CN102639748A - 清洁气体 - Google Patents
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- 238000004140 cleaning Methods 0.000 title abstract description 17
- 150000001875 compounds Chemical class 0.000 claims abstract description 14
- 229910052702 rhenium Inorganic materials 0.000 claims abstract description 13
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 8
- 229910052732 germanium Inorganic materials 0.000 claims abstract description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 7
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 6
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 6
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- 229910052741 iridium Inorganic materials 0.000 claims abstract description 6
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 6
- 229910052762 osmium Inorganic materials 0.000 claims abstract description 6
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- DCEPGADSNJKOJK-UHFFFAOYSA-N 2,2,2-trifluoroacetyl fluoride Chemical compound FC(=O)C(F)(F)F DCEPGADSNJKOJK-UHFFFAOYSA-N 0.000 description 2
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- 238000004057 DFT-B3LYP calculation Methods 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
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- 238000009835 boiling Methods 0.000 description 1
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- PBWZKZYHONABLN-UHFFFAOYSA-N difluoroacetic acid Chemical compound OC(=O)C(F)F PBWZKZYHONABLN-UHFFFAOYSA-N 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
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- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
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- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
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- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4405—Cleaning of reactor or parts inside the reactor by using reactive gases
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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Abstract
本发明公开的是包含CHF2COF而成的用于去除堆积物的清洁气体。该清洁气体可包含O2、O3、CO、CO2、F2、NF3、Cl2、Br2、I2、XFn(式中,X表示Cl、I或者Br,n表示1≤n≤7的整数。)、CH4、CH3F、CH2F2、CHF3、N2、He、Ar、Ne、Kr等,可适用于包含W、Ti、Mo、Re、Ge、P、Si、V、Nb、Ta、Se、Te、Mo、Re、Os、Ir、Sb、Ge、Au、Ag、As、Cr及其化合物等的堆积物。该清洁气体不仅清洁性能优异,且容易获取,实质上不副产对环境造成负担的CF4。
Description
技术领域
本发明涉及一种清洁气体,其用于去除在使用化学气相沉积法(CVD法)、金属有机物化学气相沉积法(MO CVD)(metalorganic chemical vapour deposition)、溅射法、溶胶凝胶法、蒸镀法等方法制造薄膜、厚膜、粉末、晶须等时堆积于装置内壁、夹具、配管等上的不需要的堆积物。
背景技术
在半导体薄膜器件制造工艺、光学器件制造工艺、超钢材料制造工艺中,使用CVD法、溅射法、溶胶凝胶法、蒸镀法等方法制造各种薄膜、厚膜、粉末、晶须等。此时,不应该是膜、晶须、粉末的堆积部位的反应器内壁或保持物品的夹具等也会生成堆积物。若生成这种不需要的堆积物,则会成为微粒发生的原因,使制造优质的膜、颗粒、晶须变得困难,因此必须随时去除。
以往,为了去除这种不需要的堆积物,使用了CF4、C2F6、C3F8等全氟化碳(PFC)的清洁气体。但是,存在以下问题:这些气体由于在环境中长时间稳定地存在,因此全球变暖潜能值被评价较高,对环境造成不良影响。例如,根据第4次IPCC报告书,它们的GWP(全球变暖潜能值Global Warming Potential)(100年值)中,CF4:7390、C2F6:12200、C3F8:8830。
进而,C2F6、C3F8等具有CF3基的部分结构的清洁气体在堆积室(腔室)内产生CF3自由基、离子等活性种,从而发挥清洁效果,但CF3活性种与F自由基、离子的F活性种接触时会再结合而副产CF4。根据环境省地球环境局环境保全对策课氟利昂等对策推进室发行(平成21年3月发行)的PFC破坏处理指导原则的记载,CF4为环境中最难分解的PFC,仅用与其他氟利昂类的破坏处理同等的条件可能无法进行充分的破坏处理。
作为替代这些PF C的、全球变暖潜能值低的含氟清洁气体,提出了COF2、CHF2OF(专利文献1),CF3COF(专利文献2、3)等。针对这些,记载了:例如,CF3COF通过对蚀刻条件进行最优化,可降低CF4的副产。
现有技术文献
专利文献
专利文献1:日本特开2000-63826
专利文献2:日本特开2000-265275
专利文献3:日本特开2002-158181
发明内容
如前述那样,根据专利文献1、2的记载,CF3COF可通过对清洁条件进行最优化来降低CF4的副产,但换言之,CF3COF与氧气之比等清洁条件并非清洁性能,不得不受CF4副产率限制。实际上,可推测以下情况:由于腔室的形状、耐腐蚀性、所希望的清洁速度等制约条件,通常难以降低CF4副产。
通常在高温、高清洁气体浓度的苛刻条件下,副产的CF4会再分解,因此有时表观上无法观察到CF4副产,但在受装置的耐腐蚀性所限制的更温和的条件下实施清洁时,有时副产CF4。因此,只要使用具有CF3基的部分结构的清洁气体,就无法从根本上回避CF3活性种和F活性种的再结合。
另外,同样地在作为替代PFC的、全球变暖潜能值低的清洁气体而提出的COF2或CF3COF的情况下,危险的CO、F2气体成为初始原料,并需要耐腐蚀性优异的、昂贵的制造设备。
因此,本发明的课题在于提供一种新型清洁气体,所述清洁气体不仅清洁性能优异,且容易获取,实质上不副产对环境造成负担的CF4。
本发明人等进行深入研究,结果发现通过使用二氟乙酰氟(CHF2COF),能将前述课题全部克服,从而完成了本发明。
