CN108695063B - 氧氮化物薄膜及电容元件 - Google Patents
氧氮化物薄膜及电容元件 Download PDFInfo
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- CN108695063B CN108695063B CN201810293209.XA CN201810293209A CN108695063B CN 108695063 B CN108695063 B CN 108695063B CN 201810293209 A CN201810293209 A CN 201810293209A CN 108695063 B CN108695063 B CN 108695063B
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- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 5
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- 229910052719 titanium Inorganic materials 0.000 claims abstract description 5
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- 238000009499 grossing Methods 0.000 description 1
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- 238000002156 mixing Methods 0.000 description 1
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- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
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- 238000004611 spectroscopical analysis Methods 0.000 description 1
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- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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Abstract
本发明提供一种制造效率高、介电特性优异的具有由氧氮化物构成的主组成的电介质薄膜及包含其的电容元件。所述电介质薄膜其特征在于,该电介质薄膜具有由以组成式AaBbOoNn(a+b+o+n=5)表示的氧氮化物构成的主组成,所述A为Sr、Ba、Ca、La、Ce、Pr、Nd、Na的任意一种以上,所述B为Ta、Nb、Ti、W的任意一种以上,构成所述电介质薄膜的晶粒为未向某特定的晶面方向取向的多晶,而且由柱状的颗粒构成。
Description
技术领域
本发明涉及具有由氧氮化物构成的主组成的电介质薄膜及包含其的电容元件。
背景技术
近年来,随着数码设备的小型化、高性能化,寻求使用了高性能的电介质薄膜的电容元件。
一直以来,作为电介质薄膜,广泛使用着使用了金属氧化物材料的薄膜。但是,由金属氧化物材料带来的电介质薄膜的特性提高遇到了极限,正在寻求具有更高特性的新的材料。
作为电介质薄膜的材料,可以举出氧氮化物。氧氮化物能够以ABO2N表示,但在例如以组成式SrTaO2N表示的氧氮化物中,成为其前体的氧化物为Sr2Ta2O7。SrTaO2N也能够由含有Sr、Ta、O及N的化合物直接合成,通过将Sr2Ta2O7氮化也可以得到。Sr2Ta2O7的相对介电常数根据合成法不同而各异,大致为100左右(非专利文献1)。另一方面,SrTaO2N的相对介电常数报告有数千以上的值(非专利文献2、专利文献1)。即,通过向氧氮化物的晶格内掺入氮,从而相对介电常数飞跃性地增大。
