CN1642855B - 高纯度硅石粉末、其制造方法及装置 - Google Patents
高纯度硅石粉末、其制造方法及装置 Download PDFInfo
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- CN1642855B CN1642855B CN03806359XA CN03806359A CN1642855B CN 1642855 B CN1642855 B CN 1642855B CN 03806359X A CN03806359X A CN 03806359XA CN 03806359 A CN03806359 A CN 03806359A CN 1642855 B CN1642855 B CN 1642855B
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- Prior art keywords
- silica powder
- powder
- pyrolysis
- silica
- implement
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- 239000000843 powder Substances 0.000 title claims abstract description 115
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 266
- 239000000377 silicon dioxide Substances 0.000 title claims description 100
- 238000000034 method Methods 0.000 title claims description 48
- 230000008569 process Effects 0.000 title description 2
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- 239000005350 fused silica glass Substances 0.000 claims description 29
- 229910003902 SiCl 4 Inorganic materials 0.000 claims description 27
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 24
- 238000004140 cleaning Methods 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 16
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 12
- 229910052742 iron Inorganic materials 0.000 claims description 12
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- 239000004411 aluminium Substances 0.000 claims description 9
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- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 8
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 7
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 5
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- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 2
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- 206010022998 Irritability Diseases 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
- C01B33/183—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process by oxidation or hydrolysis in the vapour phase of silicon compounds such as halides, trichlorosilane, monosilane
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- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/10—Forming beads
