JPH0336282A - Gold-plating - Google Patents
Gold-platingInfo
- Publication number
- JPH0336282A JPH0336282A JP14327490A JP14327490A JPH0336282A JP H0336282 A JPH0336282 A JP H0336282A JP 14327490 A JP14327490 A JP 14327490A JP 14327490 A JP14327490 A JP 14327490A JP H0336282 A JPH0336282 A JP H0336282A
- Authority
- JP
- Japan
- Prior art keywords
- bath
- gold
- gold plating
- treated
- tungsten
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000007747 plating Methods 0.000 title claims abstract description 20
- 229910052737 gold Inorganic materials 0.000 claims abstract description 38
- 239000010931 gold Substances 0.000 claims abstract description 38
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000000919 ceramic Substances 0.000 claims abstract description 21
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 19
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 15
- 238000000576 coating method Methods 0.000 claims abstract description 8
- 239000011248 coating agent Substances 0.000 claims abstract description 6
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 18
- 239000010937 tungsten Substances 0.000 claims description 17
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 14
- 239000011733 molybdenum Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000001465 metallisation Methods 0.000 claims description 8
- 239000011260 aqueous acid Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 229910001854 alkali hydroxide Inorganic materials 0.000 claims 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims 1
- 239000000356 contaminant Substances 0.000 claims 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 4
- 230000002378 acidificating effect Effects 0.000 abstract description 4
- 239000005368 silicate glass Substances 0.000 abstract description 4
- 229910003638 H2SiF6 Inorganic materials 0.000 abstract description 3
- ZEFWRWWINDLIIV-UHFFFAOYSA-N tetrafluorosilane;dihydrofluoride Chemical compound F.F.F[Si](F)(F)F ZEFWRWWINDLIIV-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052681 coesite Inorganic materials 0.000 abstract description 2
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 2
- 239000000377 silicon dioxide Substances 0.000 abstract description 2
- 229910052682 stishovite Inorganic materials 0.000 abstract description 2
- 229910052905 tridymite Inorganic materials 0.000 abstract description 2
- 239000010409 thin film Substances 0.000 abstract 3
- 239000010408 film Substances 0.000 abstract 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000010410 layer Substances 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 229910052759 nickel Inorganic materials 0.000 description 6
- 238000005406 washing Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- OVHDZBAFUMEXCX-UHFFFAOYSA-N benzyl 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)OCC1=CC=CC=C1 OVHDZBAFUMEXCX-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- FGZBFIYFJUAETR-UHFFFAOYSA-N calcium;magnesium;silicate Chemical compound [Mg+2].[Ca+2].[O-][Si]([O-])([O-])[O-] FGZBFIYFJUAETR-UHFFFAOYSA-N 0.000 description 1
- 238000010344 co-firing Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- ASTZLJPZXLHCSM-UHFFFAOYSA-N dioxido(oxo)silane;manganese(2+) Chemical compound [Mn+2].[O-][Si]([O-])=O ASTZLJPZXLHCSM-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- IZLAVFWQHMDDGK-UHFFFAOYSA-N gold(1+);cyanide Chemical compound [Au+].N#[C-] IZLAVFWQHMDDGK-UHFFFAOYSA-N 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- HHIQWSQEUZDONT-UHFFFAOYSA-N tungsten Chemical compound [W].[W].[W] HHIQWSQEUZDONT-UHFFFAOYSA-N 0.000 description 1
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten(VI) oxide Inorganic materials O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
-
- 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
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/48—Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
- H01L21/4814—Conductive parts
- H01L21/4846—Leads on or in insulating or insulated substrates, e.g. metallisation
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Metallurgy (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Chemically Coating (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Manufacturing Of Printed Wiring (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、セラミック本体の表面に付着させたタングス
テン又はモリブデンの表筒に金を無電解めっきする方法
に関する５、より詳しく（・ま、本発明は、エレクトロ
ニクスに使用するためのセラミック製のコンポーネント
の場合、例えば集積回路用の基体又はハウジングの場合
に、タングステン又はモリブデンを無電解金めつきする
方法に関する。Detailed Description of the Invention [Field of Industrial Application] The present invention relates to a method for electroless plating gold on a tungsten or molybdenum face cylinder attached to the surface of a ceramic body. The invention relates to a method for electroless gold plating of tungsten or molybdenum in the case of ceramic components for use in electronics, for example in the case of substrates or housings for integrated circuits.
