Valstybinis mokslinių tyrimų institutas Fizinių ir technologijos mokslų centras
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Priority to LT2020542ApriorityCriticalpatent/LT6899B/en
Priority to US17/122,269prioritypatent/US20220064801A1/en
Priority to PCT/IB2021/057786prioritypatent/WO2022043889A1/en
Priority to KR1020237010227Aprioritypatent/KR20230056751A/en
Priority to JP2023513700Aprioritypatent/JP2023538951A/en
Priority to CN202180053197.3Aprioritypatent/CN116324032A/en
Priority to EP21759163.5Aprioritypatent/EP4204599A1/en
Publication of LT2020542ApublicationCriticalpatent/LT2020542A/en
Publication of LT6899BpublicationCriticalpatent/LT6899B/en
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
C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
C23C18/1601—Process or apparatus
C23C18/1633—Process of electroless plating
C23C18/1635—Composition of the substrate
C23C18/1637—Composition of the substrate metallic substrate
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
C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
C23C18/1601—Process or apparatus
C23C18/1603—Process or apparatus coating on selected surface areas
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
C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
C23C18/1601—Process or apparatus
C23C18/1633—Process of electroless plating
C23C18/1646—Characteristics of the product obtained
C23C18/165—Multilayered product
C23C18/1651—Two or more layers only obtained by electroless plating
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
C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
C23C18/18—Pretreatment of the material to be coated
C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
C23C18/1837—Multistep pretreatment
C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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
C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
C23C18/18—Pretreatment of the material to be coated
C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
C23C18/1848—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by electrochemical pretreatment
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
C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
C23C18/31—Coating with metals
C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
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
C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
C23C18/31—Coating with metals
C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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
C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
C23C18/31—Coating with metals
C23C18/38—Coating with copper
C23C18/40—Coating with copper using reducing agents
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
C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
C—CHEMISTRY; METALLURGY
C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
C25D11/02—Anodisation
C25D11/34—Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32
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
C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
C23C18/18—Pretreatment of the material to be coated
C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
Abstract
The invention relates to selective deposition of a nickel layer on a copper surface. The invention may be used in the production of electrically conductive areas for electronic circuits. Method for nickel deposition on the surface of copper comprises immersing an item, which surface is to be deposited with the nickel layer, into one or more baths, of which at least one contains a reducing agent and of which at least one is adapted for (electroless) plating of nickel. In order to extend the field of application and to obtain practically pure nickel coatings, said reducing agent comprises boronic or phosphoric compounds, comprising morpholine borane (C4H9BNO), or dimethylamine borane (C2H7BN), or sodium tetrahydroborate (NaBH4), or sodium hypophosphite (NaH2PO2) and said reducing agent directly or indirectly reduces insoluble copper(I) or copper(II) compounds on the copper surface. At least one of the mention baths comprises a ligand or mixture thereof.
Claims (19)
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.A method of chemical nickel plating of a copper surface, where the surface of the copper may be the surface of a product or part thereof made of copper, or the surface of a product coated with a layer of copper, comprising immersing the product in one or more solutions, at least one of solutions are reducing agents; - of which at least one solution is adapted for the chemical coating of nickel, characterized in that - said reducing agent is a boron or phosphorus compound comprising morpholine borane (C4H9BNO), or dimethylamino borane (C2H7BN), or sodium tetrahydroborate (NaBH4), (NaH2PO2), wherein said reducing agent directly or indirectly reduces insoluble copper (I) and copper (II) compounds on the copper surface; - at least one of said solutions also contains a ligand or mixture of ligands which helps to dissolve the incompletely reduced insoluble copper compounds by binding them to soluble complexes, leaving a substantially pure copper surface on which nickel is subsequently deposited.