- C03B19/1005—Forming solid beads
- C03B19/102—Forming solid beads by blowing a gas onto a stream of molten glass or onto particulate materials, e.g. pulverising
- C03B19/1025—Bead furnaces or burners
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- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
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- C03B37/01—Manufacture of glass fibres or filaments
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- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
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- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
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- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/02—Pure silica glass, e.g. pure fused quartz
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
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Abstract
本发明涉及一种杂质的总量低于500ppb的硅石粉末。
Description
技术领域
本发明涉及高纯度硅石粉末及在热区内制造该高纯度硅石粉末的方法及装置。
背景技术
高纯度硅石粉末已经在许多技术领域采用。这些应用场合的实例包含:光纤、用以抽拉硅单晶的石英坩埚、光电子材料(例如:透镜及反射镜)、电子材料内所用惰性成分的填料及晶片的抛光悬浮液(化学机械抛光)。上述诸应用场合对粉末纯度的要求极高。
在光学通讯上所用由SiO2所制光纤内,作为资讯载体的光,其放射强度不应由杂质(例如:OH、铁及铜)所引起的吸收作用、或泡沫、结晶核及不匀性引起的散射作用而减弱。结晶核是由杂质(例如:钙及镁)所形成。
在石英玻璃坩埚内,在抽拉硅单晶期间对坩埚内表面所发生的腐蚀作用是随杂质的数量及类型而变化。腐蚀作用减低潜在拉晶时间。再者,每多一种杂质即增加结晶核的数量,在单晶冷却期间,结晶核处可形成氧的沉淀。
例如,在光学玻璃中,玻璃内的传送损失是由钠及过渡金属所引起。所以,过渡金属的浓度需不超过100ppb。唯独如此方可确保:波长为248纳米的传送大于99.5%及波长为193纳米的传送大于98%。再者,光纤、石英坩埚及玻璃所用的硅石粉末必须不含有机杂质,否则在烧结步骤期间会形成许多气泡。
若元素铁、钠及钾的浓度不超过0.2ppm及元素铝及钛的浓度不超过1ppm,高纯度SiO2也可用作环氧树脂的填料以保护IC晶片。这些元素改变惰性元件的热膨胀系数、电导率及抗腐蚀性。如此可使晶片的保护功能产生去活化作用。
抛光悬浮液是用于半导体表面的直接抛光。例如,作此用途的SiO2,其铝的浓度必须不能超过4ppm。
制造高纯度硅石粉末的已知方法是:含硅母体的水解作用。例如,该方法可借下列诸方式加以实施:在有有机溶剂存在的情况下,在水中将SiCl4水解(Degussa的DE 3937394);将氟硅酸铵首先与氨水混合,之后再与氢氟酸混合(Nissan,JP 04175218),或通过添加稀无机酸于碱金属硅酸盐而得硅石沉淀(日本、EP 9409167,武汉大学,CN1188075)。如此形成的硅石也称作沉淀型硅石且主要是用途催化剂载体及作为环氧树脂填料以保护LSI及VLSI电路装置。上述方法制备多孔性、含有气泡的、流动性能差的非完美球状微粒。这些方法的另一非常重大缺点是纯度受到限制,因为这些方法会引进一定程度的某些杂质,例如:OH、碳、氟、氮及碱金属,例如:钠及钾。这些缺点导致大量光散射及吸收,以及应用产品的机械及热稳定性减低。所以,该方法基本上不适用于光纤、坩埚及玻璃工业。
由于严格的纯度要求,天然石英也不能作上述用途。但,已经尝试,通过将不够纯的石英作进一步纯化的另外加工步骤以达成合格的纯度等级。依照DE 3123024(Siemens),天然石英是通过熔化作用转化为细纤维,随后利用酸及碱将这些纤维施以许多沥滤加工步骤.由于这些纤维的表面积高及厚度小,过渡金属离子的含量可降到低于1ppm.因这些纤维是直接应用于光纤工业界,此方法相当低廉.依照DE 3741393(Siemens),若作为其他用途或制成不同成形体几何形状,这些经纯化的纤维是加以研磨,并借助于水、分散剂及其他助剂转化成泥浆,随后施以流铸加工及烧结加工,最后结果是带有许多污染源的繁复加工方法。
