0.9~10.15μm和11.45~20μm谱段的光信号进行抑制。因此亟需设计一种在10.3~11.3μm谱段具有高透过率,在0.9~10.15μm和11.45~20μm谱段宽截止,同时膜层质量较好的长波红外滤光片。The optical filter with high transmittance in the 10.3-11.3 μm spectral band is a key optical filter in the current remote sensing detection system. In order to reduce the influence of signal noise, the optical signals in the 0.9-10.15 μm and 11.45-20 μm spectral bands need to be suppressed in the remote sensing detection system. Therefore, it is urgent to design a long-wave infrared filter with high transmittance in the 10.3-11.3 μm spectral band, wide cut-off in the 0.9-10.15 μm and 11.45-20 μm spectral bands, and better film quality.
发明内容Contents of the invention
针对现有技术中尚无一种在10.3~11.3μm谱段具有高透过率,同时在0.9~10.15μm和11.45~20μm谱段宽截止的长波红外滤光片。本发明的目的之一在于提供一种10.3~11.3μm透过的长波红外滤光片,所述滤光片在10.3~11.3μm谱段具有高透过率,同时在0.9~10.15μm和11.45~20μm谱段宽截止。Aiming at the prior art, there is no long-wave infrared filter with high transmittance in the 10.3-11.3 μm spectral band and wide cut-off in the 0.9-10.15 μm and 11.45-20 μm spectral bands. One of the objectives of the present invention is to provide a long-wave infrared filter that passes through 10.3-11.3 μm. 20μm broad cut-off.
本发明的目的之二在于提供一种10.3~11.3μm透过的长波红外滤光片的制备方法。The second object of the present invention is to provide a method for preparing a long-wave infrared filter that transmits at 10.3-11.3 μm.
本发明的目的通过以下技术方案实现。The purpose of the present invention is achieved through the following technical solutions.
一种10.3~11.3μm透过长波红外滤光片,所述滤光片包括基底、基底一侧的长波通膜系和基底另一侧的短波通膜系。Disclosed is a 10.3-11.3 μm long-wave infrared filter, which includes a substrate, a long-wave pass film system on one side of the substrate, and a short-wave pass film system on the other side of the substrate.
其中,所述基底材料为锗,优选尺寸为:长29.5mm,宽1.36mm,厚1.2mm,优选表面光洁度为40/20;Wherein, the base material is germanium, the preferred size is: length 29.5mm, width 1.36mm, thickness 1.2mm, and the preferred surface finish is 40/20;
长波通膜系包括交替叠加的硫化锌(ZnS)膜层和碲化铅(PbTe)膜层,结构为:(0.5hl0.5h)^9(0.574l1.148h0.574l)^5(0.36h0.72l0.36h)^5,中心波长为7300nm;其中,h为碲化铅膜层,0.5、1.148和0.36分别为碲化铅膜层厚度对应基本厚度的系数,0.5h表示碲化铅膜层厚度为0.5个基本厚度,1.148h表示碲化铅膜层厚度为1.148个基本厚度,0.36h表示碲化铅膜层厚度为0.36个基本厚度,l为硫化锌膜层,1、0.574和0.72分别为硫化锌膜层厚度对应基本厚度的系数,l表示硫化锌膜层厚度为1个基本厚度,0.574l表示硫化锌膜层厚度为0.574个基本厚度,0.72l表示硫化锌膜层厚度为0.72个基本厚度,所述基本厚度为光学厚度中心波长的四分之一,基本膜堆(0.5hl0.5h)的周期数为9,基本膜堆(0.574l1.148h0.574l)和基本膜堆(0.36h0.72l0.36h)的周期数均为5。The long-wave pass film system includes alternately stacked zinc sulfide (ZnS) film layers and lead telluride (PbTe) film layers, and the structure is: (0.5hl0.5h)^9 (0.574l1.148h0.574l)^5 (0.36h0. 72l0.36h)^5, the central wavelength is 7300nm; where h is the lead telluride film layer, 0.5, 1.148 and 0.36 are the coefficients of the lead telluride film thickness corresponding to the basic thickness, and 0.5h represents the lead telluride film thickness is 0.5 basic thickness, 1.148h means the lead telluride film thickness is 1.148 basic thickness, 0.36h means the lead telluride film thickness is 0.36 basic thickness, l is the zinc sulfide film layer, 1, 0.574 and 0.72 are respectively The coefficient of the zinc sulfide film thickness corresponding to the basic thickness, l means that the thickness of the zinc sulfide film is 1 basic thickness, 0.574l means that the thickness of the zinc sulfide film is 0.574 basic thickness, and 0.72l means that the thickness of the zinc sulfide film is 0.72 basic Thickness, the basic thickness is a quarter of the central wavelength of the optical thickness, the cycle number of the basic film stack (0.5hl0.5h) is 9, the basic film stack (0.574l1.148h0.574l) and the basic film stack (0.36h0 .72l0.36h) are all 5 cycles.
