CN114014663B - 一种碲硒砷镉化合物、靶材及其制备方法 - Google Patents
一种碲硒砷镉化合物、靶材及其制备方法 Download PDFInfo
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- 239000013077 target material Substances 0.000 title claims abstract description 31
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 53
- 239000010439 graphite Substances 0.000 claims abstract description 53
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 claims abstract description 52
- FSIONULHYUVFFA-UHFFFAOYSA-N cadmium arsenide Chemical compound [Cd].[Cd]=[As].[Cd]=[As] FSIONULHYUVFFA-UHFFFAOYSA-N 0.000 claims abstract description 30
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- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 23
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- 229910052711 selenium Inorganic materials 0.000 claims description 22
- 239000011669 selenium Substances 0.000 claims description 22
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- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 12
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Abstract
本发明公开了一种碲硒砷镉化合物/靶材及制备方法,由摩尔比为(60‑90):(0.999‑39.99):(0.001~0.01)的碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒研磨成粉、混匀,将混匀的物料装入石墨坩埚中,或者将混匀的物料放入模具中室温压片成靶材坯,压片成形的靶材坯装入石墨治具内,石墨治具放入真空烧结炉内,在真空烧结炉内压实,真空状态加热烧结,自然降温至室温,打开真空烧结炉即得到碲硒砷镉化合物/靶材。上述制备方法能够适应市场规模化生产需求,工序简单、环境友好。制备出的碲硒砷镉化合物结晶度好,制备出的碲硒砷镉靶材相对密度高于90%(晶粒尺寸小于300nm)。
Description
技术领域
本发明属于半导体材料领域,具体涉及一种碲硒砷镉化合物、靶材及其制备方法。
背景技术
Ⅱ-Ⅵ族化合物半导体材料在微电子、红外调制、红外探测器和太阳电池等方面有着广泛的应用。其中,由Ⅱ-Ⅵ族元素碲与镉组成的二元化合物碲化镉(CdTe)带隙值为1.5eV,与太阳可见光谱匹配,处于理想的太阳电池带隙范围,有很好的光电转换效率,成为薄膜太阳电池研究热点。
