CN105839053B - 一种一碘化铟多晶薄膜的制备方法 - Google Patents
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- FOVZCYAIUZHXGB-UHFFFAOYSA-M indium(1+);iodide Chemical compound I[In] FOVZCYAIUZHXGB-UHFFFAOYSA-M 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000010408 film Substances 0.000 claims abstract description 60
- 238000001704 evaporation Methods 0.000 claims abstract description 28
- 230000008020 evaporation Effects 0.000 claims abstract description 28
- 238000000151 deposition Methods 0.000 claims abstract description 12
- 230000008021 deposition Effects 0.000 claims abstract description 10
- 239000011521 glass Substances 0.000 claims abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 5
- 244000061458 Solanum melongena Species 0.000 claims abstract description 4
- 239000002932 luster Substances 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000002207 thermal evaporation Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000012085 test solution Substances 0.000 claims description 5
- 239000010409 thin film Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims 1
- 229910052738 indium Inorganic materials 0.000 claims 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims 1
- 229910052740 iodine Inorganic materials 0.000 claims 1
- 239000011630 iodine Substances 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 8
- 239000004615 ingredient Substances 0.000 abstract description 3
- 238000000427 thin-film deposition Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 11
- 239000012535 impurity Substances 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 229910017115 AlSb Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910052571 earthenware Inorganic materials 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- RQQRAHKHDFPBMC-UHFFFAOYSA-L lead(ii) iodide Chemical compound I[Pb]I RQQRAHKHDFPBMC-UHFFFAOYSA-L 