CN113667944A - Mn-Zn-O系溅射靶及其制备方法 - Google Patents
Mn-Zn-O系溅射靶及其制备方法 Download PDFInfo
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- CN113667944A CN113667944A CN202110716455.3A CN202110716455A CN113667944A CN 113667944 A CN113667944 A CN 113667944A CN 202110716455 A CN202110716455 A CN 202110716455A CN 113667944 A CN113667944 A CN 113667944A
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- 238000005477 sputtering target Methods 0.000 title claims abstract description 63
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- 229910052725 zinc Inorganic materials 0.000 claims abstract description 14
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 53
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 37
- 239000011572 manganese Substances 0.000 claims description 30
- 229910052751 metal Inorganic materials 0.000 claims description 27
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 26
- 238000005245 sintering Methods 0.000 claims description 25
- 239000011701 zinc Substances 0.000 claims description 25
- 239000002184 metal Substances 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 21
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- 229910052715 tantalum Inorganic materials 0.000 claims description 10
- 229910052720 vanadium Inorganic materials 0.000 claims description 10
- 229910052771 Terbium Inorganic materials 0.000 claims description 9
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- 229910052749 magnesium Inorganic materials 0.000 claims description 9
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- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
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- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(III) oxide Inorganic materials O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 2
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- 238000005303 weighing Methods 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
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- DLINORNFHVEIFE-UHFFFAOYSA-N hydrogen peroxide;zinc Chemical compound [Zn].OO DLINORNFHVEIFE-UHFFFAOYSA-N 0.000 description 1
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- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910000471 manganese heptoxide Inorganic materials 0.000 description 1
- 229910000473 manganese(VI) oxide Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
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- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- HBEQXAKJSGXAIQ-UHFFFAOYSA-N oxopalladium Chemical compound [Pd]=O HBEQXAKJSGXAIQ-UHFFFAOYSA-N 0.000 description 1
- 229910003445 palladium oxide Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
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- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 239000012856 weighed raw material Substances 0.000 description 1
- 229940105296 zinc peroxide Drugs 0.000 description 1
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Abstract
本发明提供可供于DC溅射的Mn‑Zn‑O系溅射靶及其制备方法。本发明的Mn‑Zn‑O系溅射靶的特征在于,在成分组成中含有Mn、Zn、O和元素X,其中,X为选自W和Mo的单独1种元素或2种元素,上述靶的被溅射面的算术平均粗糙度Ra为1.5μm以下、或最大高度Ry为10μm以下。
Description
本申请是申请日为2017年7月11日,申请号为201780042540.8 (PCT/JP2017/025276),发明名称为“Mn-Zn-O系溅射靶及其制备方法”的发明专利申请的分案申请。
技术领域
本发明涉及Mn-Zn-O系溅射靶及其制备方法,特别是涉及适合供于形成光信息记录介质的记录层的、在成分组成中含有元素X (X为W或Mo)的Mn-Zn-O系溅射靶及其制备方法。
背景技术
使Ar离子等与包含合金或烧结体的溅射靶碰撞的溅射法在玻璃涂层、半导体元件制备、平板显示器制备、光信息记录介质(记录型光盘)的记录层形成等广泛的技术领域中得到实施。
这些之中,例如在光信息记录介质的技术领域,随着处理的数据的增大,越发需要大容量化。在这里,光信息记录介质大致分为只读和记录型,其中记录型可分为一次性写入型和可重写型这2种类型。作为一次性写入型光盘的记录层材料,以往广泛研究有机色素材料,但随着近年来的大容量化,无机材料也得到广泛研究。
目前,作为一次性写入型光盘的无机系记录层材料,实际应用钯氧化物系材料。但是,由于Pd为稀有金属,所以材料成本高。因此,作为以廉价的材料成本得到充分良好的记录特性的材料,开发了锰氧化物系材料。
