LT6899B - Vario paviršiaus cheminio nikeliavimo būdas, nenaudojant aktyvavimo paladžiu - Google Patents

Vario paviršiaus cheminio nikeliavimo būdas, nenaudojant aktyvavimo paladžiu Download PDF

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LT6899B
LT6899B LT2020542A LT2020542A LT6899B LT 6899 B LT6899 B LT 6899B LT 2020542 A LT2020542 A LT 2020542A LT 2020542 A LT2020542 A LT 2020542A LT 6899 B LT6899 B LT 6899B
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concentration
copper
nickel
ligand
reducing agent
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LT2020542A
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LT2020542A (lt
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Aldona JAGMINIENĖ
JAGMINIENĖ Aldona
Ina STANKEVIČIENĖ
STANKEVIČIEN Ina
Karolis RATAUTAS
RATAUTAS Karolis
Eugenijus Norkus
Norkus Eugenijus
Gediminas RAČIUKAITIS
RAČIUKAITIS Gediminas
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Valstybinis mokslinių tyrimų institutas Fizinių ir technologijos mokslų centras
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Priority to LT2020542A priority Critical patent/LT6899B/lt
Priority to US17/122,269 priority patent/US20220064801A1/en
Priority to PCT/IB2021/057786 priority patent/WO2022043889A1/en
Priority to KR1020237010227A priority patent/KR20230056751A/ko
Priority to CN202180053197.3A priority patent/CN116324032A/zh
Priority to JP2023513700A priority patent/JP2023538951A/ja
Priority to EP21759163.5A priority patent/EP4204599A1/en
Publication of LT2020542A publication Critical patent/LT2020542A/lt
Publication of LT6899B publication Critical patent/LT6899B/lt

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    • C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
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Abstract

Išradimas siejamas su selektyviu nikelio sluoksnio nusodinimu ant vario paviršiaus. Išradimas gali būti panaudotas, gaminant elektrai laidžias sritis elektronikos grandynams. Vario paviršiaus cheminio nikeliavimo būdas, apima gaminio, kurio vario paviršius dengiamas nikeliu, panardinimą į vieną arba daugiau tirpalų, iš kurių bent viename iš minėtų tirpalų yra reduktorius ir iš kurių bent vienas tirpalas yra pritaikytas cheminiam nikelio padengimui. Siekiant išplėsti jo panaudojimo sritį, bei gauti, praktiškai grynas nikelio dangas, minėtas reduktorius, yra boro arba fosforo junginiai, apimantys morfolino boraną (C4H9BNO) arba dimetilamino boraną (C2H7BN), arba natrio tetrahidroboratą (NaBH4), arba natrio hipofosfitą (NaH2PO2), kur minėtas reduktorius tiesiogiai arba netiesiogiai redukuoja netirpius vario(I) ir vario(II) junginius vario paviršiuje.

Claims (19)

  1. Vario paviršiaus cheminio nikeliavimo būdas, kur vario paviršius gali būti gaminio, arba jo dalies, pagaminto/os iš vario, paviršius, arba gaminio, padengto vario sluoksniu, paviršius, apimantis gaminio panardinimą į vieną arba daugiau tirpalų, - iš kurių bent viename iš minėtų tirpalų yra reduktorius; - iš kurių bent vienas tirpalas yra pritaikytas cheminiam nikelio padengimui, b e s i s k i r i a n t i s tuo, kad - minėtas reduktorius, yra boro arba fosforo junginiai, apimantys morfolino boraną (C4H9BNO), arba dimetilamino boraną (C2H7BN), arba natrio tetrahidroboratą (NaBH4), arba natrio hipofosfitą (NaH2PO2), kur minėtas reduktorius tiesiogiai arba netiesiogiai redukuoja netirpius vario(I) ir vario(II) junginius vario paviršiuje; - bent viename iš minėtų tirpalų yra ir ligandas arba ligandų mišinys, kuris padeda nutirpinti nepilnai suredukuotus netirpius vario junginius, surišdamas juos į tirpius kompleksinius junginius, paliekant iš esmės gryno vario paviršių, ant kurio vėliau nusodinamas nikelis.