依照EP 0737653(Heraeus),天然石英是施以研磨、筛选、预热至1000℃、用Cl2/HCl加以处理、冷却及去脱附等加工步骤。此耗时加工法所得纯度仍含约70ppb的铁。来自碱土金属及铝的杂质(可形成方英石,所以(例如)减低坩埚品质)无法移除至此种程度,因为这些元素可形成低挥发性的氯化物(主要地:钠=1100ppb,钾=1050ppb,锂=710ppb,钙>370ppb,铝=16000ppb,铁=410ppb;随后:钠<10ppb,钾>80ppb,锂=700ppb,钙>120ppb,铝=16000ppb,铁>30ppb)。
依照US 4818510(石英技术),可用HF将石英进一步纯化。但,HF仅对若干元素(例如:铁)作选择性反应,而形成容易溶解的复合物。
进一步纯化作用也可对SiO2颗粒实施。依照US 6180077及EP1088789(Heraeus),SiO2颗粒是借助于HCl在高温下制造及纯化。一项优点是:这些颗粒的表面积高,所以HCl可较为容易地及较为快速地与其作用。若起始点是纯度为钠<50ppb,铁=250ppb,铝<1ppm的颗粒,进一步纯化作用可达到纯度非常高的等级(纳=5ppb,铁=10ppb,铝=15ppb)。一项缺点是:首先需要制造高度多孔性的硅石颗粒(孔洞体积0.5立方厘米,孔洞直径50纳米,BET表面积100平方米/克,密度0.7克/立方厘米,粒径180至500微米),这是一个耗时加工方法,且这些颗粒并不代表最终产品,仍须加以烧结。再者,该高孔隙率隐藏着成型(例如:形成坩埚)后烧结期间所含剩余气体的潜在风险。
依照US 4956059(Heraeus),除高温下所用纯化气体Cl2/HCl之外,在硅石颗粒进一步纯化作用中也可使用电场(通常为652伏特/厘米)。在有电场存在的情况下(尤其碱金属离子受此影响,在电场中容易移动),可使进一步纯化作用的效果更佳。此方法可使钠的等级由1ppm减至50ppb。
依照EP 1006087(Heraeus),进一步纯化作用可用适当的方式实施,以便在气流内将不纯的粉末加热,使杂质软化并形成熔融附聚物可附着在该表面上。该方法仅对非常不纯的起始原料粉末有用。但,此种方法对高熔点氧化物(例如:MgO及Al2O3)无法产生进一步的纯化作用。为达成此目的需要使用大量气体,这是另一缺点。
利用溶胶-凝胶加工法(其中由有机硅烷及水,首先形成溶胶及随后形成凝胶可达成高纯度(金属杂质<1ppm,碳<5ppm,硼<50ppm,磷<10ppb)。随后利用惰性气体加以烘干、煅烧及烧结(Mitsubishi,EP 0831060、EP 0801026、EP 0474158)。因为将高纯度有机硅氧烷用作起始原料,此方法非常耗时而且昂贵。通常,在制造程序中使用以有机物为主要成分的流变性助剂、分散剂及溶剂,结果最终产品中可含有黑色碳微粒及CO及CO2气泡。使用水可导致高OH含量,因而产品中有气泡形成及产品的热稳定性低。若将该材料用作利用Czochralski法制造硅单晶的硅石坩埚,由于温度高及压力低,这些气泡及孔洞会膨胀。在拉晶期间,这些气泡不仅在硅熔体内形成涡流而且形成结晶瑕疵以及降低坩埚的长期稳定性。
原则上,高纯度硅石也可在有氧-燃料焰存在的情况下,利用CVD或OVD法,由高纯度有机硅烷或SiCl4产生硅石沉淀而制得(Corning,US 5043002、US 5152819、EP 0471139、WO 01/17919、WO 97/30933、WO 97/22553、EP 0978486、EP 0978487、WO 00/17115)。但,方法不能制成粉末,而是具有特定、简单几何形状的玻璃体。这些简单几何形状包含光学玻璃及透镜。光纤可借抽拉作用自所制高纯度形式的玻璃体制得。为自这些简单玻璃体制造任何预期几何形状的玻璃体,所制玻璃体必须首先加以研磨成为粉末状,之后加以分散、成型及烧结。但,此种方法可产生广泛污染(尤其在研磨步骤期间)。
此方法的另一缺点是:为达成特别高的纯度,须使用昂贵、高纯度有机硅烷,例如:八甲基环四硅氧烷(OMCTS)。
高纯度SiO2薄层也可通过沉淀在高纯度底材上而制得(例如:通过等离子体CVD/OVD,GB 2208114、EP 1069083)。其缺点是:仅可达成150纳米/分钟的低沉淀速率(例如:J.C.Alonso等人,J.VAC.Sci.Technol.A 13(6),1995、第2924等页)。涂覆方法需要高制造成本。由这些方法,无法制得高纯度硅石粉末。
简单替代方法是在火焰中形成硅石。在此方面有两种不同的方式经公开。依照JP 5-193908(Toyota/ShinEtsu),借助于C3H2n+2/O2焰(其中C3H2n+2仅是燃烧作用所需),高纯度硅金属粉末可氧化成高纯度硅石粉末。但,发明人自己承认有反应产生许多未燃烧微粒的问题。除非起始微粒非常纤细(0.2微米),甚难达到充分氧化作用。但,几乎不能制得如此纤细的高纯度硅微粒。
