CN113233870B - 一种掺杂氧化镉靶材及其制备方法与应用 - Google Patents
一种掺杂氧化镉靶材及其制备方法与应用 Download PDFInfo
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Abstract
本发明公开了一种氧化铟掺杂氧化镉的靶材及其制备方法与应用,所述掺杂氧化镉靶材的制备方法包括如下步骤:(1)将氧化镉粉末和氧化铟粉末按CdO:In2O3=95~99.5:0.5~5的质量比进行球磨混合均匀;(2)将步骤(1)所得混料装入模具中,然后放入真空热压炉中;(3)对真空热压炉进行抽真空,当真空度≤10Pa后,开启加热,700~800℃保温1~3h,其中,保温10~50min后开始加压,加压压力为10~40MPa,保压时间为20~40min,当温度降至400~600℃后,将压力降至3~15MPa;(4)当温度降至室温后,开炉门,脱模,即得所述掺杂氧化镉靶材。本发明的靶材的晶粒尺寸<10μm,抗弯强度>80MPa,溅射效果好,用于溅射制备CdO基导电薄膜时可使薄膜中含In,扩宽了薄膜的透光波段,不会引入其它杂质,溅射条件的要求低。
Description
技术领域
本发明涉及溅射靶材制备技术领域,具体涉及一种氧化铟掺杂氧化镉的靶材及其制备方法与应用。
背景技术
氧化镉(CdO)是一种新型的半导体氧化物,它的禁带宽度约为2.2eV。CdO薄膜透明呈浅黄色,在可见光范围(380~780nm)内具有较高的光学透过率(80%~90%),是一种具有高迁移率、高载流子浓度的薄膜,被广泛应用于太阳能电池的窗口和光敏探测器等电子器件中。
CdO中添加In,可以实现CdO基导电薄膜透光波段的可调性,使更多的阳光被太阳能电池半导体结构吸收,从而最大程度地提高太阳能电池的光利用效率。为达到上述技术效果,现有的解决方法为:同时采用两种靶材,CdO靶材和ITO靶材共同溅射制备薄膜,以此向CdO基导电薄膜中掺入In。但是,由于ITO靶材中含有Sn,导致所制备的薄膜中也同时掺入了Sn杂质,而杂质含量越高,对薄膜的负面影响越大。此外,同时使用两种靶材进行溅射对溅射条件的要求较高,溅射过程不易控制,产品不良率高。
发明内容
为解决上述现有技术中存在的缺点和不足,本发明的目的在于提供一种掺杂氧化镉靶材及其制备方法与应用。本发明在制备靶材过程中直接向氧化镉中掺入氧化铟,并通过调控氧化铟的掺入量,制得晶粒尺寸<10μm及抗弯强度>80MPa的掺杂氧化镉靶材,该掺杂氧化镉靶材具有良好的溅射效果,可用于制备含In的CdO基导电薄膜,且不会向薄膜中引入其它杂质,溅射条件的要求低,溅射过程容易控制。
为实现上述目的,本发明采取的技术方案为:
一种掺杂氧化镉靶材的制备方法,包括如下步骤:
(1)将氧化镉粉末和氧化铟粉末按CdO:In2O3=95~99.5:0.5~5的质量比进行球磨混合均匀;
(2)将步骤(1)所得混料装入模具中,然后放入真空热压炉中;
(3)对真空热压炉进行抽真空,当真空度≤10Pa后,开启加热,700~800℃保温1~3h,其中,保温10~50min后开始加压,加压压力为10~40MPa,保压时间为20~40min,当温度降至400~600℃后,将压力降至3~15MPa;
(4)当温度降至室温后,开炉门,脱模,即得所述掺杂氧化镉靶材。
靶材的晶粒尺寸和抗弯强度是影响靶材溅射效果的重要参数,其中,晶粒尺寸会影响靶材溅射薄膜的厚度和均匀性,晶粒尺寸越小越好,而抗弯强度低会导致溅射时靶材容易开裂。本发明通过调控氧化铟的掺入量、以及混料和真空热压的条件,可成功制得氧化铟掺杂氧化镉的靶材,而且靶材的晶粒尺寸<10μm,抗弯强度>80MPa,具有较好的溅射效果。
优选地,所述氧化镉粉末和氧化铟粉末的纯度为5N以上。以该纯度的粉末制得的掺杂氧化镉靶材具有较好的溅射效果。
优选地,所述氧化镉粉末的平均粒径D90<5μm。
优选地,所述球磨混合的球料比为2~2.5:1,球磨时间为3~6h。使用常规的混料方法难以将氧化镉均匀分散于微米级的氧化镉粉末中,而使用本发明上述的球磨条件,可将氧化镉均匀分散于微米级的氧化镉粉末中,达到较好的掺杂效果。
