CN113322394A - 一种封装用高性能键合铂合金微细材及其制备方法 - Google Patents
一种封装用高性能键合铂合金微细材及其制备方法 Download PDFInfo
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- CN113322394A CN113322394A CN202110523285.7A CN202110523285A CN113322394A CN 113322394 A CN113322394 A CN 113322394A CN 202110523285 A CN202110523285 A CN 202110523285A CN 113322394 A CN113322394 A CN 113322394A
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- 229910001260 Pt alloy Inorganic materials 0.000 title claims abstract description 55
- 239000000463 material Substances 0.000 title claims abstract description 55
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 67
- 239000000956 alloy Substances 0.000 claims abstract description 67
- 238000000137 annealing Methods 0.000 claims abstract description 47
- 238000010438 heat treatment Methods 0.000 claims abstract description 33
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000009749 continuous casting Methods 0.000 claims abstract description 23
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 20
- 238000005096 rolling process Methods 0.000 claims abstract description 16
- 229910052790 beryllium Inorganic materials 0.000 claims abstract description 15
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 14
- 229910052732 germanium Inorganic materials 0.000 claims abstract description 14
- 238000005266 casting Methods 0.000 claims abstract description 11
- 238000007711 solidification Methods 0.000 claims abstract description 10
- 230000008023 solidification Effects 0.000 claims abstract description 10
- 238000005275 alloying Methods 0.000 claims abstract description 9
- 238000003280 down draw process Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 44
- 230000008569 process Effects 0.000 claims description 25
- 238000012545 processing Methods 0.000 claims description 23
- 238000002844 melting Methods 0.000 claims description 18
- 230000008018 melting Effects 0.000 claims description 18
- 229910052697 platinum Inorganic materials 0.000 claims description 15
- 239000000498 cooling water Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 238000003723 Smelting Methods 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 8
