CN1258211C - 门氧化膜形成用硅化铪靶及其制造方法 - Google Patents

门氧化膜形成用硅化铪靶及其制造方法 Download PDF

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CN1258211C
CN1258211C CNB028117050A CN02811705A CN1258211C CN 1258211 C CN1258211 C CN 1258211C CN B028117050 A CNB028117050 A CN B028117050A CN 02811705 A CN02811705 A CN 02811705A CN 1258211 C CN1258211 C CN 1258211C
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gate oxide
hfsi
targe
powder
hafnium
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CN1515029A (zh
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入间田修一
铃木了
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JX Nippon Mining and Metals Corp
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Nikko Materials Co Ltd
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Abstract

本发明涉及由HfSi1.02-2.00构成的门氧化膜形成用硅化铪靶。得到了适合形成可代替SiO2膜作为高介电率门绝缘膜使用的HfSiO和HfSiON膜，加工性和耐脆化性卓越的硅化铪钯，及其制备方法。

Description

门氧化膜形成用硅化铪靶及其制造方法
技术领域
本发明涉及适合形成可以作为高介电率门绝缘膜使用的HfSiO和HfSiON膜，加工性和耐脆化性卓越的硅化铪钯，及其制造方法。另外，本说明书中使用的单位“ppm”全部指wtppm(重量ppm)。
背景技术
介电门绝缘膜的膜厚对MOS晶体管的性能影响很大，并且与硅基片的界面是电学上平滑的以及载体的运动性不劣化是必要的。
以往，SiO2膜用作该门绝缘膜，在界面质量方面是最优越的。另外，具有用作该门绝缘膜的SiO2膜越薄，载体的数目(即，电子或电子空穴)增加，并且漏电流也由此增加的特性。
在这样的情况下，每一次由于布线的微型化导致电源电压下降，总是在不损害电介质击穿的可靠性的范围内将门SiO2膜作得尽可能薄。然而，当门膜的厚度为3nm或更小时，隧道漏电流直接流动，引起该膜不能起到绝缘膜作用的问题。
另一方面，尽管试图将晶体管小型化，但是既然作为前述的门绝缘膜的SiO2膜的膜厚有限制，则晶体管的小型化会损失其价值，产生性能不能改善的问题。
另外，为降低LSI的电源电压以及降低电力消耗，需要使门绝缘膜更进一步薄。然后，由于当SiO2膜的膜厚被作成3nm或更小时存在上述的门电介质击穿方面的问题，因此膜的变薄本身存在限制。
考虑到以上的情况，最近正考虑用高介电率门绝缘膜作为SiO2膜的替代品。作为该高介电率门绝缘膜引起注目的是HfSiO膜和HfSiON膜。
该高电介质绝缘膜是较厚的膜，能够获得与SiO2膜同等的容量，其特征在于，其能够抑制隧道漏电流。另外，由于其可以看作是在SiO2中添加了Hf的膜，因此可以预计界面质量与SiO2膜相近。
因此，所寻找的是能够容易且稳定地形成优质HfSiO和HfSiON高介电率门绝缘膜的溅射靶。
发明内容
为克服以上问题，本发明提供作为高介电率门绝缘膜使用，适合形成HfSiO和HfSiON膜，加工性和耐脆化性卓越的硅化铪钯，及其制造方法。
本发明提供：
1.一种门氧化膜形成用硅化铪靶，其由HfSi1.02-2.00构成(但是在该组成比中，不包括Si：1.02。换句话说，意味着仅Si的下限值为1.02(或更高)。本说明书中也同样如此)；
2.如上述1所述的门氧化膜形成用硅化铪靶，其特征在于，氧含量为500～10000ppm；
3.如上述1～2所述的门氧化膜形成用硅化铪靶，其特征在于，锆含量为2.5重量％或更低；
4.如上述1～3任一项所述的门氧化膜形成用硅化铪靶，其特征在于，杂质为C：300ppm或更低，Ti：100ppm或更低，Mo：100ppm或更低，W：10ppm或更低，Nb：10ppm或更低，Fe：10ppm或更低，Ni：10ppm或更低，Cr：10ppm或更低，Na：0.1ppm或更低，K：0.1ppm或更低，U：0.01ppm或更低，和Th：0.01ppm或更低；
5.如上述1～4任一项所述的门氧化膜形成用硅化铪靶，其特征在于，平均结晶粒径为5～200μm；
6.一种门氧化膜形成用硅化铪靶制造方法，其中该门氧化膜形成用硅化铪靶由HfSi1.02-2.00构成，含有主要包括HfSi相和HfSi2相的混合相，和相对密度为95％或更高，该方法的特征在于，合成由HfSi1.02-2.00构成的粉，将其粉碎到100目或更小，然后在1400℃～1535℃热压；
