CN111926307A - 石墨烯薄膜、多孔二氧化硅粉末和透明导电层的制作方法 - Google Patents
石墨烯薄膜、多孔二氧化硅粉末和透明导电层的制作方法 Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 65
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 52
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 27
- 229910021426 porous silicon Inorganic materials 0.000 title claims abstract description 25
- 239000011148 porous material Substances 0.000 claims abstract description 129
- 239000003054 catalyst Substances 0.000 claims abstract description 94
- 239000002184 metal Substances 0.000 claims abstract description 78
- 229910052751 metal Inorganic materials 0.000 claims abstract description 78
- 239000000843 powder Substances 0.000 claims abstract description 58
- 238000000231 atomic layer deposition Methods 0.000 claims abstract description 49
- 238000000151 deposition Methods 0.000 claims abstract description 25
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 41
- 239000002243 precursor Substances 0.000 claims description 27
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 20
- 229910052802 copper Inorganic materials 0.000 claims description 20
- 239000010949 copper Substances 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 18
- 239000012691 Cu precursor Substances 0.000 claims description 15
- 239000011261 inert gas Substances 0.000 claims description 14
- 229910052759 nickel Inorganic materials 0.000 claims description 14
- 238000010926 purge Methods 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 7
- 238000005229 chemical vapour deposition Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- ZKXWKVVCCTZOLD-UHFFFAOYSA-N copper;4-hydroxypent-3-en-2-one Chemical compound [Cu].CC(O)=CC(C)=O.CC(O)=CC(C)=O ZKXWKVVCCTZOLD-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 230000014759 maintenance of location Effects 0.000 claims description 3
