CN113165984A - Cr-Si系烧结体 - Google Patents
Cr-Si系烧结体 Download PDFInfo
- Publication number
- CN113165984A CN113165984A CN201980075791.5A CN201980075791A CN113165984A CN 113165984 A CN113165984 A CN 113165984A CN 201980075791 A CN201980075791 A CN 201980075791A CN 113165984 A CN113165984 A CN 113165984A
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- Prior art keywords
- sintered body
- less
- crsi
- powder
- silicon
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- 229910019819 Cr—Si Inorganic materials 0.000 title claims abstract description 25
- 239000011651 chromium Substances 0.000 claims abstract description 42
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 30
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000010703 silicon Substances 0.000 claims abstract description 19
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 17
- 229910021357 chromium silicide Inorganic materials 0.000 claims abstract description 15
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910021359 Chromium(II) silicide Inorganic materials 0.000 claims abstract description 11
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 7
- 229910019974 CrSi Inorganic materials 0.000 claims abstract description 4
- 238000005477 sputtering target Methods 0.000 claims description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 14
- 239000001301 oxygen Substances 0.000 claims description 14
- 229910052760 oxygen Inorganic materials 0.000 claims description 14
- 239000013078 crystal Substances 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 238000004544 sputter deposition Methods 0.000 claims description 6
- 239000010409 thin film Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 description 35
- 238000010304 firing Methods 0.000 description 31
- 239000000843 powder Substances 0.000 description 30
- 238000002844 melting Methods 0.000 description 25
- 230000008018 melting Effects 0.000 description 25
- 239000012535 impurity Substances 0.000 description 15
- 239000002994 raw material Substances 0.000 description 13
- 238000009689 gas atomisation Methods 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 6