- 239000000155 melt Substances 0.000 claims description 8
- 230000006698 induction Effects 0.000 claims description 7
- 229910052741 iridium Inorganic materials 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 238000007670 refining Methods 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 238000010791 quenching Methods 0.000 claims description 4
- 230000000171 quenching effect Effects 0.000 claims description 4
- 238000005496 tempering Methods 0.000 claims description 4
- 229910052787 antimony Inorganic materials 0.000 claims description 3
- 229910052797 bismuth Inorganic materials 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052745 lead Inorganic materials 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000005538 encapsulation Methods 0.000 claims 7
- 238000005260 corrosion Methods 0.000 abstract description 8
- 230000007797 corrosion Effects 0.000 abstract description 8
- 239000004065 semiconductor Substances 0.000 abstract description 8
- 238000011161 development Methods 0.000 abstract description 6
- 238000000746 purification Methods 0.000 abstract description 2
- 230000001276 controlling effect Effects 0.000 description 7
- 238000004100 electronic packaging Methods 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- -1 platinum iridium yttrium Chemical compound 0.000 description 5
- HWLDNSXPUQTBOD-UHFFFAOYSA-N platinum-iridium alloy Chemical class [Ir].[Pt] HWLDNSXPUQTBOD-UHFFFAOYSA-N 0.000 description 5
- 229910000566 Platinum-iridium alloy Inorganic materials 0.000 description 4
- 238000007669 thermal treatment Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052703 rhodium Inorganic materials 0.000 description 3
- 239000010948 rhodium Substances 0.000 description 3
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 238000010891 electric arc Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- 229910001020 Au alloy Inorganic materials 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910000946 Y alloy Inorganic materials 0.000 description 1