  2. Būdas pagal 1 punktą, b e s i s k i r i a n t i s tuo, kad ligandas arba ligandų mišinys sudarytas iš bet kurių vandenyje tirpių cheminių junginių, gebančių sudaryti patvarius kompleksinius junginius su vario jonais, ir yra parinktas iš grupės, apimančios aminoetano rūgštį (C2H5NO2), nitrilotriacto rūgštį (C6H9NO6), etilendiamintetraacto rūgštį (C10H16N2O8), dietilentriaminpentaacto rūgštį (C14H23N3O10) ir jų druskas; vyno rūgštį (C4H6O6); citrinų rūgštį (C₆H₈O₇) ir jų druskas; amoniaką (NH3), etilendiaminą (C2H8N2), dietilentriaminą (C4H13N3), N,N,N′,N′-tetrakis(2-hidroksipropil)etilendiaminą (C14H32N2O4).
  3. Būdas pagal 1 punktą, b e s i s k i r i a n t i s tuo, kad apima šiuos etapus: (i) minėtas gaminys yra panardinamas į aktyvavimo tirpalą, kuris apima minėtą reduktorių ir ligandą, kuriame esančio minėto reduktoriaus anodinės oksidacijos metu susidarę elektronai suaktyvina vario paviršių, redukuodami vario(I) ir vario(II) oksidus ir oksi-hidroksi-junginius paviršiuje iki metalinio vario, tuo pačiu metu vykstant reduktoriaus terminiam ir (arba) kataliziniam skilimui, ant paviršiaus adsorbuojasi susidaręs atominis vandenilis, kuris taip pat reaguoja kaip ant paviršiaus esančių vario(I) ir vario(II) junginių reduktorius, o tirpale taip pat esantis ligandas padeda nutirpinti nepilnai suredukuotus netirpius vario junginius, surišdamas juos į tirpius kompleksinius junginius, palikdamas iš esmės gryno vario paviršių, (ii) gaminys su aktyvuotu vario paviršiumi panardinamas į cheminio nikeliavimo tirpalą, kuriame vyksta cheminis nikelio nusodinimas ant vario paviršiaus.
  4. Būdas pagal 1 punktą, b e s i s k i r i a n t i s tuo, kad apima vieną etapą, kurio metu minėtas gaminys panardinamas į cheminio nikeliavimo tirpalą, turintį reduktorių, parinktą iš minėtų cheminių junginių grupės, pasirenkant tokias minėto reduktoriaus cheminių junginių koncentracijas, kad minėtas junginys redukuotų netirpius vario(I) ir vario(II) junginius, esančius ant gaminio vario paviršiaus; bei ligandą arba ligandų mišinį – parinktą iš minėtų cheminių junginių grupės, pasirenkant tokias minėto ligando arba ligandų mišinio cheminių junginių koncentracijas, kad minėtas junginys nutirpintų nepilnai suredukuotus netirpius vario junginius, surišdamas juos į tirpius kompleksinius junginius taip, kad liktų iš esmės gryno vario paviršius, ant kurio nusodinamas nikelis.
  5. Būdas pagal 3 punktą, b e s i s k i r i a n t i s tuo, kad aktyvavimo tirpalą sudaro natrio hipofosfitas (NaH2PO2), kurio koncentracija yra nuo 0,5 M iki tirpumo ribos, ir minėtas ligandas arba jų mišiniai, kurių koncentracija nuo 0,001 M iki tirpumo ribos, o apdorojimas vyksta 1-15 minučių, esant 80-96 ºC tirpalo temperatūrai.
  6. Būdas pagal 3 punktą, b e s i s k i r i a n t i s tuo, kad aktyvavimo tirpalą sudaro morfolino boranas (C4H9BNO), kurio koncentracija yra nuo 0,01 M iki tirpumo ribos ir minėtas ligandas arba jų mišiniai, kurių koncentracija nuo 0,001 M iki tirpumo ribos, o apdorojimas vyksta 1-15 minučių, esant 18-50 ºC tirpalo temperatūrai.
  7. Būdas pagal 3 punktą, b e s i s k i r i a n t i s tuo, kad aktyvavimo tirpalą sudaro dimetilamino boranas (C2H7BN), kurio koncentracija yra nuo 0,01 M iki tirpumo ribos ir minėtas ligandas arba jų mišiniai, kurių koncentracija nuo 0,001 M iki tirpumo ribos, o apdorojimas vyksta 1-15 minučių, esant 18-50 ºC tirpalo temperatūrai.
