CN105408244B - 金属氧化物膜的制造方法和晶体管的制造方法 - Google Patents
金属氧化物膜的制造方法和晶体管的制造方法 Download PDFInfo
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- CN105408244B CN105408244B CN201480042219.6A CN201480042219A CN105408244B CN 105408244 B CN105408244 B CN 105408244B CN 201480042219 A CN201480042219 A CN 201480042219A CN 105408244 B CN105408244 B CN 105408244B
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- 230000003287 optical effect Effects 0.000 description 1
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- 229920005989 resin Polymers 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 1
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- 238000002604 ultrasonography Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- NHXVNEDMKGDNPR-UHFFFAOYSA-N zinc;pentane-2,4-dione Chemical compound [Zn+2].CC(=O)[CH-]C(C)=O.CC(=O)[CH-]C(C)=O NHXVNEDMKGDNPR-UHFFFAOYSA-N 0.000 description 1
Classifications
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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- H01L21/02175—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal
- H01L21/02178—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal the material containing aluminium, e.g. Al2O3
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
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- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
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- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02282—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process liquid deposition, e.g. spin-coating, sol-gel techniques, spray coating
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- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
- H01L21/02318—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment
- H01L21/02321—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment introduction of substances into an already existing insulating layer
- H01L21/02323—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment introduction of substances into an already existing insulating layer introduction of oxygen
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- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
- H01L21/02318—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment
- H01L21/02334—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment in-situ cleaning after layer formation, e.g. removing process residues
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- H01L21/02107—Forming insulating materials on a substrate
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- H01L21/02337—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment treatment by exposure to a gas or vapour
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- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
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- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
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- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
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- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
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- H01L29/40—Electrodes ; Multistep manufacturing processes therefor
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- H01L29/40—Electrodes ; Multistep manufacturing processes therefor
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- H01L29/49—Metal-insulator-semiconductor electrodes, e.g. gates of MOSFET
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- H01L29/66227—Multistep manufacturing processes of devices having semiconductor bodies comprising group 14 or group 13/15 materials the devices being controllable only by the electric current supplied or the electric potential applied, to an electrode which does not carry the current to be rectified, amplified or switched, e.g. three-terminal devices
- H01L29/66409—Unipolar field-effect transistors
- H01L29/66477—Unipolar field-effect transistors with an insulated gate, i.e. MISFET