- LIXXICXIKUPJBX-UHFFFAOYSA-N [Pt].[Rh].[Pt] Chemical compound [Pt].[Rh].[Pt] LIXXICXIKUPJBX-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000005548 dental material Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000003353 gold alloy Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- DYXZHJQUDGKPDJ-UHFFFAOYSA-N iridium;oxoplatinum Chemical compound [Ir].[Pt]=O DYXZHJQUDGKPDJ-UHFFFAOYSA-N 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
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- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
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Abstract
本发明涉及一种封装用高性能键合铂合金微细材及其制备方法,属于封装键合材料技术领域。该键合铂合金微细材各组分的重量百分比为:Ir:0%~60%,Ge:0%~5.0%,Be、Dy和Eu中的一种或几种,Be、Dy和Eu总含量为0.03%~0.1%,余量为Pt。其制备步骤包括制备中间合金、下引连续+定向凝固铸造合金化、粗拉+在线退火+精拉及精密轧制+在线电阻加热软化处理。该合金具有高纯化、超细化、高精化的优点,同时具有强度高、耐腐蚀性好、使用寿命长、满足极端恶劣环境使用需求等优点,适合特殊领域的封装键合需求,特别是满足芯片窄间距微型化、高可靠、高稳定性应用需求,对高端半导体器件的发展意义重大。
Description
技术领域
本发明涉及一种封装用高性能键合铂合金微细材及其制备方法,属于封装键合材料技术领域。
背景技术
引线键合是一种使用细金属线,利用热、压力、超声波能量使金属引线与基板焊盘紧密焊合,实现芯片与基板间的电气互连和芯片间的信息互通,是微电子领域常用的封装材料。键合丝的品种从传统的键合金丝、键合铝丝发展到现在的多品种多型号,最近十几年发展起来的有键合铜丝、键合银丝、键合金合金丝、键合银合金丝、键合镀钯铜丝及键合镀金银丝等。键合丝产品的规格从20μm到50μm不等,绕在线轴上的成品长度从500米到6000米不等。键合丝主要应用在:集成电路(IC)、半导体分立器件(TR)、半导体照明(LED)、摄像头模组(COB)等。近几十年来,中国的半导体电子随着国际上大发展也有着快速发展,国家在半导体电子研发和制造上加大了投入和刺激,但国内的技术水平离国际一流的企业还有一定距离,尤其在基础的半导体材料研制方面。同时,国际上键合丝制造朝着更精细,更长,性能稳定性要求更高的方向发展,这对键合丝制造提出更高的要求,传统的键合材料已不能完全满足关键重点领域高可靠长寿命的封装键合需求。
铂合金具有高硬度、高熔点及优良的耐腐蚀性能和低的接触电阻,因此在工业中有极为广泛的应用。铂合金中铱的加入会显著提高铂的抗化学腐蚀能力,具有稳定的电化学参数,铂铱合金有高的硬度、高的熔点、高的耐腐蚀能力和低的接触电阻,且使用可靠、寿命长,常用作电接触材料,如航空发动机上的点火接触点、高灵敏度继电器和舰艇上的电螺经重力摆继电器等;铂铱合金也常被用作电极材料以及牙科材料。铂铱合金在各种电传感器也有广泛应用,如飞机、导电、舰艇的导向仪、陀螺仪等。此外,铂铱合金在热电偶等领域也有一定的应用。
国内在相关领域开展了广泛的研究。专利CN101948965 A新型铂合金电接触材料及其制备方法公开了一种铂铱合金电接触材料各组分的重量百分比为5.0-30.0%Ir,0.1-5.0%Nb,0.1-5.0%Zr,0.1-5.0%Mo,0.1-5.0%Ta,0.1-5.0%Yb,0.1-5.0Gb,0.1-5.0Tb,余量为Pt。通过高频或中频熔炼、轧制、拉拔、热处理等工艺加工,最终形状为板状、棒状或触头等成品。专利CN107916339新型铂铱钇合金电接触材料及其制备方法中提到:Ir5~25%、Y1~1.5%余量为Pt,于电弧炉中真空熔炼,得初次铸锭后,粉碎成颗粒,混料,再次真空电弧熔炼,在1000-1300℃热轧开坯。冷加工结合热处理得到成品,稀土元素可降低贵金属含量,改善电接触性能。专利CN 104294311 B公开了一种铂铱氧化物合金电极的制备方法,通过化学方法制得适于氧化电解水制备的铂铱氧化物钛阳极催化材料。专利CN101561322A弥散强化铂铑-铂热电偶丝及其生产方法中提到在正负极材料中添加Zr 0~0.5%;钇0~0.5%;钙0~0.5%;镧0~0.5%;钛0~0.5%,余量为铂;此外,正极材料中含12.87-13%的铑。通过添加元素得到的弥散强化铂的断裂寿命是普通铂的100倍以上,铂铑的寿命是普通铂铑的10倍以上。
