CN113699506B - 一种碘化亚铜薄膜的制备方法 - Google Patents
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- 229910021595 Copper(I) iodide Inorganic materials 0.000 title claims abstract description 57
- LSXDOTMGLUJQCM-UHFFFAOYSA-M copper(i) iodide Chemical compound I[Cu] LSXDOTMGLUJQCM-UHFFFAOYSA-M 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 239000010408 film Substances 0.000 claims abstract description 37
- 238000010438 heat treatment Methods 0.000 claims abstract description 37
- 238000000231 atomic layer deposition Methods 0.000 claims abstract description 32
- 239000000758 substrate Substances 0.000 claims abstract description 30
- 239000010409 thin film Substances 0.000 claims abstract description 27
- 239000010949 copper Substances 0.000 claims abstract description 21
- 238000010926 purge Methods 0.000 claims abstract description 21
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052802 copper Inorganic materials 0.000 claims abstract description 20
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011630 iodine Substances 0.000 claims abstract description 15
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 15
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 8
- 239000010703 silicon Substances 0.000 claims abstract description 8
- 239000011521 glass Substances 0.000 claims abstract description 7
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 7
- 239000010980 sapphire Substances 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 50
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 22
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 16
- 229910000043 hydrogen iodide Inorganic materials 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 claims description 6
- CLUOTFHJTGLPSG-UHFFFAOYSA-L copper;7,7-dimethyloctanoate Chemical compound [Cu+2].CC(C)(C)CCCCCC([O-])=O.CC(C)(C)CCCCCC([O-])=O CLUOTFHJTGLPSG-UHFFFAOYSA-L 0.000 claims description 3
- 229940071870 hydroiodic acid Drugs 0.000 claims description 3
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims description 2
- 239000004065 semiconductor Substances 0.000 abstract description 6
- 238000000151 deposition Methods 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 9