- 239000000956 alloy Substances 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- 238000007731 hot pressing Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 229910021332 silicide Inorganic materials 0.000 description 6
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 6
- 238000005259 measurement Methods 0.000 description 5
- 238000005498 polishing Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000005336 cracking Methods 0.000 description 4
- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000013077 target material Substances 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000007751 thermal spraying Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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Abstract
包含硅化铬(CrSi2)、硅(Si)的Cr‑Si系烧结体难以获得高强度。本发明提供一种包含Cr(铬)、硅(Si)的Cr‑Si系烧结体,其特征在于,根据X射线衍射确定的结晶结构由硅化铬(CrSi2)、硅(Si)构成,CrSi2相在块体中存在60wt%以上,烧结体密度为95%以上,CrSi2相的平均粒径为60um以下。
Description
技术领域
本发明涉及一种用于形成薄膜的Cr-Si系烧结体。
背景技术
近年来,如CrSi2这样的硅化物根据其特性而在半导体或太阳能电池等众多的领域被作为薄膜使用。薄膜的制作在工业上大多采用溅射法。但是,已知含有如CrSi2这样的硅化物的组合物通常强度低,在溅射靶材的加工时及成膜的放电时存在破裂的现象,难以用作溅射靶材。因此,在专利文献1中通过热喷涂法来制作Cr、Si的晶相的溅射靶材。但是,在热喷涂法中,在Cr的分布少的部位,强度不能充分提高,另外,使用硅化物相的粉末并通过热喷涂法制作的溅射靶材不能高强度化。
另外,在专利文献2中,通过熔融法制作具有微细的共晶组织的组合物。但是,在熔融法中共晶组织的比例少,在存在大量初生晶的组成中无法实现高强度化。进而,在大型化时,由于冷却速度的不同,结晶组织的控制变得困难,强度的不均变大。
进而,在专利文献3、4中,由于硅化物相脆,所以并未提及含有大量硅化物的体系。
现有技术文献
专利文献
专利文献1:日本特开2017-82314号公报
专利文献2:日本特表2013-502368号公报
专利文献3:日本特开2002-173765号公报
专利文献4:日本特开2003-167324号公报
发明内容
发明所要解决的问题
本发明的目的在于,提供一种包含Cr(铬)、硅(Si)的高强度Cr-Si系烧结体。
用于解决问题的技术方案
本发明人对以化学计量组成计由硅化铬(CrSi2)、硅(Si)构成、且具有特定量以上的CrSi2相的Cr-Si系烧结体的制造工艺进行了深入研究,结果发现,通过使用气雾化粉末等快淬合金粉末,能够获得高强度的Cr-Si系烧结体,从而完成了本发明。
即,本发明具有以下技术方案。
(1)一种Cr-Si系烧结体,是包含Cr(铬)、硅(Si)的Cr-Si系烧结体,其特征在于,根据X射线衍射确定的结晶结构由硅化铬(CrSi2)、硅(Si)构成,CrSi2相在块体(“块体”的日语原文为“バルク”)中存在60wt%以上,烧结体密度为95%以上,CrSi2相的平均粒径为60μm以下。
(2)根据(1)所述的Cr-Si系烧结体,其特征在于,弯曲强度为100MPa以上。
(3)根据(1)或(2)所述的Cr-Si系烧结体,其特征在于,块体中的氧量为1wt%以下。
(4)一种溅射靶材,其特征在于,包含(1)~(3)中任一项所述的Cr-Si系烧结体。
(5)一种薄膜的制造方法,其特征在于,使用(4)所述的溅射靶材进行溅射。
发明效果
本发明的Cr-Si系烧结体具有高强度,在用作溅射靶材的情况下,在高输出下也没有破裂,可得到高的生产性,而且优选氧量少,因此,在成膜时可实现低颗粒化。
附图说明
图1是实施例1和比较例3的X射线衍射图谱。
具体实施方式
以下,详细说明本发明。
本发明提供一种Cr-Si系烧结体,其包含Cr(铬)、硅(Si),其特征在于,根据X射线衍射确定的结晶结构由硅化铬(CrSi2)、硅(Si)构成,CrSi2相在块体中存在60wt%以上,烧结体密度为95%以上,CrSi2相的平均粒径为60μm以下。