  8. Būdas pagal 3 punktą, b e s i s k i r i a n t i s tuo, kad aktyvavimo tirpalą sudaro natrio tetrahidroboratas (NaBH4), kurio koncentracija yra nuo 0,01 M iki tirpumo ribos ir minėtas ligandas arba jų mišiniai, kurių koncentracija nuo 0,001 M iki tirpumo ribos, o apdorojimas vyksta 1-15 minučių, esant 18-50 ºC tirpalo temperatūrai.
  9. Būdas pagal 1 punktą, b e s i s k i r i a n t i s tuo, kad cheminio nikeliavimo tirpalą sudaro: nikelio sulfatas (NiSO4), kurio koncentracija 0,05-0,5 M; reduktorius natrio hipofosfitas (NaH2PO2), kurio koncentracija 0,25-3 M; ligandas aminoetano rūgštis (C2H5NO2), kurios koncentracija 0,25-1 M; natrio hidroksidas (NaOH), kurio koncentracija yra pakankama pasiekti tinkamam tirpalo pH.
  10. Būdas pagal 1 punktą, b e s i s k i r i a n t i s tuo, kad minėto gaminio vario paviršius padengiamas nikeliu, naudojant du skirtingus nikeliavimo tirpalus, kuriose yra reduktorius natrio hipofosfitas, pirmiausia, gaminys, kurio vario paviršių reikia nikeliuoti, panardinamas į šarminį cheminio nikeliavimo tirpalą, kurio pH yra nuo 8,5 iki 10, vėliau minėtas gaminys panardinamas į rūgštinį cheminio nikeliavimo tirpalą, kurio pH yra nuo 4,0 iki 6,0.
  11. Būdas pagal 1 punktą, b e s i s k i r i a n t i s tuo, kad cheminio nikeliavimo tirpalą sudaro nikelio sulfatas (NiSO4), kurio koncentracija yra 0,05-0,5 M; reduktorius morfolino boranas (C4H9BNO), kurio koncentracija yra 0,01-1 M; ligandas dietilentriaminas (C4H13N3), kurio koncentracija yra 0,001-0,5 M; natrio hidroksidas (NaOH), kurio koncentracija yra pakankama sureguliuoti tirpalo pH 5,0-7,8 ribose; dengimas vyksta, esant 18-35 ºC tirpalo temperatūrai.
  12. Būdas pagal 1 punktą, b e s i s k i r i a n t i s tuo, kad cheminio nikeliavimo tirpalą sudaro nikelio sulfatas (NiSO4), kurio koncentracija yra 0,05-0,5 M; reduktorius dimetilamino boranas (C2H7BN), kurio koncentracija yra 0,01-1 M; ligandas dietilentriaminas (C4H13N3), kurio koncentracija yra 0,001-0,5 M; natrio hidroksidas (NaOH), kurio koncentracija yra pakankama sureguliuoti tirpalo pH 5,0-7,8 ribose; dengimas vyksta, esant 18-35 ºC tirpalo temperatūrai.
  13. Būdas pagal 1 punktą, b e s i s k i r i a n t i s tuo, kad cheminio nikeliavimo tirpalą sudaro nikelio sulfatas (NiSO4), kurio koncentracija yra 0,05–0,5 M; reduktorius natrio tetrahidroboratas (NaBH4), kurio koncentracija yra 0,01–0,5 M; ligandas etilendiaminas (C2H8N2), kurio koncentracija yra 0,001-0,5 M; ligandas kalio natrio tartratas (KNaC4H4O6), kurio koncentracija yra 0,05–0,2 M; dinatrio tiosulfatas (Na2S2O3), kurio koncentracija yra 0,001–0,01 M; natrio hidroksidas (NaOH), kurio koncentracija yra pakankama sureguliuoti tirpalo pH 12,0-13,0 ribose; dengimas vyksta, esant 18-35 ºC temperatūrai.
  14. Būdas pagal 4 punktą, b e s i s k i r i a n t i s tuo, kad cheminio nikeliavimo tirpalą sudaro nikelio sulfatas (NiSO4); natrio šarmas (NaOH); ligandas aminoetano rūgštis (C2H5NO2) ir reduktorius natrio hipofosfitas (NaH2PO2), kurio koncentracija viršija 0,8 M.