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Abstract
本发明目的在于提供一种有效得到密合性良好的金属氧化物膜的技术。本发明中的金属氧化物膜的制造方法特征在于,其具备:将含有有机金属络合物的溶液涂布于基板上的涂布工序;将得到的涂膜暴露于臭氧的臭氧暴露工序;对所述涂膜进行加热的加热工序。
Description
技术领域
本发明涉及金属氧化物膜的制造方法和晶体管的制造方法。本发明要求2013年8月7日申请的日本专利申请号2013-164248的优先权,对于认可基于文献参照的编入的指定国,通过参照将该申请所述的内容编入本申请中。
背景技术
氧化铝、氧化硅等金属氧化物被用于半导体装置、光学薄膜等用途。期望将金属氧化物以所需膜厚形成于所需位置,若能够更简便地进行薄膜的形成,则关系到低成本高产量。
专利文献1中公开了一种成膜方法,其具有:在基板的成膜面上,形成对于成膜材料的粒子示出高亲和性的高亲和性区域和与所述亲和性区域相比示出低亲和性的低亲和性区域的工序;在与所述基板之间,使用具备电子捕捉部的溅射装置,使所述成膜材料的粒子飞向所述成膜面,使所述成膜材料选择性地堆积在所述高亲和性区域的工序。
现有技术文献
专利文献
专利文献1:日本特开2010-199402号公报
发明内容
发明要解决的课题
在专利文献1所述的成膜方法中,使用溅射装置,将成膜材料选择性地堆积在基板上。如此以使用溅射法、蒸镀法的干式法进行金属氧化物的成膜的技术是已知的。但是,干式法主要使用真空装置进行,因此与以湿式法进行的情况相比,存在成本升高、产量降低的趋势。
此外,通过对基板照射紫外线,选择性地进行金属氧化物的成膜的技术已经普及,但对基板的密合性很难说是良好的。
本发明是鉴于这种情况而完成的,目的在于提供一种有效得到密合性良好的金属氧化物膜的技术。
解决课题的手段
本发明方式是为了实现上述目的而完成的,本发明的金属氧化物膜的制造方法具备:将含有有机金属络合物的溶液涂布于基板的涂布工序;将得到的涂膜暴露于臭氧的臭氧暴露工序;对所述涂膜进行加热的加热工序。
此外,本发明方式的金属氧化物膜的制造方法特征还在于,所述加热工序中的加热温度为180度以下。
此外,本发明方式的金属氧化物膜的制造方法特征还在于,在所述臭氧暴露工序之后,进一步具备用有机溶剂对所述基板进行清洗的清洗工序,在所述臭氧暴露工序中,将所述涂膜选择性地暴露于臭氧。
此外,特征还在于所述有机金属络合物为1分子中的总碳原子数为4~30的金属络合物的至少一种。
此外,特征还在于所述有机金属络合物为乙酰丙酮金属络合物,所述含有有机金属络合物的溶液的溶剂包含醇类、酮类、醚类、卤代烃类、环状烃类的至少1种。
此外,特征还在于所述金属氧化物膜至少含有Al、O、C、H四种元素,所述四种元素之间的C与H的组成比的总量为70%以上。
此外,特征还在于在所述清洗工序中所用的所述有机溶剂包含醇类、酮类、醚类、卤代烃类、环状烃类的至少一种。
此外,本发明方式的晶体管的制造方法具备:在基板上形成栅极的工序;将含有有机金属络合物的溶液涂布于所述基板的工序;将得到的涂膜选择性地暴露于臭氧的工序;用有机溶剂对所述基板进行清洗的工序;对所述涂膜进行烧制,得到绝缘膜的工序;形成源极、漏极和半导体层的工序。
此外,本发明方式的金属氧化物膜特征在于,其为至少含有Al、O、C、H四种元素的金属氧化物膜,所述四种元素之间的C与H的组成比的总量为70%以上。
发明效果
本发明能够提供一种有效得到密合性良好的金属氧化物的金属氧化物膜的技术。
附图说明
图1为用于说明本实施方式的金属氧化物膜的制造方法的一例的截面图。
图2为用于说明本变形例的金属氧化物膜的制造方法的一例的截面图。
图3为得到的氧化铝膜的140倍的SEM图像。
图4为得到的氧化铝膜的600倍的光学显微镜图像。
图5为基于氧化铝膜的线&间隙的170倍的SEM图像。
图6为示出基于氧化铝膜的线&间隙的100倍的SEM图像和基于EDX的线扫描结果的图。
图7为得到的氧化铝膜的120倍的SEM图像。
图8为示出基于氧化铝膜的线&间隙的120倍的SEM图像和基于EDX的线扫描结果的图。
图9为氧化铝膜的170倍的SEM图像。
图10为得到的氧化铝膜的120倍的SEM图像。
图11为示出得到的氧化铝膜的120倍的SEM图像和基于EDX的线扫描结果的图。
图12为示出对加热温度和相对介电常数·绝缘击穿电压进行测定的结果的图。
图13为示出对氧化铝膜的加热温度和组成比进行测定的结果的图。
具体实施方式
以下,参照附图对于本发明的实施方式的一例进行说明。
图1为用于说明本实施方式的金属氧化物膜的制造方法的一例的截面图。
