CN113005413B - 一种微波介质陶瓷表面镀银的pvd工艺 - Google Patents
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Abstract
本发明公开了一种微波介质陶瓷表面镀银的PVD工艺,采用真空平面磁控溅射镀膜,首先陶瓷件预处理清洗,进真空室加热,并对真空室抽真空;然后真空室通入氩气,进行离子清洗;最后对陶瓷件进行镀膜,包括:关闭氩气、辅助偏压,在陶瓷件上镀膜Cr层,形成打底层;在打底层上镀膜Ag/Cu/Cr合金层,形成第一过渡层;在第一过渡层上镀膜Ag/Cu合金层,形成第二过渡层;在第二过渡层上镀膜Ag层,完成镀银。本发明的真空平面磁控溅射镀膜工艺,原材料以惰性气体和固体金属靶材为主,在100‑300℃温环境下沉积金属膜;本发明制程短、工艺制程简单、工艺流程环保、成本低且单件产品能耗比低。
Description
技术领域
本发明涉及镀银工艺技术领域,尤其涉及一种微波介质陶瓷表面镀银的PVD工艺。
背景技术
微波介质陶瓷(MWDC)是指应用于频率较高的微波频段电路中作为介质材料并完成一种或多种功能的介电陶瓷,要求其具有较高的介电常数(εr),高的电学品质因数(Q)、接近0的介电常数的温度系数(τf)、低介质损耗(tgδ),合适的线膨胀系数和足够的机械强度。微波介质陶瓷制作的滤波器、谐振器等主要用于商用无线通信(0.4-1GHz),电视接收(2-5GHz),直接广播 (11 -13GHz)和卫星通信(20-30GHz)等系统。
目前微波介质陶瓷表面涂银层是采用的“烧银法”工艺。烧银法是指在介质陶瓷表面烧渗一层银,作为电容器、滤波器的电极或集成电路基片的导电网络,其工艺流程:陶瓷件预处理、银浆的配制(含银原料、熔剂、粘合剂)、涂敷、烧银。
其中,银浆配制含多种重金属化合物和酸碱,主要成分如下:含银原料需要用到三乙醇胺[N(CH2CH2OH)3]、Ag2CO3或者AgNO3、氨水、甲醛(甲酸)进行化学合成得到;熔剂包括铅硼熔块(或者铋镉熔块)和低熔点的硼酸铅化合物;粘合剂常用松节油,松油醇及环己酮。烧银阶段工艺复杂,主要分四个阶段:室温- 350℃,主要除去黏合剂,这时有大量气体产生,所以通风排气升温速度不超过每小时150℃-200℃;350℃-500℃,碳酸银与氧化银分解为银;500℃-910℃,硼酸铅先熔化成玻璃态,氧化铋也熔化,与银颗粒构成悬浮态玻璃液,使银颗粒彼此黏结,玻璃液润湿瓷件并渗入起反应,形成过渡层,使银层与瓷件牢固结合;冷却阶段,冷却要快,为了获得结晶细密的银层。
发明内容
本发明的目的在于提供一种微波介质陶瓷表面镀银的PVD工艺,以解决上述背景技术中所提出的问题。
为达到上述目的,本发明采用的技术方案是:一种微波介质陶瓷表面镀银的PVD工艺,采用真空平面磁控溅射镀膜,包括如下步骤,
S1)陶瓷件预处理清洗,进真空室加热,并对真空室抽真空;
S2)离子清洗:通入氩气使真空室的真空度达到(5.0-9.0)*10-1Pa,Cr靶和Cu靶电流为0.1A-0.5A、或Cr靶和Cu靶电压为100V-350V,离子源功率为100W-1000W,工件偏压电压为-200V--600V,占空比为30%-80%;
S3)对陶瓷件进行镀膜,其包括:
S31)关闭氩气、辅助偏压,在陶瓷件上镀膜Cr层,形成打底层;
S32)在打底层上镀膜Ag/Cu/Cr合金层,形成第一过渡层;
S33)在第一过渡层上镀膜Ag/Cu合金层,形成第二过渡层;
S34)在第二过渡层上镀膜Ag层,完成镀银。