采用TFCalc软件对所述长波通膜系的结构进行优化,得到优选的长波通膜系,如表1所示,其中,层数为1的膜层为长波通膜系的最外层,层数为39的膜层沉积在锗基底上,为长波通膜系的最内层;Adopt TFCalc software to optimize the structure of the long-wave pass film system, obtain the preferred long-wave pass film system, as shown in table 1, wherein, the film layer that the number of layers is 1 is the outermost layer of the long-wave pass film system, and the number of layers The film layer of 39 is deposited on the germanium substrate, which is the innermost layer of the long-wave pass film system;
表1 长波通膜系Table 1 Long wave pass film system
短波通膜系包括交替叠加的硫化锌膜层和碲化铅膜层,结构为:(lh)^8,中心波长为14600nm;其中,l为硫化锌膜层,1为硫化锌膜层厚度对应基本厚度的系数,l表示硫化锌膜层厚度为1个基本厚度,h为碲化铅膜层,1为碲化铅膜层厚度对应基本厚度的系数,h表示碲化铅膜层厚度为1个基本厚度,所述基本厚度为光学厚度中心波长的四分之一,基本膜堆(lh)的周期数为8。The short-wave pass film system includes alternately stacked zinc sulfide film layers and lead telluride film layers. The coefficient of the basic thickness, l means the thickness of the zinc sulfide film layer is 1 basic thickness, h is the lead telluride film layer, 1 is the coefficient of the lead telluride film layer thickness corresponding to the basic thickness, h means the lead telluride film layer thickness is 1 a basic thickness, the basic thickness is a quarter of the central wavelength of the optical thickness, and the period number of the basic film stack (lh) is 8.
采用TFCalc软件对所述短波通膜系的结构进行优化,得到优选的短波通膜系,如表2所示,其中,层数为1的膜层为短波通膜系的最外层,层数为16的膜层沉积在锗基底上,为短波通膜系的最内层;Adopt TFCalc software to optimize the structure of the short-wave pass film system, obtain the preferred short-wave pass film system, as shown in table 2, wherein, the film layer that the number of layers is 1 is the outermost layer of the short-wave pass film system, and the number of layers The film layer of 16 is deposited on the germanium substrate, which is the innermost layer of the short-wave pass film system;
表2 短波通膜系Table 2 Short-wave pass film system
一种本发明所述的10.3~11.3μm透过长波红外滤光片的制备方法,所述方法步骤如下:A method for preparing a 10.3-11.3 μm long-wave infrared filter according to the present invention, the steps of the method are as follows:
(1)将干净的基底装入清洁的真空室中,抽真空至3.0×10-3Pa;(1) Put the clean substrate into a clean vacuum chamber and evacuate to 3.0×10 -3 Pa;
(2)将基底加热到150℃,并保持30min;(2) Heat the substrate to 150°C and keep it for 30min;
(3)打开霍尔轻型离子源通氩气,气流量为30sccm,开启阴极电压为100~200V,阳极电压为50~100V,使得阳极电流为0.5A;采用电阻蒸发法分别在基底的一侧逐层交替沉积长波通膜系中的硫化锌膜层和碲化铅膜层,在基底的另一侧逐层交替沉积短波通膜系中的硫化锌膜层和碲化铅膜层,直至完成所述膜系的沉积;其中,硫化锌膜层的沉积速率为2.0~3.0nm/s,碲化铅膜层的沉积速率为0.8~1.0nm/s;膜层厚度采用光比例法监控;(3) Turn on the Hall light ion source to pass argon gas, the gas flow rate is 30 sccm, the cathode voltage is 100-200V, and the anode voltage is 50-100V, so that the anode current is 0.5A; Alternately deposit the zinc sulfide film layer and the lead telluride film layer in the long-wave pass film system layer by layer, and alternately deposit the zinc sulfide film layer and the lead telluride film layer in the short-wave pass film system layer by layer on the other side of the substrate until the completion The deposition of the film system; wherein, the deposition rate of the zinc sulfide film layer is 2.0-3.0nm/s, and the deposition rate of the lead telluride film layer is 0.8-1.0nm/s; the thickness of the film layer is monitored by the optical ratio method;
(4)基底自然冷却至室温,得到本发明所述的10.3~11.3μm透过长波红外滤光片。(4) The substrate is naturally cooled to room temperature to obtain the 10.3-11.3 μm long-wave infrared filter according to the present invention.