随着对Ⅱ-Ⅵ族元素化合物半导体研究深入以及相关产业的飞速发展,人们逐渐认识到这类半导体具有自补偿效应。这种自补偿效应限制了该类化合物载流子浓度的增加,进而影响了尤其构成的器件的开路电压和填充因子的提高。为了提高载流子浓度及其少子寿命,于是人们尝试在二元化合物碲化镉(CdTe)中掺入硒元素。尽管硒元素掺杂碲化镉组成的三元化合物碲硒镉(CdSeTe)带隙略下降到1.4eV,较好地扩展了其红外响应,增加了器件的光电流密度,但是因硒掺杂引起带隙降低造成器件开路电压下降成为了新的挑战。为了解决这一问题,人们实验发现,通过在由Ⅱ-Ⅵ族元素碲、镉、硒组成的化合物中掺杂V族元素,尤其是掺杂元素砷能较好地钝化碲硒镉化合物薄膜中的缺陷,利于提高载流子浓度及少子寿命,使器件开路电压和电流密度增加。正如上述,碲化镉基多元化合物半导体在性能上有优良的表现,作为一种多元化合物薄膜太阳电池材料,具有广阔的发展前景。但是,目前有关在碲硒镉化合物薄膜中掺砷的方法是先沉积好碲硒镉化合物薄膜,然后再把该薄膜放置在砷源气氛中热扩散得到碲硒砷镉化合物薄膜,工艺过程中必须严苛控制砷源温度、工艺气压,工艺过程复杂且对设备要求苛刻,砷和硒的化学计量比难以控制,重金属砷、镉泄露风险也比较高。若采用碲硒砷镉化合物或靶材为原料制备碲硒砷镉化合物薄膜,上述问题迎刃而解,因此,开展碲硒砷镉化合物、靶材制备方法的研究是必要的。目前国内外关于碲硒砷镉化合物、靶材制备的方法还未见报道。
发明内容
为解决上述问题,本发明提供一种碲硒砷镉化合物、靶材及其制备方法,利用此方法合成的碲硒砷镉化合物或制备的靶材,通过热蒸发或溅射等技术可以在真空镀膜设备内一步完成预期化学计量比的碲硒砷镉薄膜制备,实现简化工艺、降低设备成本,有利于多元化合物碲硒砷镉薄膜材料的发展。
为解决上述技术问题,本发明采用的技术方案如下:一种碲硒砷镉化合物的制备方法,包括以下步骤:
1)将碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒混合均匀,置于研磨机内研磨成粉末,碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒三者的摩尔比为(60-90): (0.999-39.99): (0.001~0.01);
2)将上述研磨好的混合物料装入石墨坩埚内,将石墨坩埚放入带有液压装置的真空烧结炉内,液压装置将坩埚内的混合物料压实,抽真空至10-9Torr,然后向真空烧结炉内充保护气体,最后对石墨坩埚密封,并充保护气体使真空烧结炉内气压在0.1-100Torr之间;
3)对密封好的石墨坩埚进行加热,升温速率为1~5℃/min,加热至700~900℃,保温30~60min,保温结束后,停止加热,自然降温至室温,即得碲硒砷镉化合物。
步骤1)中碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒的纯度均为5N级以上;所述研磨机为行星研磨机。
步骤1)中碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒研磨成粉末,研磨时间4-6h,粉末粒径为不大于200微米。
步骤2)中将石墨坩埚放入带有液压装置的真空烧结炉内,抽真空与充保护气循环,循环过程中真空烧结炉内气压始终低于大气压;所述保护气为氩氢混合气。
一种碲硒砷镉化合物,由上述任一制备方法制得。
一种碲硒砷镉靶材的制备方法,包括以下步骤:
1)将碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒混合,置于研磨机内研磨成粉末,碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒三者的摩尔比为(60-90): (0.999-39.99): (0.001~0.01);
2)将上述混合均匀的物料放入模具中室温压片成靶材坯,压片成形的靶材坯装入石墨治具内,将石墨治具放入带有液压装置的真空烧结炉内,抽真空至10-9Torr,然后向真空烧结炉内充保护气体,最后对石墨治具密封,使用真空烧结炉自带的液压装置对石墨治具内的靶材坯加压保持为50MPa-80Mpa,并充保护气体使真空烧结炉内气压在0.1-100Torr之间;
3)对密封好的石墨治具进行加热,升温速率为1~3℃/min,加热至800~900℃,保温1~2h,保温结束后,停止加热,自然降温至室温,打开真空烧结炉得到碲硒砷镉靶材。
步骤1)中碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒的纯度均为5N级以上;所述研磨机为行星研磨机。
步骤2)中压片成靶材坯时的压强为50MPa-80Mpa,靶材坯为厚度6mm-10mm的平面圆形或平面长方形。
步骤2)中将石墨治具放入带有液压装置的真空烧结炉内,抽真空与充保护气循环,循环过程中真空烧结炉内气压始终低于大气压。
一种碲硒砷镉靶材,由以上任一所述制备方法制得。