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- RMUKCGUDVKEQPL-UHFFFAOYSA-K triiodoindigane Chemical compound I[In](I)I RMUKCGUDVKEQPL-UHFFFAOYSA-K 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0694—Halides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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- Physical Vapour Deposition (AREA)
- Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
Abstract
一种一碘化铟多晶薄膜，它是一种呈紫红色，具有金属光泽，表面光滑的薄膜；上述一碘化铟多晶薄膜的制备方法主要是将一碘化铟多晶放置在玛瑙研钵中研磨成粉末，放入坩埚内作为蒸发源；由涡轮分子泵实现真空腔室的背底真空度；将普通玻璃片作为蒸镀沉淀衬底，悬挂在坩埚上方处；通过电阻加热蒸发源，控制挡板精确地做出薄膜沉积；将所得的一碘化铟多晶薄膜冷却至室温，得到200～900nm的一碘化铟多晶薄膜。本发明制备的一碘化铟多晶薄膜具有厚度和成分均匀性好、附着效果好、薄膜纯度高、化学配比好、结构致密度的优点，不缺高沉积速率高、适合大面积生长、可以大规模生产。
Description
技术领域
本发明属于材料技术领域，特别涉及一种一碘化铟多晶薄膜的制备方法。
背景技术
一碘化铟(InI)单晶具有电阻率高、载流子迁移率寿命积较大、制成的γ射线探测器具有较高的能量分辨率和探测效率、并能够在室温下使用和保存等优点,使其成为一种极有前途的室温核辐射探测器材料,是近年来重点研究的室温核辐射探测器的新材料之一。
由于高电阻率、大体积一碘化铟单晶的制备存在较多困难,而小体积一碘化铟单晶不能满足大面积辐射成像器件的制备需求,近年来一碘化铟单晶的研究和应用已经受到了一定程度的限制。与生长块状化合物半导体单晶相比,多晶薄膜材料是一种非常有前途且制备更加方便,工艺也更完善的半导体材料。对于PbI2、AlSb、HgI2等拥有类似特性、同为室温核辐射探测材料的薄膜多晶,国内外在其制备以及辐射探测器件应用方面已取得了丰富的研究成果。一碘化铟多晶薄膜可以满足核探测器以及大面积辐射成像器件的需求，且相比于一碘化铟单晶，一碘化铟多晶薄膜发展和利用空间更大。但一碘化铟多晶薄膜的制备，目前国内外还未见有相关报道。
发明内容
本发明的目的在于提供一种厚度和成分均匀性好、沉积速率高、可以大规模生产的一碘化铟多晶薄膜的制备方法。
本发明的一碘化铟多晶薄膜是一种呈紫红色，具有金属光泽，表面光滑的薄膜。
上述一碘化铟多晶薄膜的制备方法包括如下步骤：
(1)将纯度>99.99％的一碘化铟多晶放置在玛瑙研钵中研磨成粉末，放入石墨坩埚内作为蒸发源；
(2)将普通玻璃片用去离子水冲洗后,再用丙酮和乙醇试液分别对其进行超声清洗10min,用高纯氮气烘干处理后，用其作为蒸镀沉淀衬底，悬挂在坩埚上方25cm处；
(3)将步骤(1)的石墨坩埚放入热蒸发真空腔室，采用涡轮分子泵使其腔室的背底真空度达到1.5×10-3Pa以下；
(4)在薄膜生长过程中，由膜厚仪监测加热速率和蒸镀厚度，以20℃/min的速率缓慢加热蒸发源至50～90℃，控制薄膜沉积速率在0.5～2.0沉积得到200～900nm的一碘化铟多晶薄膜。
(5)将步骤(4)的一碘化铟多晶薄膜冷却至室温，完成薄膜的制备。
本发明与现有技术相比具有如下优点：
1、使用真空蒸发法制备的一碘化铟多晶薄膜具有厚度和成分均匀性好、沉积速率高、适合大面积生长、可以大规模生产；
2、与衬底附着效果好；薄膜纯度高，化学配比好；结构致密度高，是一种使用十分广泛的多晶薄膜制备方法。
附图说明
图1是本发明实施例3制备的一碘化铟多晶薄膜的样品图；
图2是本发明实施例3制备的一碘化铟多晶薄膜的XRD图；
图3是本发明实施例3制备的一碘化铟多晶薄膜的表面SEM图；
图4是本发明实施例3制备的一碘化铟多晶薄膜的紫外-可见透过谱和吸收系数图。
具体实施方式
实施例1
