CN118108189A - 一种利用液态金属转移六方氮化硼的方法 - Google Patents
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0646—Preparation by pyrolysis of boron and nitrogen containing compounds
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0648—After-treatment, e.g. grinding, purification
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Abstract
本发明公开了一种利用液态金属转移六方氮化硼的方法。该方法包括如下步骤:以氨硼烷、氮气、氢气为源,以高催化性的金属如镓、铟、镍、铁、钴等与硼形成的合金等为载体高温催化氨硼烷源热分解,所得反应基元在液态金属中溶解并迁移,在高温状态下在液态金属表面析出获得高质量h‑BN薄膜。通过将生长有h‑BN催化金属覆盖在石英、蓝宝石、碳化硅等绝缘衬底上并融化的方法,实现大面积氮化硼的转移。该方法无需在湿法化学和有机胶辅助条件下对h‑BN进行化学转移等处理,避免了对晶格与结晶质量造成损害,解决了以往h‑BN生长过程中成本高、易受污染等问题。
Description
技术领域
本发明涉及h-BN材料制备与应用技术领域,具体涉及一种利用液态金属转移六方氮化硼的方法。
背景技术
二维六方氮化硼(h-BN)是一种有着广泛应用前景的二维材料,这主要归功于其与石墨烯类似的晶体结构以及非常独特的性质。h-BN的层状结构由交替排列的氮和硼原子组成,呈现出类似蜂窝状六边形的晶体结构。与石墨烯不同,h-BN是一种宽禁带绝缘材料,其能隙约为5.97电子伏特(eV),使得其在电子学应用中显示出优异的绝缘特性。
二维h-BN还具有良好的化学稳定性、热导性、机械强度以及优异的耐热性和耐化学性,为其在许多领域的应用提供了可能性。例如,在电气绝缘材料、热界面材料和防护涂层方面,h-BN都显示出极大的潜力。特别是在纳米电子学领域,由于其高的热导率和电绝缘性,h-BN被视为理想的电子器件绝缘体材料,可作为石墨烯等导电二维材料的衬底。h-BN的平滑表面和较低的表面能使得电子可以在其上高速移动,因此,它对于制造下一代高速、低能耗的纳米电子器件至关重要。在电子和光电领域,h-BN可以应用于制造电路板、半导体器件、透明导电膜以及作为纳米复合材料的强化剂。此外,由于h-BN对某些波长的光有选择性的吸收能力,它还可能被应用于可见光驱动的光催化和紫外光吸收材料。在生物医学领域,h-BN因其生物相容性和耐药性,在药物递送和生物成像领域同样有着巨大潜力。
然而,在实际应用中,二维h-BN材料的薄膜转移技术仍然面临许多难点。首先,h-BN薄膜的生长通常需要在高温下进行,这会导致对生长基板的选择有一定限制。而且,多层h-BN的转移通常需要精准控制,任何微小的缺陷或是褶皱都可能导致性能下降。其次,薄膜转移过程中的精确对准和完整剥离也是一大难题,特别是在尝试将h-BN嵌入或与其他二维材料组合时。此外,为了实现大面积的h-BN薄膜转移,所需的设备和技术支持必须有足够的精确度,以确保薄膜的完整性和一致性。目前,为了解决这些难题,科研人员正在探索多种创新的方法,包括干法转移技术、湿法转移技术以及上述的液态金属转移技术等。每种方法都有其优点和局限性,在实际操作中需要根据h-BN薄膜的具体应用和性能要求来选择合适的转移策略。
发明内容
鉴于以上所述现有技术的缺点,本发明的目的在于提供利用液态金属转移六方氮化硼(h-BN)的方法,以实现直接精确大面积h-BN的转移,且无需刻蚀、压印及化学转移。本发明具体采用如下技术方案:
通过感应加热法在催化合金上生长多层h-BN,清洗目标转移衬底,在高温下下将熔融的催化合金上的多层h-BN转移至目标绝缘衬衬底,利用在高温下的界面效应,多层h-BN与目标衬底的固-液界面的结合力大于高温熔融状态下液-液界面多层h-BN与液态合金之间的结合力,实现对Ni-B合金表面的多层h-BN进行转移。随后进行进一步的测量与表征。包括以下步骤:
1) 清洗催化合金金属;
2) 向腔室中放入催化金属合金,高温下通入反应气源生长h-BN;
3) 将生长有h-BN的合金金属与承载物的上表面紧密接触;
4) 将结构置于管式炉中,通入载气并加热至合金金属融化温度温度;
5) 降温并移除基底表面的金属催化剂,在目标基底表面得到大面积h-BN。
作为本发明的优选方案,所述反应基源包括环硼氮环、氨硼烷等含硼、氮基元。
作为本发明的优选方案,所述催化金属包括但不限于镓、铟、铋、镍、铁、钴等催化金属与硼形成的二元或多元合金。
作为本发明的优选方案,所述绝缘衬底为硅片、氧化硅片、SiO2/Si、碳化硅或蓝宝石等耐高温绝缘衬底片。
作为本发明的优选方案,步骤2)中,h-BN的生长温度为800-1300 ℃,优选为1000℃;保温10-60 min,优选为30-45 min;工作气压10-10000 Pa,优选为10-120 Pa。
作为本发明的优选方案,步骤3)中所述载气为氩气和氢气的混合气,其流量分别为1-50 sccm和100-300 sccm。
作为本发明的优选方案,步骤5)中,移除催化剂的方法为,退火温度800-1300 ℃融化金属,时间为5-10分钟,工作气压为10000-50000 Pa,载气为氢气、氮气和氩气的混合气。
本发明利用利用液态金属转移六方氮化硼,有如下优点 :
1)本发明可以在衬底上精确定位大面积h-BN的位置;
2)本发明所得h-BN无需化学过程,避免了对有机物污染及H-BN褶皱的引入;
3)本发明无需对h-BN进行光刻、离子刻蚀等工艺,避免了对h-BN的损伤与破坏。
附图说明
图1 、多层h-BN转移工艺流程示意图;
图2 、多层h-BN转移至Sapphire衬底的OM、SEM图像;转移至Sapphire衬底的XPS谱图;
图3 、多层h-BN转移前后的Raman图(左)和XRD衍射谱(右);
图4、 Ni-B合金在1250 ℃生长60 min,45 min,30 min制备和转移多层h-BN的OM及AFM表征结果。
具体实施方式
以下通过特定的具体实例说明本发明的实施方式,本领域技术人员可由本说明书所揭示的内容轻易地了解本发明的其他优点与功效。本发明还可以通过另外不同的具体实施方式加以实施或应用,本说明书中的各项细节也可以基于不同观点与应用,在没有背离本发明的精神下进行各种修饰或改变。
请参阅附图。需要说明的是,参考图是本发明的示意图,图中的表示只是示意性质的,不应该被认为限制本发明的范围。
本发明的主要创新之处在于利用高温转移的方法将催化合金上的h-BN转移至绝缘衬底上。这种避免了化学转移及刻蚀的h-BN大面积方法,在以h-BN为功能单元的微纳电子器件方面有广泛的应用前景。
实施例:利用Ni-B合金作为催化剂,利用高温生长和转移的方法在实现多层h-BN向绝缘衬底表面的转移,步骤如下:
(1)将Ni-B合金置于高温感应加热CVD炉中,将炉温升至1000℃,使硼氮聚合物在高温及催化剂的作用下分解,在NiB合金表面形成大面积的H-BN。以氩气180sccm、氢气20sccm作为载气,反应时间60min,工作气压为常压;
(2)将高温感应加热炉冷却至室温以后,将Ni-B合金从炉内取出,将其倒置于清洗干净的蓝宝石衬底表面,将其置于炉内;