本发明的有益效果是:通过配制预设摩尔比例的碲化镉、碲硒镉和砷化镉,并经研磨后根据需要压实或压片经真空炉烧结并保温保压一定时间,得到碲硒砷镉化合物或致密碲硒砷镉靶材。上述制备方法能够适应市场规模化生产需求,工序简单、环境友好。制备出的碲硒砷镉化合物结晶度好,制备出的碲硒砷镉靶材相对密度高于90%(晶粒尺寸小于300nm)。
附图说明
图1为碲硒砷镉化合物X射线衍射谱。
图2为碲硒砷镉靶材扫描电镜图。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚,下面对本发明中的技术方案进行清楚、完整地描述,显然,所描述的实施方式是本发明一部分实施方式,而不是全部的实施方式。基于本发明中的实施方式,本领域普通技术人员在没有作出创造性劳动前提下所获得的其他所有实施方式,都属于本发明保护的范围。因此,以下对本发明的实施方式的详细描述并非旨在限制要求保护的本发明的范围,而是仅仅表示本发明的选定实施方式。
本发明提出一种碲硒砷镉化合物的制备方法,包括如下步骤:
1)将碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒混合,放置在研磨机内研磨4-8小时,碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒三者的摩尔比为(60-90): (9.999-39.99): (0.001~0.01),碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒的纯度均为5N级以上,研磨机为行星研磨机;
2)将上述研磨好的物料装入石墨坩埚内,再将石墨坩埚放入真空烧结炉内,使用真空烧结炉自带的液压装置将坩埚内的物料压实,抽真空至10-9Torr,然后向真空烧结炉内充保护气体,该抽真空与充保护气完成若干次循环,以尽可能减少真空烧炉内杂质气体(比如氧)等存在,其中,该循环过程中炉内气压始终低于大气压,最后对石墨坩埚密封,并充保护气体使真空烧结炉内气压在0.1-100Torr之间;
3)对密封好的石墨坩埚进行加热,升温速率为1~5℃/min,加热至700~900℃,保温30~60min,保温结束后,停止加热,自然降温至室温,打开真空烧结炉得到碲硒砷镉化合物块体;
4)将碲硒砷镉块体根据不同客户的需求用进行破碎筛选得到不同粒径的碲硒砷镉化合物产品。
研磨机可以选用行星研磨机,其他种类的研磨机也可以用,优选行星研磨机;碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒纯度均优选5N级以上;碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒在研磨机中的研磨时间4-6h,粉末粒径为不大于200微米,保证颗粒均匀。
一种碲硒砷镉靶材的制备方法,该方法包括如下步骤:
1)将一定量碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒混合,放置在研磨机内研磨24-28小时研磨成粉末混合均匀;碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒三者的摩尔比例为:(60-90): (0.999-39.99): (0.001~0.01);
2)将上述混合均匀的一定量的物料放入模具中室温压片成平面圆形或平面长方形,压片成形压强为45MPa-60Mpa,压片厚度为6mm-10mm;压片成形的靶材坯装入石墨治具内,再将石墨治具放入带有液压装置的真空烧结炉内,抽真空至10-9Torr;然后向真空烧结炉内充保护气体,该抽空与充保护气完成若干次循环,以尽可能减少真空烧炉内杂质气体(比如氧)等存在,其中,该循环过程中炉内气压始终低于大气压;最后对石墨治具密封,使用真空烧结炉自带的液压装置对石墨治具内的的靶材坯加压保持为45MPa-60Mpa,并充保护气体使真空烧结炉内气压在0.1-100Torr之间;
3)对密封好的石墨治具进行加热,升温速率为1~3℃/min,加热至800~900℃,保温1~2h;保温结束后,停止加热,自然降温至室温,打开真空烧结炉得到碲硒砷镉靶材。
