CN106567045B - 管状旋转高纯硅溅射靶材的制备方法 - Google Patents
管状旋转高纯硅溅射靶材的制备方法 Download PDFInfo
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 30
- 239000010703 silicon Substances 0.000 title claims abstract description 30
- 239000013077 target material Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000005477 sputtering target Methods 0.000 title claims abstract description 12
- 238000005507 spraying Methods 0.000 claims abstract description 25
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000001301 oxygen Substances 0.000 claims abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 8
- 239000011248 coating agent Substances 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 6
- 239000011230 binding agent Substances 0.000 claims abstract description 4
- 238000002844 melting Methods 0.000 claims abstract description 4
- 230000008018 melting Effects 0.000 claims abstract description 4
- 238000007781 pre-processing Methods 0.000 claims abstract description 4
- 238000007788 roughening Methods 0.000 claims abstract description 4
- 238000005488 sandblasting Methods 0.000 claims abstract description 4
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 6
- 238000003754 machining Methods 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 238000007750 plasma spraying Methods 0.000 abstract description 4
- 238000004544 sputter deposition Methods 0.000 description 10
- 239000010408 film Substances 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- Aiming, Guidance, Guns With A Light Source, Armor, Camouflage, And Targets (AREA)
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Abstract
本发明公开了一种高纯度、高密度、低氧含量、低电阻率的管状旋转高纯硅溅射靶材的制备方法,包括如下步骤:靶材基管准备:选用并检验所需型号的靶材基管;基管表面预处理:将靶材基管进入基管预处理设备进行喷砂粗化、喷涂打底结合层,得到准备喷涂的靶材基管;硅粉原料准备:称取含量:99.95%‑99.99%、氧含量≤1500ppm、粒径为45‑150μm的硅粉;烘干:将所得的硅粉原料置于烘干炉中烘干;真空等离子喷涂:将靶材基管置于密封的喷涂仓内,采用大功率超音速等离子喷涂枪,使用等离子体为热源将所得硅粉加热到熔融或半熔融状态,并随高速焰流喷涂到制备好的靶材基管表面,形成致密的硅涂层。
Description
技术领域
本发明涉及溅射镀膜材料领域,尤其涉及一种管状旋转高纯硅溅射靶材的制备方法。
背景技术
由于硅材料具备良好的超硬、耐磨、抗蚀、封闭性好的特征,硅靶材在溅射镀膜工艺中已作为不可或缺的封闭、光栅涂层材料,在光电玻璃、节能玻璃、超硬耐磨工具等领域得到广泛的应用。由于生产技术的局限性,目前市场上采用热喷涂工艺制作的硅靶材,具有相对密度不够高(≤95%)、孔隙多、氧含量高的缺陷。在溅射过程中由于氧含量高,使靶材导电性变差,影响了放电起辉,溅射效果不好,同时由于氧含量高,在溅射过程中,靶材中的氧释放到溅射室真空腔中,使真空腔中的氧浓度变高,溅射出来的即将成膜的靶材分子被氧化,影响了膜的质量。由于靶材密度不够高,在溅射过程中,绕靶材高速运动的电子轰击靶材表面时,会击发出较大的靶材分子团,靶材分子团越大,沉积在基板上成膜质量就越差。
发明内容
本发明所要解决的技术问题是:提供一种高纯度、高密度、低氧含量、低电阻率的管状旋转高纯硅溅射靶材的制备方法。