7.如上述6所述的门氧化膜形成用硅化铪靶制造方法，其特征在于，热压在150～2000kgf/cm2下进行。
具体实施方式
具有代替SiO2膜的特性的高介电率门绝缘膜是通过使用HfSi靶，通过氧反应性溅射形成的。该氧化物膜被认为是由HfO2·SiO2表示的氧化物膜的混成体或用氮置换了部分氧的膜，并且通常要求靶的组成为Si/Hf＝1.0。
一般地，尽管要求Hf和Si的组成比是接近目标膜的组成比，但是富Hf的氧化膜倾向于具有高的相对介电常数，富Si的氧化膜与Si基片具有好的相容性，可以容易地成为无定形结构，因此具有漏电流低的特性。
考虑到上面这些，需要根据使用目的考虑和确定介电常数和漏电流的平衡。另外，要求器件的各制造工序具有独特的相容性，并且要求可以根据需要任意变化铪与硅的组成比的材料。
当烧结铪和硅的混合物粉时，根据组成比，形成硅化物相如HfSi相和HfSi2相，和混晶如Hf相和Si相，但一般来说，存在由于这些硅化铪间化合物的熔点高而在烧结时不能得到充分的密度，变成多孔组织的烧结体，并且然后变成粒子的产生多的靶的问题。
并且，如果不根据组成比调整热压条件，即加热温度和压力，则不能得到最佳密度的靶。
通过致力于改良密度的提高，本发明成功地获得了适合作为门氧化膜形成用硅化铪靶的靶。
本发明考虑到介电常数和漏电流的平衡，提供由HfSi1.02-2.00构成的门氧化膜形成用硅化铪靶。该硅化铪靶具有以HfSi相和HfSi2相为主相的混合相，消除了多孔结构，相对密度为95％或更高。
当相对密度低于95％时，由于密度不足而使脆性变差，并且由此加工性也变差。这也引起了由于脆性结晶的破裂和飞散导致的粒子增加。因此，优选相对密度在上述范围内。
优选门氧化膜形成用硅化铪靶中的氧含量为500～10000ppm。当氧少于500ppm时，存在在制造过程中靶发火的可能性，相反，当氧超过10000ppm时，靶中的氧作为氧化物沉积并引起溅射时的异常放电，由此粒子增加，并且结果制品的成品率下降。
另外，优选靶中的锆含量控制在2.5重量％或者更低。当锆含量超过2.5重量％时，工艺条件如用于形成氧化膜的反应性溅射时的电压、电流和基片温度变化很大，这是不优选的。
另外，优选门氧化膜形成用硅化铪靶中的杂质为C：300ppm或更低，Ti：100ppm或更低，Mo：100ppm或更低，W：10ppm或更低，Nb：10ppm或更低，Fe：10ppm或更低，Ni：10ppm或更低，Cr：10ppm或更低，Na：0.1ppm或更低，K：0.1ppm或更低，U：0.01ppm或更低，和Th：0.01ppm或更低。这是因为这些杂质将成为门电极和下部Si基片的污染源。
为制造耐脆性卓越的由HfSi1.02-2.00构成的门氧化膜形成用硅化铪靶，将由HfSi1.02-2.00构成的组合物粉混合，然后在1400℃～1535℃热压。如果温度低于1400℃，密度将不充分，并且如果温度超过1535℃，由于开始产生部分溶解而不优选。
将由HfSi1.02-2.00构成的组合物粉混合时，制备氢化铪粉和Si粉，并以1∶1.02～1∶2.00的摩尔比混合，然后在600℃～800℃烧结。
尽管也可以考虑使用Hf粉，但Hf粉由于具有强的可氧化性，并且当粉碎时存在它可能发火的问题，因此不优选Hf粉。
因此，使用氢化铪以防止这种发火的产生。优选氢化铪粉与Si粉在粉碎到100目或更小时使用。使用这种细粉使得可以实现烧结时的高密度。
通过上述烧结时的加热过程进行脱氢和硅化物生成。脱氢从约600℃开始发生。尽管烧结在真空(1×10-4～1×10-2托)中进行，但由于脱氢而变成轻微的氢气氛。
另外，加热到800℃时脱氢结束，并且可能引起Hf金属发火的部分形成硅化物，或者烧结到不用担心发火的程度(约3μm或更高)。
如上所述，通过加热合成时低温进行脱氢和生成硅化物，可以抑制晶粒生长，烧结粉的一次晶粒保持微细，并且可以在成型时变成高密度。如果烧结粉变成粗粒，烧结前的粉碎变得困难，所以残留粗大粒子，密度下降。
因此，由于低温进行烧结所以产生了晶粒生长可被抑制的显著特性，并且门氧化膜形成用硅化铪靶的平均结晶粒径可以变成5～200μm。从而，烧结时可以实现高密度化。
对于平均结晶粒径低于5μm的靶，难以使氧量成为10000ppm或更低，另外在制造过程中存在发火的担心。另外，当平均结晶粒径超过200μm时，由于粒子增加、制品成品率下降，所以优选如上述将平均结晶粒径设定为5～200μm。
通过合成由上述的HfSi1.02-2.00构成的粉末，并将其在1400℃～1535℃热压，可以实现烧结时的高密度化。
上述的热压温度是合成粉的液相生成直下的温度，并且该温度范围对于烧结是重要的。这使得可以实现相对密度为95％或者更高的高密度硅化铪靶。
本发明的高密度硅化铪靶产生的效果是防止溅射过程中由于细孔引起的粒子产生。
实施例
接下来，说明实施例。另外，这些实施例仅是示例性的，本发明不受这些实施例的限制。换句话说，本发明包括在本发明的技术思想范围内的这些实施例以外的所有形式和变形。
(实施例1)
将100目以下的HfH2粉与100目以下的Si粉混合，通过在真空中、800℃加热，同时进行脱氢反应和硅化物的合成反应，得到了HfSi1.1的合成粉。
将该硅化铪粉粉碎，得到100目以下的硅化铪粉。此时，也可以加入预先合成的硅化铪粉。通过XRD确认该硅化铪粉是由包括HfSi相和HfSi2相的混合相组成的。