- KMVUJWSUYNVYSC-UHFFFAOYSA-N copper;cycloocta-1,5-diene Chemical compound [Cu].C1CC=CCCC=C1 KMVUJWSUYNVYSC-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- LZPXVVTUQLLOKZ-UHFFFAOYSA-N copper;1,1,1,5,5,5-hexafluoropentane-2,4-dione Chemical compound [Cu].FC(F)(F)C(=O)CC(=O)C(F)(F)F LZPXVVTUQLLOKZ-UHFFFAOYSA-N 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 34
- 239000000377 silicon dioxide Substances 0.000 description 25
- 235000012239 silicon dioxide Nutrition 0.000 description 17
- 239000000243 solution Substances 0.000 description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 239000010409 thin film Substances 0.000 description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 6
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- 239000012686 silicon precursor Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 2
- JOLURLQBADSSPV-UHFFFAOYSA-N [Cu].FC(C(CC(C(F)(F)F)=O)=O)(F)F.C1=CCCC=CCC1 Chemical compound [Cu].FC(C(CC(C(F)(F)F)=O)=O)(F)F.C1=CCCC=CCC1 JOLURLQBADSSPV-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000006557 surface reaction Methods 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
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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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
- C23C16/0281—Deposition of sub-layers, e.g. to promote the adhesion of the main coating of metallic sub-layers
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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
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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
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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
- C23C16/44—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 method of coating
- C23C16/455—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 method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