作为包含这样的锰氧化物系材料的记录层,在专利文献1中提出了含有Mn的氧化物和金属Ma (其中,金属Ma选自Mg、Mo、Si和Te)的氧化物,并进一步含有金属M (选自Sn、Zn、Bi等)的Mn-Zn-Ma-O系记录层。而且,作为将上述Mn-Zn-Ma-O系记录层成膜的具体方法,专利文献1公开了共溅射(多元溅射)法。通过使用专利文献1所述的技术,可不使用作为稀有金属的Pd,而实现材料:Mn-Zn-Ma-O系记录层。
现有技术文献
专利文献
专利文献1:国际公开第2013/183277号。
发明内容
发明所要解决的课题
在这里,如包含上述材料的Mn-Zn-Ma-O系记录层,作为用溅射法形成含有多种元素的层的方法之一,如专利文献1所公开,可列举出溅射包含各自元素的多个靶的多元溅射法。作为其它的方法,可列举出将含有多种元素的1张复合靶作为单一靶来溅射的方法。在这里,多元溅射法不仅有装置大型化而导致成本上升的因素,而且有易产生组成偏差的缺点。因此,以量产化的观点,优选使用1张复合靶,且使用DC (直流)溅射法。
作为信息记录介质制作用溅射靶,上述专利文献1提出了含有Mn的氧化物,且上述Mn的氧化物的一部分或全部以Mn的价数低于+4的氧化物状态存在的靶。在专利文献1中,进一步提出了在该靶中以上述氧化物状态存在的Mn的氧化物优选为不会热分解的Mn3O4。另外,也提出了该靶可进一步含有Mn以外的金属或该金属的氧化物,上述金属为选自Sn、Zn、Bi、Ge、Co、W、Cu和Al的1种以上。此外,还提出了可添加Zr、Al、Ta、Mo、Si、Mg、Hf、V、Ti、Sb和Te中的任意的金属元素。
但是,专利文献1并未提及具体的Mn-Zn-O系复合溅射靶。到目前为止尚未确立在成分组成中含有Mn、Zn、元素X (其中,X为W或Mo)和O的Mn-Zn-O系的复合溅射靶。
因此,本发明的目的在于,提供含有元素X (其中,X为W或Mo)的Mn-Zn-O系溅射靶及其制备方法。
用于解决课题的手段
本发明人为达成上述诸多目的而进行了深入研究,以氧化锰粉末、氧化锌粉末、氧化钨粉末作为原料,尝试了制作Mn-Zn-W-O系溅射靶。另外,在上述Mn-Zn-W-O系溅射靶中,代替氧化钨粉末,以氧化钼粉末作为原料,还尝试了制作Mn-Zn-Mo-O系溅射靶。在将这些溅射靶供于DC溅射时,明确了会发生异常放电(也称为“电弧放电(arcing)”)。因此,将原料全部更换为上述元素的金属粉末,分别尝试了制作Mn-Zn-W-O系溅射靶和Mn-Zn-Mo-O系溅射靶。但是,由于金属锌的熔点比氧化锌低,所以可知溅射靶的制作本身是困难的。
因此,本发明人考虑将氧化物粉末和金属粉末组合作为原料粉末来制作Mn-Zn-O系溅射靶,本发明人发现,通过使得到的靶的被溅射面的算术平均粗糙度Ra为1.5μm以下、或使最大高度Ry为10μm以下,即使供于DC溅射,也不产生异常放电,从而完成了本发明。
本发明是基于本发明人的上述见解而成的,作为用于解决上述诸多课题的手段,如下所述。即,
<1> 溅射靶,其是在成分组成中含有Mn、Zn、O和元素X的Mn-Zn-O系溅射靶,其中,X为选自W和Mo的单独1种元素或2种元素,其特征在于,
上述靶的被溅射面的算术平均粗糙度为1.5μm以下、或最大高度Ry为10μm以下。
该<1>所述的Mn-Zn-O系溅射靶为可供于DC溅射的Mn-Zn-O系溅射靶。而且,根据该<1>所述的Mn-Zn-O系溅射靶,可不产生异常放电而进行DC溅射。
<2> 上述<1>所述的溅射靶,其中,相对于Mn、Zn和上述元素X的总计100原子%,Mn为4~40原子%,Zn为15~60原子%,上述元素X为5~40原子%。
<3> 上述<1>或<2>所述的溅射靶,其中,在上述成分组成中进一步含有选自Cu、Mg、Ag、Ru、Ni、Zr、Sn、Bi、Ge、Co、Al、In、Pd、Ga、Te、V、Si、Ta、Cr、Tb的单独1种元素或2种以上元素。
<4> 上述<3>所记载的溅射靶,其中,在上述溅射靶的构成元素中,相对于除去O以外的总计100原子%,上述选自Cu、Mg、Ag、Ru、Ni、Zr、Sn、Bi、Ge、Co、Al、In、Pd、Ga、Te、V、Si、Ta、Cr、Tb的单独1种元素或2种以上元素的含量为8~70原子%。
<5> 制备方法,其是制备上述<1>所述的Mn-Zn-O系溅射靶的方法,其特征在于,包括:
混合工序,其是将锰氧化物粉末、锌氧化物粉末、和以上述元素X作为成分含有的金属粉末湿式混合12小时以上,
烧结工序,其是在该混合工序后在700℃以上的温度下烧结上述混合粉末,和