为了解决上述技术问题,本发明的技术方案为:管状旋转高纯硅溅射靶材的制备方法,包括如下步骤:靶材基管准备:选用并检验所需型号的靶材基管;基管表面预处理:将靶材基管进入基管预处理设备进行喷砂粗化、喷涂打底结合层,得到准备喷涂的靶材基管;硅粉原料准备:称取含量:99.95%-99.99%、氧含量≤1500ppm、粒径为 45-150um的硅粉;烘干:将所得的硅粉原料置于烘干炉中烘干;真空等离子喷涂:将靶材基管置于密封的喷涂仓内,采用大功率超音速等离子喷涂枪,使用等离子体为热源将所得硅粉加热到熔融或半熔融状态,并随高速焰流喷涂到制备好的靶材基管表面,形成致密的硅涂层,在喷涂过程中,连续的往喷涂仓中通入氮气,并呈正压状态,喷涂电压95-100V、喷涂电流550-600A、等离子焰体温度10000-15000℃、焰流速150m/s、氩气流量1500-2500L/h、氢气流量600-1500L/h、氮气流量3000-4000L/h;机械加工:待喷涂所得靶材到达所定尺寸后,对成型的靶材进行外形机械加工,加工后进行清洁包装即得到管状旋转高纯硅溅射靶材。
本发明的优点是:上述管状旋转高纯硅溅射靶材的制备方法,本发明中的杂质总和≤100ppm、氧含量≤1500ppm、相对密度≥97%、电阻率≤400Ω·cm、靶材的晶粒小于等于30μm,由于硅靶材的密度得到了提高,晶粒得到细化,晶粒之间的排列更加紧密,靶材的电阻率变低,在靶材使用过程中,在相同电压下,通过靶材的电流越大,由于功率=电压*电流,功率可以越高。从而可以提高磁控溅射镀膜速率,降低成本。同一成分的靶材,细小尺寸晶粒靶材的溅射速率要比粗晶粒靶快;而晶粒尺寸相差较小的靶材,淀积薄膜的厚度分布也更加均匀致密。据日本Energy公司研究发现,若将硅靶材的晶粒尺寸控制在100μm以下,且晶粒大小的变化保持在20%以内,其溅射所得薄膜的质量可得到大幅度改善。实验证明,本发明的靶材会使溅镀薄膜更为均匀,且靶材寿命较长,但要搭配溅射功率。本发明的申请人没有在硅原料中添加任何元素的情况下,能改善和提高硅靶材关键性质量指标,极大的提高了产品性能,可广泛用于液晶显示屏镀膜、光学镀膜等领域,对行业的进步有极大的推动作用。
具体实施方式
下面通过具体实施例详细描述一下本发明的具体内容。
管状旋转高纯硅溅射靶材的制备方法,包括如下步骤:靶材基管准备:选用并检验所需型号的靶材基管;基管表面预处理:将靶材基管进入基管预处理设备进行喷砂粗化、喷涂打底结合层,得到准备喷涂的靶材基管;硅粉原料准备:称取含量:99.95%-99.99%、氧含量≤1500ppm、粒径为45-150μ m 的硅粉;烘干:将所得的硅粉原料置于烘干炉中烘干;真空等离子喷涂:将靶材基管置于密封的喷涂仓内,采用大功率超音速等离子喷涂枪,使用等离子体为热源将所得硅粉加热到熔融或半熔融状态,并随高速焰流喷涂到制备好的靶材基管表面,形成致密的硅涂层,在喷涂过程中,连续的往喷涂仓中通入氮气,并呈正压状态,以保证靶材喷涂全过程都处于惰性气体保护状态中,喷涂电压95-100V、喷涂电流550-600A、等离子焰体温度10000-15000℃、焰流速150m/s、氩气流量1500-2500L/h、氢气流量600-1500L/h、氮气流量3000-4000L/h;机械加工:待喷涂所得靶材到达所定尺寸后,对成型的靶材进行外形机械加工,加工后进行清洁包装即得到管状旋转高纯硅溅射靶材。
Claims (1)
1.管状旋转高纯硅溅射靶材的制备方法,其特征在于:包括如下步骤:靶材基管准备:选用并检验所需型号的靶材基管;基管表面预处理:将靶材基管进入基管预处理设备进行喷砂粗化、喷涂打底结合层,得到准备喷涂的靶材基管;硅粉原料准备:称取含量:99.95%-99.99%、氧含量≤1500ppm、粒径为45-150μ m 的硅粉;烘干:将所得的硅粉原料置于烘干炉中烘干;真空等离子喷涂:将靶材基管置于密封的喷涂仓内,采用大功率超音速等离子喷涂枪,使用等离子体为热源将所得硅粉加热到熔融或半熔融状态,并随高速焰流喷涂到制备好的靶材基管表面,形成致密的硅涂层,在喷涂过程中,连续的往喷涂仓中通入氮气,并呈正压状态,喷涂电压95-100V、喷涂电流550-600A、等离子焰体温度10000-15000℃、焰流速150m/s、氩气流量1500-2500L/h、氢气流量600-1500L/h、氮气流量3000-4000L/h;机械加工:待喷涂所得靶材到达所定尺寸后,对成型的靶材进行外形机械加工,加工后进行清洁包装即得到管状旋转高纯硅溅射靶材。
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CN109267019A (zh) * | 2017-07-17 | 2019-01-25 | 宁波江丰电子材料股份有限公司 | 硅旋转靶材及其制备方法 |
CN107675120B (zh) * | 2017-09-05 | 2019-11-19 | 中国科学院上海硅酸盐研究所 | 一种在钼或钼合金表面制备硅化钼涂层的方法 |
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CN112582528B (zh) * | 2020-12-28 | 2023-04-07 | 杭州博源光电科技有限公司 | 一种新型大功率激光探测器中热电堆的制备方法 |
CN112899628A (zh) * | 2021-01-18 | 2021-06-04 | 福建阿石创新材料股份有限公司 | 一种可均匀溅射旋转硅靶材及其制备方法 |
CN113481477A (zh) * | 2021-06-21 | 2021-10-08 | 芜湖映日科技股份有限公司 | 高透过率硅旋转溅射靶材的制备方法 |
CN113862621A (zh) * | 2021-09-17 | 2021-12-31 | 芜湖映日科技股份有限公司 | 一种旋转硅铬靶材制备方法 |
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CN203947155U (zh) * | 2014-06-20 | 2014-11-19 | 江阴恩特莱特镀膜科技有限公司 | 一种制备旋转高纯硅靶的烧结炉 |
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