有益效果Beneficial effect
1.本发明提供了一种10.3~11.3μm透过长波红外滤光片,所述滤光片达到优良技术指标:在10.3~11.3μm谱段具有高透过率τav≥80%,在0.9~10.15μm和11.45~20μm谱段宽截止,截止区域内截止深度τλ<1%,半功率点波长允差在50nm之内,可大大改进该谱段滤光片的通带以及截止带的特性,满足遥感探测系统的使用要求,具有高稳定性和高可靠性;1. The present invention provides a 10.3-11.3 μm long-wave infrared filter, the filter achieves excellent technical indicators: it has a high transmittance τ av ≥ 80% in the 10.3-11.3 μm spectrum, and at 0.9 ~10.15μm and 11.45~20μm wide cut-off, the cut-off depth τ λ <1% in the cut-off area, the half-power point wavelength tolerance is within 50nm, which can greatly improve the pass band and cut-off band of the filter in this spectrum. Features, meet the requirements of the remote sensing detection system, with high stability and reliability;
2.本发明提供了一种10.3~11.3μm透过长波红外滤光片,所述滤光片的膜系包括交替叠加的硫化锌膜层和碲化铅膜层,膜系层数较少;2. The present invention provides a 10.3-11.3 μm long-wave infrared filter, the film system of the filter includes alternately stacked zinc sulfide film layers and lead telluride film layers, and the number of film system layers is relatively small;
3.本发明提供了一种10.3~11.3μm透过长波红外滤光片的制备方法,所述方法可制得本发明所述的滤光片,工艺稳定,重复性好,操作简便,产品成品率高。3. The present invention provides a preparation method of a 10.3-11.3 μm long-wave infrared filter, the method can produce the filter of the present invention, the process is stable, the repeatability is good, the operation is simple, and the finished product is High rate.
附图说明Description of drawings
图1为实施例1中滤光片的透射光谱图。Fig. 1 is the transmittance spectrum diagram of the optical filter in embodiment 1.
具体实施方式Detailed ways
为了充分说明本发明的特性以及实施本发明的方式,下面给出实施例。In order to fully illustrate the characteristics of the present invention and the mode of carrying out the present invention, examples are given below.
实施例1Example 1
一种10.3~11.3μm透过长波红外滤光片,所述滤光片包括锗基底、基底一侧的长波通膜系和基底另一侧的短波通膜系。Disclosed is a 10.3-11.3 μm long-wave infrared filter, which includes a germanium substrate, a long-wave pass film system on one side of the substrate, and a short-wave pass film system on the other side of the substrate.
其中,所述基底长29.5mm,宽1.36mm,厚1.2mm,表面光洁度为40/20。Wherein, the base is 29.5mm long, 1.36mm wide, 1.2mm thick, and has a surface finish of 40/20.