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).Process according to claim 1, characterized in that the ligand or mixture of ligands consists of any water-soluble chemical compounds capable of forming stable complexes with copper ions and is selected from the group consisting of aminoacetic acid (C 2 H 5 NO 2), nitrilotriacetic acid (C 6 H 5 NO 9) ethylenediaminetetraacetic acid (C10H16N2O8), diethylenetriaminepentaacetic acid (C14H23N3O10) and their salts; tartaric acid (C4H6O6); citric acid (C₆H₈O₇) and their salts; ammonia (NH3), ethylenediamine (C2H8N2), diethylenetriamine (C4H13N3), N, N, N ′, N′-tetrakis (2-hydroxypropyl) ethylenediamine (C14H32N2O4).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.A process according to claim 1, characterized in that it comprises the steps of: (i) immersing said product in an activating solution comprising said reducing agent and a ligand in which the electrons formed during the anodic oxidation of said reducing agent activate the copper surface by reducing copper (I); copper (II) oxides and oxyhydroxy compounds on the surface up to metallic copper, with the simultaneous thermal and / or catalytic decomposition of the reducing agent adsorbing on the surface the atomic hydrogen which also reacts as the copper (I) and copper (II) a reducing agent of the compounds and a ligand also present in the solution helps to dissolve the incompletely reduced insoluble copper compounds by binding them to the soluble complexes, leaving a substantially pure copper surface; chemical deposition of nickel on a copper surface.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.A process according to claim 1, characterized in that it comprises one step of immersing said product in a chemical nickel plating solution containing a reducing agent selected from the group consisting of said reducing compounds to reduce said insoluble copper and copper (II) compounds present on the copper surface of the article; and a ligand or mixture of ligands selected from the group consisting of chemical compounds of said ligand or mixture of ligands such that said compound dissolves incompletely reduced insoluble copper compounds by binding them to soluble complexes so as to leave a substantially pure copper surface, on which nickel is deposited.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.The method according to claim 3, characterized in that the activating solution comprises sodium hypophosphite (NaH 2 PO 2) in a concentration of 0.5 M to the solubility limit, and said ligand or mixtures thereof in a concentration of 0.001 M to the solubility limit, and the treatment is carried out -15 minutes at a solution temperature of 80-96 ºC.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.The method according to claim 3, characterized in that the activating solution comprises morpholine borane (C4H9BNO) in a concentration of 0.01 M to the solubility limit and said ligand or mixtures thereof in a concentration of 0.001 M to the solubility limit, and the treatment is carried out in 1- 15 minutes at a solution temperature of 18-50 ºC.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.Process according to claim 3, characterized in that the activating solution comprises dimethylamine borane (C2H7BN) in a concentration of 0.01 M to the solubility limit and said ligand or mixtures thereof in a concentration of 0.001 M to the solubility limit, and the treatment is carried out in 1- 15 minutes at a solution temperature of 18-50 ºC.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.The method according to claim 3, characterized in that the activating solution comprises sodium tetrahydroborate (NaBH 4) in a concentration of 0.01 M to the solubility limit and said ligand or mixtures thereof in a concentration of 0.001 M to the solubility limit, and the treatment is carried out in 1- 15 minutes at a solution temperature of 18-50 ºC.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.Process according to Claim 1, characterized in that the chemical nickel-plating solution comprises: nickel sulphate (NiSO 4) in a concentration of 0.05 to 0.5 M; reducing agent sodium hypophosphite (NaH2PO2) at a concentration of 0.25-3 M; ligand aminoacetic acid (C2H5NO2) at a concentration of 0.25-1 M; sodium hydroxide (NaOH) in a concentration sufficient to reach the appropriate pH of the solution.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.Process according to claim 1, characterized in that the copper surface of said product is coated with nickel using two different nickel-plating solutions containing a reducing agent sodium hypophosphite, in particular the product whose copper surface needs to be nickel-plated is immersed in an alkaline chemical nickel solution. , 5 to 10, the said product is then immersed in an acidic chemical nickel plating solution having a pH of 4.0 to 6.0.