(第1工序)
首先,如图1的(A)所示,制备有机金属络合物溶液1。对于有机金属络合物溶液1,通过将有机金属络合物11溶解于溶剂12中来获得。作为有机金属络合物11中所用的材料,可以使用例如Cu(acac)2、Mn(acac)3、VO(acac)2、Fe(acac)3、Co(acac)3、Zn(acac)2等乙酰丙酮金属络合物。需要说明的是,“acac”表示乙酰丙酮。
溶剂12只要为可溶解有机金属络合物11的液体即可,可以使用例如乙醇、丙醇、丁醇、戊醇、己醇、辛醇、壬醇、苄醇、甲基环己醇、乙二醇、丙二醇、丁二醇、戊二醇、己二醇、辛二醇、己三醇等醇类;以及甲酸丁酯、甲酸戊酯、乙酸甲酯、乙酸乙酯、乙酸丙酯、乙酸丁酯、乙酸戊酯、乙酸己酯、乙酸苄酯、乙酸3-甲氧基丁基酯、乙酸2-乙基丁基酯、乙酸2-乙基己基酯、丙酸甲酯、丙酸乙酯、丙酸丙酯、丙酸丁酯、丙酸戊酯等酯类;二甲基甲酰胺、二甲基乙酰胺、二乙基甲酰胺、二乙基乙酰胺等酰胺类;二甲基酮、甲基乙基酮、戊酮、己酮、甲基异丁基酮、庚酮、二异丁基酮等酮类;乙腈等腈类;二乙基醚、二丙基醚、二异丙基醚、二丁基醚、二己基醚等醚类;苯甲醚、四氢呋喃、四氢吡喃等环状醚类;二甲氧基乙烷、二乙氧基乙烷、二丁氧基乙烷、二乙二醇二甲醚、二乙二醇二乙醚、乙二醇二丁醚等乙二醇醚类;甲缩醛、乙缩醛等缩醛类;戊烷、己烷、庚烷、辛烷、壬烷、癸烷、十二烷等链烷烃类;甲苯、二甲苯、乙基苯、异丙基苯、三甲基苯、四氢化萘、丁基苯、异丙基甲苯、二乙基苯、戊基苯、二戊基苯、环戊烷、环己烷、甲基环己烷、乙基环己烷、萘烷等环状烃类;氯甲烷、二氯甲烷、三氯甲烷(氯仿)、四氯甲烷、氯乙烷、二氯乙烷、三氯乙烷、四氯乙烷、五氯乙烷、氯丙烷、二氯丙烷、三氯丙烷、氯丁烷、二氯丁烷、三氯丁烷、氯戊烷、氯苯、二氯苯、氯甲苯、二氯甲苯、溴甲烷、溴丙烷、溴苯、氯溴乙烷等卤代烃类。
(第2工序)
接着,如图1的(B)所示,在基板2上涂布有机金属络合物溶液1,形成被膜10。对于基板2,可以使用通常使用的基板材料。可以使用例如聚对苯二甲酸乙二酯(PET)、聚萘二甲酸乙二酯(PEN)、聚酰亚胺等树脂基板;或硅(Si)、砷化镓(GaAs)、氮化镓(GaN)等半导体基板;或二氧化硅(SiO2)、蓝宝石、氧化锌(ZnO)等氧化物基板等。
需要说明的是,对于有机金属络合物溶液1的涂布,可以使用公知的涂布方法,例如使用旋涂法、浸涂法、喷涂法等涂布方法,在基板2上涂布有机金属络合物溶液1,形成被膜10。需要说明的是,不限于这样的涂布方法,可以根据得到的膜的均匀性、成本等,适当选择其他涂布方法。
(第3工序)
接着,如图1的(C)所示,在有机金属络合物溶液1的被膜10上,准备具有所需开口图案的掩模21。作为掩模21,可以使用例如金属掩模、经图案化的光致抗蚀剂等。需要说明的是,使用金属掩模的情况下,可以以直接接触被膜10的方式进行配置,也可以在与被膜10之间设置间隙来进行配置使其不接触被膜10。在本实施方式中,在后述的第4工序,为了使被膜10对应于掩模的开口图案暴露于臭氧中,使掩模21接触被膜10来进行配置时,能够防止臭氧暴露于掩模21的非开口部和被膜10之间,存在更容易得到所需图案的趋势。需要说明的是,使用光致抗蚀剂的情况下,通过在被膜10上形成光致抗蚀剂,并进行通常的光刻工序,能够得到经图案化的光致抗蚀剂。
(第4工序)
接着,如图1的(D)所示,使被膜10经由掩模21暴露于臭氧22中。作为暴露于臭氧22的方法,有例如使用利用紫外光中所含的波长约为250mm以下的光产生臭氧的臭氧清洗装置,使其暴露于臭氧22的方法;除此之外,有使其暴露于用臭氧发生器等产生的臭氧22中的方法;使用利用氧和等离子体的反应产生臭氧的等离子体发生装置,使其暴露于臭氧22的方法等,根据成本、产量,适当地进行选择。
图1的(E)示出使被膜10暴露于臭氧22后得到的基板2。在第3工序,利用掩模21选择性地覆盖被膜10,因此使形成有被膜10的基板2暴露于臭氧22时,形成未暴露于臭氧22的被膜10a和暴露于臭氧22的被膜10b。
有机金属络合物11对于醇、丙酮等有机溶剂是可溶的,因此未暴露于臭氧的被膜10a对有机溶剂的耐性低。另一方面,对于暴露于臭氧22的被膜10b来说,有机金属络合物中的结构内发生化学键的切断、再结合,其对醇、丙酮等有机溶剂的耐性高。即,在被膜10暴露于臭氧22的部分和未暴露于臭氧22的部分,在对于有机溶剂的溶解容易性上产生差别。
(第5工序)