另外一种方式是,通过火焰水解作用,在第一步骤内,于氢氧焰中由SiCl4可制得热解型硅石,在第二步骤内,借烧结作用可将该热解型硅石转化为熔凝硅石。
应了解的是,术语热解型硅石是指通过使硅烷在高温火焰内反应所制的超细微粒、纳米级粉末,且经常凝集及粘聚在一起。热解型硅石的一个典型实例是:Degussa制备的OX 50,BET表面积为50平方米/克。应了解的是,熔凝硅石一词是指较粗颗粒、球状玻璃粉末。熔凝硅石的一个典型实例是Tokuyama制备的平均粒径为15微米。
依照US 5,063,179(Cabot),第二个子步骤(=熔凝硅石的制造)的实施方式是:将热解型硅石分散在水中,加以过滤、烘干、利用SOCl2或Cl2进一步纯化,并于炉内加以烧结。杂质(例如:钠及铁)的浓度约为1ppm(杂质总含量<50ppm),即仍然相当高。
依照JP 5301708及JP 62-270415(德山公司),为制造熔凝硅石,用水蒸汽处理高纯度热解型硅石,加以冷却及流体化,借助于一螺杆输送器将其进给至一氢氧焰内以实施烧结作用。利用上述方法所制熔凝硅石产品含有>1000ppb的杂质,该杂质是铜、铁、钛、铝、钙、镁、钠、钾、镍、铬、锂诸元素累积的总和。例如,借助于螺杆输送器,依照上述方法实施这些热解型硅石的分散作用及输送。螺杆是移动部件,接触硅石会受到损伤,尤其边缘部位更为严重。结果,该螺杆污染到细石粉末。该项设备的其他部件也会曝露于磨蚀性硅石微粒,因而受到损伤。尤其应提及燃烧器喷嘴,在该处硅石粉末的速度特别高。
发明内容
本发明的目的是提供一种纯度非常高的硅石粉末。
本发明的另一目的是提供以廉价方式制造本发明粉末的一种方法及装置。
所制杂质总量低于500ppb的硅石粉末可达成第一个目标。
本发明硅石粉末内的杂质总量优选低于150ppb.尤其优选杂质总量低于150ppb及个别杂质含量为铜<1ppb、铁<25ppb、镍<2ppb、铬<2ppb、钛<3ppb、铝<31ppb、钙<65ppb、镁<12ppb、钠<12ppb、钾<6ppb、及锂<1ppb而且该粉末不含碳.
杂质等级是利用ICP分析法(感应性偶合等离子体,装置类型为IPC-MS HP 4500)测定,该方法的检测极限低于1ppb。这些硅石粉末可以是热解型硅石或熔凝硅石。
热解型硅石的表面积以50至300平方米/克为佳,尤以150至250平方米/克更佳。原始粒径以1纳米至1000纳米为佳,但以5纳米至100纳米较佳,尤以10纳米至30纳米更佳。
熔凝硅石的平均粒径以100纳米至200微米为佳,但以1微米至200微米较佳,尤以5微米至40微米更佳。再者该粉末的粒径分布以狭窄(D(95)-D(5)<50微米)为佳,但以D(95)-D(5)<35微米,也即平均粒径D(50)=15微米;D(5)=1微米,D(95)=50微米较佳,尤以D(5)=3微米,D(95)=35微米更佳(利用CILAS 715测量)。
本发明产品的狭窄粒径分布意谓另外加工步骤(例如:筛选)已不需要而且该粉末适于直接进一步加工。例如,图6所示是依照实施例4所制熔凝硅石粉末的非常均匀粒径分布。
本发明熔凝硅石微粒最好呈球状而且完全玻璃化。与利用溶胶-凝胶法所制粉末不同,此等熔凝硅石微粒不含任何气泡或由于使用有机溶剂、分散剂及流变性试剂所产生的碳杂质。
本发明的高纯度热解型硅石及熔凝硅石粉末可用于现有技术已知的所有应用场合。例如,这些高纯度硅石粉末特别适用于制造DE19943103(Wacker Chemie GmbH)所述的成形体。
本发明的粉末最好可借助于以下方法制造:高纯度热解型硅石是由高纯度SiCl4的水解而制得,其中作用以形成热解型硅石的SiCl4水解是在具有无金属表面的装置内实施。高纯度SiCl4的水解作用是在火焰中实施。该火焰包括含氧气体及选自以下组中的气体:烃及氢,但以包括空气或氧及选自以下组中的气体较佳:甲烷、丙烷及氢,尤以包括氧及氢者更佳。该水解作用最好在H2/O2焰内实施。另外一种方式是,水解作用是在等离子体内(例如:HF等离子体内)实施。
热解型硅石粉末的沉积作用最好也在具有无金属表面的装置内实施。
其他适当的起始原料包含:杂质<100ppb的硅烷、有机硅化合物及卤硅烷。杂质<100ppb的SiCl4极为适当,纯度如表1所示的SiCl4则更为适当。
同样高纯度的本发明熔凝硅石粉末也可通过烧结作用由本发明的热解型硅石粉末制成。
高纯度热解型硅石粉末的烧结作用最好是在用以制造本发明热解型硅石粉末的装置中,在H2/O2焰内或借助于HF等离子体实施。热解型硅石内也可添加控制量的水以控制熔凝硅石粉末的料径。
为避免遭受环境元素(例如:钠、钾、镁或钙)的污染,最好是在清洁室内情况下和/或在一层流动体的情况下进行工作。
在此情况下,该方法是在清洁室内等级100000至1(但以10000至100较佳,尤以1000更佳)时实施。
作为清洁室内情况的变通方式,该方法可在0.913巴至1.513巴(但以1.013巴至1.413巴较佳,尤以1.020巴至1.200巴更佳)的压力下实施.超大气压力可防止杂质进入设备内.