作为进一步的优化,S1中真空室加热温度为100-300℃,加热时间30-120 min;真空室的本底真空降至(1.0-6.0)*10-3Pa。
作为进一步的优化,S2中氩气流量为200-600sccm,清洗时间为30-180min。
作为进一步的优化,S3中氮气流量保持400sccm,真空室温度保持200℃,真空度为(1.0-6.0)*10-3Pa。
作为进一步的优化,S31中采用单靶电源作为Cr靶的溅射电源,Cr靶靶电流设定为15A-40A,Cr靶靶电压为300V-600V,离子源功率设定300W-1000W,镀膜时间为2-30min,工件偏压电压为-50V--350V,占空比为20%-80%。
作为进一步的优化,S32中采用中频电源作为Cu靶的溅射电源,Cu靶靶电流为10A-30A,Cu靶靶电压200V-600V,Cr靶靶电流设定为15A-40A,Cr靶靶电压为200V-600V,离子源功率设定500W-1500W,镀膜时间为10-60min,工件偏压电压为-100V-0V,占空比20%-80%。
作为进一步的优化,S33中Cu靶靶电流为10A-30A,Cu靶靶电压200V-600V,离子源功率设定500W-1500W,镀膜时间为30-120min,工件偏压电压为-100V-0V,占空比20%-80%。
作为进一步的优化,S34中离子源功率设定500W-1500W,镀膜时间为60-240min,工件偏压电压为-100V-0V,占空比20%-80%。
作为进一步的优化,溅射电源频率为20-180 KHz,功率为 20-60 KW;离子源作为Ag的靶源。
与已有技术相比,本发明的有益效果体现在:
1.本发明的真空平面磁控溅射镀膜工艺,原材料以惰性气体和固体金属靶材为主,在100-300℃温环境下沉积金属膜;
2.本发明制程短、工艺制程简单、工艺流程环保、成本低且单件产品能耗比低。
附图说明
图1为本发明的陶瓷件镀银示意图。
图中,1.陶瓷件;2.底层;3.第一过渡层;4.第二过渡层;5.银层。
具体实施方式
以下是本发明的具体实施例,结合附图对本发明的技术方案作进一步的描述,但本发明并不限于这些实施例。
一种微波介质陶瓷表面镀银的PVD工艺,采用真空平面磁控溅射镀膜,包括如下步骤,
S1)进炉抽真空:基材陶瓷件1预处理清洗后,进真空炉加热至200℃,加热时间90min,同时真空室抽真空,使真空室的本底真空降至 3.5*10-3 Pa;
S2)金属离子清洗:通入氩气使真空室的真空度达到 7.0*10-1 Pa,氩气流量为500sccm,Cr靶和Cu靶电流设定为0.2A,离子源功率设定200W,工件偏压电压为-500V,占空比35%,离子清洗时间90 min;
S3)镀膜:镀膜阶段氮气流量保持400sccm,真空室温度保持200℃;
S31)打底层2:离子清洗后,关闭氩气、辅助偏压,抽真空至真空室的真空度达到3.5*10-3 Pa,打底层为Cr层,采用单靶电源作为Cr靶的溅射电源,Cr靶靶电流设定为20A,Cr靶靶电压为450V,离子源功率设定700W,镀膜时间为10min,工件偏压电压为-200V,占空比为50%;
S32)第一过渡层3:第一过渡层为Ag/Cu/Cr合金层,采用中频电源作为Cu靶的溅射电源,Cu靶靶电流为20A,Cu靶靶电压500V,Cr靶靶电流设定为20A,Cr靶靶电压为450V,离子源功率设定700W,镀膜时间为30min,工件偏压电压为-80V,占空比50%;
S33)第二过渡层4:第二过渡层为Ag/Cu合金层,Cu靶靶电流为20A,Cu靶靶电压500V,离子源功率设定1000W,镀膜时间为60min,工件偏压电压为-50V,占空比30%;