接着,如图1的(F)所示,使施加有被膜10a和被膜10b的基板2接触有机溶剂,来进行清洗。清洗中所用的有机溶剂只要可溶解第1工序中所用的有机金属络合物即可,此处可以使用例如乙醇、丙醇、丁醇、戊醇、己醇、辛醇、壬醇、苄醇、甲基环己醇、乙二醇、丙二醇、丁二醇、戊二醇、己二醇、辛二醇、己三醇等醇类;以及甲酸丁酯、甲酸戊酯、乙酸甲酯、乙酸乙酯、乙酸丙酯、乙酸丁酯、乙酸戊酯、乙酸己酯、乙酸苄酯、乙酸3-甲氧基丁基酯、乙酸2-乙基丁基酯、乙酸2-乙基己基酯、丙酸甲酯、丙酸乙酯、丙酸丙酯、丙酸丁酯、丙酸戊酯等酯类;二甲基甲酰胺、二甲基乙酰胺、二乙基甲酰胺、二乙基乙酰胺等酰胺类;二甲基酮、甲基乙基酮、戊酮、己酮、甲基异丁基酮、庚酮、二异丁基酮等酮类;乙腈等腈类;二乙基醚、二丙基醚、二异丙基醚、二丁基醚、二己基醚等醚类;苯甲醚、四氢呋喃、四氢吡喃等环状醚类;二甲氧基乙烷、二乙氧基乙烷、二丁氧基乙烷、二乙二醇二甲醚、二乙二醇二乙醚、乙二醇二丁醚等乙二醇醚类;甲缩醛、乙缩醛等缩醛类;戊烷、己烷、庚烷、辛烷、壬烷、癸烷、十二烷等链烷烃类;甲苯、二甲苯、乙基苯、异丙基苯、三甲基苯、四氢化萘、丁基苯、异丙基甲苯、二乙基苯、戊基苯、二戊基苯、环戊烷、环己烷、甲基环己烷、乙基环己烷、萘烷等环状烃类;氯甲烷、二氯甲烷、三氯甲烷(氯仿)、四氯甲烷、氯乙烷、二氯乙烷、三氯乙烷、四氯乙烷、五氯乙烷、氯丙烷、二氯丙烷、三氯丙烷、氯丁烷、二氯丁烷、三氯丁烷、氯戊烷、氯苯、二氯苯、氯甲苯、二氯甲苯、溴甲烷、溴丙烷、溴苯、氯溴乙烷等卤代烃类。被膜10a对于有机溶剂的耐性低,因此利用清洗发生溶解,但被膜10b未溶解而残存。因此,在臭氧暴露部分与未暴露部分可以形成图案化。需要说明的是,对于清洗,通过浸渍放置于有机溶剂中是足够的,通过使用超声波清洗,或是进行搅拌,能够缩短处理时间。需要说明的是,清洗时间过短时,被膜10a不能充分溶解,此外清洗时间过长时,有时连被膜10b也发生溶解,因此清洗时间根据有机金属络合物、有机溶剂的种类适当设定。
(第6工序)
接着,如图1的(G)所示,对被膜10b进行加热处理(烧制)。对于加热处理,在加热温度为180℃以下的情况下,能够得到高介电常数,因此优选在180℃以下进行加热。利用加热处理,能够形成被膜10c,该被膜10c为被膜10b与基板2具有高密合性的金属氧化物。
加热处理的结果如图1的(H)所示,能够得到具有高绝缘性的金属氧化物,其以被膜10c的形状被图案化。
以上,在本实施方式中,利用湿式法进行被膜形成,并使用臭氧进行图案化,由此可以有效得到选择性的金属氧化物膜。无需为了图案化而使用腐蚀性高的强酸作为蚀刻溶液,因此能够防止给配线、基板带来损坏。
(变形例)
接着,对本实施方式的变形例进行说明。
图2为用于说明本变形例的金属氧化物膜的制造方法的一例的截面图。在本变形例中,使用利用上述实施方式形成的金属氧化物膜制造晶体管。
(第1工序)
首先,如图2的(A)所示,在基板2a上形成栅极31。栅极是使用公知的光刻技术形成的。
(第2工序)
接着,如图2的(B)所示,对与上述实施方式同样地制备得到的有机金属络合物溶液1进行涂布,形成被膜10A。之后被膜10A成为晶体管的绝缘体层,因此优选以覆盖栅极31的方式进行涂布。
(第3工序)
接着,如图2的(C)所示,在利用有机金属络合物溶液1形成的被膜上准备掩模21。掩模21可以为金属掩模,也可以通过涂布抗蚀剂,并进行图案化来形成掩模21。需要说明的是,掩模21可以以接触利用有机金属络合物溶液1形成的被膜10A的方式形成。
(第4工序)
接着,如图2的(D)所示,使被膜10A暴露于臭氧22中。暴露方法与上述实施方式相同。
(第5工序)
接着,如图2的(E)所示,与上述实施方式同样地用有机溶剂对被膜10A进行清洗。有机溶剂与上述实施方式相同,为丙酮等。通过清洗,暴露于臭氧22的被膜10Ab部分残留于基板2a上,臭氧未暴露部分发生溶解。之后,对被膜10Ab进行加热处理,得到绝缘膜。需要说明的是,得到氧化铝作为绝缘膜的情况下,为了得到相对介电常数高的绝缘膜,优选将加热温度设为180℃以下。
(第6工序)
接着,如图2的(F)所示,在绝缘膜上形成源极32和漏极33。源极32和漏极33的形成也与栅极相同,使用光刻等公知的技术。
(第7工序)
接着,如图2的(G)所示,使用公知的技术,在基板2a上形成有机或无机的半导体层40。
根据本变形例,不使用强酸性的有机溶剂,就能够有效得到密合性高的绝缘膜。此外,与常规的绝缘膜相比,相对介电常数高,因此作为晶体管的栅极绝缘膜,具有高性能,是优选的。
以下,示出实施例,对本发明方式进行更具体的说明。其中,本发明并不限于这些实施例。
<实施例1>
(涂布)
首先,对于乙酰丙酮铝0.003mol(东京化成工业(株)制造),添加乙醇(和光纯药工业(株)制造)35ml,进行充分搅拌,确认乙酰丙酮铝全部溶解。将作为得到的混合溶液的有机金属络合物溶液1滴注在由Si构成的基板2上,利用旋涂机进行转速700rpm、30秒的旋转涂布。
(臭氧暴露和清洗)