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.Process according to Claim 1, characterized in that the chemical nickel-plating solution comprises nickel sulphate (NiSO 4) in a concentration of 0.05 to 0.5 M; reducing agent morpholine borane (C4H9BNO) at a concentration of 0.01-1 M; the ligand diethylenetriamine (C4H13N3) at a concentration of 0.001-0.5 M; sodium hydroxide (NaOH) in a concentration sufficient to adjust the pH of the solution to 5.0-7.8; coating takes place at a solution temperature of 18-35 ºC.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.Process according to Claim 1, characterized in that the chemical nickel-plating solution comprises nickel sulphate (NiSO 4) in a concentration of 0.05 to 0.5 M; a reducing agent dimethylamino borane (C2H7BN) in a concentration of 0.01-1 M; the ligand diethylenetriamine (C4H13N3) at a concentration of 0.001-0.5 M; sodium hydroxide (NaOH) in a concentration sufficient to adjust the pH of the solution to 5.0-7.8; coating takes place at a solution temperature of 18-35 ºC.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.Process according to Claim 1, characterized in that the chemical nickel-plating solution consists of nickel sulphate (NiSO 4) in a concentration of 0.05 to 0.5 M; reducing agent sodium tetrahydroborate (NaBH4) in a concentration of 0.01-0.5 M; ligand ethylenediamine (C2H8N2) at a concentration of 0.001-0.5 M; the ligand is potassium sodium tartrate (KNaC4H4O6) in a concentration of 0,05 to 0,2 M; Disodium thiosulphate (Na2S2O3) in a concentration of 0,001 to 0,01 M; sodium hydroxide (NaOH) in a concentration sufficient to adjust the pH of the solution to 12.0-13.0; coating takes place at a temperature of 18-35 ºC.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.Process according to Claim 4, characterized in that the chemical nickel-plating solution comprises nickel sulphate (NiSO 4); sodium hydroxide (NaOH); ligand aminoacetic acid (C2H5NO2) and reducing agent sodium hypophosphite (NaH2PO2) in a concentration exceeding 0.8 M.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.Process according to Claims 4 and 14, characterized in that the chemical nickel-plating solution comprises nickel sulphate (NiSO 4) in a concentration of 0.05 to 0.5 M; reducing agent sodium hypophosphite (NaH2PO2) at a concentration of 0.8-3 M; ligand aminoacetic acid (C2H5NO2) at a concentration of 0.25-1 M; NaOH (sodium hydroxide), the concentration of which is sufficient to adjust the pH of the solution to 4.0-6.0, is applied at a solution temperature of 80-96 ºC.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.Process according to Claim 4, characterized in that the chemical nickel-plating solution comprises nickel sulphate (NiSO 4) in a concentration of 0.05 to 0.5 M; reducing agent morpholine borane (C4H9BNO) at a concentration of 0.1-1 M; the ligand diethylenetriamine (C4H13N3) at a concentration of 0.001-0.5 M; Sodium hydroxide (NaOH), the concentration of which is sufficient to adjust the pH of the solution to 5,0 to 7,8, is applied at a temperature of 18 to 35 ºC.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.Process according to Claim 4, characterized in that the chemical nickel-plating solution comprises nickel sulphate (NiSO 4) in a concentration of 0.05 to 0.5 M; a reducing agent dimethylamino borane (C2H7BN) in a concentration of 0.1-1 M; the ligand diethylenetriamine (C4H13N3) at a concentration of 0.001-0.5 M; Sodium hydroxide (NaOH), the concentration of which is sufficient to adjust the pH of the solution to 5,0 to 7,8, is applied at a temperature of 18 to 35 ºC.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.Process according to Claim 4, characterized in that the chemical nickel-plating solution comprises nickel sulphate (NiSO 4) in a concentration of 0.05 to 0.5 M; reducing agent sodium tetrahydroborate (NaBH4) at a concentration of 0.02-0.5 M; ligand ethylenediamine (C2H8N2) in a concentration of 0.001-0.5 M; the ligand is potassium sodium tartrate (KNaC4H4O6) in a concentration of 0,05 to 0,2 M; disodium thiosulfate (Na2S2O3) at a concentration of 0.001-0.01 M; Sodium hydroxide (NaOH), in a concentration sufficient to adjust the pH of the solution to 12,0 to 13,0, is applied at a temperature of 18 to 35 ºC.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.Method according to any one of claims 1 to 18, characterized in that the concentration of the solutions and / or the duration of the process are determined experimentally or by computer-controlled or semi-automatic method, in which real-time information on the quality of the nickel coating , and the concentration of solutions required for the process and / or the duration of the chemical process is calculated in real time.
LT2020542A2020-08-272020-08-27Method for electroless nickel deposition onto copper without activation with palladium
LT6899B
(en)
A pretreating-activating solution for an electroless nickel plating, a method for electroless plating a thin-nickel and a method for surface-treating using the same, and a printed circuit board comprising an electroless thin-nickel