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Abstract
本申请公开了一种石墨烯薄膜、多孔二氧化硅粉末和透明导电层的制作方法,所述石墨烯薄膜的制作方法,包括以下步骤:提供一多孔材料粉末;在原子层沉积装置中放入多孔材料粉末;在原子层沉积装置中沉积金属催化层;使金属催化层沉积在所述多孔材料粉末的孔内,形成孔内有金属催化层的多孔材料粉末;使用孔内有金属催化层的多孔材料粉末,形成孔内有金属催化层的多孔材料模板;在多孔材料模板上制备石墨烯薄膜,这种制作方法产出的石墨烯薄膜孔隙率高,比表面积大,易于控制且致密度高,适合工业化使用。
Description
技术领域
本申请涉及显示技术领域,尤其涉及一种石墨烯薄膜、多孔二氧化硅粉末和透明导电层的制作方法。
背景技术
显示面板近年来得到了飞速地发展和广泛地应用。就主流市场上的TFT-LCD(ThinFilm Transistor-LCD,薄膜晶体管液晶显示屏)而言,包括阵列基板和彩膜基板,在阵列基板上形成薄膜晶体管,薄膜晶体管控制像素电极的开关,薄膜晶体管打开时,像素电极产生电压,使得液晶分子发生偏转,显示画面。
像素电极等透明导电层一般使用ITO(Indium tin oxide)铟锡氧化物材料,而ITO材料导电率较低,可见光范围内表现出不均匀光吸收,而石墨烯薄膜是最合适代替ITO的一种材料,石墨烯薄膜透明性及导电性都优于ITO材料,并且具有ITO在柔性领域所不具备的特性,如何生产石墨烯薄膜并提高其性能成了越来越多的人需要关注的问题。
发明内容
本申请的目的是提供一种石墨烯薄膜、多孔二氧化硅粉末和透明导电层的制作方法,以制得性能更好的透明导电层,替代ITO材料在显示面板中的作用。
本申请公开了一种石墨烯薄膜的制作方法,包括步骤:
提供一多孔材料粉末;
在原子层沉积装置中放入多孔材料粉末;
在原子层沉积装置中沉积金属催化层;使金属催化层沉积在所述多孔材料粉末的孔内,形成孔内有金属催化层的多孔材料粉末;
使用孔内有金属催化层的多孔材料粉末,形成孔内有金属催化层的多孔材料模板;以及
在多孔材料模板上制备石墨烯薄膜。
可选的,所述提供一多孔材料粉末的步骤中:
所述多孔材料粉末包括分级多孔二氧化硅粉末。
可选的,所述在原子层沉积装置中沉积金属催化层,使金属催化层沉积在所述多孔材料粉末的孔内,形成孔内有金属催化层的多孔材料粉末的步骤中:
所述金属催化层包括铜催化层或镍催化层。
可选的,所述在原子层沉积装置中沉积金属催化层,使金属催化层沉积在所述多孔材料粉末的孔内,形成孔内有金属催化层的多孔材料粉末的步骤中包括:
在原子层沉积装置中持续通入预设时间的铜前驱体或镍前驱体,停留预设时间,持续通入预设时间的惰性气体吹扫;
在原子层沉积装置中持续通入预设时间的还原气体,停留预设时间,持续通入预设时间的惰性气体吹扫;以及
重复执行上述两个步骤直至达到预设重复次数,形成所述铜催化层或镍催化层。
可选的,所述铜催化层或镍催化层的厚度为10-30nm。
可选的,所述铜前驱体或镍前驱体的持续通入预设时间为0.01s-0.2s,停留预设时间为2s-20s;所述还原性气体的持续通入预设时间为0.01s-0.5s,停留预设时间为2s-20s。
可选的,所述铜前驱体包括:N,N-二异丙基乙酸铜、1,5-环辛二烯(六氟-2,4-戊二酮)铜、乙酰丙酮铜中的至少一种。
可选的,所述在在多孔材料模板上制备石墨烯薄膜的步骤中包括以下步骤:
将多孔材料模板放入化学气相淀积腔室内,通入Ar/H2混合气体,加热至预设温度;
通入碳源前驱体,生长预设时间后冷却降温,形成带有多孔材料模板的石墨烯薄膜;以及
将带有二氧化硅模板的石墨烯薄膜浸入到剥离液中形成石墨烯薄膜。
本申请还公开了一种孔内含金属催化层的多孔二氧化硅粉末的制作方法,包括步骤:
A:在原子层沉积装置中放入多孔二氧化硅粉末;
B:在原子层沉积装置中持续通入预设时间的金属前驱体,停留预设时间,持续通入预设时间的惰性气体吹扫;
C:在原子层沉积装置中持续通入预设时间的还原气体,停留预设时间,持续通入预设时间的惰性气体吹扫;以及
D:循环重复所述步骤B和C预设次数,得到孔内有金属催化层的多孔二氧化硅粉末。
本申请还公开了一种显示面板的透明导电层的制作方法,包括以下步骤:
提供一多孔材料粉末;
在原子层沉积装置中放入多孔材料粉末;
在原子层沉积装置中沉积金属催化层,使金属催化层沉积在所述多孔材料粉末的孔内,形成孔内有金属催化层的多孔材料粉末;
使用孔内有金属催化层的多孔材料粉末,形成孔内有金属催化层的多孔材料模板;以及
在多孔材料模板上制备得到石墨烯薄膜,作为显示面板的基板的透明导电层。
本申请突破性的使用原子层沉积技术在多孔材料粉末的孔中沉积金属催化层,粉末状的多孔材料不仅在外表面会沉积形成金属催化层,同时,在粉末状的多孔材料的孔道内这一相对于外表面很难生长出金属催化层的位置来说,也会沉积形成金属催化层,使得生产出的多孔材料模板的孔隙率和比表面积更高,可以吸附的金属催化层更多,为后续沉积石墨烯提供更多的可能沉积的空间,其产出的石墨烯薄膜孔隙率高,易于控制且致密度高,导电性、透明度等性能优良,适合在大小各尺寸面板中工业化应用。
附图说明
所包括的附图用来提供对本申请实施例的进一步的理解,其构成了说明书的一部分,用于例示本申请的实施方式,并与文字描述一起来阐释本申请的原理。显而易见地,下面描述中的附图仅仅是本申请的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动性的前提下,还可以根据这些附图获得其他的附图。
图1是本申请的一实施例的一种石墨烯薄膜的制作方法的步骤示意图;
图2是本申请的一实施例的一种分级多孔二氧化硅粉末的制作方法的步骤示意图;
图3是本申请的一实施例的一种多孔二氧化硅粉末的制作方法的步骤示意图;
图4是本申请的另一实施例的一种石墨烯薄膜的制作方法的步骤示意图;
图5是本申请的另一实施例的一种石墨烯薄膜的制作方法的步骤示意图;
图6是本申请的一实施例的一种显示面板的透明电极层的制作方法的步骤示意图;
图7是本申请的另一实施例的一种多孔二氧化硅粉末的制作方法的步骤示意图。
具体实施方式
需要理解的是,这里所使用的术语、公开的具体结构和功能细节,仅仅是为了描述具体实施例,是代表性的,但是本申请可以通过许多替换形式来具体实现,不应被解释成仅受限于这里所阐述的实施例。
在本申请的描述中,术语“第一”、“第二”仅用于描述目的,而不能理解为指示相对重要性,或者隐含指明所指示的技术特征的数量。由此,除非另有说明,限定有“第一”、“第二”的特征可以明示或者隐含地包括一个或者更多个该特征;“多个”的含义是两个或两个以上。术语“包括”及其任何变形,意为不排他的包含,可能存在或添加一个或更多其他特征、整数、步骤、操作、单元、组件和/或其组合。
另外,“中心”、“横向”、“上”、“下”、“左”、“右”、“竖直”、“水平”、“顶”、“底”、“内”、“外”等指示的方位或位置关系的术语,是基于附图所示的方位或相对位置关系描述的,仅是为了便于描述本申请的简化描述,而不是指示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作,因此不能理解为对本申请的限制。
此外,除非另有明确的规定和限定,术语“安装”、“相连”、“连接”应做广义理解,例如可以是固定连接,也可以是可拆卸连接,或一体地连接;可以是机械连接,也可以是电连接;可以是直接相连,也可以通过中间媒介间接相连,或是两个元件内部的连通。对于本领域的普通技术人员而言,可以根据具体情况理解上述术语在本申请中的具体含义。
下面参考附图和可选的实施例对本申请作详细说明。
原子层沉积(atomic layer deposition,ALD)技术是一种特殊的化学气相沉积技术,是通过将气相前驱体脉冲交替通入原子层沉积装置的反应室并在沉积基体表面发生化学吸附反应形成薄膜的一种方法。当前驱体分子达到沉积基体表面,它们会在其表面化学吸附并发生表面反应,原子层沉积的表面反应具有自限制性,即化学吸附自限制性和顺次反应自限制性,这种自限制性特征是原子层沉积的基础,通过不断重复这种自限制性反应形成纳米颗粒或薄膜,生产极好的三维保形性化学计量薄膜。
本申请公开了一种利用ALD技术制作石墨烯薄膜的制作方法,如图1所示,包括以下步骤:
S1:提供一多孔材料粉末;
S2:在原子层沉积装置中放入多孔材料粉末;
S3:在原子层沉积装置中沉积金属催化层;使金属催化层沉积在所述多孔材料粉末的孔内,形成孔内有金属催化层的多孔材料粉末;
S4:使用孔内有金属催化层的多孔材料粉末,形成孔内有金属催化层的多孔材料模板;