由此可见,铂合金因具有特殊的高强度、高硬度以及耐腐蚀性能等优点,在电接触材料等国民经济领域具有广泛的应用,产品形态主要有板状、带状、棒状以及丝状,而针对铂合金作为封装键合材料目前鲜有报道,且有关微细材的报道也较少。作为封装键合材料与电接触材料不同的是,除了要求具有高的机械性能、良好的电性能外,还要求具有良好的键合性能、高强度、低弧度等特性。且随着半导体器件的小型化、高密度、高可靠、大功率、耐恶劣环境、长寿命等方向发展的需要,一方面对高性能封装键合微细丝提出了迫切的需求,另一方面封装键合微型窄薄带材成为解决半导体器件小间距高密度技术发展的亟需。
发明内容
本发明针对高端封装键合材料要求,通过优化合金成分、改进工艺等技术,获得了一种满足LQFP、SIP等高端封装用高性能铂合金键合微细丝及键合扁带。
本发明的主要目的在于提供一种电子封装键合用高性能铂合金微细材,通过优化合金成分,提高键合铂合金丝的机械性能,提高再结晶温度,缩小热影响区,改善键合丝的焊接性能,使其满足高端封装要求。
本发明的另一目的在于提供上述铂合金微细材的制备方法,通过改进工艺,改善高强度、高硬度铂合金丝的加工性能,合金化过程中避免晶内偏析和减少树枝状结构的生成,为微后续细材的成形提供保障。
为了达到上述目的,本发明采用的技术方案为:
一种高端电子封装用高性能键合铂合金微细材,铂合金各组分的重量百分比为:Ir:0%~60%,Ge:0%~5.0%,Be、Dy和Eu中的一种或几种,Be、Dy和Eu总含量为0.03%~0.1%,余量为Pt。
其中,Ir的质量含量可为0.01%~60%,Ge的质量含量可为0.01%~5.0%。
进一步地,Ir的质量含量为0.1%~50%,Ge的质量含量为0.1%~4.0%。
优选的,Ir的质量含量为0.5%~40%,Ge的质量含量为0.5%~3.5%。
更优选的,Ir的质量含量为1.0%~35%,Ge的质量含量为1.0%~3.0%。
最优选的,Ir的质量含量为10%~30%,Ge的质量含量为1.5%~2.5%。
本发明通过添加Ir提高铂合金的强度并显著提高铂的抗化学腐蚀能力;通过添加Ge和Be降低铂合金的熔点,降低贵金属铂和铱的用量,同时可进一步提高合金的强度,保证键合微细材的性能;通过添加稀土元素Dy、Eu可起到细化晶粒的作用,有利于后续的加工,保证加工性能。通过Ir、Ge、Be及Dy和/或Eu的共同作用,可提供铂合金微细材的综合性能,特别是力学性能,保证关键型号器件的键合强度和封装可靠性,从而满足重点工程发展需求。
所述的电子封装用高性能键合铂合金微细材包括键合微细丝和键合微细扁带,微细丝直径≥25μm,微细丝直径优选为25-100μm;微细扁带规格:厚度为12.5~25μm,宽度为50~500μm。
上述铂合金微细材的制备方法,包括以下步骤:
(1)中间合金制备:以Pt与Dy或Eu为原材料,采用真空中频感应熔炼方法制备Pt-Dy和/或Pt-Eu中间合金;
(2)“下引连铸+定向凝固”合金化:以Pt、Ir、Ge、Be以及Pt-Dy和/或Pt-Eu中间合金为原材料,采用真空中频感应熔炼方法制备合金熔体;采用下引连续铸造方法,并在凝固过程中通过控制熔体温度、连铸速度和冷却水流量等,在凝固合金和未凝固合金熔体中建立起特定方向的温度梯度,从而使熔体沿着与热流相反的方向凝固,最终得到具有特定取向(单晶)显微组织的合金圆棒;
(3)将上述的合金圆棒通过真空退火和拉拔加工制成微细丝,丝材直径为25-100μm;
(4)对成品微细材进行调质热处理,得到键合微细丝;
或者,将制得的微细丝通过精密轧制和在线加热软化处理一体工艺,得到键合微细扁带。
在上述方案的步骤(1)和(2)中,所述原材料Pt、Dy、Eu、Be、Ge纯度均≥99.99%,Ir纯度≥99.95%,中间合金及合金锭坯中Pb、Sb、Bi、Fe等杂质元素含量小于15ppm,杂质总量小于50ppm。
步骤(1)中,采用真空中频感应熔炼方法制备Pt-Dy、Pt-Eu中间合金过程中,真空度为1.0×10-3Pa~1.0×10-4Pa,熔炼温度为1600~2000℃,完全熔化后,静置1~3min精炼,然后关闭真空,充入氩气,快速浇铸到水冷铜模中得到中间合金锭坯。
步骤(2)中,将Pt、Pt-Dy中间合金、Pt-Eu中间合金、Ir、Ge和/或Be放入坩埚内,抽真空加热熔化,得到合金熔体;在连铸过程中,合金熔体温度为1750~1950℃,拉铸速度为50~150mm/min,冷却水流量为150~300L/h。合金圆棒的直径为Φ8mm。
步骤(3)中,所述合金圆棒的退火条件:在真空退火炉中热处理,真空度为1.0×10-3Pa~1.0×10-4Pa,温度为1100~1300℃,保温2~3.5h;拉拔加工过程中道次加工变形量为5~10%,两次退火间的总加工量≤50%;道次间退火的真空度为1.0×10-3Pa~1.0×10-4Pa,温度为800-900℃,保温时间1.5-2h。