通过在1500℃、300kg/cm2×2小时的条件下热压该硅化物粉，得到了密度为99.3％的烧结体。进一步将其进行机械加工，制作了φ300mm×6.35mmt的靶。得到了几乎没有细孔的组织。
用如上制作的靶进行溅射，在测定6英寸晶片上的粒子时，仅发现了尺寸为0.2μm或更大的粒子总计12个，粒子的产生显著减少。
通过以上的方法，得到了加工性、耐脆化性卓越的硅化铪靶。另外，由于该靶可以在湿式加工中使用，因此不再存在对于加工时发火的担心。
(实施例2)
将100目以下的HfH2粉与100目以下的Si粉混合，通过在真空中、800℃加热，同时进行脱氢反应和硅化物的合成反应，得到了HfSi1.5的合成粉。
将该硅化铪粉粉碎，得到100目以下的硅化铪粉。此时，也可以加入预先合成的硅化铪粉。通过XRD确认该硅化铪粉是由包括HfSi相和HfSi2相的混合相组成的。
通过在1420℃、300kg/cm2×2小时的条件下热压该硅化物粉，得到了密度为99.8％的烧结体。进一步将其进行机械加工，制作了φ300mm×6.35mmt的靶。
用如上制作的靶进行溅射，在测定6英寸晶片上的粒子时，仅发现了尺寸为0.2μm或更大的粒子总计18个，粒子的产生显著减少。
通过以上的方法，得到了加工性、耐脆化性卓越的硅化铪靶。另外，不再存在对于加工时发火的担心。
(实施例3)
将100目以下的HfH2粉与100目以下的Si粉混合，通过在真空中、800℃加热，同时进行脱氢反应和硅化物的合成反应，得到了HfSi1.9的合成粉。
将该硅化铪粉粉碎，得到100目以下的硅化铪粉。此时，也可以加入预先合成的硅化铪粉。通过XRD确认该硅化铪粉是由包括HfSi相和HfSi2相的混合相组成的。
通过在1520℃、300kg/cm2×2小时的条件下热压该硅化物粉，得到了密度为98.4％的烧结体。进一步将其进行机械加工，制作了φ300mm×6.35mmt的靶。
用如上制作的靶进行溅射，在测定6英寸晶片上的粒子时，仅发现了尺寸为0.2μm或更大的粒子总计20个，粒子的产生显著减少。
通过以上的方法，得到了加工性、耐脆化性卓越的硅化铪靶。另外，不再存在对于加工时发火的担心。
(比较例1)
将100目以下的HfH2粉与100目以下的Si粉混合，通过在真空中、800℃加热，同时进行脱氢反应和硅化物的合成反应，得到了HfSi1.3的合成粉。将该硅化铪粉粉碎，得到100目以下的硅化铪粉。此时，也可以加入预先合成的硅化铪粉。通过XRD确认该硅化铪粉是由包括HfSi相和HfSi2相的混合相组成的。
通过在1500℃、120kg/cm2×2小时的条件下热压该硅化物粉，得到了烧结体。所得到的烧结体的密度低，为92.7％。进一步将其进行机械加工，制作了φ300mm×6.35mmt的靶。
由于该靶密度低，所以存在贯通孔。因此，制作实际的器件制作中使用的靶时的加工中，由于极难消除加工液的污染，所以不能进行湿式加工。因此，为防止加工粉的发火，必须采取特殊措施，如在惰性气氛中进行干式加工。
用如上制作的靶进行溅射，在测定6英寸晶片上的粒子时，总共发现了尺寸为0.2μm或更大的粒子270个。另外，在靶面的外周上产生了许多称为结节的突起。
如上所述，在本发明的范围以外的高温下烧结时，不能提高密度，这也导致了大量粒子的产生。
(比较例2)
将100目以下的HfH2粉与100目以下的Si粉混合，通过在真空中、800℃加热，同时进行脱氢反应和硅化物的合成反应，得到了HfSi1.3的合成粉。
将该硅化铪粉粉碎，得到100目以下的硅化铪粉。此时，也可以加入预先合成的硅化铪粉。通过XRD确认该硅化铪粉是由包括HfSi相和HfSi2相的混合相组成的。
通过在1380℃、300kg/cm2×2小时的条件下热压该硅化物粉，得到了烧结体。所得到的烧结体的密度低，为90.6％。进一步将其进行机械加工，制作了φ300mm×6.35mmt的靶。
由于该靶密度低，所以存在贯通孔。因此，制作实际的器件制作中使用的靶时的加工中，由于极难消除加工液的污染，所以不能进行湿式加工。因此，为防止加工粉的发火，必须采取特殊措施，如在惰性气氛中进行干式加工。
用如上制作的靶进行溅射，在测定6英寸晶片上的粒子时，总共发现了尺寸为0.2μm或更大的粒子490个。另外，产生了许多结节。
如上所述，在本发明的范围以外的低温下烧结时，不能提高密度，这也导致了大量粒子的产生。
实施例1～3的各靶的相对密度为95％或更高。另外，粒子数为20个或更少。在1400℃～1535℃的热压条件下同样地实现了相对密度的提高。
如上所述，确认了在上述的条件下可以稳定制造Hf∶Si比为1∶1.02～2.00的硅化铪靶，与此同时提高了烧结体的密度。
相反，比较例1的相对密度低，为92.7％。其结果是，产生了粒子数为270个，产生结节的不好结果。
另外，比较例2的相对密度低，为90.6％。其结果是，产生了粒子数为490个，同样地产生了结节的不好结果。
因此，本发明的实施例的优越性是明显的，本发明具有优良的特性也是明显的。
发明的效果
本发明的特征在于，可以得到适合形成可代替SiO2膜作为高介电率门绝缘膜使用的HfSiO和HfSiON膜，加工性和耐脆化性卓越的硅化铪钯。
本发明的硅化铪靶的相对密度为95％或更高，为高密度，具有优良的强度。
另外，本发明的高密度化的硅化物靶能够防止溅射时由细孔引起的粒子产生或脆性组织破坏飞散引起的粒子产生，产生了加工时或者靶的制造过程中不会发火的显著优点。