长波通膜系包括交替叠加的硫化锌膜层和碲化铅膜层,中心波长为7300nm;各膜层参数如表3所示,其中,层数为1的膜层为长波通膜系的最外层,层数为39的膜层沉积在锗基底上,为长波通膜系的最内层;The long-wave pass film system includes alternately stacked zinc sulfide film layers and lead telluride film layers, and the center wavelength is 7300nm; the parameters of each film layer are shown in Table 3, and the film layer with the number of layers is 1. The outer layer, the film layer with 39 layers is deposited on the germanium substrate, which is the innermost layer of the long-wave pass film system;
表3 长波通膜系及膜层厚度监控Table 3 Long-wave pass film system and film thickness monitoring
短波通膜系包括交替叠加的硫化锌膜层和碲化铅膜层,中心波长为14600nm,各膜层参数如表4所示,其中,层数为1的膜层为短波通膜系的最外层,层数为16的膜层沉积在锗基底上,为短波通膜系的最内层;The short-wave pass film system includes alternately stacked zinc sulfide film layers and lead telluride film layers, and the center wavelength is 14600nm. The parameters of each film layer are shown in Table 4, and the film layer with the number of layers is 1. The outer layer, with 16 layers deposited on the germanium substrate, is the innermost layer of the short-wave pass film system;
表4 短波通膜系及膜层厚度监控Table 4 Short-wave pass film system and film thickness monitoring
本实施例所述滤光片的制备方法步骤如下:The steps of the preparation method of the optical filter described in this embodiment are as follows:
(1)用吸尘器清除真空室内杂质,然后用脱脂纱布蘸无水乙醇擦拭干净真空室内壁;用分析纯丙酮超声清洗基底10min,再用分析纯乙醇超声清洗基底10min的锗基片,将干净的基底装入清洁的真空室中,抽真空至3.0×10-3Pa;(1) Use a vacuum cleaner to remove impurities in the vacuum chamber, and then wipe the inner wall of the vacuum chamber with degreasing gauze dipped in absolute ethanol; ultrasonically clean the substrate with analytical pure acetone for 10 minutes, and then ultrasonically clean the germanium substrate with analytical pure ethanol for 10 minutes. Put the substrate into a clean vacuum chamber and evacuate to 3.0×10 -3 Pa;
(2)将基底加热到150℃,并保持30min;(2) Heat the substrate to 150°C and keep it for 30min;
(3)打开霍尔轻型离子源通氩气,气流量为30sccm,开启阴极电压为100~200V,阳极电压为50~100V,使得阳极电流为0.5A;采用电阻蒸发法分别在基底的一侧逐层交替沉积长波通膜系中的硫化锌膜层和碲化铅膜层,在基底的另一侧逐层交替沉积短波通膜系中的硫化锌膜层和碲化铅膜层,直至完成所述膜系的沉积;其中,硫化锌膜层的沉积速率为2.0~3.0nm/s,碲化铅膜层的沉积速率为0.8~1.0nm/s;膜层厚度采用光比例法监控,监控波长和次数如表3和表4所示;(3) Turn on the Hall light ion source to pass argon gas, the gas flow rate is 30 sccm, the cathode voltage is 100-200V, and the anode voltage is 50-100V, so that the anode current is 0.5A; Alternately deposit the zinc sulfide film layer and the lead telluride film layer in the long-wave pass film system layer by layer, and alternately deposit the zinc sulfide film layer and the lead telluride film layer in the short-wave pass film system layer by layer on the other side of the substrate until the completion The deposition of the film system; wherein, the deposition rate of the zinc sulfide film layer is 2.0-3.0nm/s, and the deposition rate of the lead telluride film layer is 0.8-1.0nm/s; the thickness of the film layer is monitored by the light ratio method, and the monitoring The wavelength and times are shown in Table 3 and Table 4;
(4)基底自然冷却至室温,得到本实施例所述的10.3~11.3μm透过长波红外滤光片。(4) The substrate is naturally cooled to room temperature to obtain the 10.3-11.3 μm long-wave infrared filter described in this embodiment.
对所述滤光片进行如下性能测试:Carry out following performance test to described optical filter:
采用PE公司system 2000红外傅里叶光谱仪测试,得到透射光谱如图1所示,用UVWINLAB软件对图1中的谱线进行计算,可知所述滤光片在10.3~11.3μm谱段的平均透过率为84.61%,在0.9~10.15μm谱段的平均透过率为0.43%和,1.45~20μm谱段的平均透过率为0.01%。The system 2000 infrared Fourier spectrometer of PE Company was used to test, and the transmission spectrum was obtained as shown in Figure 1. The spectral lines in Figure 1 were calculated with UVWINLAB software, and it can be known that the average transmission of the filter in the 10.3-11.3 μm spectral segment The transmittance is 84.61%, the average transmittance in the 0.9-10.15μm spectrum is 0.43% and the average transmittance in the 1.45-20μm spectrum is 0.01%.
本发明包括但不限于以上实施例,凡是在本发明的精神和原则之下进行的任何等同替换或局部改进,都将视为在本发明的保护范围之内。The present invention includes but is not limited to the above embodiments, and any equivalent replacement or partial improvement made under the spirit and principle of the present invention will be considered within the protection scope of the present invention.
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CN105137514B (en) * | 2015-09-11 | 2017-07-28 | 兰州空间技术物理研究所 | 4.2~4.45 μm pass through medium-wave infrared optical filter and preparation method |
CN106324738B (en) * | 2016-11-04 | 2019-02-01 | 天津津航技术物理研究所 | A kind of LONG WAVE INFRARED optical filter and preparation method thereof |
CN114460677B (en) * | 2022-04-13 | 2022-09-16 | 翼捷安全设备(昆山)有限公司 | Infrared filter for MEMS black body packaging and preparation method thereof |
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