这样的氧氮化物中,作为新的材料的候补之一,可以举出将钙钛矿晶体结构的氧八面体中的氧原子的一部分置换成氮原子的金属氧氮化物材料。但是,难以得到具有金属氧氮化物材料的电介质薄膜。
例如,在专利文献2及专利文献3中记载有一种制作钙钛矿型氧氮化物ABO2N的粉末的方法。但是,专利文献2及专利文献3中,关于得到使用了钙钛矿型氧氮化物ABO2N的薄膜没有任何公开。
另外,非专利文献3及非专利文献4中记载有制作由钙钛矿型氧氮化物ABO2N构成的薄膜的内容。但是,非专利文献3及非专利文献4中得到的薄膜为外延膜。
外延膜存在在其制造时花费大量时间的缺点。非专利文献1中记载有制造厚度20nm以下的外延膜时花费530小时以下的较长的时间的内容。
现有技术文献
专利文献
专利文献1:日本特开2004-296603号公报
专利文献2:日本特开昭61-122108号公报
专利文献3:日本特开2013-001625号公报
非专利文献
非专利文献1:Journal of Materials Science:Materials in Electronics,11(2000),p.575-578
非专利文献2:Chem.Master.,Vol.16,No.7,2004,p.1267-1276
非专利文献3:Scientific Reports 4.DOI:10.1038/srep04987
非专利文献4:KAST平成25年度研究概要32-33页
发明内容
发明所要解决的课题
本发明鉴于这样的实际状况,其目的在于提供一种制造效率高、介电特性优异的具有由氧氮化物构成的主组成的电介质薄膜及包含其的电容元件。
用于解决课题的技术手段
本发明所涉及的电介质薄膜其特征在于,所述电介质薄膜具有由以组成式AaBbOoNn(a+b+o+n=5)表示的氧氮化物构成的主组成,
所述A为Sr、Ba、Ca、La、Ce、Pr、Nd、Na的任意一种以上,
所述B为Ta、Nb、Ti、W的任意一种以上,
构成所述电介质薄膜的晶粒为未向某特定的晶面方向取向的多晶,而且由柱状的颗粒构成。
本发明所涉及的电介质薄膜通过具有上述的特征,能够提高介电特性。
优选所述柱状的颗粒向相对于形成所述电介质薄膜的基板交叉的方向延伸。
优选从电介质薄膜的表面贯通至背面的所述柱状的颗粒的构成比率为30%以上。
在厚度方向上距电介质薄膜的表面为1/4的深度位置、1/2的深度位置、3/4的深度位置测定氮的组成比率的情况下,优选这3个位置的氮组成的变动率最大在±55%以内。
优选的是,所述A为Sr,所述B为Ta及/或Nb,所述n大于0且小于1。
本发明所涉及的电容元件具有所述电介质薄膜。
附图说明
图1是本发明的一个实施方式的薄膜电容器的概略图。
图2是以虚线表示本发明的一个实施方式的电介质薄膜中的柱状颗粒的形状的示意图。
图3是实施例1的电介质薄膜样品的TEM图像,虚线表示颗粒的形状。
图4是实施例2的电介质薄膜样品的TEM图像,虚线表示颗粒的形状。
符号的说明:
1…薄膜电容器
11…基板
12…下部电极
13…电介质薄膜
14…上部电极
15…中间层
X…柱状的颗粒
具体实施方式
以下,基于实施方式来说明本发明。
图1中表示本实施方式的薄膜电容器(电容元件)的示意图。图1所示的薄膜电容器1在基板11上依次形成下部电极12、电介质薄膜13,并且在电介质薄膜13上具备上部电极14。
基板11的材质没有特别限制,但使用Si单晶基板作为基板11时获取容易性及成本方面优异。在重视挠性的情况下,也能够使用Ni箔作为基板。
下部电极12及上部电极14的材质没有特别限制,只要作为电极发挥作用即可。例如,可以举出Pt、Ag、Ni等。下部电极12的厚度优选为0.01~10μm。上部电极14的厚度优选为0.01~10μm。
电介质薄膜13具有由以组成式AaBbOoNn(a+b+o+n=5)表示的氧氮化物构成的主组成。