Claims (7)

1.一种门氧化膜形成用硅化铪靶，其特征在于由HfSix构成，含有主要包括HfSi相和HfSi2相的混合相和相对密度为95％或更高，其中1.02＜x≤2.00。
2.权利要求1所述的门氧化膜形成用硅化铪靶，其特征在于，氧含量为500～10000ppm。
3.权利要求1或2所述的门氧化膜形成用硅化铪靶，其特征在于，锆含量为2.5重量％或更低。
4.权利要求1或2所述的门氧化膜形成用硅化铪靶，其特征在于，杂质为C：300ppm或更低，Ti：100ppm或更低，Mo：100ppm或更低，W：10ppm或更低，Nb：10ppm或更低，Fe：10ppm或更低，Ni：10ppm或更低，Cr：10ppm或更低，Na：0.1ppm或更低，K：0.1ppm或更低，U：0.01ppm或更低和Th：0.01ppm或更低。
5.权利要求1或2所述的门氧化膜形成用硅化铪靶，其特征在于，平均结晶粒径为5～200μm。
6.一种门氧化膜形成用硅化铪靶制造方法，其中该门氧化膜形成用硅化铪靶由HfSix构成，含有主要包括HfSi相和HfSi2相的混合相和相对密度为95％或更高，该方法的特征在于，合成由HfSix构成的粉，将其粉碎到100目或更小，然后在1400℃～1535℃热压，其中1.02＜x≤2.00。
7.权利要求6所述的门氧化膜形成用硅化铪靶制造方法，其特征在于，热压在150～2000kgf/em2下进行。
CNB028117050A 2001-07-18 2002-06-05 门氧化膜形成用硅化铪靶及其制造方法 Expired - Fee Related CN1258211C (zh)

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