- 230000008021 deposition Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 239000012159 carrier gas Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- BYDBZRCFZPIVLK-UHFFFAOYSA-N CP(C)C.[Cu] Chemical compound CP(C)C.[Cu] BYDBZRCFZPIVLK-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000005234 chemical deposition Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000026045 iodination Effects 0.000 description 1
- 238000006192 iodination reaction Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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- C23C16/45525—Atomic layer deposition [ALD]
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Abstract
本申请公开了一种碘化亚铜薄膜的制备方法,涉及半导体器件技术领域,所述方法包括:在原子层沉积反应腔室中放置衬底,将所述反应腔室抽真空并开始进行加热处理,其中,加热对象包括基底、反应腔室、管路、反应源;所述衬底包括硅、蓝宝石、玻璃中的一种;待所述加热对象稳定在特定温度时,往所述原子层沉积反应腔室内通入铜源0.001‑5s,吹扫1‑180s,通入碘源0.001‑5s,吹扫1‑180s,在所述反应腔室中进行原子层沉积,获得碘化亚铜薄膜;沉积完所述碘化亚铜薄膜后,让所述基底在真空中自然冷却到室温后取出;得到均匀的碘化亚铜薄膜置于真空干燥箱中备用。
Description
技术领域
本申请涉及半导体器件技术领域,尤其涉及一种碘化亚铜薄膜的制备方法。
背景技术
碘化亚铜(CuI)在常温下呈白色粉末状或者白色晶体状。熔点为606℃,沸点为1290℃。室温下就可以结晶析出,不易被可见光分解,溶于水和乙醇,本征为P型半导体材料,相较于其他P型半导体材料(如CuCl,Cu2O) 性能更加稳定。CuI禁带宽度的理论值和实验值为3.1eV到3.2eV,对可见光透明,作为本征为P型的材料,铜空位为主要的浅能级(大约0.5eV)受主缺陷。CuI的亲和能大约为2.1eV,费米能级约为5.1eV,对比于其他半导体材料(如Si,TiO2,ZnO,ZnS等)CuI是价带顶能级最小的材料。如此的特性使得CuI很容易与金属电极或者ITO等透明电极形成良好的欧姆接触。相反,如P型的ZnO的费米能级达到大约7.3eV,很难与金属形成欧姆接触。因此CuI既可以做透明电极又可以做PN结的P型材料,同时在透明电子器件应用中是一个不错的选择。
目前CuI薄膜的制备方式有铜膜碘化法、热蒸发法、激光脉冲沉积法(PLD)、反应磁控溅射法、化学沉积法等。目前测得的最高霍尔空穴迁移率来自水热法制备的CuI晶体,达到43.9cm2/Vs,空穴浓度为4.3×10-16cm-3。如此高的迁移率在宽禁带化合物中非常罕见,但是,目前的沉积方法制备的CuI 薄膜在迁移率上与水热法制备的CuI晶体相比差距很大,亟待新的沉积方案来提高CuI薄膜的沉积质量。
原子层沉积(ALD)是一种自我限制的表面生长方式,所以ALD可以实现薄膜厚度在单原子层量级的精确可控和在三维纳米结构上100%均匀保形的薄膜覆盖。ALD技术在微电子领域已经作为一种制备动态随机存取存储器 (DRAMs)沟槽电容器的高质量电介质层和CMOS晶体管的高介电常数的栅极氧化物层制备的关键技术。采用ALD技术沉积CuI薄膜,既能够与现有的半导体生产线兼容,又能够适合大规模生产。
但本申请发明人在实现本申请实施例中技术方案的过程中,发现上述现有技术至少存在如下技术问题:
现有技术中碘化亚铜薄膜沉积技术中,薄膜迁移率低,性能差的技术问题。
发明内容
本申请实施例通过提供一种碘化亚铜薄膜的制备方法,解决了现有技术中碘化亚铜薄膜沉积技术中,薄膜迁移率低,性能差的技术问题,达到了方法操作简单,有利于量产和与现有IC工艺兼容;所述方法制备的碘化亚铜薄膜具有很好的三维保形性,薄膜厚度在单原子层量级的精确可控的技术效果。
为了解决上述问题,本申请实施例提供了一种碘化亚铜薄膜的制备方法,所述方法包括:在原子层沉积反应腔室中放置衬底,将所述反应腔室抽真空并开始进行加热处理,其中,加热对象包括基底、反应腔室、管路、反应源;所述衬底包括硅、蓝宝石、玻璃中的一种;待所述加热对象稳定在特定温度时,往所述原子层沉积反应腔室内通入铜源0.001-5s,吹扫1-180s,通入碘源0.001-5s,吹扫1-180s,在所述反应腔室中进行原子层沉积,获得碘化亚铜薄膜;沉积完所述碘化亚铜薄膜后,让所述基底在真空中自然冷却到室温后取出;得到均匀的碘化亚铜薄膜置于真空干燥箱中备用。