若本发明的粉末是在H2/O2焰内制造,本发明的装置是喷嘴,该喷嘴包括位于外管内的内管,所用起始原料选自以下组中:SiCl4、SiCl4与O2的混合物、热解型硅石及热解型硅石与O2的混合物,且通过该内管,其中该内管是由以硅为主要组分的含硅材料(例如:石英玻璃、熔凝石英、SiC、Si3N4、琺瑯或硅金属)组成。
最好该内管是由以硅为主要组分的含硅材料(例如:石英玻璃、熔凝石英、SiC、Si3N4、琺瑯或硅金属)组成,该材料的表面已经利用含氯气体(例如:SOCl2、HCl或Cl2)加以纯化。
该装置最好是喷嘴,在该喷嘴中,内管是由石英玻璃或附有石英玻璃表面的材料所组成,该石英玻璃表面最好已经利用含氯气体(例如:SOCl2、HCl或Cl2)加以纯化。
最好整个喷嘴是由石英玻璃或具有石英玻璃表面的材料组成。若石英玻璃或该具有石英玻璃表面的材料已经利用SOCl2、HCl或Cl2加以纯化,纯度仍可进一步提高。
若仅供应热解型硅石或SiCl4的内管是由石英玻璃组成,而喷嘴的其余部分是由(例如)钢组成,所制粉末的纯度较喷嘴由石英玻璃喷嘴制备的略差,但仍较已知硅石粉末高。
所以,本发明还涉及喷嘴,该喷嘴包括位于外管内的内管,其中该内管是由以硅为主要组分的含硅材料组成。该材料最好选自以下组中:石英玻璃、熔凝石英、SiC、Si3N4、琺瑯或硅金属。
该喷嘴优选由选自以下组中的材料组成:石英玻璃、熔凝石英、SiC、Si3N4、琺瑯或硅金属,尤其优选由石英玻璃组成。
喷嘴以不将燃料气体预先加以混合的喷嘴为佳。在此型喷嘴内,燃料气体H2及O2是分别进给至燃烧室内。在本发明喷嘴1的一个实施方案中,SiCl4和/或热解型硅石是在先导室7(pilot chamber)内预先与一种燃料气体(以O2为佳)混合,随后将该混合物进给至燃烧室内。该喷嘴包括供应O2及热解型硅石(SiCl4)混合物的内管5及供应H2的外管6(图3及4)。
在本发明喷嘴1的另一实施方案中,所有反应成分(H2、O2、SiCl4和/或热解型硅石)是分别进给至燃烧室内。该喷嘴包括同心配置的管2、3、4以供应热解型硅石(SiCl4)、O2及H2。一种可能的配置包括:内管以供应热解型硅石(SiCl4)、中管以供应O2及外管以供应H2(图1)。
借助于H2/O2焰以制造本发明粉末的燃烧炉10最好包括许多本发明的喷嘴1。若是一个喷嘴(图1),该燃烧炉传送一种粒径分布狭窄的粉末,传送一种粒径分布甚为狭窄的粉末则使用许多喷嘴,其中起始原料是经由三个同心管供应(图2),传送一种粒径极为狭窄的粉末则使用许多喷嘴及O2/热解型硅石预混室,起始原料是经由两个同心管5、6供应(图3及4)。该配置可使SiCl4(或制造熔凝硅石粉末时的热解型硅石粉末)在火焰中分布得特别均匀。
所以本发明还涉及包含1至30个(但以6至13个较佳,尤以7个更佳)本发明喷嘴1的燃烧炉10.燃烧炉面向燃烧室的表面最好同样由石英玻璃组成.图4所示附有7个本发明此型喷嘴1的燃烧炉10.图3所示是此型燃烧炉的平面图,图2所示是附有7个喷嘴的燃烧炉,其中所有上述3种起始原料是分别送入燃烧室内.