之后,将金属掩模载置于得到的试样上,利用UV臭氧清洗机(OC-2506:岩崎电气(株)制造)暴露于臭氧中10分钟。金属掩模的形状为200μm宽的线&间隙。据预测臭氧暴露后,在暴露的部分与未暴露部分产生对比度差,引起相变化。臭氧暴露后,浸渍于作为有机溶剂的丙酮中,放置5分钟。之后,从丙酮中取出试样,用空气喷枪吹,用乙醇、蒸馏水依次进行清洗,并进行鼓风。
(加热处理)
之后,将得到的试样在150℃进行加热并进行烧制。由此,可以形成氧化铝膜作为被膜10c,能够形成与金属掩模的线&间隙相同的图案化形状。
(评价)
图3为得到的氧化铝膜的140倍的SEM图像。可知没有缺陷、裂缝,被膜均匀。
图4为得到的氧化铝膜的600倍的光学显微镜图像。图4左侧示出Si基板的区域,右侧示出氧化铝的区域。在图4所示的光学显微镜图像中,可以确认氧化铝膜和Si基板的分界线。利用该阶差,用触针式阶差计(P16+:Tencor公司制造)测定膜的膜厚时,为50nm。
图5为基于氧化铝膜的线&间隙的170倍的SEM图像。纵剖图5中央的为氧化铝的区域,其他部分为Si基板的区域。可以形成与阴影掩模的宽度相同的200μm的线&间隙,图案化成功。
图6为示出基于氧化铝膜的线&间隙的100倍的SEM图像和基于能量分散型X射线分析(Energy dispersive X-ray spectrometry:EDX)的线扫描结果的图。沿着线(a)进行线扫描,进行Al和源自基板的Si的元素分析。根据线(b)可知,在臭氧暴露部检测出源自氧化铝膜的Al,根据线(c)可知,在臭氧未暴露部分,检测出源自Si基板的Si。由此可以判断能够形成图案化。
如上所述,使用湿式法能够形成金属氧化物膜,能够确认不使用氟化物等蚀刻溶液,就能够简便地形成经图案化的膜。
<实施例2>
作为有机金属络合物11,与实施例1同样地准备乙酰丙酮铝,与实施例1同样地使用乙醇制备有机金属络合物溶液1,涂布于基板2上,并进行臭氧暴露。之后,与实施例1不同,不进行上述第5工序的清洗,就在150℃进行10分钟烧制。
图7为之后得到的氧化铝膜的120倍的SEM图像。由该结果可知,在臭氧暴露部与未暴露部能够形成线&间隙。对于作为臭氧未暴露部的被膜10a,没有经过清洗工序,且在加热工序中发现一定程度的升华,因此能够形成线&间隙。
图8为示出基于氧化铝膜的线&间隙的120倍的SEM图像和基于EDX的线扫描结果的图。对于线扫描,与实施例1同样地对于Al和Si进行扫描。线(b)示出Al的扫描结果,据此可知,在臭氧暴露部与未暴露部,Al的检出量存在不同。利用阶差计测定线&间隙的膜厚差时,与实施例1相同,为50nm。但是,与在实施例1中进行的试样不同,行程中没有进行基于有机溶剂的清洗,因此发现有残渣。
图9为氧化铝膜的170倍的SEM图像。残渣10d示出残留于Si基板上的残渣。可知即使为臭氧未暴露部,被膜10a也未完全升华,残渣10d根据场所不同而残留。
为了除去残渣10d,本实施例中在烧制后进行使用了有机溶剂的清洗。在图8的状态下,将基板2浸渍于丙酮中5分钟,用鼓风机使其干燥。
图10为得到的氧化铝膜的120倍的SEM图像。
图11为示出得到的氧化铝膜的120倍的SEM像和基于EDX的线扫描结果的图。可知Al与Si基板的对比度高,残渣减少。
<实施例3>
作为有机金属络合物11,与实施例1同样地准备乙酰丙酮铝,与实施例1同样地使用乙醇制备有机金属络合物溶液1,涂布于基板2上,并进行臭氧暴露。之后,以除去臭氧未暴露部为目的,使用乙醇进行清洗。之后,在150℃进行烧制,用SEM图像进行确认时,与实施例1同样地确认到臭氧暴露部残留而仅臭氧未暴露部被选择性地除去所导致的金属氧化物膜的图案化。
<实施例4>
作为有机金属络合物11,与实施例1同样地准备乙酰丙酮铝。作为溶解有机金属络合物11的溶剂,使用丙酮35ml,使有机金属络合物11溶解,制备有机金属络合物溶液1。接着,用与实施例1相同的方法,在基板2上涂布有机金属络合物溶液1,并进行臭氧暴露。之后,以除去臭氧未暴露部为目的,使用丙酮进行清洗。之后,在150℃进行烧制,用SEM图像进行确认时,与实施例1同样地确认到臭氧暴露部残留于基板2上而臭氧未暴露部被除去所导致的金属氧化物膜的图案化。
<实施例5>
作为有机金属络合物11,与实施例1同样地准备乙酰丙酮铝,作为溶解有机金属络合物11的溶剂,使用丙酮35ml。使有机金属络合物11溶解,制备有机金属络合物溶液1。接着,用与实施例1相同的方法,在基板2上涂布有机金属络合物溶液1,并进行臭氧暴露。之后,以除去臭氧未暴露部为目的,使用乙醇进行清洗。之后,在150℃进行烧制,用SEM图像进行确认时,与实施例1同样地确认到臭氧暴露部残留于基板2上而臭氧未暴露部被除去所导致的金属氧化物膜的图案化。
<实施例6>