即,本发明如下所述。
[发明1]一种清洁气体,其包含CHF2COF而成,用于去除在使用化学气相沉积法(CVD法)、金属有机物化学气相沉积法(MOCCD)、溅射法、溶胶凝胶法或者蒸镀法制造薄膜、厚膜、粉末或者晶须时附带地堆积于制造装置的内壁或其附属装置的堆积物。
[发明2]根据发明1的清洁气体,其中,堆积物为堆积于成膜装置的堆积物。
[发明3]根据发明1或2的清洁气体,其中,堆积物为包含W、Ti、Mo、Re、Ge、P、Si、V、Nb、Ta、Se、Te、Mo、Re、Os、Ir、Sb、Ge、Au、Ag、As、Cr、Hf、Zr、Ni、Co及其化合物的堆积物。
[发明4]根据发明1~3的清洁气体,其中,堆积物为含硅附着物。
[发明5]根据发明1~4的清洁气体,其中,清洁气体包含选自由O2、O3、CO、CO2、F2、NF3、Cl2、Br2、I2、XFn、CH4、CH3F、CH2F2、CHF3、N2、He、Ar、Ne、Kr中的至少1种气体作为添加物,式XFn中,X表示Cl、I或者Br,n表示1≤n≤7的整数。
[发明6]根据发明1~5的清洁气体,其中,清洁气体至少包含CHF2COF和O2。
[发明7]根据发明1~6的清洁气体,其中,清洁气体至少包含CHF2COF和O2和CO。
[发明8]一种堆积物的去除方法,其使用发明5~7的清洁气体。
[发明9]根据发明8的堆积物的去除方法,其中,堆积物为堆积于成膜装置的堆积物。
[发明10]根据发明8或者9的堆积物的去除方法,其中,堆积物为包含W、Ti、Mo、Re、Ge、P、Si、V、Nb、Ta、Se、Te、Mo、Re、Os、Ir、Sb、Ge、Au、Ag、As、Cr、Hf、Zr、Ni、Co及其化合物的堆积物。
[发明11]根据发明8~10的堆积物的去除方法,其中,堆积物为含硅附着物。
[发明12]一种堆积物的去除方法,其用基于远程等离子体的高频或者微波将发明5~7的清洁气体活化后使用。
附图说明
图1为实施例、比较例中使用的远程等离子体装置的示意图。
附图标记说明
1 腔室
2 接地
3 高频电源
4 第一气体导入口
5 第二气体导入口
6 第三气体导入口
7 蓝宝石管
8 感应线圈
9 电子压力计
10 排气通路
11 试样支架
12 试样
具体实施方式
本发明的清洁气体由于含有CHF2COF,因而不仅具有对环境的负担轻这一特征,还发挥以下效果:其具有蚀刻速度快且不引起装置腐蚀等半导体的制膜装置等中的优异的清洁性能。另外,使用了该清洁气体的清洁方法同样地发挥优异的清洁性能。因此,本发明的清洁气体对去除CVD法等的薄膜制造装置的堆积物是有用的。
以下,对本发明进行详细说明。
CHF2COF可通过将作为清洗剂、发泡剂等而使用的HFE-254pc(CHF2CF2OMe)、HFE-374pc-f(CHF2CF2OEt)等CHF2CF2OR(R为甲基、乙基、正丙基、异丙基、正丁基、仲丁基、异丁基、叔丁基等烷基)的1-烷氧基-1,1,2,2-四氟乙烷催化分解而容易且定量地合成。另外,HFE-254pc、HFE-374pc-f可通过向工业上大量生产的四氟乙烯加成甲醇、乙醇来合成,因此是非常容易获取的化合物。
CHF2COF的沸点为0℃,因此无论是作为液体、还是作为气体均为处理方便性高的清洁气体。另外,CHF2COF与水反应分解为二氟乙酸(CHF2COOH)和氟化氢(HF),因此通常可用水洗器(water scrubber)进行清除,还优选使用碱性水洗器。即使万一从清除工序中逃逸而释放至大气中,也会与大气中的雨、水蒸气发生反应,而容易地分解,因此对全球变暖的影响也是极轻度的。
作为现有的CF3COF与本发明的CHF2COF在性质上显著的不同点,可列举出烯酮结构的获取难易度。已知CHF2COF如下述的反应式那样可获取CF2=C=O的烯酮结构。在CF3COF的情况下,根据计算,获取烯酮结构的反应为165.9kcal的吸热反应,为了推进反应,在该自由能的基础上还需要活化能,因此可以说现实上发生该反应的可能性非常低。
CHF2COF→CF2=C=O+HF+48.9kcal/mol
CF3COF→CF2=C=O+F2+165.9kcal/mol
反应热、B3LYP/6-311G+**的计算值。
如实施例所示的那样,在使用CHF2COF作为清洁气体的情况下,在各种条件下均完全未检出CF4,从这一方面来看,可推测其通过与CF3COF完全不同的机理来进行清洁。
