CN113930733B - 用于铁氧体加工的磁控溅射方法 - Google Patents
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 44
- 238000001755 magnetron sputter deposition Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 23
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- 239000000758 substrate Substances 0.000 claims abstract description 48
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910018487 Ni—Cr Inorganic materials 0.000 claims abstract description 8
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003814 drug Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 229910052786 argon Inorganic materials 0.000 claims abstract description 6
- 239000012459 cleaning agent Substances 0.000 claims abstract description 6
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- 238000004321 preservation Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 11
- 239000011651 chromium Substances 0.000 claims description 7
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 5
- 238000004544 sputter deposition Methods 0.000 description 5
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- 229910001120 nichrome Inorganic materials 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- BIJOYKCOMBZXAE-UHFFFAOYSA-N chromium iron nickel Chemical compound [Cr].[Fe].[Ni] BIJOYKCOMBZXAE-UHFFFAOYSA-N 0.000 description 3
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- 241001330002 Bambuseae Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 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
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- 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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
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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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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Abstract
本发明公开了用于铁氧体加工的磁控溅射方法,(1)、清洗铁氧体裸基板:清洗剂水浴超声震荡→QDR清洗→纯水超声→QDR清洗→纯水超声→QDR清洗→纯水超声→无水乙醇超声→无水乙醇保存;(2)、镀膜:将铁氧体裸基板从无水乙醇取出,使用镊子逐片夹取,吹干表面残余药液,现取现用,镍铬靶材功率为1kw,氩气流量200sccm,对铁氧体裸基板进行磁控溅镀,得到对应膜层厚度0.04um‑0.06um的板材。本发明的有益效果是经过对磁控溅射的工艺进行改进,得到了膜层厚度在0.06um以下的板材,且膜层与基板的结合力满足要求。
Description
技术领域
本发明涉及半导体器件制造工艺技术领域,尤其涉及用于铁氧体加工的磁控溅射方法。
背景技术
铁氧体材料具有很高的导磁率,可以使电感的线圈绕组之间在高频高阻的情况下产生的电容最小。由于上述特性,铁氧体材料广泛应用于印制电路板、电源线和数据线上,可以有效防止近场通信(Near Field Communication,NFC)信号被金属、电池等所吸收,增加天线的磁场强度,有效增加通信感应距离。
在印制电路板中,铁氧体材料是电路装置中的基板,而电路元件会穿过基板中的导通孔,另外铁氧体表面会镀上一层导电材料作为介质层,再将金属材料电镀在金属层上成为导线,称为金属化。如果导通孔表面有熔渣和热影响,介质层容易剥离,从而导致整个电路不能工作。因此要求导通无锥度,孔内部光滑无毛刺,表面无翻渣无热影响。
中国发明专利公开号CN113097684A公开了一种微波铁氧体隔离器基板的制作方法,包括:磁控溅射镍铬铁合金靶材在铁氧体基片表面沉积形成打底层复合膜。本发明通过定制特定比例的镍铬铁合金靶材,以磁控溅射的方式完成镍铬铁复合膜在铁氧体基片上的淀积;
又如中国发明专利授权公告号CN104733179B公开了铁氧体基板FePt永磁薄膜的制备方法,包括如下步骤:(A)将基片放入盛有去离子水的结晶皿中,用超声波清洗机清洗,再将基片放入盛有去离子水的陶瓷坩埚中,在可调功率设备上加热至去离子水沸腾,最后用竹镊子将基片放于红外灯下烘烤;(B)用N2气枪吹N2气洁净基片,用镊子把基片放置在基片托上;给预真空室充气;给预真空室排气。采取直流磁控溅射厚度为1-2nm的Cr层,作为缓冲层,直流共溅射 Fe ,Pt 靶的方式沉积厚度为2-4nm的FePt 层,这两种膜层结构交替沉积5-50次。