精加工工序,其是在该烧结工序后使上述靶的被溅射面变得平滑。
根据该<5>所述的制备方法,可制备能够供于DC溅射的Mn-Zn-O系溅射靶。而且,利用通过该<5>所述的方法制备的Mn-Zn-O系溅射靶,可不产生异常放电而进行DC溅射。
<6> 上述<5>所述的制备方法,其中,上述混合粉末进一步含有包含选自Cu、Mg、Ag、Ru、Ni、Zr、Sn、Bi、Ge、Co、Al、In、Pd、Ga、Te、V、Si、Ta、Cr、Tb的单独1种元素或2种以上元素的单体或化合物的粉末。
发明效果
根据本发明,可解决以往的上述诸多问题,而达成上述目的,可提供能够供于DC溅射的Mn-Zn-O系溅射靶及其制备方法。
附图简述
[图1]是用于说明本发明的一个实施方式的溅射靶的制备方法的流程图。
具体实施方式
(Mn-Zn-O系溅射靶)
本发明的Mn-Zn-O系溅射靶为在成分组成中含有Mn、Zn、元素X和O的Mn-Zn-O系溅射靶。以下,将本发明的Mn-Zn-O系溅射靶简称为“靶”,详细地说明本发明的靶。需说明的是,元素X为选自W和Mo的单独1种元素或2种元素,以下,简记为“(元素) X为W或Mo”。
<靶>
本发明的一个实施方式的靶在成分组成中含有Mn、Zn、元素X和O,此外根据需要含有其它的成分组成。
<<元素X>>
如上所述,元素X为W或Mo。即,元素X可包含单独1种W,元素X可包含单独1种Mo。另外,元素X也可包含W和Mo这2种元素。在这里,元素X包含W和Mo这2种元素是指在靶的成分组成中同时含有W和Mo。
<<算术平均粗糙度Ra和平均高度Ry>>
本实施方式的靶,重要的是其被溅射面的算术平均粗糙度Ra为1.5μm以下、或最大高度Ry为10μm以下。如下述实施例所示,本发明人的研究结果明确了,如果靶的被溅射面的算术平均粗糙度Ra为1.5μm以下、或最大高度Ry为10μm以下,则在DC溅射时不会产生异常放电。
需说明的是,在本发明中“算术平均粗糙度Ra”是指基于JIS B0601 (1994)的算术平均粗糙度(Ra) (单位:μm)。另外,在本发明中“最大高度(Ry)”是指基于JIS B0601(1994)的最大高度(Ry) (单位:μm)。
如上所述,本实施方式的溅射靶为可供于DC溅射的Mn-Zn-O系溅射靶,可不产生异常放电而进行DC溅射。另外,本实施方式的靶特别适合供于形成光信息记录介质的记录层,但用途无任何限定。
<<成分比>>
在这里,作为本实施方式的靶的成分比,无特殊限制,可根据目的适宜选择,相对于Mn、Zn和元素X的总计100原子%,可设为Mn:4~40原子%、Zn:15~60原子%、元素X:5~40原子%。
<<其它成分>>
在本实施方式的靶中,可根据需要进一步含有其它的金属元素。通过适宜含有这些金属元素,在将本实施方式的靶供于形成例如信息记录介质的记录层的情况下,可改变记录层的透过率、反射率和记录灵敏度,制成多层结构的记录层。为了该目的,本实施方式的靶优选在成分组成中进一步含有选自Cu、Mg、Ag、Ru、Ni、Zr、Sn、Bi、Ge、Co、Al、In、Pd、Ga、Te、V、Si、Ta、Cr、Tb的单独1种元素或2种以上元素。
-其它成分的成分比-
在溅射靶的构成元素中,相对于除去O (氧)以外的总计100原子%,上述选自Cu、Mg、Ag、Ru、Ni、Zr、Sn、Bi、Ge、Co、Al、In、Pd、Ga、Te、V、Si、Ta、Cr、Tb的单独1种元素或2种以上元素的含量可设为8~70原子%,可在该范围内根据用途适宜选择。
需说明的是,本实施方式的靶的形状无任何限定,可制成圆盘状、圆筒状、四边形板状、长方形板状、正方形板状等任意的形状,可根据靶的用途适宜选择。另外,对于靶的宽度和深度的大小(在圆形的情况下为直径),也可在毫米(mm)级~米(m)级程度的范围内,根据靶的用途适宜选择。例如在靶为圆形的情况下,通常直径为50mm~300mm左右。对于厚度也是相同的,通常为1mm~20mm左右。
<溅射靶的制备方法>
接着,使用图1,说明上述本发明的一个实施方式的靶的制备方法。本发明的一个实施方式的靶的制备方法包括混合工序(S10)、烧结工序(S20)和精加工工序(S30),此外包括根据需要适宜选择的其它工序。
<<混合工序(S10)>>
混合工序(S10)是将以下混合粉末湿式混合12小时以上的工序,所述混合粉末含有锰氧化物粉末、锌氧化物粉末、和以元素X作为成分含有的金属粉末。