优选的,所述衬底的加热温度范围为室温-500℃。
优选的,所述管路的加热温度范围为室温-200℃。
优选的,所述腔室的加热温度范围为室温-200℃。
优选的,所述反应源的加热温度范围为室温-200℃。
优选的,所述铜源包括新癸酸铜、2,2,6,6-四甲基-3,5-庚二酮酸、三氟乙酰丙酮化铜、三甲基膦铜、乙酰丙酮亚铜中的一种。
优选的,所述碘源包括碘单质、碘化氢,氢碘酸中的一种。
优选的,所述铜源为乙酰丙酮亚铜蒸汽时,所述方法包括:通入所述乙酰丙酮亚铜蒸汽的时间范围为0.8-1.2s,用惰性气体进行吹扫的时间范围为 0-60s。
优选的,所述碘源为碘化氢时,所述方法包括:通入碘化氢蒸汽的时间范围为0.2-0.8s,用惰性气体进行吹扫的时间范围为20-60s。
优选的,所述乙酰丙酮亚铜蒸汽通过将固态乙酰丙酮亚铜在原子层沉积设备的固态源加热装置中加热至60-100℃获得。
上述说明仅是本申请技术方案的概述,为了能够更清楚了解本申请的技术手段,而可依照说明书的内容予以实施,并且为了让本申请的上述和其它目的、特征和优点能够更明显易懂,以下特举本申请的具体实施方式。
附图说明
图1为本申请实施例一提供的一种碘化亚铜薄膜的制备方法的流程示意图;
图2为本申请实施例二提供的一种碘化亚铜薄膜的制备方法的流程示意图;
图3为本申请实施例中的沉积碘化亚铜薄膜工艺结果的截面示意图。
具体实施方式
本申请实施例提供了一种碘化亚铜薄膜的制备方法,解决了现有技术中碘化亚铜薄膜沉积技术中,薄膜迁移率低,性能差的技术问题。
为了解决上述技术问题,本申请提供的技术方案总体思路如下:通过在原子层沉积反应腔室中放置衬底,将所述反应腔室抽真空并开始进行加热处理,其中,加热对象包括基底、反应腔室、管路、反应源;所述衬底包括硅、蓝宝石、玻璃中的一种;待所述加热对象稳定在特定温度时,往所述原子层沉积反应腔室内通入铜源0.001-5s,吹扫1-180s,通入碘源0.001-5s,吹扫1-180s,在所述反应腔室中进行原子层沉积,获得碘化亚铜薄膜;沉积完所述碘化亚铜薄膜后,让所述基底在真空中自然冷却到室温后取出;得到均匀的碘化亚铜薄膜置于真空干燥箱中备用,达到了方法操作简单,有利于量产和与现有IC工艺兼容;所述方法制备的碘化亚铜薄膜具有很好的三维保形性,薄膜厚度在单原子层量级的精确可控的技术效果。
下面通过附图以及具体实施例对本申请技术方案做详细的说明,应当理解本申请实施例以及实施例中的具体特征是对本申请技术方案的详细的说明,而不是对本申请技术方案的限定,在不冲突的情况下,本申请实施例以及实施例中的技术特征可以相互组合。
实施例一
图1为本发明实施例中一种碘化亚铜薄膜的制备方法的流程示意图,如图1所示,所述方法包括:
步骤110:在原子层沉积反应腔室中放置衬底,将所述反应腔室抽真空并开始进行加热处理,其中,加热对象包括基底、反应腔室、管路、反应源;所述衬底包括硅、蓝宝石、玻璃中的一种;
进一步的,所述衬底的加热温度范围为室温-500℃,所述管路的加热温度范围为室温-200℃,所述腔室的加热温度范围为室温-200℃,所述反应源的加热温度范围为室温-200℃。
步骤120:待所述加热对象稳定在特定温度时,往所述原子层沉积反应腔室内通入铜源0.001-5s,吹扫1-180s,通入碘源0.001-5s,吹扫1-180s,在所述反应腔室中进行原子层沉积,获得碘化亚铜薄膜;
进一步的,所述铜源包括新癸酸铜、2,2,6,6-四甲基-3,5-庚二酮酸、三氟乙酰丙酮化铜、三甲基膦铜、乙酰丙酮亚铜中的一种;所述碘源包括碘单质、碘化氢,氢碘酸中的一种。
进一步的,所述铜源为乙酰丙酮亚铜蒸汽时,所述方法包括:通入所述乙酰丙酮亚铜蒸汽的时间范围为0.8-1.2s,用惰性气体进行吹扫的时间范围为0-60s;所述乙酰丙酮亚铜蒸汽通过将固态乙酰丙酮亚铜在原子层沉积设备的固态源加热装置中加热至60-100℃获得。
进一步的,所述碘源为碘化氢时,所述方法包括:通入碘化氢蒸汽的时间范围为0.2-0.8s,用惰性气体进行吹扫的时间范围为20-60s。
步骤130:沉积完所述碘化亚铜薄膜后,让所述基底在真空中自然冷却到室温后取出;
步骤140:得到均匀的碘化亚铜薄膜置于真空干燥箱中备用。
具体而言,原子层沉积技术是一种可以将物质以单原子膜形式一层一层的镀在基底表面的方法。原子层沉积与普通的化学沉积有相似之处。但在原子层沉积过程中,新一层原子膜的化学反应是直接与之前一层相关联的,这种方式使每次反应只沉积一层原子。本申请实施例通过原子层沉积技术在原子层沉积设备中的反应腔室中放置硅、蓝宝石、玻璃等衬底,其中衬底还可以包括其他能够达到起到相同作用,达到同等效果的物质,所述反应腔室抽真空并开始对基底、腔室、管路、反应源等进行加热。等反应腔室基底、管路及反应源等加热并稳定在特定温度时,往反应腔室内通入铜源0.001-5s,吹扫1-180s,通入碘源0.001-5s,吹扫1-180s,在腔体中进行原子层沉积,获得碘化亚铜薄膜,碘化亚铜薄膜结构如图3所示,沉积完所述碘化亚铜薄膜后,让所述基底在真空中自然冷却到室温后取出;得到均匀的碘化亚铜薄膜置于真空干燥箱中备用。解决了现有技术中碘化亚铜薄膜沉积技术中,薄膜迁移率低,性能差的技术问题,达到了方法操作简单,有利于量产和与现有IC工艺兼容;所述方法制备的碘化亚铜薄膜具有很好的三维保形性,薄膜厚度在单原子层量级的精确可控的技术效果。