研磨机可以选用行星研磨机,其他种类的研磨机也可以用,优选行星研磨机;碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒纯度均优选5N级以上;碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒在研磨机中的研磨时间24-28h,保证碲化镉、碲硒镉和砷化镉混合均匀,研磨后的颗粒粒度均匀,确保靶材晶粒成形更好。
本发明公开的上述碲硒砷镉化合物及靶材的制备方法,能够规模化生产,适应市场规模化生产需求。
实施例1
碲硒砷镉化合物的制备方法:将5N级以上的碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒按摩尔比为60: 39.99: 0.01进行配比。将上述混合物料放入行星球磨机研磨4h,将上述混合均匀的物料装入一石墨坩埚内,再将石墨坩埚放入一真空烧结炉内,使用真空烧结炉自带的液压装置使物料在坩埚内被压实,抽真空至10-9Torr,然后向真空烧结炉内充保护气体,该抽空与充保护气完成若干次循环,以尽可能减少真空烧炉内杂质气体(比如氧)等存在,其中,该循环过程中炉内气压始终低于大气压,所述保护气为氩氢混合气;最后对石墨坩埚密封,并充保护气体使真空烧结炉内气压在10Torr之间;对密封好的石墨坩埚进行加热,升温速率为1~5℃/min,加热至800℃,保温60min,保温时温度会有几度的上下浮动,属于正常范围;保温结束后,停止加热,自然降温至室温,打开真空烧结炉得到碲硒砷镉化合物块体。将碲硒砷镉块体根据不同客户的需求进行破碎筛选,得到不同粒径的碲硒砷镉化合物产品。
碲硒砷镉靶材的制备:将5N级以上的碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒按摩尔比为60: 39.99: 0.01进行配比,将上述混合物料放入行星球磨机研磨28h。将上述混合均匀的一定量的物料放入模具中室温压片成平面圆形,压片成形压强为50MPa,压片厚度为8mm;压片成形的靶材坯装入石墨治具内,再将石墨治具放入带有液压装置的真空烧结炉内,抽真空至10-9Torr;然后向真空烧结炉内充保护气体,该抽空与充保护气完成若干次循环,以尽可能减少真空烧炉内杂质气体(比如氧)等存在,其中,该循环过程中炉内气压始终低于大气压;最后对石墨治具密封,使用真空烧结炉自带的液压装置对石墨治具内的的靶材坯加压保持为50MPa,并充保护气体使真空烧结炉内气压在10Torr之间;对密封好的石墨治具进行加热,升温速率为1~3℃/min,加热至800℃,保温1h;保温结束后,停止加热,自然降温至室温,打开真空烧结炉得到碲硒砷镉靶材。
由实施例1制备的碲硒砷镉化合物X射线衍射谱见图1,从图1可以看出碲硒砷镉化合物结晶度高。由实施例1制备的碲硒砷镉靶材扫描电镜图见图2,从图2可以看出碲硒砷镉靶材致密,晶粒尺寸小于300nm,分布均匀。
实施例2
将5N级以上的碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒按摩尔比为90: 9.999:0.001进行配比。将上述混合物料放入行星球磨机研磨8h。将上述混合均匀的物料装入一石墨坩埚内,再将石墨坩埚放入一真空烧结炉内,使用真空烧结炉自带的液压装置使物料在坩埚内被压实,抽真空至10-9Torr,然后向真空烧结炉内充保护气体,该抽空与充保护气完成若干次循环,以尽可能减少真空烧炉内杂质气体(比如氧)等存在,其中,该循环过程中炉内气压始终低于大气压;最后对石墨坩埚密封,并充保护气体使真空烧结炉内气压在,1Torr之间;对密封好的石墨坩埚进行加热,升温速率为1~5℃/min,加热至700℃,保温40min;保温结束后,停止加热,自然降温至室温,打开真空烧结炉得到碲硒砷镉化合物块体。将碲硒砷镉块体根据不同客户的需求用进行破碎筛选得到不同粒径的碲硒砷镉化合物产品。
采用上述配方制备碲硒砷镉靶材时,将混合物料放入行星球磨机研磨24h,将混合均匀的物料放入模具中室温压片成平面长方形,压片成形的压强为60Mpa,压片厚度为6mm;压片成形的靶材坯装入石墨治具内,再将石墨治具放入带有液压装置的真空烧结炉内,抽真空至10-9Torr,然后向真空烧结炉内充保护气体;最后对石墨治具密封,使用真空烧结炉自带的液压装置对石墨治具内的的靶材坯加压保持为60Mpa,并充保护气体使真空烧结炉内气压在1Torr之间;对密封好的石墨治具进行加热,升温速率为1~3℃/min,加热至900℃,保温1.5h;保温结束后,停止加热,自然降温至室温,打开真空烧结炉得到碲硒砷镉靶材。