本发明的Cr-Si系烧结体的晶相的特征在于,根据XRD,其是包含硅化铬(CrSi2)相、硅(Si)相的体系。如果硅化反应未充分进行而本来在组成上不应存在的其它硅化物相(Cr3Si、Cr5Si3、CrSi)或铬(Cr)相局部存在,则因密度差使得内含微裂纹,特别是在大型的烧结体中容易破裂,不能以高成品率制造烧结体。另外,在使用这种烧结体且通过溅射投入高功率的情况下,在放电过程中容易发生破裂,从而成为使成膜工序的生产性降低的原因,故而不予优选。
本发明的Cr-Si系烧结体的特征在于,CrSi2相在块体中存在60wt%以上。优选为70wt%以上,特别优选为80wt%以上。
本发明的特征在于,Cr-Si系烧结体的烧结体密度以相对密度计为95%以上。如果烧结体密度低于95%,则强度减小。并且,在被用作溅射靶材的情况下,发生打火的频率变高,因此,优选为97%以上,更优选为98%以上。
另外,本发明的特征在于,Cr-Si系烧结体的硅化铬的粒径为60μm以下。如果大于60μm,则强度急剧降低。为了稳定地获得高强度,粒径优选为1μm~60μm,更优选为1μm~20μm,特别优选为1μm~10μm。
从制成膜时的颗粒的产生及膜制品的成品率的观点出发,本发明的Cr-Si系烧结体的块体中的氧量优选为1wt%以下,更优选为0.5wt%以下,进一步优选为0.1wt%以下,更进一步优选为0.05wt%以下。
本发明的Cr-Si系烧结体的弯曲强度优选为100MPa以上,更优选为100MPa~500MPa,进一步优选为150MPa~500MPa,特别优选为200MPa~500MPa。如果烧结体的强度高,则在抛光加工、接合工序中也不易产生破裂,成品率高,因此生产性良好。进而,在溅射过程中投入了高功率的情况下,也不易产生破裂的问题。
本发明的Cr-Si系烧结体可以含有总量为1wt%以下的除Cr(铬)、硅(Si)以外的不可避免的金属杂质,优选为0.5wt%以下、进一步优选为0.05wt%以下、更进一步优选为0.01wt%以下。
作为除Cr(铬)、硅(Si)以外的不可避免的金属杂质,特别是可以含有总量为1wt%以下的Fe、Ni、Al、Mn、Cu等金属杂质,优选为0.5wt%以下、进一步优选为0.05wt%、更进一步优选为0.01wt%以下。
作为各元素,Fe可以含有0.1wt%以下、优选为0.05wt%以下、进一步优选为0.01wt%以下。Ni可以含有0.01wt%以下、优选为0.005wt%以下、进一步优选为0.001wt%以下。Al可以含有0.1wt%以下、优选为0.05wt%以下、进一步优选为0.01wt%以下。Mn可以含有0.005wt%以下、优选为0.001wt%以下、进一步优选为0.005wt%以下。Cu可以含有0.01wt%以下、优选为0.005wt%以下、进一步优选为0.001wt%以下。
接着,对本发明的Cr-Si系烧结体的制造方法进行说明。
本发明的Cr-Si系烧结体的制造方法可包含(1)合金原料调整工序、(2)烧成工序;所述(1)合金原料调整工序中使用铬、硅,利用气雾化法、电弧熔炼法等进行;所述(2)烧成工序中使用热压炉等加压烧成炉,在压力50MPa以下、烧成温度1100℃~1300℃下对所得的原料粉末进行烧成。
以下,关于本发明的Cr-Si系烧结体的制造方法,对每个工序进行说明。
(1)合金原料调整工序
原料使用铬、硅。原料的纯度优选为99.9%以上,更优选为99.99%以上。如果含有大量的杂质,则杂质会成为烧成工序中的异常晶粒生长的原因或成膜时的颗粒的产生源。另外,优选原料的氧量较少。如果原料中的氧量多,则最终溅射靶材中的氧量变多,从而成为颗粒产生的原因。
合成原料粉末可通过气雾化法、电弧熔炼法而制造。
合金原料粉末优选通过气雾化法等快速冷却而制作具有微细组织的粉末。特别是通过气雾化法制作的粒子成为几十μm左右的球状,成为在球状内具有微细的CrSi2相和Si相的粉末。由于表面积小且为微细晶粒,所以可以使烧成后的烧结体为低氧量且高强度。虽然通过微粉混合也可以制作高强度的块体,但氧量变多。相反,如果为粗粒的混合,则虽然可以实现低氧化,但强度变低。作为其它的原料制作方法,有快淬薄带、电弧熔炼等快速冷却的方法。
气雾化法的条件优选设为熔融温度+50~300℃。进一步优选设为+100~250℃。这里,所谓熔融温度表示原料粉末熔融的温度,通常为1300~1500℃。在与熔融温度的差较小的情况下,2相的晶相之中熔点较高的一方先析出,粒子的微细化变得困难。另一方面,在与熔融温度的差较高时,在雾化后粒子彼此烧结,固着于壁面,因此,粉末的回收率变差。
另外,气雾化后的粉末优选在真空中或氮气、氩气等不活泼气氛中进行管理。如果在大气下放置粉末,则从表面开始发生氧化,粉末中的氧量变多。
电弧熔炼法的条件中,电弧的输出功率是重要的。由此,决定了是否能够将熔点差距大的材料合金化。例如在铬和硅的情况下,由于铬的熔点为1863℃,硅的熔点为1414℃,因此需要以50~200A的输出进行熔化。若电弧电流过高,则铬的升华量增加,因此,电弧熔炼的输出优选为50~150A的范围。
(2)烧成工序
接着,优选对所得的粉末使用热压炉等加压烧成炉。在无加压炉中,因为硅的扩散系数低,所以难以进行高密度化。
烧成时的热压压力优选为设为50MPa以下。如果超过50MPa,则难以制备可加压的热压模具。在制作大型的烧结体时,热压压力优选为5~50MPa,进一步优选为5~10MPa,特别优选为5~10MPa。