优选地,所述模具为石墨模具。石墨模具耐高温和热膨胀系数低的特性,在本发明的制备条件下,石墨不会与氧化镉和氧化铟发生反应,可确保靶材的纯度。
优选地,所述加热的升温速率为2~10℃/min。以该速率进行升温,烧结效果较好,可制得密度较高的靶材。若升温速率过快,会影响烧结密度,不利于排气,最终导致靶材密度较小,溅射效果不好。
本发明还提供了一种掺杂氧化镉靶材,其由本发明上述的制备方法制得。所述掺杂氧化镉靶材的晶粒尺寸<10μm,抗弯强度>80MPa。
本发明还提供了所述掺杂氧化镉靶材在导电薄膜制备中的应用。本发明的掺杂氧化镉靶材可用于溅射制备CdO基导电薄膜,且由于靶材中掺入了In2O3,因此溅射形成的CdO基导电薄膜中会含有In,实现了CdO基导电薄膜透光波段的可调性。与现有技术同时使用两种靶材进行溅射的方法相比,使用本发明的掺杂氧化镉靶材进行溅射,可避免引入对薄膜有不利影响的其它杂质,而且溅射要求更低。
本发明还提供了一种导电薄膜,其由所述掺杂氧化镉靶材通过溅射工艺制得。
与现有技术相比,本发明的有益效果在于:本发明制备的靶材为氧化铟掺杂氧化镉靶材,靶材的晶粒尺寸<10μm,抗弯强度>80MPa,具有较好的溅射效果,可用于溅射制备CdO基导电薄膜,溅射形成的CdO基导电薄膜中含In,扩宽了薄膜的透光波段,不会向薄膜中引入其它杂质,溅射条件的要求低,溅射过程容易控制。
具体实施方式
为更好的说明本发明的目的、技术方案和优点,下面将通过下列实施例进一步说明。应理解,以下实施例仅用于说明本发明而非用于限制本发明的范围。实施例中,所用方法如无特别说明,均为常规方法。实施例中使用的氧化镉粉末和氧化铟粉末的纯度均为5N,且氧化镉粉末的平均粒径D90<5μm。
实施例1
一种掺杂氧化镉靶材的制备方法,步骤如下:
(1)氧化镉粉末和氧化铟粉末按CdO:In2O3=95:5的质量比混合,放入球磨桶中,球磨4h,球料比为2:1;
(2)将步骤(1)所得混料装入石墨模具中,然后放入真空热压炉中;
(3)对真空热压炉进行抽真空,当真空度达到10Pa后,开启加热,以10℃/min升温至750℃,保温2h;其中,保温20min后开始加压,加压压力为40MPa,保压时间为30min,当温度降至600℃后,将压力降至15MPa;
(4)当温度降至室温后,开炉门,脱模,即得掺杂氧化镉靶材。
实施例2
一种掺杂氧化镉靶材的制备方法,步骤如下:
(1)氧化镉粉末和氧化铟粉末按CdO:In2O3=99.5:0.5的质量比混合,放入球磨桶中,球磨4h,球料比为2.5:1;
(2)将步骤(1)所得混料装入石墨模具中,然后放入真空热压炉中;
(3)对真空热压炉进行抽真空,当真空度达到10Pa后,开启加热,以5℃/min升温至700℃,保温1h;其中,保温50min后开始加压,加压压力为25MPa,保压时间为20min,当温度降至400℃后,将压力降至3MPa;
(4)当温度降至室温后,开炉门,脱模,即得掺杂氧化镉靶材。
实施例3
一种掺杂氧化镉靶材的制备方法,步骤如下:
(1)氧化镉粉末和氧化铟粉末按CdO:In2O3=98:2的质量比混合,放入球磨桶中,球磨4h,球料比为2.1:1;
(2)将步骤(1)所得混料装入石墨模具中,然后放入真空热压炉中;
(3)对真空热压炉进行抽真空,当真空度达到10Pa后,开启加热,以6℃/min升温至700℃,保温3h;其中,保温10min后开始加压,加压压力为40MPa,保压时间为40min,当温度降至500℃后,将压力降至10MPa;
(4)当温度降至室温后,开炉门,脱模,即得掺杂氧化镉靶材。
对比例1
一种掺杂氧化镉靶材的制备方法,步骤如下:
(1)氧化镉粉末和氧化铟粉末按CdO:In2O3=98:2的质量比混合,放入球磨桶中,球磨4h,球料比为2.1:1;
(2)将步骤(1)所得混料装入石墨模具中,然后放入真空热压炉中;
(3)对真空热压炉进行抽真空,当真空度达到10Pa后,开启加热,以13℃/min升温至700℃,保温3h;其中,保温10min后开始加压,加压压力为5MPa,保压时间为40min,当温度降至500℃后,将压力降至3MPa;