上述铁氧体基板的磁控溅镀对厚度都没有说明,而在实际生产中客户往往会对膜层厚度有要求,一般要求膜层厚度越薄越好,最好能控制在0.06um以下,但膜层越薄结合力就越弱,为了达到客户的要求需要对现有的磁控溅镀工艺进行改进,同时还要满足膜层结合力的要求。
发明内容
本发明要解决的技术问题是现有的铁氧体基片的磁控溅射靶材选用镍铬合金溅镀时厚度无法控制,为此提供一种以镍铬合金作为靶材的用于铁氧体加工的磁控溅射方法。
用于铁氧体加工的磁控溅射方法,包括以下步骤:(1)、清洗铁氧体裸基板:清洗剂水浴超声震荡→QDR清洗→纯水超声→QDR清洗→纯水超声→ QDR清洗→纯水超声→无水乙醇超声→无水乙醇保存;(2)、镀膜:将铁氧体裸基板从无水乙醇取出,使用镊子逐片夹取,吹干表面残余药液,现取现用,镍铬靶材功率为1kw,氩气流量200sccm,对铁氧体裸基板进行磁控溅镀,得到对应膜层厚度0.04um -0.06um的板材。
上述方案中所述步骤(1)中清洗剂水浴超声震荡时间为30min,水浴的温度是常温,药水配比为1:20。
上述方案中所述步骤(1)中QDR清洗的时间为15min。
上述方案中所述步骤(1)中纯水超声的时间为15min。
上述方案中所述步骤(1)中无水乙醇超声的时间为15min。
上述方案中所述步骤(1)的铁氧体裸基板放在清洗治具内清洗。
上述方案中所述步骤(2)的镍铬重量比例为54%:46%。
上述方案中所述铁氧体裸基板规格为57*57*0.5mm或者50.8*50.8*0.4mm。
上述方案中所述步骤(2)之后磁控溅射Cu靶材,Cu靶材功率4250W,氩气流量200sccm。
本发明的有益效果是经过对磁控溅射的工艺进行改进,得到了膜层厚度在0.06um以下的板材,且膜层与基板的结合力满足要求。
附图说明
图1是现有磁控溅镀工艺中经过清洗的基板照片;
图2是本发明的磁控溅镀工艺中经过清洗的基板照片;
图3-1是本发明的基板附着力测试中划片时的照片;
图3-2是本发明的基板附着力测试中剥离时的照片。
具体实施方式
下面结合附图,对本发明实施例中的技术方案进行清楚、完整地描述。显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所有其他实施例,都属于本发明的保护范围。
铁氧体加工工艺流程为:来料检验→清洗→SPU镀膜→干膜湿贴→曝光显影→真空包装(厂内制程)→电镍金→退膜→蚀刻。
1、来料检验:目检基板表面是否有划伤,裂纹等异常;基板尺寸:L*W*H(长*宽*厚), 铁氧体裸基板规格为57*57*0.5mm或者50.8*50.8*0.4mm,基板粗糙度Ra=0.019-0.03之间(为抛光片)
2、清洗:
①目的:清洗表面油渍等有机物污渍、去除表面异物等;
②原先的清洗流程如下: QDR→NaOH→QDR→HCl→QDR→IPA→晾干→150摄氏度烘烤2H以上。
通过外观检验,如图1所示,发现基板表面存在白印,为此申请人通过对清洗流程做出改进,清洗剂水浴超声震荡(30min,常温,药水配比1:20)→QDR(15min)→纯水超声(15min)→QDR(15min)→纯水超声(15min)→QDR(15min)→纯水超声→无水乙醇超声(15min)→无水乙醇保存,保鲜膜封口,基片完全浸没在无水乙醇内,如图2所示,除吹干时镊子夹持点外,无其他表面不良,结果较优。
以上的清洗工艺可以称之为磁控溅镀的前工艺,清洗工艺的效果直接对磁控溅镀的效果产生影响,如果基板表面存在白印,会给磁控溅镀带来不利的影响,甚至影响成品的良品率。
3、磁控溅镀:
现有的镍铬靶材溅镀功率为3000W(对应的工作电压是380V-398V),或者4000 W(对应的工作电压是389V-420V),或者5000w (对应的工作电压是410V-426V),或者6000w(对应的工作电压是417V-446V),对应膜层厚度0.15um、0.26um、0.32um、0.4um,超出预期值0.08μm。
由此申请人想通过调试镍铬靶材溅镀功率以此来降低膜层厚度,将铁氧体裸基板从无水乙醇取出,使用镊子逐片夹取,吹干表面残余药液,现取现用,镍铬靶材功率为1kw,氩气流量200sccm,对铁氧体裸基板进行磁控溅镀,得到对应膜层厚度0.04um -0.05um的板材。
在对该板材未经溅射区域进行取样,以SEM-EDS方式测量元素含量,ICP方式未测,因为主基体为铬时无法进行测量,仅支持主基体为铜或铁进行杂质元素的测量。测量前不进行清洗处理,测量结果是镍铬的重量比约为Ni:Cr=4:6 ,镍铬的重量比对镀层厚度也有影响,不同的镍铬比例会影响激发效率。
申请人通过降低镍铬靶材的溅镀功率,做了以下如表2所示的试验:
表2
从表2推知镍铬靶材与磁控溅镀成膜速度之间的关系,如表3所示
表3
最终确认为使用NiCr靶功率1KW进行制样,对应膜层厚度约0.05-0.06μm。
对板材进行附着力测试如图3-1、图3-2所示,划片后使用胶带无法剥离。说明本发明的经过改变膜层厚度的基板附着力符合要求。
Claims (4)
1.用于铁氧体加工的磁控溅射方法,其特征是:包括以下步骤:(1)、清洗铁氧体裸基板:清洗剂水浴超声震荡→QDR清洗→纯水超声→QDR清洗→纯水超声→ QDR清洗→纯水超声→无水乙醇超声→无水乙醇保存;(2)、镀膜:将铁氧体裸基板从无水乙醇取出,使用镊子逐片夹取,吹干表面残余药液,现取现用,镍铬靶材功率为1kW,氩气流量200sccm,对铁氧体裸基板进行磁控溅射,得到对应膜层厚度0.04μm -0.06μm的板材;所述清洗剂水浴超声震荡时间为30min,水浴的温度是常温,药水配比为1:20;所述QDR清洗的时间为15min;所述纯水超声的时间为15min;所述无水乙醇超声的时间为15min;所述镍铬靶材中镍铬重量比例为4:6。
2.如权利要求1所述的用于铁氧体加工的磁控溅射方法,其特征是:所述步骤(1)的铁氧体裸基板放在清洗治具内清洗。
3.如权利要求1所述的用于铁氧体加工的磁控溅射方法,其特征是:所述铁氧体裸基板规格为57*57*0.5mm或者50.8*50.8*0.4mm。
4.如权利要求1所述的用于铁氧体加工的磁控溅射方法,其特征是:所述步骤(2)之后磁控溅射Cu靶材,Cu靶材功率4250W,氩气流量200sccm。
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