例えば酸化アルミニウム（（よる金属被覆を形成したセ
ラミックのコンポーネントは、工１／りトロニクス用と
して、例えば出力半導体に多用されている。これらのコ
ンポーネントの金属被覆は、タングステン又はモリブデ
ンから通常或っている。Ceramic components with a metallization of aluminum oxide (for example) are often used in engineering/retronics applications, e.g. in power semiconductors. The metallization of these components is usually made from tungsten or molybdenum. .
別の金属、通常はニッケル又は金の層は、半田付は性を
高め、導電性を改善するために、電気めっき又は無電解
工程によって、金属被覆上に付着される。ニッケルと金
とをこの順に付着させることもできるが、その理由は、
ニッケルがタングステンとモリブデンどの両者に付着し
、金はこのニッケルにも付着するためである。しかし、
成る場合には、金を直接にタングステン又はモリブデン
上に、中間層を合さずに付着させることが必要となる。A layer of another metal, usually nickel or gold, is deposited over the metallization by electroplating or an electroless process to enhance solderability and improve conductivity. Nickel and gold can be deposited in this order, but the reason is
This is because nickel adheres to both tungsten and molybdenum, and gold also adheres to nickel. but,
In this case, it would be necessary to deposit the gold directly onto the tungsten or molybdenum without intervening interlayers.
それは、ニッケルの中間層が、金めつきの後でさえも（
電子コンポーネントのカプセル封入のために必要な）後
の半田付は工程の間に（例えば金もしくは錫との）脆い
中間ニッケル相となりうるためである。これらの相は、
気体に対する透過性が比較的高いため、セラ□ツク製の
ハウジングの気密な閉止を不可能とする。That is, even after gold plating, the nickel interlayer (
This is because subsequent soldering (necessary for encapsulation of electronic components) can result in brittle intermediate nickel phases (eg with gold or tin) during processing. These phases are
The relatively high gas permeability makes it impossible to close the ceramic housing in an airtight manner.
セラミック製のコンポーネントの幾何学的形状と、小さ
な寸法とのため、多（の場合において、（３）
給電用の短絡接続を設けろことは不経済である。Due to the geometry and small dimensions of ceramic components, it is uneconomical to provide short-circuit connections for multiple (3) power supplies.
従って、無電解例着技術によって金の層をイ」看させる
ことが望ましい。Therefore, it is desirable to expose the gold layer by electroless deposition techniques.
タングステン面特にセラミック部品のタングステン面上
に金の被覆を直接に無電解付着させろ方法は、ドイツ公
開特許第２２３９６７６号及び米国特許第３９９３８０
８号によって、公知となっている。A method for the electroless deposition of gold coatings directly on tungsten surfaces, particularly on tungsten surfaces of ceramic components, is described in German Published Patent No. 2239676 and US Pat. No. 399380.
No. 8, it is publicly known.
しかし、このようにして形成した金の層が、タングステ
ン又はモリブデンの層上に屡々不適切な接着強度しか示
さないことが見出されている。これらの金属がンリケー
トペーストを用いてセラミックに対して焼成された場合
に←４−特にそう１．Ｃる。However, it has been found that gold layers formed in this way often exhibit inadequate adhesion strength on tungsten or molybdenum layers. ←4-especially when these metals are fired to ceramics using hydrate pastes 1. Cru.
このペーストは、焼成の際に生ずる連続力゛ラス相が金
属（Ｆ Ｍｏ）とセラミックどの間の接着を改善する
ため、産業上多用されている。（−かし、例えば、いわ
ゆる共焼成技術の場合のタングステンについて普通に行
なわれているように、純金属ベストを用いて形成された
金属被覆面に対する接着力も、十分ではない。この場合
（（は、七う□ツ（４）
り中のわずかな比率のシリケートがおそらくは原因とな
っている。This paste is widely used in industry because the continuous force-filled phase produced during firing improves the adhesion between the metal (FMo) and the ceramic. (-However, the adhesion to metallized surfaces formed using pure metal vests, as is customary for example for tungsten in the case of so-called co-firing techniques, is also not sufficient. In this case (( , Seven U□tsu(4) A small proportion of silicates in the solution is probably responsible.