作为有机金属络合物11,与实施例1同样地准备乙酰丙酮铝,作为溶解有机金属络合物11的溶剂,使用甲苯15ml。使有机金属络合物11溶解,制备有机金属络合物溶液1。接着,用与实施例1相同的方法,在基板2上涂布有机金属络合物溶液1,并进行臭氧暴露。之后,以除去臭氧未暴露部为目的,使用丙酮进行清洗。之后,在150℃进行烧制,用SEM图像进行确认时,与实施例1同样地确认到臭氧暴露部残留于基板2上而臭氧未暴露部被除去所导致的金属氧化物膜的图案化。
<实施例7>
作为有机金属络合物11,与实施例1同样地准备乙酰丙酮铝,作为溶解有机金属络合物11的溶剂,使用氯仿35ml。使有机金属络合物11溶解,制备有机金属络合物溶液1。接着,用与实施例1相同的方法,在基板2上涂布有机金属络合物溶液1,并进行臭氧暴露。之后,以除去臭氧未暴露部为目的,使用丙酮进行清洗。之后,在150℃进行烧制,用SEM图像进行确认时,与实施例1同样地确认到臭氧暴露部残留于基板2上而臭氧未暴露部被除去所导致的金属氧化物膜的图案化。
<比较例>
作为有机金属络合物11,与实施例1同样地准备乙酰丙酮铝,与实施例1相同地使用乙醇作为溶剂制备有机金属络合物溶液1,涂布于基板2上,并进行臭氧暴露。之后,以除去臭氧未暴露部为目的,使用水,结果与其他实施例不同,臭氧暴露部和臭氧未暴露部的被膜均被除去了。根据本实施例可知,用含有水的无机溶液进行清洗时,难以进行金属氧化物膜的图案化,因此,对于清洗,优选使用无水的有机溶剂。
<实施例8>
作为有机金属络合物11,使用乙酰丙酮锌0.003mol(东京化成工业(株)制造),使用乙醇35ml作为溶剂。使有机金属络合物11溶解于溶剂中,制成有机金属络合物溶液1。之后,用与实施例1相同的方法,在基板2上涂布有机金属络合物溶液1,并进行臭氧暴露,使用丙酮进行清洗,在150℃进行烧制。其结果得到线&间隙的SEM图像,能够确认到氧化锌膜的图案化形状。
<实施例9>(加热温度的调整)
作为有机金属络合物11,与实施例1同样地准备乙酰丙酮铝,与实施例1同样地使用乙醇作为溶剂12,制备有机金属络合物溶液1。将有机金属络合物溶液1涂布于基板2时,以膜厚成为200nm的方式进行涂布。接着,以除去附着于涂膜上的细微的垃圾为目的,用丙酮清洗涂膜。接着,不进行使用掩模的图案化就用与实施例1相同的方法使涂膜暴露于臭氧中。之后,在120℃到200℃的范围,进行数个图案的烧制。烧制后,利用溅射法,在得到的氧化铝膜上形成直径2mm的金电极,将基板2和金电极作为上部·下部电极,对膜的电特性进行测定。对于测定,使用半导体参数测定器(4200-SCS:keithley公司制造)。
图12为示出对加热温度和相对介电常数·绝缘击穿电压进行测定的结果的图。α表示加热温度与绝缘击穿电压的关系,β表示加热温度与相对介电常数的关系。此外,将图12所示的测定结果的数值列于下述表1。
[表1]
试样 | 加热温度(℃) | 相对介电常数 | 绝缘击穿电压(MV/cm) |
No.1 | 120 | 28 | 1 |
No.2 | 150 | 20 | 2.5 |
No.3 | 180 | 20 | 4.4 |
No.4 | 200 | 8 | 8.75 |
常规氧化铝的相对介电常数为10以下,参照β可知,在加热温度为180℃以下的区域中,存在相对介电常数高于常规氧化铝的趋势。
该结果示出本实施例的氧化铝的组成与化学计量组成不同。与常规氧化铝相比,相对介电常数高,这可以说明基于本实施例的氧化铝适合用作晶体管等栅极绝缘膜。
<实施例10>
作为有机金属络合物11,与实施例1同样地准备乙酰丙酮铝,使用异丙醇作为溶剂,制备有机金属络合物溶液1。与实施例1同样地在基板2上涂布有机金属络合物溶液1,并进行臭氧暴露。之后,与实施例1不同,不进行第5工序的清洗就以4个图案不同的温度进行加热处理。作为结果,得到以120℃、150℃、180℃或200℃进行加热处理的4种氧化铝膜。
对于得到的各个氧化铝膜,使用卢瑟福背散射分析(Rutherford BackscatteringSpectrometry:RBS)、氢前向散射分析(Hydrogen Forward scattering Spectrometry:HFS)、核反应分析(Nuclear Reaction Analysis:NRA),对Al、O、C、H四种元素之间的组成比(相对值)进行测定。
图13为示出对氧化铝膜的加热温度和组成比进行测定的结果的图。此外,将图13所示的测定结果的数值列于下述表2。
[表2]
试样 | 加热温度(℃) | Al(atomic%) | O(atomic%) | C(atomic%) | H(atomic%) |
No.5 | 120 | 5.4 | 16.1 | 28.9 | 49.6 |