(3)在Ar(300 sccm)气氛下以200 ℃/min快速升温至1100 ℃。利用在高温下的界面效应,多层h-BN与sapphire衬底的固-液界面的结合力大于高温熔融状态下液-液界面多层h-BN与液态Ni-B合金之间的结合力,实现对Ni-B合金表面的多层h-BN进行转移;
(4)退火保温5 min后,在H2(30 sccm)和Ar(300 sccm)下快速冷却,Ar和H2主要其保护气作用;
(5)待炉内温度冷却至室温,使用专用夹具将石墨件取出,使用洁净的镊子将带有多层h-BN的sapphire样品取出,用N2吹干备用。
通过光学显微镜和原子力显微镜表征证明了其转移后表面形貌的均匀性,对其转移前后的Raman进行了表征测试,发现其转移前后曲线未有明显变化,表明转移前后多层h-BN未造成较大破坏,最后通过XPS表征测试也进一步证明了制备得到的多层h-BN B/N比符合多层h-BN的特征。
Claims (6)
1.一种利用液态金属转移六方氮化硼的方法,其特征在于,包括如下步骤:
(1)衬底清洗工艺过程:使用去离子水清洗催化金属片15 min,使用夹具将其浸入丙酮溶液中超声清洗15 min,用去离子水清洗后,用5%稀释盐酸以及去离子水冲洗衬底,最后高纯氮气吹干备用,将目标绝缘衬底先使用大量去离子水冲洗后浸入丙酮溶液中超声清洗15min,去除表面残留有机物等; 衬底分别浸入H2SO4/H2O2(摩尔比4:1)清洗液中在65 ℃水浴加热30 min; 最后利用去离子水将衬底清洗干净,使用高纯氮气吹干备用;
(2)多层h-BN生长工艺:将清洗吹干后的合金与反应基源置于感应加热线圈温区中部,抽真空后再通入Ar使高温感应加热系统至常压;通入Ar/H2混合气体并以200 ℃/min的升温速率升至800 ℃退火,随后保温20 min,目的是去除合金衬底表面的杂质;设备以200℃/min加热至1250 ℃,通入N2/H2混合气体并生长15-60 min; 生长结束后,通入Ar/H2混合气体,随后自然冷却至室温,用洁净镊子取出h-BN样品备用;
(3)多层h-BN的转移工艺:将生长有h-BN催化金属覆盖在绝缘衬底上,在Ar气氛下升温融化催化金属,在H2和N2气氛下保温5min。利用在高温下的界面效应, h-BN与衬底的固-液界面的结合力大于高温熔融状态下液-液界面h-BN与液态合金之间的结合力,实现对合金表面的多层h-BN进行转移。保温5 min后,在H2和Ar下使腔体快速冷却,待炉内温度冷却至室温,使用夹具将重新凝固的催化合金取出,使用洁净的镊子将带有多层h-BN的样品取出,用N2吹干备用。
2.根据权利要求1 所述的一种利用液态金属转移六方氮化硼方法,其特征在于:所述步骤1)中催化金属选自高催化性的金属如镓、铟、镍、铁、钴等与硼形成的合金。
3.根据权利要求1 所述的一种利用液态金属转移六方氮化硼方法,其特征在于:步骤2)中所述反应基源包括环硼氮环、氨硼烷等含硼、氮基元。
4.根据权利要求1 所述的一种利用液态金属转移六方氮化硼方法,其特征在于:所述步骤3)中的绝缘衬底为硅片、氧化硅片、SiO2/Si、碳化硅、或蓝宝石等。
5.根据权利要求1 所述的一种利用液态金属转移六方氮化硼方法,其特征在于:所述步骤2)中h-BN的生长温度为800-1300 ℃,时间为10-60分钟,工作气压为10-10000 Pa,载气为氢气、氮气和氩气的混合气。
6.根据权利要求1 所述的一种利用液态金属转移六方氮化硼方法,其特征在于:所述步骤3)中,移除催化剂的方法为,退火温度800-1300 ℃融化金属,时间为5-10分钟,工作气压为10000-50000 Pa,载气为氢气、氮气和氩气的混合气。
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