A为选自Sr、Ba、Ca、La、Ce、Pr、Nd、Na中的一种以上的元素。优选A为选自Sr、Ba、La、Nd中的一种以上的元素。更优选A为Sr。通过使用上述元素作为A,可以得到较高的电容。B为选自Ta、Nb、Ti、W中的一种以上的元素。优选B为选自Ta、Nb中的一种以上的元素。更优选B为Ta。通过使用上述元素作为B,可以得到异相较少的电介质薄膜13。
另外,组成式AaBbOoNn中,优选a<1。另外,优选a/b>1,更优选a/b≧1.05。另外,优选1>n>0,更优选1>n≧0.3,进一步优选1>n≧0.5。通过将a、b及n设为上述的范围,可以得到良好的介电特性。
构成电介质薄膜13的晶粒为未向某特定的晶面方向取向的多晶。而且,如图2所示,构成电介质薄膜13的晶粒由柱状的颗粒X构成,上述柱状的颗粒X优选向相对于形成电介质薄膜13的基板11交叉的方向延伸。另外,如图2所示,上述柱状的颗粒X优选从电介质薄膜13的上部电极14侧的表面贯通至基板11侧的背面。本实施方式中,构成电介质薄膜13的晶粒为未向某特定的晶面方向取向的多晶,且由柱状的颗粒X构成,由此,介电特性提高。
认为构成电介质薄膜13的晶粒通过为未向某特定的晶面方向取向的多晶,且由柱状的颗粒X构成,从而氮高效地进入晶粒内,电介质薄膜的介电特性提高。
通常,取向膜为了得到其取向性而通过比较慢的成膜速度来形成,但这样的较慢的成膜速度时,不能充分得到成为氮的扩散路径的膜厚方向的晶界。本实施方式中,认为通过构成电介质薄膜13的晶粒为柱状的颗粒形状,从而在膜厚方向上形成氮的扩散路径,使氮能够高效地进入结晶内。其结果,本实施方式的电介质薄膜中,相对介电常数提高,可以得到较高的介电特性。
进一步,这样贯通电介质薄膜13的柱状的颗粒X相对于构成电介质薄膜13的全部晶粒的构成比率优选为30%以上。上述构成比率是基于电介质薄膜13的透射电子显微镜(TEM)图像观察的全部晶粒的数量中贯通的柱状的颗粒X的数量的比率。通过将贯通的柱状的颗粒X的构成比率设为上述范围,介电特性提高。
另外,电介质薄膜13的氮组成优选在厚度方向上距其表面为1/4的深度位置(表层侧)、1/2的深度位置(膜中央)、3/4的深度位置(基板侧),变动较少。更优选上述各深度位置中的氮组成的变动率最大在±55%以内,更优选为±25%以内,进一步优选为±20%以内,特别优选为±16%以内。通过将氮组成的变动率最大设为上述范围,介电特性提高。此外,电介质薄膜13中的氮组成能够通过X射线光电子能谱分析来进行确认。
变动率的最大X如下算出。首先,在上述各深度位置测定不同的5个点以上的氮组成。接着,基于上述不同的5个点以上的氮组成,求得各深度位置的氮平均组成。即,算出上述不同的5点以上的、在1/4的深度位置的氮平均组成X1、在1/2的深度位置的氮平均组成X2、在3/4的深度位置的氮平均组成X3。在此,将各深度位置的氮平均组成的平均值(X1+X2+X3)/3设为薄膜的氮组成的平均值Xa。然后,求得各深度位置的变动率Xn’=(Xn-Xa)/Xa(n=1、2、3)。即,算出在1/4的深度位置的变动率X1’、在1/2的深度位置的变动率X2’、在3/4的深度位置的变动率X3’。将X1’、X2’、X3’中与平均值Xa的差最大的变动率设为变动率的最大X。
关于氮的定量,优选AlN等的氮化单晶片进行定量,但也能够根据由同组成构成的氧氮化物粉算出灵敏度因子并修正定量值。在利用氧氮化物粉进行修正的情况下,也可以预先对氧氮化物粉使用脉冲加热熔融提取法等进行定量。另外,也能够用装置内标准进行代用。
电介质薄膜13的厚度没有特别限制,但优选为10nm~2μm,更优选为10nm~1μm。
电介质薄膜的介电损耗角正切(tanδ)优选为60%以下,更优选为40%以下,进一步优选为15%以下,特别优选为10%以下。通过将介电损耗角正切(tanδ)设为上述范围,可以得到介电特性优异的电介质薄膜。
此外,电介质薄膜的介电损耗角正切(tanδ)能够使用LCR仪,并在电压1V/rms、频率1kHz的条件下进行测定。
电介质薄膜的相对介电常数优选为355以上,更优选为450以上,进一步优选为700以上,特别优选为1110以上。通过将相对介电常数设为上述范围,可以得到介电特性优异的电介质薄膜。
此外,相对介电常数能够使用LCR仪,测定电压1V/rms、频率1kHz下的静电容量,并基于静电容量、电介质薄膜的厚度及电极面积算出。