S5:在多孔材料模板上制备石墨烯薄膜。
本申请使用原子层沉积技术在多孔材料粉末的孔中沉积金属催化层,因为原子层沉积的表面具有自吸附特性,粉末状的多孔材料不仅在外表面会沉积形成金属催化层,同时,在粉末状的多孔材料的孔道内,相对于外表面很难生长出金属催化层的位置来说,也会沉积形成金属催化层,使得生产出的多孔材料模板的孔隙率和比表面积更高,可以吸附的金属催化层更多,为后续沉积石墨烯提供更多的可能沉积的空间,其产出的石墨烯薄膜孔隙率高,比表面积大,易于控制且致密度高,导电性、透明度等性能优良,适合在大小各尺寸面板中工业化应用。
其中,所述的多孔材料粉末可选用分级多孔二氧化硅粉末,而所述金属催化层可以包括铜催化层或镍催化层甚至两者混合,以二氧化硅材料作模板,以铜或镍作催化剂,在大规模生产中,生产成本较低,其原材料容易获得,且制得的石墨烯薄膜的效果优良。
在一具体的实施例中,所述分级多孔二氧化硅可以使用溶胶-凝胶制备分级多孔二氧化硅(HPSi)粉末。如图2所示,在所述提供一分级多孔二氧化硅的步骤中包括:
S101:按比例添加水和有机溶剂的混合液;
S102:添加硅前驱体源和表面活性剂;
S103:添加催化剂;
S104:在20-50℃下,400-800rpm(转每分)快速分散4-10小时;离心分离得到分级多孔二氧化硅。
其中,水/有机溶剂的比例范围为0.3-0.5;催化剂的PH范围在8-10,有机溶剂可以为乙醇、异丙醇、丁醇等,硅前驱体源可以为正硅酸乙酯(TEOS,Si(OC2H5)4),表面活性剂可以为CTAB(Hexadecyl trimethyl ammonium Bromide,十六烷基三甲基溴化铵)、CTAC(Hexadecyl trimethyl ammonium Chloride,十六烷基三甲基氯化铵);催化剂可以为氨水。
如图3所示,在另一个具体的实施例中,所述在原子层沉积装置中沉积金属催化层;使金属催化层沉积在所述多孔材料粉末的孔内,形成孔内有金属催化层的多孔材料粉末的步骤包括:
S301:在原子层沉积装置中持续通入预设时间的铜前驱体或镍前驱体,停留预设时间,持续通入预设时间的惰性气体吹扫;
S302:在原子层沉积装置中持续通入预设时间的还原气体,停留预设时间,持续通入预设时间的惰性气体吹扫;
S303:重复循环执行上述S301和S302两个步骤直至达到预设重复次数,形成所述铜催化层或镍催化层。
通过控制各种前驱体通入预设时间和停留预设时间,进而控制反应程度,适合控制在多孔二氧化硅粉末这种复杂的孔道内沉积铜催化层或镍催化层的厚度。比如,所述铜前驱体或镍前驱体的持续通入预设时间为0.01s-0.2s,停留预设时间为2s-20s;所述还原性气体的持续通入预设时间为0.01s-0.5s,停留预设时间为2s-20s。所述铜前驱体或镍前驱体、还原性气体的持续通入速率在5标准毫升/分钟至30标准毫升/分钟之间而根据实验数据证明,在设置范围为0.01s-0.2s的通入预设时间,可以满足足够一个循环使用的量,因为各种前驱体的材料价格较贵,通过控制通入预设时间,控制通入的量,防止浪费原材料,而停留预设时间设置为2s-20s,足够满足当前通入量的反应时间,其中,还原气体的停留预设时间越长,与铜前驱体或镍前驱体反应越充分,停留预设时间越短,生产效率越高;对应铜前驱体或镍前驱体的停留预设时间控制该前驱体的吸附程度,对应的停留预设时间越长,吸附量越多,对应的停留预设时间越短,生产效率越高。
具体的,所述铜催化层或镍催化层的厚度可选的控制为10-30nm,对应的,所述循环上述步骤的预设次数在50次至200次,需要说明的是,根据需要形成的铜催化层或镍催化层的厚度,可以对应设置不同循环预设次数。
所述铜前驱体可选用N,N-二异丙基乙酸铜、1,5-环辛二烯(六氟-2,4-戊二酮)铜、乙酰丙酮铜中的至少一种,对应的还原气体为氢气;这几种前驱体的原材料活性较高,反应速度较快,有利于节省原材料,同时有利于提高上生产效率。本申请选择的铜前驱体和还原气体在ALD装置的反应腔无需设置太高温度即可满足需求,所述原子层沉积装置的压强设置为0.05-10torr,温度150-300℃。低温的工作环境对于开发柔性显示设备和在OLED中应用产生带来了有利条件,便于铟镓锌氧化物在开发柔性显示设备和在OLED中应用的广泛使用,提高显示面板的稳定性等。