步骤(4)中,键合微细丝/带的拉断力和延伸率呈反向关系,为获得良好的使用效果,在满足延伸率指标要求的基础上,微细丝/扁带拉断力应控制在一定范围,当拉断力过高时,会造成弹力过大及回旋等不足。进一步通过热处理,对成品微细丝/扁带进行调质热处理,将拉断力和延伸率调控到合理范围。成品微细丝/扁带的退火温度为650~800℃,在线退火速度为10~15m/min;或采用在线电阻加热,功率为15-20Kw,在线退火速度为10~15m/min。
步骤(4)中,制备微细扁带时,采用多棍轧机进行精密轧制。
制备键合微细扁带所需微细丝的尺寸通过以下公式换算:
本发明的有益效果:
(1)本发明通过添加微量元素结合下引连铸方法制得的铂合金锭坯组织均匀细小,且合金成分均匀无偏析、产品的纯净度高、没有表面裂纹、冷隔、夹杂、表面氧化等缺陷,表面光洁度高。保证合金强度的同时有利于后续的冷加工,可以减少加工过程中的中间退火次数,为微细材的成形提供保障。
(2)与普通铸造相比,本发明采用下引连铸减少了铸锭中的轴向晶界,减少了变形过程中的位错堆积,冷加工之后可得到纤维晶组织,抗拉强度大幅度提高。同时,铸锭中的轴向晶界的减少,降低了金属的电阻,且由于真空熔炼很大程度上消除了杂质,大大优化了铸坯的导电性能。
(3)同时,本发明在软化处理过程中,利用丝材或扁带自身的导电能力通过电阻自热实现退火软化处理,清洁高效,性能均匀可调。结合成分设计、加工工艺及退火工艺控制,键合微细材的拉断力可根据需求控制在15g~50g或150-300g;延伸率可根据需求控制在1~3%或3~12%等。
(4)本发明的铂合金封装键合材料具有强度高、耐腐蚀性好、尺寸精度高等优点,而且使用寿命长,产品涵盖微细丝以及微细扁带,满足特殊领域的封装键合需求,特别是满足窄间距的芯片微型化、高可靠、高稳定性发展的应用需求。
附图说明
图1为下引连铸方法制得的铂合金锭坯组织。
具体实施方式
下面对本发明的具体实施方式作进一步描述。以下实施例仅用于更加清楚地说明本发明的技术方案,不限制本发明的保护范围。
本发明的高端电子封装用高性能键合铂合金微细材,铂合金各组分的重量百分百为:Ir:0%~60%,Ge:0%~5.0%,Dy、Eu、Be中的一种或两种以上(包括Be+Dy,Be+Eu,Dy+Eu和Be+Dy+Eu),(Be+Dy+Eu)总含量为0.03%~0.1%,余量为Pt。键合微细材料包括微细丝及微细扁带。
上述铂合金微细材的制备方法,包括以下步骤:1、制备中间合金;2、“下引连续+定向凝固”铸造合金化;3、“粗拉+在线退火+精拉”;4、“精密轧制+在线电阻加热软化处理”。
1)中间合金制备:为减少烧损、保证合金成分的均匀性,采用真空中频感应熔炼方法先制备Pt-Dy、Pt-Eu中间合金;条件为:真空度1.0×10-3Pa~1.0×10-4Pa,熔炼温度为1600~2000℃,完全熔化后,静置1~3min精炼,然后关闭真空,充入氩气,快速浇铸到水冷铜模中得到中间合金锭坯。
2)合金化:采用下引连续铸造方法,并在凝固过程中采用强制手段,在凝固合金和未凝固合金熔体中建立起特定方向的温度梯度,从而使熔体沿着与热流相反的方向凝固,最终得到具有特定取向(单晶)显微组织的Φ8mm的合金圆棒。连铸过程中,熔体温度控制在1750~1950℃,拉铸速度50~150mm/min,冷却水流量范围在150~300L/h。
3)将上述的合金圆棒经“在线退火+拉拔”加工制得不同规格的微细键合丝材,丝材直径包括:Φ25μm、Φ35μm、Φ50μm、Φ100μm等等;退火条件:在1100~1300℃,1.0×10- 3Pa~1.0×10-4Pa的真空下,在真空退火炉中热处理,保温2~3.5h;拉拔过程中道次加工变形量控制在5~10%,两次退火间的总加工量控制在≤50%。
进一步地,将制得的不同规格微细键合丝,通过“精密轧制+在线电阻加热软化处理”一体工艺,得到微细扁带,扁带尺寸包括≠12.5×75μm、≠12.7×150μm、≠25.0×150μm等等不同规格。
键合扁带的制备所需微细键合丝尺寸通过以下公式换算:
4)键合微细丝/带的拉断力和延伸率呈反向关系,为获得良好的使用效果,在满足延伸率指标要求的基础上,微细丝/扁带拉断力应控制在一定范围,当拉断力过高时,会造成弹力过大及回旋等不足。进一步通过热处理,对成品微细丝/扁带进行调质热处理,将拉断力和延伸率调控到合理范围。成品退火温度:650~800℃,在线退火速度为10~15m/min。或为电阻加热,功率:15-20Kw。
Pt-Dy、Pt-Eu中间合金及合金锭坯中Pb、Sb、Bi、Fe等杂质元素含量小于15ppm,杂质总量小于50ppm。
实施例1
制备Pt-10Dy、Pt-10Eu中间合金:
将500gPt放入坩埚内,抽真空至1×10-3Pa以下,升温至2000℃,Pt全部熔化后,温度降至1600℃时采用后加料的方式加50gDy或Eu,直至熔体全熔后温度降至1400℃,静置精炼3-5min,然后在氩气或氮气保护下迅速浇铸至水冷铜模中,从而通过瞬间冷却实现成分的均匀性,得到Pt-10Dy及Pt-10Eu中间合金。
实施例2
制备厚度为12.5μm,宽度为75μm的高端电子封装用高性能键合铂合金微细扁带,铂合金中,Ir:0.5wt%,Ge:1.0wt%,(Be+Dy):0.03wt%,余量为Pt.