热解型硅石在火焰内的分散作用仍可在本发明喷嘴的变化中获得进一步改善,其中O2及热解型硅石粉末是在进给至燃烧室之前加以预先混合。
若本发明的粉末是在等离子体内制造,则本发明的装置是等离子体吹管11,其中包括粉末喷嘴12、中间管13及外管14(图4),且粉末喷嘴、中间管及外管的表面是由以硅石为主要组分的含硅材料制成。最好该表面是由选自以下组中的材料组成:石英玻璃、熔凝石英、SiC、Si3N4、琺瑯或硅金属。最好该表面是利用一种气体(例如:SOCl2、Cl2或HCl)加以纯化,热解型硅石粉末是经由该粉末喷嘴计量加入,等离子体气体O2是经由中间管13计量加入,遮蔽气体混合物O2及H2是经由外管送入。
最好使用等离子枪,其中粉末喷嘴、中间管及外管的表面是由石英玻璃制成。
尤其最好使用表面是由石英玻璃制成的等离子枪。
等离子枪11还具有感应线圈15及水冷却16与水冷却夹套17。
高纯度粉末可利用本发明的装置直接制得。通常所需的进一步纯化加工步骤则可省去。利用传统方法未曾达成的极高纯度热解型及熔凝硅石粉末(表1),可利用本发明的喷嘴制得。在清洁室内情况下,通过在石英玻璃制喷嘴内的燃烧作用仍可将纯度进一步提高。再者,如果与粉状起始原料或本发明产品接触的制造本发明热解型或熔凝硅石粉末设备的所有表面是经设计得无污染,则属有利。所以,用以制造本发明硅石粉末的装置,其所有与硅石粉末接触的表面最好不含金属。公知制造硅石粉末的设备包括:a)计量装置、b)燃烧炉、c)燃烧室、d)旋风器及e)储藏器。若是制造热解型硅石,旋风器与储藏器之间通常以流化床连接。
前述用以制造本发明喷嘴的材料,最好也形成计量装置、燃烧室、旋风器、流化床及储藏器的表面。在另一实施方案中,计量装置及储藏器的表面也可以是纯塑料。例如,该塑料可以是PFA(全氟烷氧基共聚物)、PTFE(聚四氟乙烯)、GFK(玻璃纤维强化聚酯树脂)及PP(聚丙烯)。在计量区内,硅石粉末的输送最好不使用移动零件,例如:借助于压缩空气,利用气动输送。
附图说明
在下列附图中:
图1:显示燃烧炉的出口作为3-管燃烧炉喷嘴,O2不与SiCl4或热解型硅石预先混合,
图2:所示为包括7个喷嘴的燃烧炉出口,O2不与SiCl4或热解型硅石预先混合,
图3:所示为包括7个喷嘴的燃烧炉出口,O2与SiCl4或热解型硅石预先混合,
图4:所示为包括7个石英玻璃喷嘴的燃烧炉,O2与SiCl4或热解型硅石预先混合,
图5:所示为等离子枪,
图6:所示为由实施例4所制熔凝硅石粉末。
具体实施方式
下列诸实施例用于将本发明作进一步说明。
实施例1:在无清洁室条件下借助于氢氧焰由SiCl4制造热解型硅石粉末
为由SiCl4制造热解型硅石粉末,借助于石英玻璃喷嘴,未经预先混合,将反应成分SiCl4、O2及H2送至燃烧室内。利用16.6克/分钟的SiCl4+6.3升/分钟的O2+8.9升/分钟的H2实施该反应。该燃烧室是在超出大气压力20毫巴的压力下操作。表1所示是分析结果。
实施例2:利用清洁室条件,借助于氢氧焰由SiCl4制造热解型硅石粉末
为由SiCl4制造热解型硅石粉末,借助于石英玻璃喷嘴,未经预先混合,将反应成分SiCl4、O2及H2送至燃烧室内。利用16.6克/分钟的SiCl4+6.3升/分钟的O2+8.9升/分钟的H2实施该反应。整个设备是在属于清洁室等级10000的清洁室内。表1所示是分析结果。
实施例3:在无清洁室条件下借助于氢氧焰由热解型硅石粉末制造熔凝硅石粉末
为由热解型硅石粉末制造熔凝硅石粉末,借助于石英玻璃喷嘴,未经预先混合,将反应成分热解型硅石、O2及H2送至燃烧室内。利用180升/分钟的H2+90升/分钟的O2+60.3克/分钟的热解型硅石粉末实施该反应。该燃烧室是在超出大气压力40毫巴的压力下操作。表1所示是分析结果。
实施例4:在清洁室条件下借助于氢氧焰由热解型硅石粉末制造熔凝硅石粉末