具体的,在所述使用孔内有金属催化层的多孔材料粉末,形成孔内有金属催化层的多孔材料模板的步骤中,通过将沉积有铜催化层或镍催化层的多孔二氧化硅粉末分散在有机醇溶液中,压制成二氧化硅模板,其中,有机醇溶液可以为乙醇、丙三醇、正丁醇等,该方法相较于直接成膜工艺,可以使得二氧化硅模板为后续沉积石墨烯提供更多的孔道空间。
如图4所示,在另一个具体的实施例中,所述在在多孔材料模板上制备石墨烯薄膜的步骤可包括以下步骤:
S501:将二氧化硅模板放入化学气相淀积腔室内,通入氩气(Ar)和氢气(H2)混合气体,加热至预设温度;其中,氢气通入速率为80-120标况毫升每分;
S502:通入碳源前驱体,生长预设时间后冷却降温,形成带有多孔二氧化硅模板的石墨烯薄膜;其中,碳源前驱体通入速率可选为10-30标况毫升每分,加热至800-1200℃,碳源前驱体包括:CH4、C2H2和C2H6等,生长预设时间设置为1-5分钟;
S503:将带有二氧化硅模板的石墨烯薄膜浸入到剥离液中形成石墨烯薄膜。所述剥离液可以为FeCl3溶液和氢氟酸溶液的混合液,也可以为FeCl3溶液和氢氟酸溶液的混合液,也可以依次将石墨烯薄膜浸入到FeCl3溶液和氢氧化钠溶液,或FeCl3溶液和氢氟酸溶液中。FeCl3溶液可以去除带有二氧化硅模板的石墨烯薄膜中的铜催化层,氢氟酸溶液和氢氟酸溶液可以去除带有二氧化硅模板的石墨烯薄膜中的二氧化硅模板。
如图5所示,作为本申请的一具体的实施例,公开了一种石墨烯薄膜的制作方法,包括步骤:
S11:按比例添加水和有机溶剂(如乙醇、异丙醇、丁醇)的混合液;
S21:添加硅前驱体源(如正硅酸乙酯)和表面活性剂(如CTAB、CTAC);
S31:添加催化剂(如氨水);
S41:在20-50℃下,400-800rpm(转每分)快速分散4-10小时;离心分离得到分级多孔二氧化硅;
S51:在原子层沉积装置中放入分级多孔二氧化硅;
S61:在原子层沉积装置中持续通入0.02s时间的铜前驱体(如N,N-二异丙基乙酸铜、1,5-环辛二烯(六氟-2,4-戊二酮)铜、乙酰丙酮铜中的至少一种)或镍前驱体,停留10s的时间,持续通入5时间的惰性气体(如氩气)吹扫;
S71:在原子层沉积装置中持续通入0.03s时间的还原气体(氢气),停留10s时间,持续通入5时间的惰性气体(如氩气)吹扫;
S81:重复执行上述S61和S71的步骤直至达到预设次数(如50次),形成铜催化层或镍催化层;
S91:将沉积有铜催化层或镍催化层的分级多孔二氧化硅分散在有机醇溶液中,压制成二氧化硅模板;
S101:将二氧化硅模板放入化学气相淀积腔室内,通入Ar/H2混合气体,加热至预设温度;
S111:通入碳源前驱体,生长预设时间后冷却降温,形成带有二氧化硅模板的石墨烯薄膜。
S121:将带有二氧化硅模板的石墨烯薄膜浸入到剥离液中形成石墨烯薄膜。
作为本申请一具体的实施例,如图6所示,本申请还公开了一种显示面板的制作方法,包括形成石墨烯薄膜作为显示面板的透明导电层的步骤;所述显示面板的透明导电层制作方法包括:
S12:提供一多孔材料粉末;
S22:在原子层沉积装置中放入多孔材料粉末;
S32:在原子层沉积装置中沉积金属催化层;使金属催化层沉积在所述多孔材料粉末的孔内,形成孔内有金属催化层的多孔材料粉末;
S42:使用孔内有金属催化层的多孔材料粉末,形成孔内有金属催化层的多孔材料模板;
S52:在多孔材料模板上制备得到石墨烯薄膜,作为显示面板的基板的透明导电层。
同时,本申请还公开了一种孔内含金属催化层的多孔二氧化硅粉末的制作方法,如图7所示,包括以下步骤:
A:在原子层沉积装置中放入多孔二氧化硅粉末;
B:在原子层沉积装置中持续通入预设时间的金属前驱体,停留预设时间,持续通入预设时间的惰性气体吹扫;
C:在原子层沉积装置中持续通入预设时间的还原气体,停留预设时间,持续通入预设时间的惰性气体吹扫;
D:循环重复上述步骤B和C预设次数,形成孔内有金属催化层的多孔二氧化硅粉末。
通过本方法制得的孔内含金属催化层的多孔二氧化硅粉末的金属催化层的分布更多更广,上述孔内含金属催化层的多孔二氧化硅粉末除可用于制作多孔二氧化硅模板以用于进一步制作石墨烯薄膜外,还可以根据需要用于制备碳纳米管、碳纤维等材料的制备。
需要说明的是,本方案中涉及到的各步骤的限定,在不影响具体方案实施的前提下,并不认定为对步骤先后顺序做出限定,写在前面的步骤可以是在先执行的,也可以是在后执行的,甚至也可以是同时执行的,只要能实施本方案,都应当视为属于本申请的保护范围。