1、“下引连铸+定向凝固”合金化。将5gIr、10gGe、0.2gBe、1gPt-10Dy中间合金(实施例1制备)以及983.8gPt放入坩埚内,抽真空加热到2000℃熔化;进行下引连铸,连铸速度控制在50mm/min,合金熔体温度控制在1750℃,连铸出口处控制冷却水水温在25℃以下,冷却水流量范围在150L/h,以保证熔体结晶速度,确保定向凝固的稳定性,从而实现Φ8mm单晶棒坯的近净成形。
2、“在线退火+拉拔”。将合金棒坯经过多道次拉拔结合中间热处理制备出Φ35μm的微细铂合金丝。合金棒坯在真空退火炉中热处理条件:真空度1.0×10-4Pa,1100℃保温3h;拉拔过程中道次加工变形量控制在5~10%,两次退火间的总加工量控制在≤50%。道次间退火的真空度为1.0×10-4Pa,温度为800℃,保温2h。
4、使用多棍轧机及在线退火装置,将上述铂合金丝采用“精密轧制+在线电阻加热软化处理”方法,利用丝材或扁带自身的导电能力通过电阻自热实现退火软化处理,电阻加热的功率为20Kw,在线退火速度为15m/min,得到≠12.5×75μm的微细超薄铂合金扁带。
实施例3
制备厚度为25μm,宽度为150μm的高端电子封装用高性能键合铂合金微细扁带,铂合金中,Ir:10wt%,Ge:2.5wt%,(Be+Eu):0.06wt%,余量为Pt。
1、“下引连铸+定向凝固”合金化。将100gIr、25gGe、0.5gBe以及873.5gPt放入坩埚内,抽真空加热到2000℃熔化。采用后加料方式,利用熔炼炉内的加料装置加入1gPt-10Eu中间合金(实施例1制备),熔炼1-3min;合金熔体温度控制在1850℃,冷却水水温在25℃以下,控制冷却水流量为150L/h,开展连铸,调节连铸速度控制在52mm/min,实现Φ8mm单晶棒坯的近净成形,如图1所示,为下引连铸方法制得的铂合金锭坯组织。
2、“在线退火+拉拔”。将合金棒坯经过多道次拉拔结合中间热处理制备出Φ69μm的微细铂合金丝。合金棒坯在真空退火炉中热处理条件:真空度1.0×10-4Pa,1100℃保温2.5h;拉拔过程中道次加工变形量控制在5~10%,两次退火间的总加工量控制在≤50%。道次间退火的真空度为1.0×10-4Pa,温度为850℃,保温1.5h。
4、使用多棍轧机及在线退火装置,将上述铂合金丝采用“精密轧制+在线电阻加热软化处理”方法,利用丝材或扁带自身的导电能力通过电阻自热实现退火软化处理,电阻加热的功率为15Kw,在线退火速度为12m/min,得到≠25×150μm的微细超薄铂合金扁带。
实施例4
制备厚度为12.7μm,宽度为150μm的高端电子封装用高性能键合铂合金微细扁带,铂合金中,Ir:60wt%,Ge:5.0wt%,(Be+Dy+Eu):0.1wt%,余量为Pt.
1、“下引连铸+定向凝固”合金化。将将600gIr、50gGe、0.4gBe以及343.6gPt放入坩埚内,抽真空加热到2200℃熔化,然后调节加热功率,使温度降到1950℃,采用后加料方式,利用熔炼炉内的加料装置加入3gPt-10Dy和3gPt-10Eu中间合金(实施例1制备),熔炼1-3min;合金熔体温度控制在1950℃,冷却水水温在25℃以下,控制冷却水流量范围在150L/h,开展连铸,调节连铸速度控制在55mm/min,实现Φ8mm单晶棒坯的近净成形。
2、“在线退火+拉拔”。将合金棒坯经过多道次拉拔结合中间热处理制备出Φ50μm的微细铂合金丝。合金棒坯在真空退火炉中热处理条件:真空度1.0×10-4Pa,1100℃保温2.5h;拉拔过程中道次加工变形量控制在5~10%,两次退火间的总加工量控制在≤50%。道次间退火的真空度为1.0×10-3Pa,温度为900℃,保温时间2h。
4、使用多棍轧机及在线退火装置,将上述铂合金丝采用“精密轧制+在线电阻加热软化处理”方法,利用丝材或扁带自身的导电能力通过电阻自热实现退火软化处理,电阻加热的功率为18Kw,在线退火速度为10m/min,得到≠12.7×150μm的微细超薄铂合金扁带。