作为湿式混合的方法,无特殊限制,可根据目的适宜选择,例如可列举出使用以往公知的球磨装置的湿式混合方法等。以下说明在本工序中混合的混合粉末和混合条件。
混合粉末包含锰氧化物粉末、锌氧化物粉末、和以元素X作为成分含有的金属粉末,可根据需要含有其它的粉末。
-锰氧化物粉末-
作为锰氧化物粉末,可根据目的适宜选择,除了Mn3O4 (氧化锰(二价、三价))和Mn2O3 (氧化锰(三价))以外,还可使用MnO、MnO2、MnO3和Mn2O7等Mn3O4、Mn2O3等。这些可单独使用1种或组合使用2种以上。
这些之中,更优选Mn3O4粉末。这是由于烧结温度与熔点的关系的缘故。
需说明的是,作为锰氧化物粉末的平均粒径,可根据目的适宜选择。作为Mn3O4粉末的平均粒径,可设为市售的3μm~7μm左右。
-锌氧化物粉末-
作为锌氧化物粉末,可根据目的适宜选择,例如可列举出氧化锌(ZnO)粉末、过氧化锌(ZnO2)粉末等。这些可单独使用1种或组合使用2种以上。
这些之中,更优选ZnO粉末。这是由于烧结温度与熔点的关系的缘故。
需说明的是,作为锌氧化物粉末的平均粒径,可根据目的适宜选择。另外,作为ZnO粉末的平均粒径,可设为市售的1μm~3μm左右。
-以元素X作为成分含有的金属粉末-
作为以元素X作为成分含有的金属粉末,可根据目的适宜选择,例如可列举出包含W的单体的金属钨粉末、包含Mo的单体的金属钼粉末等。这些可单独使用1种或组合使用2种以上。在X为W和Mo的情况下,同时使用金属钨粉末和金属钼粉末。
需说明的是,作为以元素X作为成分含有的金属粉末的平均粒径,可根据目的适宜选择。作为金属钨粉末的平均粒径,可设为市售的2μm~5μm左右。另外,作为金属钼粉末的平均粒径,可设为市售的1μm~5μm左右。
-其它粉末-
作为其它粉末,可根据目的适宜选择,例如可列举出包含选自Cu、Mg、Ag、Ru、Ni、Zr、Sn、Bi、Ge、Co、Al、In、Pd、Ga、Te、V、Si、Ta、Cr、Tb的单独1种元素或2种以上元素的单体或化合物的粉末等。在这里,可根据制备的靶的所期望的目的,在混合粉末中含有所述的粉末。
-混合时间-
在这里,在本实施方式中重要的是将混合粉末湿式混合12小时以上。由于通过将混合时间设为12小时以上,可充分地将混合粉末混合,所以可促进烧结中的氧化锰的固相反应,抑制烧结后的氧化锰结晶相的残留。另外,在上述范围中,优选将混合时间设为16小时以上,更优选设为20小时以上,最优选设为24小时以上。若混合24小时,则混合的效果饱和,但也可混合24小时以上,虽然未设计上限,但考虑工业上的生产能力,可将上限设定为168小时。
<<烧结工序(S20)>>
烧结工序(S20)是在混合工序(S10)后进行的工序,是在700℃以上的温度下烧结混合粉末的烧结工序。
-烧结-
作为烧结方法,无特殊限制,可根据目的适宜选择,例如可列举出惰性气体气氛中的热压、热等静压加压法(HIP法:Hot Isostatic Pressing)等。
在这里,在本实施方式中重要的是在700℃以上的温度下烧结混合粉末。通过将烧结温度设为700℃以上,可抑制烧结后的氧化锰结晶相的残留。
需说明的是,烧结时间无特殊限定,可适宜选择,只要设为通常实施的1小时~6小时左右的烧结时间即可。
<<精加工工序(S30)>>
精加工工序(S30)是在烧结工序(S20)后进行的工序,是使靶的被溅射面变得平滑的工序。
上述精加工工序可使用平面磨削机来进行。具体而言,使用金刚石磨石或砂粒磨石,进行磨削。然后,用SCOTCHBRITE (注册商标)等研磨用垫进行精加工,使靶的被溅射面变得平滑。
经过以上的工序,可制备靶的被溅射面的算术平均粗糙度Ra为1.5μm以下、或最大高度Ry为10μm以下的Mn-Zn-O系溅射靶。
<<其它工序>>
作为其它工序,无特殊限制,可根据目的适宜选择,例如可列举出混合粉末的成型工序等。
-成型工序-
需说明的是,上述混合粉末的成型工序在本发明中不是必不可少的,有时为了成型靶的形状而实施。
实施例1
以下,使用实施例来更详细地说明本发明,但本发明绝不限定于以下的实施例,可在不偏离本发明的宗旨的范围内加入各种的变更。
如下所述,使用W作为元素X,制作实施例1-1~1-2作为本发明的靶,制作比较例1-1~1-2作为对照用靶,评价了异常放电的次数。
(实施例1-1)
作为原料粉末,准备了以下的粉末。
纯度:99.9%以上,平均粒径:5μm,Mn3O4粉末