烧成温度设为1100℃~1300℃。如果低于1100℃,则密度不能充分提高;如果超过1300℃,则根据热压的压力而有可能熔化。另外,降温速度没有特别限定,可考虑烧成炉的容量、烧结体的尺寸及形状、破裂容易度等适当决定
烧成时的保持时间设为1~5小时以内。在短于1小时时,在炉内及热压模具中会产生温度不均,难以获得均匀的组织。反之,在保持时间长时,生产性变差。
作为烧成时的气氛,没有特别限制,优选为真空或氩气等不活泼气氛。
本发明的Cr-Si系烧结体可使用平面磨床、外圆磨床、车床、切割机、加工中心等机械加工机,抛光加工成板状形状。
本发明的Cr-Si系烧结体可制成包含本发明的Cr-Si系烧结体的溅射靶材。作为溅射靶材的制造方法,可根据需要通过使用铟焊料等与含有无氧铜或钛等的背板、背管进行接合(bonding)而获得溅射靶材。
另外,也可以通过使用获得的溅射靶材进行溅射而制造薄膜。
实施例
以下,通过实施例更具体地说明本发明,但本发明不限定于此。需要说明的是,本实施例中的各测定如下进行。
(1)烧结体的密度
关于烧结体的相对密度,根据JIS R 1634通过阿基米得法测定堆积密度,并除以真密度而求出相对密度。烧结体的真密度使用CrSi2相的重量a[g]及Si相的重量b[g]、各自的真密度4.98[g/cm3]、2.3[g/cm3],根据下式表示的算术平均来算出。
d=(a+b)/((a/4.98)+(b/2.3))
(2)X射线衍射试验
测定镜面抛光后的烧结体试样的2θ=20~70°的范围的X射线衍射谱图。
扫描方法:步进扫描法(FT法)
X射线源:Cu Kα
功率:40kV、40mA
步长:0.01°
(3)烧结体粒径
进行镜面抛光,并利用扫描电子显微镜进行观察,根据所得的烧结体组织的照片通过直径法测定烧结体粒径。至少观察任意3点以上,进行300个以上的粒子的测定。
(扫描电子显微镜的观察条件)
加速电压:10kV
(4)弯曲强度
依据JIS R 1601进行测定。
(弯曲强度的测定条件)
试验方法:三点弯曲试验
支点间距离:30mm
试样尺寸:3mm×4mm×40mm
压头速度:0.5mm/分钟。
(5)氧量的分析
对烧成后的烧结体表面抛光1mm以上之后,从任意的部分切出样品,将该样品的分析值作为测定数据。
测定方法:脉冲炉熔融-红外线吸收法
装置:LECO TC436氧·氮分析装置
(6)金属杂质量的分析
对烧成后的烧结体表面抛光1mm以上之后,从任意的部分切出样品,将该样品的分析值作为测定数据。
测定方法:辉光放电质谱(GDMS)
(实施例1)
在碳坩埚内熔化Cr薄片(4N):42wt%、Si薄片(5N):58wt%,将熔融温度设为1650℃,通过气雾化法制作粉末。将粉末在大气下利用筛子(筛孔尺寸:300μm)实施粉末的粒度调整。
接着,将该粉末放入碳模具(53mmφ)中,通过热压法进行烧成,获得烧结体。
(烧成条件)
烧成炉:热压炉
升温速度:200℃/小时
升温气氛:真空减压气氛
烧成温度:1250℃
压力:10MPa
烧成时间:3小时
获得烧结体尺寸为53mmφ×7mmt的无微裂纹的烧结体。烧结体特性示于表1。
(实施例2~5)
除变更烧成条件以外,通过与实施例1同样的方法制作烧结体。烧结体的烧结体特性示于表1。
(实施例6)
在输出100A的条件下通过电弧熔炼法熔化Cr薄片(4N):29wt%、Si薄片(5N):71wt%。将获得的块体利用乳钵粉碎,在实施例3的条件下进行烧成。烧结体的特性示于表1。
(实施例7)
在碳坩埚内熔化Cr薄片(4N):42wt%、Si薄片(5N):58wt%,将熔融温度设为1650℃,通过气雾化法制作粉末。将粉末在手套箱内(氧浓度:0.1wt%以下)利用筛(筛孔尺寸:300μm)实施粉末的粒度调整。
接着,将该粉末放入碳模具(53mmφ)中,通过热压法进行烧成,获得烧结体。
(烧成条件)
烧成炉:热压炉
升温速度:200℃/小时
升温气氛:真空减压气氛
烧成温度:1200℃
压力:20MPa
烧成时间:3小时
获得烧结体尺寸为53mmφ×7mmt的无微裂纹的烧结体。烧结体特性示于表1。
另外,对金属杂质量进行GDMS分析,Cr、Si以外的金属杂质总量为0.034wt%以下,就各种杂质量而言,Fe为0.0066wt%,Ni为0.00082wt%,Al为0.000048wt%,Mn为0.00011wt%,Cu为0.000051wt%。
(实施例8)
在碳坩埚内熔化Cr薄片(4N):29wt%、Si薄片(5N):71wt%,将熔融温度设为1540℃,通过气雾化法制作粉末。将粉末在手套箱内(氧浓度:0.1wt%以下)利用筛(筛孔尺寸:300μm)实施粉末的粒度调整。
接着,将该粉末放入碳模具(53mmφ)中,通过热压法进行烧成,获得烧结体。
(烧成条件)
烧成炉:热压炉
升温速度:200℃/小时
升温气氛:真空减压气氛
烧成温度:1200℃
压力:20MPa
烧成时间:3小时
获得烧结体尺寸为53mmφ×7mmt的无微裂纹的烧结体。烧结体特性示于表1。另外,对金属杂质量进行GDMS分析,Cr、Si以外的金属杂质总量为0.026wt%以下,就各种杂质量而言,Fe为0.0027wt%,Ni为0.00039wt%,Al为0.000022wt%,Mn为0.000041wt%,Cu为0.000012wt%。