薄膜电容器1的制造方法
接着,说明薄膜电容器1的制造方法。以下,对具有由以组成式AaBbOoNn表示的氧氮化物构成的主组成的电介质薄膜13中,A原子为Sr,且B原子为Ta的情况进行说明,但在使用其它种类的原子的情况下也同样。
最终成为电介质薄膜13的薄膜的成膜方法没有特别限制。例如,可以列举:真空蒸镀法、溅射法、PLD法(脉冲激光蒸镀法)、MO-CVD(有机金属化学气相沉积法)、MOD(有机金属分解法)、溶胶凝胶法、CSD(化学溶液堆积法)等。另外,有时在成膜时使用的原料中含有微少的杂质或副成分,但只要是不大幅损坏薄膜性能的程度的量,就没有特别的问题。另外,本实施方式的电介质薄膜13也可以在不大幅损坏性能的程度内含有微少的杂质或副成分。
上述的成膜方法中,在通过PLD法、溅射法及CSD法等的方法成膜时,最终得到的薄膜容易成为多晶膜。CVD法中也能够进行合成,但由于成分元素数较多,因此,PLD法或溅射法其组成控制性更高。本实施方式中,对利用PLD法的成膜方法进行说明。
首先,作为基板11,准备Si单晶基板。接着,在Si单晶基板上,按照SiO2、TiOx、Pt的顺序进行成膜,形成由Pt构成的下部电极12。形成下部电极12的方法没有特别限制。例如可以举出溅射法或CVD法等。
接着,在下部电极12上通过PLD法将金属氧化物薄膜成膜。为了使下部电极12的一部分露出,也可以使用金属掩模形成薄膜一部分未成膜的区域。
PLD法中,首先,将含有作为目标的电介质薄膜的构成元素的靶材设置于成膜室内。接着,向靶材的表面上照射脉冲激光。通过脉冲激光较强的能量,使靶材的表面瞬间蒸发。然后,在以与靶材相对的方式配置的基板上沉积蒸发物,将金属氧化物薄膜成膜。
作为靶材,能够使用例如具有组成式A2B2O7的前体。该前体优选为被称为钙钛矿板层的、钙钛矿单元和O过量层交替堆积而成的钙钛矿层状化合物。
靶材的种类没有特别限制,也能够使用将氧氮化物粉进行压缩成型后的颗粒。但是,由于需要充分管理含有的N量,因此,使用A2B2O7的颗粒时控制性良好。另外,靶材中优选各元素平均地分布,但也可以在不影响得到的电介质薄膜的品质的范围内分布存在不均。进一步,靶材未必需要为一个,也能够准备多个含有电介质薄膜的构成元素的一部分的靶材并用于成膜。靶材的形状也没有限制,只要设为适于使用的成膜装置的形状即可。另外,通过调整成膜条件(氧的气压、氮的气压、成膜室的大小及气体导入管的位置等),能够控制最终得到的电介质薄膜的a及b。例如,如果增大靶材的a/b,则能够增大成膜后的膜中的a/b。
例如,在最终得到的电介质薄膜的组成为SraTabOoNn的情况下,作为靶材,准备含有Sr2Ta2O7的烧结体。而且,通过调整成膜条件(例如氧的气压、氮的气压、成膜室的大小及气体导入管的位置等),能够控制最终得到的电介质薄膜的a及b。
成膜条件也非常重要。是由于通过脉冲激光从靶材蒸发的金属元素受到构成成膜室中的气氛的元素的影响,到达基板的成膜面。从超高真空到大气压附近大范围地设置气氛压力为PLD法的特征,但真空度较高时容易得到结晶性高的膜,另一方面,氧等的气氛压力较高时容易得到氧等的缺陷较少的膜。在并用等离子体的情况下,等离子体决定能够维持的压力范围宽度,因此,在该范围内,只要鉴于结晶性及缺陷等决定适当的压力即可。在为了将氧氮化物成膜而导入氧和氮的情况下,氧阻碍氮掺入膜中,因此,优选其压力较低。即使不导入氧,也能够通过导入被等离子体活化后的氮,形成钙钛矿结构。此外,溅射法中,作为成膜室中的气氛,优选并用氩。
另外,在PLD法时,为了使成膜的金属氧化物薄膜结晶化,优选在成膜时将基板11通过红外线激光进行加热。成膜时的基板11的加热温度根据金属氧化物薄膜及基板11的构成元素及组成等进行变化,但优选为550~850℃,更优选为600~800℃,进一步优选为650~750℃。通过将成膜时的基板的加热温度设为上述范围,容易形成柱状的颗粒。另外,难以形成空隙,介电特性提高。进一步,通过将基板11的温度设为适当的温度,金属氧氮化物薄膜容易结晶化,并且能够防止在冷却时产生的裂纹的产生。