另外,在CF3COF的情况下,在使用了例如等离子体的清洁工序中,暂时生成的CF3活性种以某种概率与F活性种接触而再结合,从而副产CF4。与此相对,在CHF2COF的情况下,即使CHF2活性种与F活性种进行接触,也只是副产较容易分解的CHF3。从概率上来说,也可以认为存在CHF3进一步分解而产生CF3活性种、并通过其与F活性种的再结合而副产CF4的情况。但可容易地推测,与具有CF3基的部分结构的CF3COF等清洁气体相比较其概率显著较低。根据这些理由,可以认为CHF2COF实质上不副产CF4,实际上在各实施例中也未观察到CF4的副产。
作为本发明的清洁气体的对象的堆积物是在使用化学气相沉积法(CVD法)、金属有机物化学气相沉积法(MOCCD)、溅射法、溶胶凝胶法、蒸镀法等方法制造薄膜、厚膜、粉末、晶须等时附带地堆积于制造装置的内壁或者夹具、配管等附属装置的不需要的堆积物。在本说明书中,只要未另行定义,则“堆积物”是指此处所述的“不需要的堆积物”。
作为可通过本发明的清洁气体清洁的堆积物,可列举出W、Ti、Mo、Re、Ge、P、Si、V、Nb、Ta、Se、Te、Mo、Re、Os、Ir、Sb、Ge、Au、Ag、As、Cr、Hf、Zr、Ni、Co及其化合物,具体而言,可列举出SiO2、WSix、TiN、Ta2O5、Si3N4、SiB等的氧化物、氮化物、碳化物、硼化物以及它们的再结合物。这些之中,W、WSix、Ti、TiN、Ta2O5、Mo、Re、Ge、Si3N4、Si、SiO2等是优选的,作为去除的对象物,特别优选至少包含硅或其化合物的堆积物即含硅堆积物。
考虑应去除的堆积物的种类及厚度以及制造薄膜等的装置中使用的材料的种类,本发明的清洁气体可添加O2、O3、CO、CO、F2、NF3、Cl2、Br2、I2、XFn(式中,X表示Cl、I或者Br,n表示1≤n≤7的整数。具体而言,可例示出ClF、ClF3、BrF、BrF3、IF5、IF7。)、CH4、CH3F、CH2F2、CHF3、N2、He、Ar、Ne、Kr中的任一种作为添加物。氧气的添加对提高清洁速度是有效的。具体而言,优选CHF2COF:O2(摩尔比)为10:1~1:5,进一步优选为5:1~1:3。另外,进一步添加氧气以外的添加剂时,也可超过该范围而进行添加。该范围依赖于CH4等含氢添加剂的添加量,但优选CHF2COF:O2(摩尔比)大致为20:1~1:20。
另外,O2与前述碳原子数1的化合物(CO、CO2、CH4、CH3F、CH2F2、CHF3)的组合是适合的,特别优选添加O2和CO。CO将烯酮产生时等副产的HF以HCOF的形式捕获,其自身作为清洁剂起作用,因此是有效率的。CO的添加量为CHF2COF:CO(摩尔比)=10:1~1:5、优选为5:1~1:1。N2、He、Ne、Ar、Kr、Xe等非活性气体不仅具有稀释效果,特别是Ar对等离子体的稳定是有效的,通过与CHF2COF的协同效果而使清洁速度提高。F2、NF3、Cl2、Br2、I2、XFn(X=Cl、I、Br,1≤n≤7)、CH4、CH3F、CH2F2、CHF3的添加对于根据去除对象堆积物的种类来控制清洁速度而言是有效的。
另外,关于反应条件,只要考虑被处理装置的材质进行适当选择则无特别限定,对于温度,在装置材质为石英的情况下优选为800℃以下,作为部分或整体的材质而使用陶瓷、铝等金属的情况下优选为500℃以下。在这些温度以上时会发生腐蚀因此不优选。接着,关于压力,若超过500℃则优选设为13.3kPa(100Tor)以下,更优选6.6kPa(50Torr)以下。若超过100Torr则会发生腐蚀,因此不优选。
基于本发明的清洁气体的清洁使用热分解法、光分解法、等离子体法均可,优选等离子体法。等离子体法可以使用高频或者微波在腔室内产生,但优选采用在腔室外产生并导入至腔室内的远程等离子体法。作为本发明的清洁方法的被处理装置,可以适用于通过CVD法形成半导体器件、液晶器件、光器件、涂覆工具等的薄膜的制膜装置或制造晶须、粉末等的制造装置。这些之中,特别优选适用于制膜装置,进一步优选适用于半导体器件、液晶器件等使用了硅化合物的制膜装置。
实施例
以下,通过实施例对本发明进行详细地说明。
实施例1~4、比较例1~5