  15. Būdas pagal 4 ir 14 punktus, b e s i s k i r i a n t i s tuo, kad cheminio nikeliavimo tirpalą sudaro nikelio sulfatas (NiSO4), kurio koncentracija yra 0,05-0,5 M; reduktorius natrio hipofosfitas (NaH2PO2), kurio koncentracija yra 0,8-3 M; ligandas aminoetano rūgštis (C2H5NO2), kurios koncentracija yra 0,25-1 M; NaOH (natrio hidroksidas), kurio koncentracija yra pakankama sureguliuoti tirpalo pH 4,0-6,0 ribose, dengimas vyksta, esant 80-96 ºC tirpalo temperatūrai.
  16. Būdas pagal 4 punktą, b e s i s k i r i a n t i s tuo, kad cheminio nikeliavimo tirpalą sudaro nikelio sulfatas (NiSO4), kurio koncentracija yra 0,05-0,5 M; reduktorius morfolino boranas (C4H9BNO), kurio koncentracija yra 0,1-1 M; ligandas dietilentriaminas (C4H13N3), kurio koncentracija yra 0,001-0,5 M; natrio hidroksidas (NaOH), kurio koncentracija yra pakankama sureguliuoti tirpalo pH 5,0-7,8 ribose, dengimas vyksta, esant 18-35 ºC tirpalo temperatūrai.
  17. Būdas pagal 4 punktą, b e s i s k i r i a n t i s tuo, kad cheminio nikeliavimo tirpalą sudaro nikelio sulfatas (NiSO4), kurio koncentracija yra 0,05-0,5M; reduktorius dimetilamino boranas (C2H7BN), kurio koncentracija yra 0,1-1 M; ligandas dietilentriaminas (C4H13N3), kurio koncentracija yra 0,001-0,5 M; natrio hidroksidas (NaOH), kurio koncentracija yra pakankama sureguliuoti tirpalo pH 5,0-7,8 ribose, dengimas vyksta, esant 18-35 ºC tirpalo temperatūrai.
  18. Būdas pagal 4 punktą, b e s i s k i r i a n t i s tuo, kad cheminio nikeliavimo tirpalą sudaro nikelio sulfatas (NiSO4), kurio koncentracija yra 0,05-0,5 M; reduktorius natrio tetrahidroboratas (NaBH4), kurio koncentracija yra 0,02-0,5 M; ligandas etilendiaminas (C2H8N2), kurio koncentracija yra 0,001-0,5 M; ligandas kalio natrio tartratas (KNaC4H4O6), kurio koncentracija yra 0,05–0,2 M; dinatrio tiosulfatas (Na2S2O3), kurio koncentracija yra 0,001-0,01 M; natrio hidroksidas (NaOH), kurio koncentracija yra pakankama sureguliuoti tirpalo pH 12,0-13,0 ribose, dengimas vyksta, esant 18-35 ºC temperatūrai.
  19. Būdas pagal bet kurį iš 1-18 punktų, b e s i s k i r i a n t i s tuo, kad tirpalų koncentraciją ir (arba) proceso trukmę nustato eksperimentiškai arba kompiuteriu valdomu arba pusiau automatiniu būdu, kurio metu realiu laiku nuskaitoma informacija apie ant gaminio paviršiaus dengiamo nikelio sluoksnio kokybę ir reagentų tirpaluose koncentraciją, bei realiu laiku apskaičiuojama procesui vykdyti reikalinga tirpalų koncentracija ir (arba) cheminio proceso trukmė.
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US17/122,269 US20220064801A1 (en) 2020-08-27 2020-12-15 Method for electroless nickel deposition onto copper without activation with palladium
PCT/IB2021/057786 WO2022043889A1 (en) 2020-08-27 2021-08-25 Method for electroless nickel deposition onto copper without activation with palladium
KR1020237010227A KR20230056751A (ko) 2020-08-27 2021-08-25 팔라듐에 의한 활성화가 없는 구리 상에서 무전해 니켈 증착 방법
CN202180053197.3A CN116324032A (zh) 2020-08-27 2021-08-25 在不用钯活化的情况下在铜上无电镀镍沉积的方法
JP2023513700A JP2023538951A (ja) 2020-08-27 2021-08-25 パラジウムで活性化することなく銅上に無電解ニッケルを析出させる方法
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