S34)镀银层5:镀银层为Ag金属层,离子源功率设定1000W;镀膜时间为120min;工件偏压电压为-50V,占空比30%。
通过上述步骤镀膜后,陶瓷表面Lab值为:L*= 99.82,a*= 1.40,b*=4.25;用万用表测试镀银陶瓷样品表面接触电阻为2-4mΩ,焊接性能良好。
本文中所描述的具体实施例仅仅是对本发明精神作举例说明。本发明所属技术领域的技术人员可以对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,但并不会偏离本发明的精神或者超越所附权利要求书所定义的范围。
Claims (8)
1.一种微波介质陶瓷表面镀银的PVD工艺,其特征在于,采用真空平面磁控溅射镀膜,包括如下步骤,
S1)陶瓷件预处理清洗,进真空室加热,并对真空室抽真空;
S2)离子清洗:通入氩气使真空室的真空度达到(5.0-9.0)*10-1Pa,Cr靶和Cu靶电流为0.1A-0.5A、或Cr靶和Cu靶电压为100V-350V,离子源功率为100W-1000W,工件偏压电压为-200V--600V,占空比为30%-80%;
S3)对陶瓷件进行镀膜,其包括:
S31)关闭氩气、辅助偏压,在陶瓷件上镀膜Cr层,形成打底层;
S32)在打底层上镀膜Ag/Cu/Cr合金层,形成第一过渡层;
S33)在第一过渡层上镀膜Ag/Cu合金层,形成第二过渡层;
S34)在第二过渡层上镀膜Ag层,完成镀银;
其中,S31中采用单靶电源作为Cr靶的溅射电源,Cr靶靶电流设定为15A-40A,Cr靶靶电压为300V-600V,离子源功率设定300W-1000W,镀膜时间为2-30min,工件偏压电压为-50V--350V,占空比为20%-80%。
2.根据权利要求1所述的微波介质陶瓷表面镀银的PVD工艺,其特征在于,S1中真空室加热温度为100-300℃,加热时间30-120min;真空室的本底真空降至(1.0-6.0)*10-3Pa。
3.根据权利要求1所述的微波介质陶瓷表面镀银的PVD工艺,其特征在于,S2中氩气流量为200-600sccm,清洗时间为30-180min。
4.根据权利要求1所述的微波介质陶瓷表面镀银的PVD工艺,其特征在于,S3中氮气流量保持400sccm,真空室温度保持200℃,真空度为(1.0-6.0)*10-3Pa。
5.根据权利要求1所述的微波介质陶瓷表面镀银的PVD工艺,其特征在于,S32中采用中频电源作为Cu靶的溅射电源,Cu靶靶电流为10A-30A,Cu靶靶电压200V-600V,Cr靶靶电流设定为15A-40A,Cr靶靶电压为200V-600V,离子源功率设定500W-1500W,镀膜时间为10-60min,工件偏压电压为-100V-0V,占空比20%-80%。
6.根据权利要求1所述的微波介质陶瓷表面镀银的PVD工艺,其特征在于,S33中Cu靶靶电流为10A-30A,Cu靶靶电压200V-600V,离子源功率设定500W-1500W,镀膜时间为30-120min,工件偏压电压为-100V-0V,占空比20%-80%。
7.根据权利要求1所述的微波介质陶瓷表面镀银的PVD工艺,其特征在于,S34中离子源功率设定500W-1500W,镀膜时间为60-240min,工件偏压电压为-100V-0V,占空比20%-80%。
8.根据权利要求1所述的微波介质陶瓷表面镀银的PVD工艺,其特征在于,溅射电源频率为20-180kHz ,功率为20-60kW ;离子源作为Ag的靶源。
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