为由热解型硅石粉末制造熔凝硅石粉末,借助于石英玻璃喷嘴,将经预先混合的反应成分热解型硅石粉末、O2及H2送至燃烧室内。利用180升/分钟的H2+90升/分钟的O2+60.3克/分钟的热解型硅石粉末实施该反应。整个设备是在属于清洁室等级10000的清洁室内。表1所示是分析结果。
实施例5:在清洁室条件下,借助于HF等离子体由热解型硅石粉末制造熔凝硅石粉末
为由热解型硅石粉末制造熔凝硅石粉末,经由包括石英玻璃筒的枪将反应成分热解型硅石粉末、空气及H2通至燃烧室内。利用45升/分钟的O2作为中央等离子体气体,90升/分钟的O2及25升/分钟的H2作为遮蔽气体及15千克/小时的热解型硅石粉末(经由粉末喷嘴计量加入)。燃烧室内的压力为300托,HF等离子体的总功率为90千瓦。在本案例中,依照固态技术的原理,该等离子体是HF等离子体,本领域技术人员均对其熟悉。整个设备是在属于清洁室等级10000的清洁室内。表1所示是分析结果。
实施例6:在清洁室条件下,利用非石英玻璃制的标准喷嘴借助于氢氧焰由热解型硅石粉末制造熔凝硅石粉末
为由热解型硅石粉末制造熔凝硅石粉末,借助于不锈钢喷嘴,经预先混合,将反应成分热解型硅石粉末、O2及H2送至燃烧室内。利用180升/分钟的H2+90升/分钟的O2+60.3克/分钟的热解型硅石粉末实施该反应。整个设备是在属于清洁室等级10000的清洁室内。表1所示是分析结果。
比较例7:依照JP 59152215借助于氢氧焰由热解型硅石制造熔凝硅石
经由螺杆输送器将高纯度热解型硅石粉末送入氧流体内,之后将其送入燃烧炉管内。该燃烧炉包括3个管,经由内管及外管将7.6立方米/小时的H2送至燃烧室内,而中间管含有3.8立方米/小时的O2及1.8千克/小时的热解型硅石粉末。表1所示是分析结果。
表1
利用ICP/MS测定各个实施例所制产品及所用SiCl4的杂质含量(ppb)
实施例 | 铜 | 铁 | 钛 | 铝 | 钙 | 镁 | 钠 | 钾 | 镍 | 铬 | 锂 |
1 | <1 | 22 | 2 | 24 | 54 | 9 | 8 | 5 | 2 | 2 | <1 |
2 | <1 | 10 | <1 | 10 | 11 | 2 | 4 | 1 | <1 | <1 | <1 |
3 | <1 | 25 | 2 | 31 | 64 | 11 | 11 | 5 | 2 | 2 | <1 |
4 | <1 | 10 | <1 | 9 | 13 | 3 | 5 | 1 | <1 | <1 | <1 |
5 | <1 | 12 | <1 | 15 | 14 | 3 | 6 | 1 | <1 | <1 | <1 |
6 | <1 | 250 | 4 | 63 | 15 | 7 | 7 | 2 | 43 | 27 | <1 |
7 | 4 | 730 | <1 | 62 | 66 | 134 | 19 | 9 | 167 | 235 | <1 |
SiCl<sub>4</sub> | <1 | 10 | <1 | 3 | 8 | <1 | 3 | 2 | <1 | <1 | <1 |
Claims (21)
1.一种硅石粉末,其中杂质的总量低于500ppb。
2.一种硅石粉末,其中杂质的总量低于150ppb。
3.如权利要求1的硅石粉末,其中所述杂质的总量低于150ppb,且个别杂质含量为:铜<1ppb,铁<25ppb,镍<2ppb,铬<2ppb,钛<3ppb,铝<31ppb及钙<65ppb,镁<12ppb,钠<12ppb,钾<6ppb,锂<1ppb,并且该粉末不含碳。
4.如权利要求1、2或3的硅石粉末,其中所述粉末是热解型硅石粉末,其BET表面积为50-300平方米/克。
5.如权利要求4的硅石粉末,其BET表面积为150-250平方米/克。