No.6 | 150 | 6 | 17.1 | 28.8 | 48.1 |
No.7 | 180 | 7.6 | 19.5 | 29.9 | 43 |
No.8 | 200 | 11.9 | 26.4 | 25.3 | 36.2 |
参照图13时,可知随着加热温度升高,H与C的组成比的总量减少,同时Al与O的组成比的总量增加。由该结果可认为,源自有机金属络合物11的碳氢(CH)键随着加热温度的上升而消失。
考察<实施例9>和<实施例10>的结果。<实施例9>中,在加热温度为180℃以下的区域中,存在相对介电常数高于常规氧化铝的趋势,根据<实施例10>,在加热温度为180℃以上的区域中,C与H的组成比的总量减少。因此,可认为在180℃以下的区域的高相对介电常数源自CH键,被膜10中的CH键多时,相对介电常数高。换言之,在200℃以上的加热温度进行加热的情况下,能够得到用以往技术获得的那样的氧化铝膜,但得到的氧化铝膜并没有示出高相对介电常数。
此外,根据<实施例10>和表2可知,在<实施例9>中示出高介电常数的加热温度180℃以下的情况下,C与H的组成比的总量为70%以上。即,氧化铝膜中的Al、O、C、H四种元素之间的C与H的组成比的总量为70%以上的情况下,能够得到示出高介电常数的氧化铝膜。
符号说明
1:有机金属络合物溶液、2、2a:基板、10、10A、10a、10b、10Ab:被膜、11:有机金属络合物、12:溶剂、31:栅极、32:源极、33:漏极、40:半导体层。
Claims (6)
1.一种金属氧化物膜的制造方法,其中,其具备:
将含有有机金属络合物的溶液涂布于基板的涂布工序;
将得到的涂膜暴露于臭氧的臭氧暴露工序;和
在180度以下对所述涂膜进行加热的加热工序,
在所述臭氧暴露工序之后,进一步具备使所述涂膜接触有机溶剂的清洗工序,
在所述臭氧暴露工序中,将所述涂膜选择性地暴露于臭氧。
2.如权利要求1所述的金属氧化物膜的制造方法,
其中,所述有机金属络合物为1分子中的总碳原子数为4~30的金属络合物的至少一种。
3.如权利要求1或2所述的金属氧化物膜的制造方法,
其中,所述有机金属络合物为乙酰丙酮金属络合物,
所述含有有机金属络合物的溶液的溶剂包含醇类、酮类、醚类、卤代烃类、环状烃类的至少1种。
4.如权利要求1或2所述的金属氧化物膜的制造方法,
其中,所述金属氧化物膜至少含有Al、O、C、H四种元素,所述四种元素之间的C与H的组成比的总量为70%以上。
5.如权利要求1所述的金属氧化物膜的制造方法,
其中,在所述清洗工序中所用的所述有机溶剂包含醇类、酮类、醚类、卤代烃类、环状烃类的至少一种。
6.一种晶体管的制造方法,其中,其具备:
在基板上形成栅极的工序;
将含有有机金属络合物的溶液涂布于所述基板的工序;
将得到的涂膜选择性地暴露于臭氧的工序;
用有机溶剂对所述基板进行清洗的工序;
在180度以下对所述涂膜进行加热,得到绝缘膜的工序;和
形成源极、漏极和半导体层的工序。
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EP2660870A4 (en) * | 2010-12-27 | 2014-03-05 | Panasonic Corp | FIELD EFFECT TRANSISTOR AND METHOD FOR MANUFACTURING THE SAME |
JP5916761B2 (ja) * | 2011-01-28 | 2016-05-11 | ノースウェスタン ユニバーシティ | 金属酸化物薄膜およびナノ材料から誘導される金属複合薄膜の低温製造 |
JP5929132B2 (ja) * | 2011-11-30 | 2016-06-01 | 株式会社リコー | 金属酸化物薄膜形成用塗布液、金属酸化物薄膜の製造方法、及び電界効果型トランジスタの製造方法 |
JP6454974B2 (ja) * | 2013-03-29 | 2019-01-23 | 株式会社リコー | 金属酸化物膜形成用塗布液、金属酸化物膜の製造方法、及び電界効果型トランジスタの製造方法 |
KR101433857B1 (ko) * | 2013-07-05 | 2014-08-26 | 연세대학교 산학협력단 | 과산화수소를 이용한 산화물 박막 형성 방법 및 산화물 박막 트랜지스터 제조 방법 |
JP6651714B2 (ja) * | 2014-07-11 | 2020-02-19 | 株式会社リコー | n型酸化物半導体製造用塗布液、電界効果型トランジスタ、表示素子、画像表示装置、及びシステム |
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