本申请的技术方案可以广泛用于各种显示面板的透明导电层的制作,如TN(Twisted Nematic,扭曲向列型)显示面板、IPS(In-Plane Switching,平面转换型)显示面板、VA(Vertical Alignment,垂直配向型)显示面板、MVA(Multi-Domain VerticalAlignment,多象限垂直配向型)显示面板,当然,也可以是其他类型的显示面板,如OLED(Organic Light-Emitting Diode,有机发光二极管)显示面板,均可适用上述方案。
以上内容是结合具体的可选实施方式对本申请所作的进一步详细说明,不能认定本申请的具体实施只局限于这些说明。对于本申请所属技术领域的普通技术人员来说,在不脱离本申请构思的前提下,还可以做出若干简单推演或替换,都应当视为属于本申请的保护范围。
Claims (10)
1.一种石墨烯薄膜的制作方法,其特征在于,包括以下步骤:
提供一多孔材料粉末;
在原子层沉积装置中放入多孔材料粉末;
在原子层沉积装置中沉积金属催化层,使金属催化层沉积在所述多孔材料粉末的孔内,形成孔内有金属催化层的多孔材料粉末;
使用孔内有金属催化层的多孔材料粉末,形成孔内有金属催化层的多孔材料模板;以及
在多孔材料模板上制备得到石墨烯薄膜。
2.如权利要求1所述的一种石墨烯薄膜的制作方法,其特征在于,所述提供一多孔材料粉末的步骤中:
所述多孔材料粉末为分级多孔二氧化硅粉末。
3.如权利要求1所述的一种石墨烯薄膜的制作方法,其特征在于,所述在原子层沉积装置中沉积金属催化层,使金属催化层沉积在所述多孔材料粉末的孔内,形成孔内有金属催化层的多孔材料粉末的步骤中:
所述金属催化层包括铜催化层或镍催化层。
4.如权利要求3所述的一种石墨烯薄膜的制作方法,其特征在于,所述铜催化层或镍催化层的厚度为10-30nm。
5.如权利要求3所述的一种石墨烯薄膜的制作方法,其特征在于,所述在原子层沉积装置中沉积金属催化层,使金属催化层沉积在所述多孔材料粉末的孔内,形成孔内有金属催化层的多孔材料粉末的步骤包括:
在原子层沉积装置中持续通入预设时间的铜前驱体或镍前驱体,停留预设时间,持续通入预设时间的惰性气体吹扫;
在原子层沉积装置中持续通入预设时间的还原气体,停留预设时间,持续通入预设时间的惰性气体吹扫;以及
重复执行上述两个步骤直至达到预设重复次数,形成所述铜催化层或镍催化层。
6.如权利要求5所述的一种石墨烯薄膜的制作方法,其特征在于,所述铜前驱体或镍前驱体的持续通入预设时间为0.01s-0.2s,停留预设时间为2s-20s;所述还原性气体的持续通入预设时间为0.01s-0.5s,停留预设时间为2s-20s。
7.如权利要求5所述的一种石墨烯薄膜的制作方法,其特征在于,所述铜前驱体包括:N,N-二异丙基乙酸铜、1,5-环辛二烯铜、六氟-2,4-戊二酮铜、乙酰丙酮铜中的至少一种。
8.如权利要求1所述的一种石墨烯薄膜的制作方法,其特征在于,所述在在多孔材料模板上制备石墨烯薄膜的步骤包括以下步骤:
将多孔材料模板放入化学气相淀积腔室内,通入氩气(Ar)和氢气(H2)混合气体,加热至预设温度;
通入碳源前驱体,生长预设时间后冷却降温,形成带有多孔材料模板的石墨烯薄膜;以及
将带有多孔材料模板的石墨烯薄膜浸入到剥离液中形成石墨烯薄膜。
9.一种孔内含金属催化层的多孔二氧化硅粉末的制作方法,其特征在于,包括以下步骤:
A:在原子层沉积装置中放入多孔二氧化硅粉末;
B:在原子层沉积装置中持续通入预设时间的金属前驱体,停留预设时间,持续通入预设时间的惰性气体吹扫;
C:在原子层沉积装置中持续通入预设时间的还原气体,停留预设时间,持续通入预设时间的惰性气体吹扫;以及
D:循环重复所述步骤B和C预设次数,得到孔内有金属催化层的多孔二氧化硅粉末。
10.一种显示面板的透明导电层的制作方法,其特征在于,包括以下步骤:
提供一多孔材料粉末;
在原子层沉积装置中放入多孔材料粉末;
在原子层沉积装置中沉积金属催化层,使金属催化层沉积在所述多孔材料粉末的孔内,形成孔内有金属催化层的多孔材料粉末;
使用孔内有金属催化层的多孔材料粉末,形成孔内有金属催化层的多孔材料模板;以及
在多孔材料模板上制备得到石墨烯薄膜,作为显示面板的基板的透明导电层。
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