在成膜中,通过导入氮自由基进行氮化处理,能够得到由钙钛矿型氧氮化物构成的电介质薄膜13。也可以在将金属氧化物膜成膜后,导入氮自由基进行氮化处理,但在成膜中导入氮自由基时能够进一步增加成膜后的薄膜中的氮量。
基板上的电介质薄膜13也可以在成膜后进行高速热退火处理(RTA)。退火在比成膜温度高100℃的温度以下,更优选在成膜温度以下进行,由此,能够维持在成膜时形成的柱状结构。在成膜温度以下进行退火的情况下,得到的膜的XRD图案在退火的前后未发现有重大的变化,因此,推测在成膜时决定柱状的晶体结构,在退火中产生缺陷的填补、应力缓和等。
最后,通过在电介质薄膜13上形成上部电极14,能够制造薄膜电容器1。此外,上部电极14的材质没有特别限制,能够使用Ag、Au、Cu等。另外,上部电极14的形成方法也没有特别限制。例如,能够通过溅射法或蒸镀来形成。
此外,也可以在电介质薄膜13与下部电极12之间、及电介质薄膜13与上部电极14之间具有中间层15。中间层15可以由绝缘材料构成,也可以由导电材料构成。作为绝缘材料,能够使用含有铝、硅、锶及钽中的至少一种的氧化物或氮化物等的化合物等。作为导电材料,能够使用Cu、Al、Ni、Au、及Ni-Cr等。作为中间层15的形成方法,能够采用与上述的电介质薄膜13的形成方法、或下部电极12及上部电极14的形成方法同样的方法。而且,中间层15可以作为绝缘层、应力缓和层、或用于将电极面的凹凸平滑化的层等发挥作用。
中间层15可以处于电介质薄膜13与下部电极12之间、及电介质薄膜13与上部电极14之间两者,也可以处于任一方。在中间层具有多个的情况下,各个中间层也可以具有不同的功能。
中间层15的厚度优选为电介质薄膜13的厚度的20%以下,更优选为10%以下。
本实施方式的电介质薄膜能够用作例如能够电压调谐的电容器、或如去耦薄膜电容器那样的高密度电容器装置的电介质层。
本实施方式的电容元件为利用了本实施方式的电介质薄膜的优异的介电性的元件,包括电容器、热敏电阻、滤波器、双工器、谐振器、发射器、天线、压电元件、晶体管、铁电体存储器等。本实施方式的电介质薄膜适用于特别是要求介电特性高的电容元件。
作为本实施方式的电容元件,作为例如电容器的制造方法,可以举出在基板上形成具有适当的电极的高调谐装置结构的方法。作为该高调谐装置结构,没有特别限定,例如也可以使用与SAW双工器、利用RF-MEMS的开关、压电驱动型的MEMS气隙可变电抗器、固定(低调谐性)高密度薄膜电容器、TFBAR电路、电阻器、电感器、以氧化物为基体的TFT及传感器等其它薄膜装置集成化后的装置结构。
以上,说明了本发明的实施方式,但本发明不被限定于这样的实施方式,当然可以在不脱离本发明的要点的范围内以各种不同的方式进行实施。
实施例
以下,基于更详细的实施例来说明本发明,但本发明不限定于这些实施例。
实施例1
首先,作为用作成膜用靶材的Sr2Ta2O7烧结体的原料,准备SrCO3粉末及Ta2O5粉末。以Sr/Ta的摩尔比成为1的方式称量SrCO3粉末及Ta2O5粉末。
接着,对于SrCO3粉末及Ta2O5粉末,利用使用了乙醇溶剂的湿式球磨机混合16小时,得到混合浆料。
接着,将上述混合浆料利用恒温干燥机以80℃干燥12小时,得到混合物。
接着,将上述混合物在乳钵中轻微粉碎,并放入陶瓷制的坩埚中。然后,使用电炉在大气气氛中以1000℃进行2小时热处理,得到煅烧物。
接着,对于上述煅烧物,再次利用使用了乙醇溶剂的湿式球磨机混合16小时,得到煅烧后浆料。
将得到的煅烧后浆料利用恒温干燥机以80℃干燥12小时,得到煅烧后混合物。
对于上述煅烧后混合物,添加作为粘合剂的聚乙烯醇溶液,并进行混合,得到造粒物。聚乙烯醇溶液的添加量相对于粉碎物100重量%设为0.6重量%。
将上述造粒物成型为直径约23mm、高度约9mm的圆柱形状,得到成型物。成型方法设为CIP成型。
对于上述成型物,使用电炉在大气气氛中,以1400℃烧成2小时,得到烧结物。进一步,将上述烧结物的上表面及下表面进行镜面研磨,得到高度5mm的成膜靶材。此外,确认了得到的成膜靶材的相对密度为96~98%。
将如上所述得到的成膜用靶材设置于成膜装置中,以与成膜用靶材相对的方式设置Si基板。作为该Si基板,使用了在表面具有作为下部电极的Pt膜的基板。