纯度:99.9%以上,平均粒径:1.4μm,ZnO粉末
纯度:99.9%以上,平均粒径:2μm,W粉末
称量上述Mn3O4粉末、ZnO粉末和W粉末,使得各种金属元素的比例为Mn:Zn:W=20:50:30 (原子%)。将秤量的各种原料粉末、各种原料粉末的总计重量3倍的氧化锆球(直径为5mm)和乙醇放入聚乙烯容器中,用球磨装置,进行了24小时的湿式混合。在将混合粉末干燥后,过筛孔为500μm的筛子。接着,在烧结温度:900℃、烧结时间:2小时、压力:200kgf/cm2、惰性气体气氛中进行了热压。接着,利用平面磨削机将通过煅烧得到的靶的表面进行了精加工,使得算术平均粗糙度Ra为0.5μm、最大高度Ry为4μm。在这里,上述算术平均粗糙度Ra和最大高度Ry的值是使用东京精密株式会社制Surfcom 480A测定而得的值。最后,在无氧铜制的背板上用In焊料进行焊接(bonding),制作了实施例1-1所涉及的靶。
(实施例1-2)
与实施例1-1相同地制作了靶。其中,靶的被溅射面的精加工通过变更砂粒尺寸,使得表面的算术平均粗糙度Ra为1.5μm、最大高度Ry为10μm来进行,制作了实施例1-2所涉及的靶。其它的条件与实施例1-1完全相同。
(比较例1-1)
与实施例1-1相同地制作了靶。其中,靶的被溅射面的精加工通过变更砂粒尺寸,使得表面的算术平均粗糙度Ra为1.6μm、最大高度Ry为12μm来进行,制作了比较例1-1所涉及的靶。其它的条件与实施例1-1完全相同。
(比较例1-2)
与实施例1-1相同地制作了靶。其中,靶的被溅射面的精加工通过变更砂粒尺寸,使得表面的算术平均粗糙度Ra为1.6μm、最大高度Ry为12μm来进行,制作了比较例1-2所涉及的靶。其它的条件与实施例1-1完全相同。
<异常放电的发生次数的评价>
对于以上的实施例1-1~1-2和比较例1-1~1-2所涉及的靶,进行了异常放电的发生次数的评价。具体而言,将实施例1-1~1-2和比较例1-1~1-2所涉及的靶安装在溅射装置上,分别进行了DC溅射。即,将溅射装置内真空排气至1×10-4Pa以下,导入Ar气和O2气,将装置内压力设为0.3Pa。氧的分压([O2]/[Ar+O2])设为70%。用DC电源施加5W/cm2的电流,进行30分钟的溅射,利用电弧计数器测量了溅射中的异常放电的发生次数。需说明的是,刚放电后的异常放电排除在外。将得到的结果示出于表1中。
[表1]
靶 | 算术平均粗糙度Ra (μm) | 最大高度Ry (μm) | 异常放电发生次数 |
实施例1-1 | 0.5 | 4.0 | 0 |
实施例1-2 | 1.5 | 10.0 | 0 |
比较例1-1 | 1.6 | 12.0 | 30 |
比较例1-2 | 2.0 | 20.0 | 80 |
由表1可知,在元素X为W的情况下,满足靶的被溅射面的算术平均粗糙度Ra为1.5μm以下或最大高度Ry为10μm以下的实施例1-1、1-2所涉及的靶,发生异常放电的次数为0次,可不发生异常放电而进行溅射。与之相对的是,在靶的被溅射面的算术平均粗糙度Ra超过1.5μm或最大高度Ry超过10μm的比较例1-1和1-2的情况下,可知异常放电至少发生30次。
实施例2
如下所述,使用Mo作为元素X,制作实施例2-1~2-2作为本发明的靶,制作比较例2-1~2-2作为对照用的靶,评价了有无异常放电。
(实施例2-1)
作为原料粉末,准备了以下的粉末。
纯度:99.9%以上,平均粒径:5μm,Mn3O4粉末
纯度:99.9%以上,平均粒径:1.4μm,ZnO粉末
纯度:99.9%以上,平均粒径:2μm,Mo粉末
称量上述Mn3O4粉末、ZnO粉末和W粉末,使得各种金属元素的比例为Mn:Zn:Mo=20:50:30 (原子%)。将称量的各种原料粉末、各种原料粉末的总计重量3倍的氧化锆球(直径为5mm)和乙醇放入聚乙烯容器中,用球磨装置,进行了24小时的湿式混合。在将混合粉末干燥后,过筛孔为500μm的筛子。接着,在烧结温度:900℃、烧结时间:2小时、压力:200kgf/cm2、惰性气体气氛中进行了热压。接着,利用平面磨削机将通过煅烧得到的靶的表面进行了精加工,使得算术平均粗糙度Ra为0.5μm、最大高度Ry为4μm。在这里,上述算术平均粗糙度Ra和最大高度Ry使用东京精密株式会社制Surfcom 480A进行测定。最后,在无氧铜制的背板上用In焊料进行焊接(bonding),制作了实施例2-1所涉及的靶。