将实验所使用的装置的示意图记于图1。使用高频电源3(13.56MHz、50W),在安装于反应腔室1的上部的蓝宝石管7内对以表1所示的流量由气体导入口供给的试样气体(二氟乙酰氟(CHF2COF)、氧气(O2)、一氧化碳(CO))进行激发,利用气流(gas flow)将所生成的活性种供给至腔室内,对固定于试样支架11的试样12(掺杂了P的Si基板)进行了蚀刻。
对于试样气体,介由质量流量控制器(未图示)分别将CHF2COF、CF3COF、CF4、C2F6从第一气体导入口4导入,将O2从第二气体导入口5导入,将CO从第三气体导入口6导入。将基板(试样支架11)温度设定为25℃、压力设定为13.3Pa(0.1torr)。通过在机械增压泵(mechanical boo ster pump)的排气侧以2升/分种的速度添加氮气来稀释排气,并通过FT-IR利用标准曲线法对CF4进行了定量。
实施例1~4结束后,对装置内进行检查,未观察到腐蚀等。为了与CHF2COF进行比较,作为比较例对现有的清洁气体(CF3COF、CF4、C2F6)的蚀刻速度也进行了测定。将它们的结果示于表1。予以说明,表中的ND表示检测下限以下。蚀刻速度通过蚀刻前后的膜厚差除以蚀刻时间而求出。
[表1]
CHF2COF:二氟乙酰氟
CF3COF:三氟乙酰氟
O2:氧气
CO:一氧化碳
CF4:四氟化碳
C2F6:六氟乙烷
Claims (12)
1.一种清洁气体,其包含CHF2COF而成,用于去除在使用化学气相沉积法即CVD法、金属有机物化学气相沉积法即MOCCD、溅射法、溶胶凝胶法或者蒸镀法制造薄膜、厚膜、粉末或者晶须时附带地堆积于制造装置的内壁或其附属装置的堆积物。
2.根据权利要求1所述的清洁气体,其中,堆积物为堆积于成膜装置的堆积物。
3.根据权利要求1或2所述的清洁气体,其中,堆积物为包含W、Ti、Mo、Re、Ge、P、Si、V、Nb、Ta、Se、Te、Mo、Re、Os、Ir、Sb、Ge、Au、Ag、As、Cr、Hf、Zr、Ni、Co及其化合物的堆积物。
4.根据权利要求1~3中任一项所述的清洁气体,其中,堆积物为含硅附着物。
5.根据权利要求1~4中任一项所述的清洁气体,其中,清洁气体包含选自由O2、O3、CO、CO2、F2、NF3、Cl2、Br2、I2、XFn、CH4、CH3F、CH2F2、CHF3、N2、He、Ar、Ne、Kr中的至少1种气体作为添加物,式XFn中,X表示Cl、I或者Br,n表示1≤n≤7的整数。
6.根据权利要求1~5中任一项所述的清洁气体,其中,清洁气体至少包含CHF2COF和O2。
7.根据权利要求1~6中任一项所述的清洁气体,其中,清洁气体至少包含CHF2COF和O2和CO。
8.一种堆积物的去除方法,其使用权利要求5~7中任一项所述的清洁气体。
9.根据权利要求8所述的堆积物的去除方法,其中,堆积物为堆积于成膜装置的堆积物。
10.根据权利要求8或9所述的堆积物的去除方法,其中,堆积物为包含W、Ti、Mo、Re、Ge、P、Si、V、Nb、Ta、Se、Te、Mo、Re、Os、Ir、Sb、Ge、Au、Ag、As、Cr、Hf、Zr、Ni、Co及其化合物的堆积物。
11.根据权利要求8~10所述的堆积物的去除方法,其中,堆积物为含硅附着物。
12.一种堆积物的去除方法,其用基于远程等离子体的高频或者微波将权利要求5~7中任一项所述的清洁气体活化后使用。
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Also Published As
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TW201139622A (en) | 2011-11-16 |
US20120234351A1 (en) | 2012-09-20 |
TWI411662B (zh) | 2013-10-11 |
KR101363440B1 (ko) | 2014-02-14 |
WO2011068038A1 (ja) | 2011-06-09 |
JP2011117014A (ja) | 2011-06-16 |
EP2505687A4 (en) | 2013-07-24 |
KR20120056295A (ko) | 2012-06-01 |
JP5691163B2 (ja) | 2015-04-01 |
EP2505687A1 (en) | 2012-10-03 |
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