实施例1中,通过PLD法以频率10Hz照射脉冲激光,并以厚度成为500nm的方式成膜。此时,不向成膜室中导入氮,仅导入氧,形成电介质氧化膜。另外,成膜中,照射0.5小时的等离子体。成膜温度设为700℃。刚成膜后,导入氮自由基,将氮化处理进行30分钟,得到电介质薄膜样品。如下评价得到的电介质薄膜样品。
多晶膜及其取向性的评价
对于得到的样品,使用Rigaku株式会社制造的全自动水平型多目标X射线衍射装置SmartLab进行XRD测定,根据其XRD图案确认是否为向特定的面取向的取向膜和是否具有多晶性。在具有多晶性且不是相对于特定的面取向的取向膜的情况下,评价为“良”,在不具有多晶性的情况及为取向膜的情况下,评价为“不良”。另外,得到的薄膜样品所包含的氧氮化物的组成使用ULVAC-PHI,Inc.制造的PHI Quantera IITM并通过光电子分光分析进行定量。一边进行Ar蚀刻,一边定量薄膜的深度方向的组成。
氮组成的变动率的测定
对于得到的样品,在厚度方向上距薄膜的表面为1/4的深度位置,将不同的5点的氮组成(atm%)利用X射线光电子分光分析装置进行测定,并算出其平均。在厚度方向上距薄膜的表面为1/2的深度位置、及3/4的深度位置,也同样地测定氮组成(atm%),并分别算出平均。根据这些平均算出最大变动率。将结果在表1中表示。
空隙的有无及柱状颗粒的评价
对于的得到的样品,使用扫描电子显微镜(SEM)进行薄膜截面的观察。根据SEM图像,确认在1.2μm×1.5μm的3个视野的观察视野内30nm以上的空隙的有无。另外,根据使用透射电子显微镜(TEM)得到的TEM图像,确认柱状的颗粒的有无。进一步,在具有柱状的颗粒的情况下,确认柱状的颗粒是否向相对于基板交叉的方向延伸。然后,基于TEM图像,算出贯通的柱状颗粒的比率。将结果在表1中表示。另外,将实施例1中得到的TEM图像在图3中表示。
介电特性(tanδ及相对介电常数)的测定
使用LCR仪,在电压1V/rms、频率1kHz下测定试样的静电电容及tanδ。然后,基于薄膜的厚度、电极面积及静电电容算出相对介电常数。
晶体结构
通过XRD测定,确认得到的样品的晶体结构。
实施例2
实施例2中,通过PLD法以厚度成为1000nm的方式将电介质氧化膜成膜。另外,在成膜时导入氮自由基,进行氮化处理,但在成膜后不导入氮自由基。其它条件与实施例1同样地进行,得到电介质薄膜样品。与实施例1同样地评价。将结果在表1中表示。另外,将TEM图像在图4中表示。
实施例3
实施例3中,通过PLD法以厚度成为500nm的方式将电介质氧化膜成膜。成膜温度设为600℃。其它条件与实施例1同样地进行,得到电介质薄膜样品。与实施例1同样地评价。将结果在表1中表示。
实施例4
除了以下所示以外,与实施例1同样地进行,得到电介质薄膜样品。即,实施例4中,作为用作成膜用靶材的La2Ti2O7烧结体的原料,准备La2O3粉末及TiO2粉末。以La/Ti的摩尔比成为1的方式称量La2O3粉末及TiO2粉末。另外,通过PLD法以厚度成为500nm的方式将电介质氧化膜成膜。与实施例1同样地评价。将结果在表1中表示。
实施例5
除了以下所示以外,与实施例1同样地进行,得到电介质薄膜样品。即,实施例5中,作为用作成膜用靶材的Ba/Ta的摩尔比为1的氧化物的烧结体的原料,准备BaCO3粉末及Ta2O5粉末。以Ba/Ta的摩尔比成为1的方式称量Ba2CO3粉末及Ta2O5粉末。另外,通过PLD法以厚度成为500nm的方式将电介质氧化膜成膜。不存在作为Ba2Ta2O7的组合物,因此,即使以成为1的方式调整靶材烧结体的Ba/Ta的摩尔比,对于通过成膜条件得到的薄膜的摩尔比,也难以转移靶材组成。因此,对于调整成膜时的分压等,Ba/Ta的摩尔比成为1的样品,与实施例1同样地评价。将结果在表1中表示。
实施例6
实施例6中,除了将成膜温度设为500℃以外,与实施例1同样地进行,得到电介质薄膜样品。与实施例1同样地评价。将结果在表1中表示。
实施例7
实施例7中,除了将成膜温度设为850℃以外,与实施例1同样地进行,得到电介质薄膜样品。与实施例1同样地评价。将结果在表1中表示。