对实施例2-4制备得到的键合铂合金微细扁带进行性能测试,结果见表1。
表1本发明实施例2-4的测试性能
本发明封装用高性能键合铂合金微细材包括微细丝及微细扁带,尺寸精度及力学性能可控,满足不同应用需求。本发明微细材制备过程中使用丝材或扁带自身的导电能力实现退火软化处理,性能均匀可调,方法简单且可操作性强,易于批量生产。所述合金具有高纯化、超细化、高精化的优点,同时具有强度高、耐腐蚀性好、使用寿命长、满足极端恶劣环境使用需求等优点,产品涵盖微细丝以及微细扁带,适合特殊领域的封装键合需求,特别是满足芯片窄间距微型化、高可靠、高稳定性应用需求,对高端半导体器件的发展意义重大。
Claims (10)
1.一种封装用高性能键合铂合金微细材,其特征在于:各组分的重量百分比为:Ir:0%~60%,Ge:0%~5.0%,Be、Dy和Eu中的一种或几种,Be、Dy和Eu的总含量为0.03%~0.1%,余量为Pt。
2.根据权利要求1所述的封装用高性能键合铂合金微细材,其特征在于:所述的铂合金微细材包括键合微细丝和键合微细扁带,微细丝直径≥25μm;微细扁带的厚度为12.5~25μm,宽度为50~500μm。
3.根据权利要求1或2所述的封装用高性能键合铂合金微细材的制备方法,包括以下步骤:
(1)中间合金制备:以Pt、Dy或Eu为原材料,采用真空中频感应熔炼方法制备Pt-Dy和/或Pt-Eu中间合金;
(2)合金化:以Pt、Ir、Ge、Be、Pt-Dy和Pt-Eu中间合金为原材料,采用真空中频感应熔炼方法制备合金熔体;采用下引连续铸造方法,并在凝固过程中通过控制熔体温度、连铸速度和冷却水流量,在凝固合金和未凝固合金熔体中建立起特定方向的温度梯度,从而使熔体沿着与热流相反的方向凝固,最终得到具有特定取向显微组织的合金圆棒;
(3)将所述的合金圆棒通过真空退火和拉拔加工制成微细丝,丝材直径为25-100μm;
(4)对成品微细材进行调质热处理,得到键合微细丝;
或者,将制得的微细丝通过精密轧制和在线加热软化处理一体工艺,得到键合微细扁带。
4.根据权利要求3所述的封装用高性能键合铂合金微细材的制备方法,其特征在于:原材料Pt、Dy、Eu、Be和Ge纯度≥99.99%,Ir纯度≥99.95%,中间合金及合金锭坯中Pb、Sb、Bi或Fe杂质元素含量小于15ppm,杂质总量小于50ppm。
5.根据权利要求3所述的封装用高性能键合铂合金微细材的制备方法,其特征在于:采用真空中频感应熔炼方法制备Pt-Dy、Pt-Eu中间合金过程中,真空度为1.0×10-3Pa~1.0×10-4Pa,熔炼温度为1600~2000℃,完全熔化后,静置1~3min精炼,然后关闭真空,充入氩气,浇铸到水冷铜模中得到中间合金锭坯。
6.根据权利要求3所述的封装用高性能键合铂合金微细材的制备方法,其特征在于:在连铸过程中,合金熔体温度为1750~1950℃,拉铸速度为50~150mm/min,冷却水流量为150~300L/h;所述合金圆棒的直径为Φ8mm。
7.根据权利要求3所述的封装用高性能键合铂合金微细材的制备方法,其特征在于:所述合金圆棒的退火条件:在真空退火炉中热处理,真空度为1.0×10-3Pa~1.0×10-4Pa,温度为1100~1300℃,保温2~3.5h;拉拔加工过程中道次加工变形量为5~10%,两次退火间的总加工量≤50%;道次间退火的真空度为1.0×10-3Pa~1.0×10-4Pa,温度为800-900℃,保温时间1.5-2h。
8.根据权利要求3所述的封装用高性能键合铂合金微细材的制备方法,其特征在于:成品微细丝/扁带的退火温度为650~800℃,在线退火速度为10~15m/min;或采用在线电阻加热,功率为15-20Kw,在线退火速度为10~15m/min。
9.根据权利要求3所述的封装用高性能键合铂合金微细材的制备方法,其特征在于:制备微细扁带过程中,采用多棍轧机进行精密轧制。
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