6.如权利要求1、2或3的硅石粉末,其中所述粉末是熔凝硅石粉末,其平均粒径为100纳米至200微米。
7.如权利要求6的硅石粉末,其平均粒径为1微米至200微米。
8.如权利要求6的硅石粉末,其平均粒径为5微米至40微米。
9.如权利要求6的硅石粉末,其具有狭窄的粒径分布:D(95)-D(5)<50微米。
10.如权利要求9的硅石粉末,其具有狭窄的粒径分布:D(95)-D(5)<35微米。
11.如权利要求6的硅石粉末,其具有球状形貌且完全玻璃化。
12.一种制备权利要求1-4之一的硅石粉末的方法,在该方法中,通过高纯度SiCl4的火焰水解得到高纯度热解型硅石粉末,其中该SiCl4的火焰水解是在具有无金属表面的装置内实施。
13.一种制备权利要求6-11之一的硅石粉末的方法,在该方法中,通过高纯度热解型硅石粉末的烧结得到高纯度熔凝硅石粉末,其中该热解型硅石粉末的烧结是在具有无金属表面的装置内实施。
14.如权利要求12或13的方法,其是在清洁室条件下实施。
15.如权利要求14的方法,其中所使用的清洁室条件等级为100000至1。
16.如权利要求15的方法,其中所使用的清洁室条件等级为10000至100。
17.如权利要求15的方法,其中所使用的清洁室条件等级为1000。
18.如权利要求12或13的方法,其是在0.913巴至1.513巴的压力下实施。
19.如权利要求18的方法,其是在1.013巴至1.413巴的压力下实施。
20.如权利要求18的方法,其是在1.020巴至1.200巴的压力下实施。
21.一种用于制备权利要求1-11之一的硅石粉末的装置,其中所有与该硅石粉末接触的表面都不含金属,并且该装置是喷嘴包括位于外管内的内管,并且整个喷嘴由石英玻璃或具有石英玻璃表面的材料组成。
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- 2003-03-06 RU RU2004130850/15A patent/RU2295492C2/ru not_active IP Right Cessation
- 2003-03-06 CN CN03806359XA patent/CN1642855B/zh not_active Expired - Fee Related
- 2003-03-06 EP EP08164313A patent/EP1997778A1/de not_active Withdrawn
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JP2005531475A (ja) | 2005-10-20 |
DE10211958A1 (de) | 2003-10-16 |
DE50310806D1 (de) | 2009-01-02 |
US20050129603A1 (en) | 2005-06-16 |
EP1503957A1 (de) | 2005-02-09 |
KR20040107485A (ko) | 2004-12-20 |
JP4381149B2 (ja) | 2009-12-09 |
RU2295492C2 (ru) | 2007-03-20 |
CN1642855A (zh) | 2005-07-20 |
UA80274C2 (en) | 2007-09-10 |
WO2003078321A1 (de) | 2003-09-25 |
RU2004130850A (ru) | 2005-06-10 |
EP1997778A1 (de) | 2008-12-03 |
EP1503957B1 (de) | 2008-11-19 |
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