比较例1
比较例1中,除了将成膜温度设为400℃以外,与实施例2同样地进行,得到电介质薄膜样品。与实施例1同样地评价。将结果在表1中表示。
比较例2
比较例2中,除了将成膜温度设为300℃以外,与实施例2同样地进行,得到电介质薄膜样品。与实施例1同样地评价。将结果在表1中表示。
比较例3
比较例3中,除了将成膜温度设为900℃以外,与实施例1同样地进行,得到电介质薄膜样品。与实施例1同样地评价。将结果在表1中表示。
根据表1及图3、4的TEM图像,确认了在实施例1~7中,得到了没有空隙、未向特定的晶面方向取向的多晶,而且由向相对于基板交叉的方向延伸的柱状的颗粒构成的电介质薄膜样品,N组成的最大变动率为±55%以下,膜厚方向上均匀。另一方面,比较例1的电介质薄膜样品中,观察到空隙,未观察到柱状的颗粒。比较例2的薄膜样品中,未观察到空隙,但不具有晶体结构,也未观察到柱状的颗粒。另外,比较例1及2中,未检测到氮。比较例3的薄膜样品中,未观察到柱状的颗粒,N组成的最大变动率超过±55%。
实施例8
实施例8中,除了进一步延长成膜时的等离子体照射时间以外,与实施例1同样地进行,得到电介质薄膜样品。与实施例1同样地评价。将结果在表2中表示。此外,对于晶体结构,与实施例1相比,得到了“无峰移动”的结果。“无峰移动”是指通过X射线衍射得到的图案的峰位置没有移动,表示不管氮N的含有状态,与实施例1相比,晶格的大小均没有变化。
实施例9
实施例9中,除了进一步延长成膜时的等离子体照射时间以外,与实施例1同样地进行,得到电介质薄膜样品。与实施例1同样地评价。将结果在表2中表示。此外,对于晶体结构,与实施例8同样地,与实施例1相比,得到了“无峰移动”的结果。
实施例10、11
实施例10、11中,除了变更脉冲激光的频率及成膜气氛以外,与实施例1同样地进行,得到电介质薄膜样品。与实施例1同样地评价。将结果在表2中表示。此外,对于晶体结构,与实施例2相比,得到了“无峰移动”的结果。即,可知在实施例10、11中,不管氮N的含有状态,与实施例2相比,晶格的大小均没有变化。
[表2]
Claims (7)
1.一种电介质薄膜,其特征在于,
所述电介质薄膜具有由以组成式AaBbOoNn表示的氧氮化物构成的主组成,其中,a+b+o+n=5,
所述A为Sr、Ba、Ca、La、Ce、Pr、Nd、Na的任意一种以上,
所述B为Ta、Nb、Ti、W的任意一种以上,
构成所述电介质薄膜的晶粒为未向某特定的晶面方向取向的多晶,而且由柱状的颗粒构成,
所述柱状的颗粒向相对于形成所述电介质薄膜的基板交叉的方向延伸,
从所述电介质薄膜的表面贯通至背面的所述柱状的颗粒的数量的构成比率为30%以上。
2.根据权利要求1所述的电介质薄膜,其中,
在厚度方向上距所述电介质薄膜的表面为1/4的深度位置、1/2的深度位置、3/4的深度位置测定氮的组成比率的情况下,这3个位置的氮组成的变动率最大在±55%以内。
3.一种电介质薄膜,其特征在于,
所述电介质薄膜具有由以组成式AaBbOoNn表示的氧氮化物构成的主组成,其中,a+b+o+n=5,
所述A为Sr、Ba、Ca、La、Ce、Pr、Nd、Na的任意一种以上,
所述B为Ta、Nb、Ti、W的任意一种以上,
构成所述电介质薄膜的晶粒为未向某特定的晶面方向取向的多晶,而且由柱状的颗粒构成,
在厚度方向上距所述电介质薄膜的表面为1/4的深度位置、1/2的深度位置、3/4的深度位置测定氮的组成比率的情况下,这3个位置的氮组成的变动率最大在±55%以内。
4.根据权利要求3所述的电介质薄膜,其中,
所述柱状的颗粒向相对于形成所述电介质薄膜的基板交叉的方向延伸。
5.根据权利要求4所述的电介质薄膜,其中,
从所述电介质薄膜的表面贯通至背面的所述柱状的颗粒的数量的构成比率为30%以上。
6.根据权利要求1~5中任一项所述的电介质薄膜,其中,
所述A为Sr,所述B为Ta及/或Nb,所述n大于0且小于1。
7.一种电容元件,其中,
具有权利要求1~6中任一项所述的电介质薄膜。
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