(实施例2-2)
与实施例2-1相同地制作了靶。其中,靶的被溅射面的精加工通过变更砂粒尺寸,使得表面的算术平均粗糙度Ra为1.5μm、最大高度Ry为10μm来进行,制作了实施例2-2所涉及的靶。其它的条件与实施例2-1完全相同。
(比较例2-1)
与实施例2-1相同地制作了靶。其中,靶的被溅射面的精加工通过变更砂粒尺寸,使得表面的算术平均粗糙度Ra为1.6μm、最大高度Ry为12μm来进行,制作了比较例2-1所涉及的靶。其它的条件与实施例2-1完全相同。
(比较例2-2)
与实施例2-1相同地制作了靶。其中,靶的被溅射面的精加工通过变更砂粒尺寸,使得表面的算术平均粗糙度Ra为1.6μm、最大高度Ry为12μm来进行,制作了比较例2-2所涉及的靶。其它的条件与实施例2-1完全相同。
<异常放电的发生次数的评价>
对于以上的实施例2-1~2-2和比较例2-1~2-2所涉及的靶,进行了异常放电的发生次数的评价。具体而言,将实施例2-1~2-2和比较例2-1~2-2所涉及的靶安装在溅射装置上,分别进行了DC溅射。即,将溅射装置内真空排气至1×10-4Pa以下,导入Ar气和O2气,将装置内压力设为0.3Pa。氧的分压([O2]/[Ar+O2])设为70%。用DC电源施加5W/cm2的电流,进行30分钟的溅射,利用电弧计数器测量了溅射中的异常放电的发生次数。需说明的是,刚放电后的异常放电排除在外。将得到的结果示出于表2中。
[表2]
靶 | 算术平均粗糙度Ra (μm) | 最大高度Ry (μm) | 异常放电发生次数 |
实施例2-1 | 0.5 | 4.0 | 0 |
实施例2-2 | 1.5 | 10.0 | 0 |
比较例2-1 | 1.6 | 12.0 | 20 |
比较例2-2 | 2.0 | 20.0 | 70 |
由表2可知,在元素X为W的情况下,满足靶的被溅射面的算术平均粗糙度Ra为1.5μm以下或最大高度Ry为10μm以下的实施例2-1、2-2所涉及的靶,发生异常放电的次数为0次,可不发生异常放电而进行溅射。与之相对的是,在靶的被溅射面的算术平均粗糙度Ra超过1.5μm或最大高度Ry超过10μm的比较例2-1、2-2的情况下,可知异常放电至少发生20次。
产业上的可利用性
根据本发明,可提供特别适合供于形成光信息记录介质的记录层的、可供于DC溅射的Mn-Zn-O系溅射靶及其制备方法。
符号说明
S10···混合工序;
S20···烧结工序;
S30···精加工工序。
Claims (6)
1.溅射靶,其是在成分组成中含有Mn、Zn、O和元素X的Mn-Zn-O系溅射靶,其中,X为选自W和Mo的单独1种元素或2种元素,其特征在于,
上述靶的被溅射面的算术平均粗糙度Ra为1.5μm以下、或最大高度Ry为10μm以下。
2.权利要求1所述的溅射靶,其中,相对于Mn、Zn和上述元素X的总计100原子%,Mn为4~40原子%,Zn为15~60原子%,上述元素X为5~40原子%。
3.权利要求1或2所述的溅射靶,其中,在上述成分组成中进一步含有选自Cu、Mg、Ag、Ru、Ni、Zr、Sn、Bi、Ge、Co、Al、In、Pd、Ga、Te、V、Si、Ta、Cr、Tb的单独1种元素或2种以上元素。
4.权利要求3所述的溅射靶,其中,在上述溅射靶的构成元素中,相对于除去O以外的总计100原子%,上述选自Cu、Mg、Ag、Ru、Ni、Zr、Sn、Bi、Ge、Co、Al、In、Pd、Ga、Te、V、Si、Ta、Cr、Tb的单独1种元素或2种以上元素的含量为8~70原子%。
5.溅射靶的制备方法,其是制备权利要求1所述的Mn-Zn-O系溅射靶的方法,其特征在于,包括:
混合工序,其是将以下混合粉末湿式混合12小时以上,所述混合粉末包含锰氧化物粉末、锌氧化物粉末、和以上述元素X作为成分含有的金属粉末,
烧结工序,其是在该混合工序后在700℃以上的温度下烧结上述混合粉末,和
精加工工序,其是在该烧结工序后使上述靶的被溅射面变得平滑。
6.权利要求5所述的溅射靶的制备方法,其中,上述混合粉末进一步含有包含选自Cu、Mg、Ag、Ru、Ni、Zr、Sn、Bi、Ge、Co、Al、In、Pd、Ga、Te、V、Si、Ta、Cr、Tb的单独1种元素或2种以上元素的单体或化合物的粉末。
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