(实施例9)
除了变更烧成条件以外,通过与实施例8同样的方法制作烧结体。烧结体的烧结体特性示于表1。
(实施例10)
在碳坩埚内熔化Cr薄片(4N):47wt%、Si薄片(5N):53wt%,将熔融温度设为1540℃,通过气雾化法制作粉末。将粉末在手套箱内(氧浓度:0.1wt%以下)利用筛(筛孔尺寸:300μm)实施粉末的粒度调整。
接着,将该粉末放入碳模具(53mmφ)中,通过热压法进行烧成,获得烧结体。
(烧成条件)
烧成炉:热压炉
升温速度:200℃/小时
升温气氛:真空减压气氛
烧成温度:1200℃
压力:20MPa
烧成时间:3小时
获得烧结体尺寸为53mmφ×7mmt的无微裂纹的烧结体。烧结体特性示于表1。另外,对金属杂质量进行GDMS分析,Cr、Si以外的金属杂质总量为0.03wt%以下,就各种杂质量而言,Fe为0.0062wt%,Ni为0.00078wt%,Al为0.000035wt%,Mn为0.000068wt%,Cu为0.000041wt%。
(实施例11)
除了变更烧成条件以外,通过与实施例10同样的方法制作烧结体。烧结体的烧结体特性示于表1。
(比较例1)
通过电弧熔炼法熔化Cr薄片(4N):42wt%、Si薄片(5N):58wt%。熔化后所得的块体的特性示于表1。
(比较例2)
将比较例1中制作的块体利用乳钵粉碎,通过热压法制作。烧结体特性示于表1。
(比较例3)
通过V型混合法混合Cr粉末(45μm)、Si粉末(9μm),对混合粉末进行热压,制作烧结体。烧结体特性示于表1。
(比较例4)
变更烧成条件,对通过气雾化法制作的粉末进行烧成。烧结体特性示于表1。
(比较例5)
通过电弧熔炼法熔化Cr薄片(4N):29wt%、Si薄片(5N):71wt%。熔化后所得的块体的特性示于表1。
[表1]
以上参照特定的实施方式详细说明了本发明,但本领域技术人员而言可以理解,在不脱离本发明的精神和范围的情况下可以进行各种变更及修正。
此外,本申请基于2018年11月22日申请的日本国专利申请(特愿2018-218832)及2019年06月11日申请的日本国专利申请(特愿2019-108661),其整体通过引用而并入本申请。另外,在此引用的所有参照作为整体被并入本申请。
Claims (5)
1.一种Cr-Si系烧结体,其为包含Cr(铬)、硅(Si)的Cr-Si系烧结体,其特征在于,根据X射线衍射确定的结晶结构由硅化铬(CrSi2)、硅(Si)构成,CrSi2相在块体中存在60wt%以上,烧结体密度为95%以上,CrSi2相的平均粒径为60μm以下。
2.根据权利要求1所述的Cr-Si系烧结体,其特征在于,弯曲强度为100MPa以上。
3.根据权利要求1或2所述的Cr-Si系烧结体,其特征在于,块体中的氧量为1wt%以下。
4.一种溅射靶材,其特征在于,包含权利要求1~3中任一项所述的Cr-Si系烧结体。
5.一种薄膜的制造方法,其特征在于,使用权利要求4所述的溅射靶材进行溅射。
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JP2018218832 | 2018-11-22 | ||
JP2019108661 | 2019-06-11 | ||
JP2019-108661 | 2019-06-11 | ||
PCT/JP2019/045113 WO2020105591A1 (ja) | 2018-11-22 | 2019-11-18 | Cr-Si系焼結体 |
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US20230121940A1 (en) * | 2020-03-26 | 2023-04-20 | Tosoh Corporation | Cr-si sintered body, sputtering target, and method for producing thin film |
CN115666820A (zh) * | 2020-05-26 | 2023-01-31 | 东曹株式会社 | 金属-Si系粉末、其制造方法、以及金属-Si系烧结体、溅射靶和金属-Si系薄膜的制造方法 |
EP4190762A1 (en) * | 2020-07-31 | 2023-06-07 | Tosoh Corporation | Cr-si-c-based sintered body |
CN112376023A (zh) * | 2020-11-04 | 2021-02-19 | 宁波江丰电子材料股份有限公司 | 一种铬硅合金溅射靶材的制备方法 |
KR20230132862A (ko) * | 2021-03-29 | 2023-09-18 | 도소 가부시키가이샤 | Cr-Si 계 막 |
JP7394085B2 (ja) * | 2021-04-05 | 2023-12-07 | Jx金属株式会社 | スパッタリングターゲット及びその製造方法 |
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