(4)当温度降至室温后,开炉门,脱模,即得掺杂氧化镉靶材。
对比例2
一种掺杂氧化镉靶材的制备方法,步骤如下:
(1)氧化镉粉末和氧化铟粉末按CdO:In2O3=98:2的质量比混合,放入球磨桶中,球磨4h,球料比为2.1:1;
(2)将步骤(1)所得混料装入石墨模具中,然后放入真空热压炉中;
(3)对真空热压炉进行抽真空,当真空度达到10Pa后,开启加热,以6℃/min升温至600℃,保温3h;其中,保温10min后开始加压,加压压力为40MPa,保压时间为40min,当温度降至500℃后,将压力降至10MPa;
(4)当温度降至室温后,开炉门,脱模,即得掺杂氧化镉靶材。
对比例3
一种掺杂氧化镉靶材的制备方法,步骤如下:
(1)氧化镉粉末和氧化铟粉末按CdO:In2O3=98:2的质量比混合,放入球磨桶中,球磨4h,球料比为2.1:1;
(2)将步骤(1)所得混料装入石墨模具中,然后放入真空热压炉中;
(3)对真空热压炉进行抽真空,当真空度达到10Pa后,开启加热,以6℃/min升温至900℃,保温3h;其中,保温10min后开始加压,加压压力为40MPa,保压时间为40min,当温度降至500℃后,将压力降至10MPa;
(4)当温度降至室温后,开炉门,脱模,即得掺杂氧化镉靶材。
性能测试:
靶材的晶粒尺寸用晶相显微镜观察。
靶材的抗弯强度按照GB/T 14452-93《金属弯曲力学性能试验方法》标准进行测试。
实施例1~3和对比例1~3制备的掺杂氧化镉靶材的晶粒尺寸和抗弯强度如下表所示:
掺杂氧化镉靶材 | 晶粒尺寸,μm | 抗弯强度,MPa |
实施例1 | <9 | 81.5 |
实施例2 | <9 | 80.8 |
实施例3 | <10 | 82.1 |
对比例1 | <10 | 73.2 |
对比例2 | <10 | 69.5 |
对比例3 | <15 | 75.6 |
最后所应当说明的是,以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制,尽管参照较佳实施例对本发明作了详细说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的实质和范围。
Claims (9)
1.一种掺杂氧化镉靶材的制备方法,其特征在于,包括如下步骤:
(1)将氧化镉粉末和氧化铟粉末按CdO:In2O3=95~99.5:0.5~5的质量比进行球磨混合均匀;
(2)将步骤(1)所得混料装入模具中,然后放入真空热压炉中;
(3)对真空热压炉进行抽真空,当真空度≤10Pa后,开启加热,700~800℃保温1~3h,其中,保温10~50min后开始加压,加压压力为10~40MPa,保压时间为20~40min,当温度降至400~600℃后,将压力降至3~15MPa;所述加热的升温速率为2~10℃/min;
(4)当温度降至室温后,开炉门,脱模,即得所述掺杂氧化镉靶材。
2.如权利要求1所述的掺杂氧化镉靶材的制备方法,其特征在于,所述氧化镉粉末和氧化铟粉末的纯度为5N以上。
3.如权利要求1所述的掺杂氧化镉靶材的制备方法,其特征在于,所述氧化镉粉末的平均粒径D90<5μm。
4.如权利要求1所述的掺杂氧化镉靶材的制备方法,其特征在于,所述球磨混合的球料比为2~2.5:1,球磨时间为3~6h。
5.如权利要求1所述的掺杂氧化镉靶材的制备方法,其特征在于,所述模具为石墨模具。
6.一种掺杂氧化镉靶材,其特征在于,由如权利要求1~5任一项所述的掺杂氧化镉靶材的制备方法制得。
7.如权利要求6所述的掺杂氧化镉靶材,其特征在于,所述掺杂氧化镉靶材的晶粒尺寸<10μm,抗弯强度>80MPa。
8.如权利要求6或7所述的掺杂氧化镉靶材在导电薄膜制备中的应用。
9.一种导电薄膜,其特征在于,由如权利要求6或7所述的掺杂氧化镉靶材通过溅射工艺制得。
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