实施例3-20
碲硒砷镉化合物的制备:原料碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒摩尔比,研磨时间、加热温度及保温时间等工艺变量均见表1,其余制备步骤同实施例1中碲硒砷镉化合物的制备方法;碲硒砷镉靶材的制备原料与上述碲硒砷镉化合物制备原料相同,研磨时间、压片压力、靶材坯加压压力、真空烧结炉内气压等工艺变量均见表2,其余制备步骤同实施例中碲硒砷镉靶材的制备方法。
表1
表2
Claims (9)
1.一种碲硒砷镉化合物的制备方法,其特征在于,包括以下步骤:
1)将碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒混合均匀,置于研磨机内研磨成粉末,碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒三者的摩尔比为(60-90): (0.999-39.99): (0.001~0.01);
2)将上述研磨好的混合物料装入石墨坩埚内,将石墨坩埚放入带有液压装置的真空烧结炉内,液压装置将坩埚内的混合物料压实,抽真空至10-9Torr,然后向真空烧结炉内充保护气体,抽真空与充保护气循环,循环过程中真空烧结炉内气压始终低于大气压,最后对石墨坩埚密封,并充保护气体使真空烧结炉内气压在0.1-100Torr之间;所述保护气为氩氢混合气;
3)对密封好的石墨坩埚进行加热,升温速率为1~5℃/min,加热至700~900℃,保温30~60min,保温结束后,停止加热,自然降温至室温,即得碲硒砷镉化合物。
2.根据权利要求1所述碲硒砷镉化合物的制备方法,其特征在于,步骤1)中碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒的纯度均为5N级以上;所述研磨机为行星研磨机。
3.根据权利要求1所述碲硒砷镉化合物的制备方法,其特征在于,步骤1)中碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒研磨成粉末,研磨时间4-6h,粉末粒径为不大于200微米。
4.一种碲硒砷镉化合物,其特征在于,由权利要求1-3任一所述制备方法制得。
5.一种碲硒砷镉靶材的制备方法,其特征在于,包括以下步骤:
1)将碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒混合,置于研磨机内研磨成粉末,碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒三者的摩尔比为(60-90): (0.999-39.99): (0.001~0.01);
2)将上述混合均匀的物料放入模具中室温压片成靶材坯,压片成形的靶材坯装入石墨治具内,将石墨治具放入带有液压装置的真空烧结炉内,抽真空至10-9Torr,然后向真空烧结炉内充保护气体,最后对石墨治具密封,使用真空烧结炉自带的液压装置对石墨治具内的靶材坯加压保持为50MPa-80MPa ,并充保护气体使真空烧结炉内气压在0.1-100Torr之间;
3)对密封好的石墨治具进行加热,升温速率为1~3℃/min,加热至800~900℃,保温1~2h,保温结束后,停止加热,自然降温至室温,打开真空烧结炉得到碲硒砷镉靶材。
6.根据权利要求5所述碲硒砷镉靶材的制备方法,其特征在于,步骤1)中碲化镉颗粒、碲硒镉颗粒和砷化镉颗粒的纯度均为5N级以上;所述研磨机为行星研磨机。
7.根据权利要求5所述碲硒砷镉靶材的制备方法,其特征在于,步骤2)中压片成靶材坯时的压强为50MPa-80MPa ,靶材坯为厚度6mm-10mm的平面圆形或平面长方形。
8.根据权利要求5所述碲硒砷镉靶材的制备方法,其特征在于,步骤2)中将石墨治具放入带有液压装置的真空烧结炉内,抽真空与充保护气循环,循环过程中真空烧结炉内气压始终低于大气压。
9.一种碲硒砷镉靶材,其特征在于,由权利要求5-8任一所述制备方法制得。
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