将纯度>99.99％的一碘化铟多晶放置在玛瑙研钵中研磨，称取5g一碘化铟多晶粉末放入石墨坩埚内作为蒸发源；将厚度为1mm的普通玻璃片用去离子水对其冲洗,再用丙酮和乙醇试液分别对其进行超声清洗10min,高纯氮气烘干处理后，迅速放入热蒸发高真空腔室中，悬挂在坩埚上方25cm处；将石墨坩埚放入热蒸发真空腔室，通过涡轮分子泵实现腔室的背底真空度达到1.0×10-3Pa；在蒸发过程中，升温过快会导致蒸发源材料和坩埚中吸附的杂质不能充分脱附，对沉积的薄膜样品造成污染，为使蒸发源材料和坩埚上吸附的杂质完全脱附，因此应由旁镜观察加在坩埚上电流的加热情况，在薄膜生长过程中，由膜厚仪监测加热速率和蒸镀厚度，以20℃/min的速率缓慢加热蒸发源至60℃，并保持薄膜沉积速率0.6得到沉积厚度为300nm的一碘化铟多晶薄膜，将制得的一碘化铟多晶薄膜冷却至室温。
实施例2
将纯度>99.99％的一碘化铟多晶放置在玛瑙研钵中研磨，称取10g一碘化铟多晶粉末放入石墨坩埚内作为蒸发源；将厚度为1mm的普通玻璃片用去离子水对其冲洗,再用丙酮和乙醇试液分别对其进行超声清洗10min,高纯氮气烘干处理后，迅速放入热蒸发高真空腔室中，悬挂在坩埚上方25cm处；将石墨坩埚放入热蒸发真空腔室，通过涡轮分子泵实现腔室的背底真空度达到0.8×10-3Pa；在蒸发过程中，升温过快会导致蒸发源材料和坩埚中吸附的杂质不能充分脱附，对沉积的薄膜样品造成污染。为使蒸发源材料和坩埚上吸附的杂质完全脱附，因此应由旁镜观察加在坩埚上电流的加热情况。在薄膜生长过程中，由膜厚仪监测加热速率和蒸镀厚度，以20℃/min的速率缓慢加热蒸发源至70℃，并保持薄膜沉积速率0.8得到沉积厚度为700nm的一碘化铟多晶薄膜，将制得的一碘化铟多晶薄膜冷却至室温。
实施例3
将纯度>99.99％的一碘化铟多晶放置在玛瑙研钵中研磨，称取15g一碘化铟多晶粉末放入石墨坩埚内作为蒸发源；将厚度为1mm的普通玻璃片用去离子水对其冲洗,再用丙酮和乙醇试液分别对其进行超声清洗10min,高纯氮气烘干处理后，迅速放入热蒸发高真空腔室中，悬挂在坩埚上方25cm处；将石墨坩埚放入热蒸发真空腔室，通过涡轮分子泵实现腔室的背底真空度达到0.5×10-3Pa；在蒸发过程中，升温过快会导致蒸发源材料和坩埚中吸附的杂质不能充分脱附，对沉积的薄膜样品造成污染。为使蒸发源材料和坩埚上吸附的杂质完全脱附，因此应由旁镜观察加在坩埚上电流的加热情况。在薄膜生长过程中，由膜厚仪监测加热速率和蒸镀厚度，以20℃/min的速率缓慢加热蒸发源至80℃，并保持薄膜沉积速率1.0得到沉积厚度为800nm的一碘化铟多晶薄膜，将制得的一碘化铟多晶薄膜冷却至室温。
如图1所示，制得的一碘化铟多晶薄膜呈紫红色具有金属光泽，表面光滑与衬底结合良好。图2所示，其中(040)晶面的衍射峰最强，峰形尖锐且对称，说明薄膜沿(040)面择优取向生长良好，膜层结晶质量高。图3所示，制得的一碘化铟多晶薄膜呈块状生长，结构均匀、表面较为致密。图4所示，制得的薄膜的光谱吸收边比较陡直，薄膜光谱透过率较高，在600nm以后波段平均透过率可以达到60％，这表明一碘化铟多晶薄膜具有较高的沉积质量、缺陷态较少。
Claims (4)
1.一种一碘化铟多晶薄膜，其特征是：它是一种呈紫红色，具有金属光泽，表面光滑的薄膜。
2.权利要求1的一碘化铟多晶薄膜的制备方法，其特征是：它包括如下步骤：
(1)将一碘化铟多晶放置在玛瑙研钵中研磨成粉末，放入石墨坩埚内作为蒸发源；
(2)将普通玻璃片作为蒸镀沉淀衬底，悬挂在坩埚上方25cm处；
(3)将步骤(1)的石墨坩埚放入热蒸发真空腔室，采用涡轮分子泵使其腔室的背底真空度达到1.5×10-3Pa以下；
(4)在薄膜生长过程中，由膜厚仪监测加热速率和蒸镀厚度，以20℃/min的速率缓慢加热蒸发源至50～90℃，控制薄膜沉积速率在沉积得到200～900nm的一碘化铟多晶薄膜；
(5)将步骤(4)的一碘化铟多晶薄膜冷却至室温，完成薄膜的制备。
3.根据权利要求2所述的一碘化铟多晶薄膜的制备方法，其特征是：所述一碘化铟多晶纯度大于99.99％。
4.根据权利要求2所述的一碘化铟多晶薄膜的制备方法，其特征是：所述的普通玻璃片的厚度为1mm,使用去离子水对其冲洗后,再用丙酮和乙醇试液分别对其进行超声清洗10min，然后用高纯氮气烘干处理。
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