实施例二
如图2所示,本申请实施例以乙酰丙酮亚铜作为铜源,以碘化氢作为碘源为例进行解释说明:
a、在原子层沉积反应腔室中放置硅衬底,将所述反应腔室抽真空并开始对基底、腔室加热;
b、在手套箱中将乙酰丙酮亚铜装入原子层沉积设备的固态源加热源瓶内,设定源瓶加热温度对源进行加热,直到每次脉冲的蒸汽压稳定为止,由于乙酰丙酮亚铜室温下为固态,饱和蒸气压较低,所以需要将其用原子层沉积设备自带的固态源加热装置将其加热到60-100℃;以保证乙酰丙酮亚铜有足够的蒸气压脉冲进入载气系统,最后由载气输运至反应腔室。由于碘化氢室温下是气态,直接由载气输运至反应腔室。
c、待基底温度达到预设值100-200℃,温度稳定后,执行设定好的原子层沉积程序,具体程序如下:
第一脉冲为乙酰丙酮亚铜脉冲,脉冲时间为1-4s;氮气清洗脉冲时间为 20-60s;碘化氢脉冲时间为0.2-0.8s;氮气清洗脉冲时间为20-60s。乙酰丙酮亚铜和碘化氢载气流量为45sccm,其他源管线的氮气的流量均设为 30sccm。生长厚度为执行200-800个上述原子层沉积循环。
综上所述,本发明方法首次以原子层沉积技术沉积碘化亚铜薄膜,方法操作简单,有利于量产和与现有IC工艺兼容;方法制备的碘化亚铜薄膜具有很好的三维保形性,薄膜厚度在单原子层量级的精确可控。本申请实施例所述的方法对于碘化亚铜薄膜在存储、光电、透明电子以及柔性器件等领域应用具有重要意义。
本申请实施例中的上述一个或多个技术方案,至少具有如下一种或多种技术效果:
本申请实施例通过提供一种碘化亚铜薄膜的制备方法,通过在原子层沉积反应腔室中放置衬底,将所述反应腔室抽真空并开始进行加热处理,其中,加热对象包括基底、反应腔室、管路、反应源;所述衬底包括硅、蓝宝石、玻璃中的一种;待所述加热对象稳定在特定温度时,往所述原子层沉积反应腔室内通入铜源0.001-5s,吹扫1-180s,通入碘源0.001-5s,吹扫1-180 s,在所述反应腔室中进行原子层沉积,获得碘化亚铜薄膜;沉积完所述碘化亚铜薄膜后,让所述基底在真空中自然冷却到室温后取出;得到均匀的碘化亚铜薄膜置于真空干燥箱中备用,解决了现有技术中碘化亚铜薄膜沉积技术中,薄膜迁移率低,性能差的技术问题,达到了方法操作简单,有利于量产和与现有IC工艺兼容;所述方法制备的碘化亚铜薄膜具有很好的三维保形性,薄膜厚度在单原子层量级的精确可控的技术效果。
尽管已描述了本发明的优选实施例,但本领域内的技术人员一旦得知了基本创造性概念,则可对这些实施例做出另外的变更和修改。所以,所附权利要求意欲解释为包括优选实施例以及落入本发明范围的所有变更和修改。
显然,本领域的技术人员可以对本发明实施例进行各种改动和变型而不脱离本发明实施例的精神和范围。这样,倘若本发明实施例的这些修改和变型属于本发明权利要求及其等同技术的范围之内,则本发明也意图包含这些改动和变型在内。
Claims (10)
1.一种碘化亚铜薄膜的制备方法,其中,所述方法包括:
在原子层沉积反应腔室中放置衬底,将所述反应腔室抽真空并开始进行加热处理,其中,加热对象包括衬底、反应腔室、管路、反应源;所述衬底包括硅、蓝宝石、玻璃中的一种;
待所述加热对象稳定在特定温度时,往所述原子层沉积反应腔室内通入铜源0.001-5s,吹扫1-180s,通入碘源0.001-5s,吹扫1-180s,在所述反应腔室中进行原子层沉积,获得碘化亚铜薄膜;
沉积完所述碘化亚铜薄膜后,让所述衬底在真空中自然冷却到室温后取出;
得到均匀的碘化亚铜薄膜置于真空干燥箱中备用。
2.如权利要求1所述的方法,其中,所述衬底的加热温度范围为室温-500℃。
3.如权利要求1所述的方法,其中,所述管路的加热温度范围为室温-200℃。
4.如权利要求1所述的方法,其中,所述腔室的加热温度范围为室温-200℃。
5.如权利要求1所述的方法,其中,所述反应源的加热温度范围为室温-200℃。
6.如权利要求1所述的方法,其中,所述铜源包括新癸酸铜、三氟乙酰丙酮化铜、三甲基膦铜、乙酰丙酮亚铜中的一种。
7.如权利要求1所述的方法,其中,所述碘源包括碘单质、碘化氢,氢碘酸中的一种。
8.如权利要求6所述的方法,其中,所述铜源为乙酰丙酮亚铜蒸汽时,所述方法包括:通入所述乙酰丙酮亚铜蒸汽的时间范围为0.8-1.2s,用惰性气体进行吹扫的时间范围为0-60s。
9.如权利要求7所述的方法,其中,所述碘源为碘化氢时,所述方法包括:通入碘化氢蒸汽的时间范围为0.2-0.8s,用惰性气体进行吹扫的时间范围为20-60s。
10.如权利要求8所述的方法,其中,所述乙酰丙酮亚铜蒸汽通过将固态乙酰丙酮亚铜在原子层沉积设备的固态源加热装置中加热至60-100℃获得。
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