モリブデンもしくはタングステンの粉末と珪酸マンガン
とから成る金属被覆ペーストを用いることは、ドイツセ
ラミック学会＠（、Ｂｅｒ 、ｄ 、ｃｌｅｎｔ 。The use of a metallization paste consisting of molybdenum or tungsten powder and manganese silicate has been proposed by the German Ceramic Society.
Ｋｅｒ、ＧｅＳ、 １９６５ ＋ ４５２頁）によって
、以前から知られている。ドイツ特許８３８０３２２７
号によって提案された、α）微細に分割されたタングス
テンもしくはモリブデンの粉末とｂ）液状の有機結合剤
とｃ） １２００°−１５００℃の融点をもった珪酸
カルシウムマグネシウムの粉末とを含有する金属破壊ペ
ーストを使用してもよい。Ker, GeS, 1965 + p. 452). German patent 83803227
A metal fracture containing α) finely divided tungsten or molybdenum powder, b) a liquid organic binder and c) calcium magnesium silicate powder with a melting point of 1200°-1500°C was proposed by No. Paste may also be used.
〔発明によって解決しようとする課題〕本発明の目的は
、特に珪酸塩含有金属被覆ペーストを使用して、無電解
的に、強い接着性を示す金の層と共に、セラ□ツク上に
おいて焼成された５タングステン又はモリブデンの層を
提供することにある。[Problem to be Solved by the Invention] It is an object of the present invention to provide a metal coating paste which is fired electrolessly on ceramics with a gold layer exhibiting strong adhesion properties, in particular using a silicate-containing metallization paste. 5 to provide a layer of tungsten or molybdenum.
本発明によれば、金属被覆によってセラミック本体上に
付着させた薄いタングステン又はモリブデンの表面に無
電解金めつきするに当り、ｌｉＦ及びＨ２Ｓ ７ Ｆ６
の水溶液によって該表面をＯ・と先す処理した後、ｐｌ
ｉが１０以上の水性アルカリ浴中及びｐＨが３以下の水
性酸浴中において核表面を次々に処理する。アルカリ浴
中の処理を最初に行１（い、酸浴中の処理を次に行なう
ことが望ましい。According to the invention, in the electroless gold plating of thin tungsten or molybdenum surfaces deposited on ceramic bodies by metallization, liF and H2S 7 F6
After prior treatment of the surface with O. by an aqueous solution of pl
The nuclear surfaces are sequentially treated in an aqueous alkaline bath with i of 10 or more and an aqueous acid bath with a pH of 3 or less. It is desirable to carry out treatment in an alkaline bath first, and then carry out treatment in an acid bath.
次に水性の金含有浴中において金めつきを行なう。Gold plating is then carried out in an aqueous gold-containing bath.
ｌＩＦ及びＨ２ＳｉＦ６の水溶液による処理によって、
セラ□ツクの金属被覆ペーストに由来するＳｉｎ。By treatment with an aqueous solution of lIF and H2SiF6,
Sin derived from the metal coating paste of Cera□Tsuku.
及び珪酸塩ガラスも除去されると推定される。It is estimated that silicate glass and silicate glass are also removed.
有利には、金を錯塩として含有するアルカリ性浴中にお
いて金めつきを行なう。しかし酸性金浴を用いてもよい
。Gold plating is preferably carried out in an alkaline bath containing gold as a complex salt. However, acidic gold baths may also be used.
実際には、金属被横後に、金めつきされたセラミック製
のコンポーネントを清浄にすることが必要どなる。この
コンポーネントは、−例どして、水性浴を入れた回転ド
ラム中において超音波に曝露させつつ清浄にすることが
できる。アルカリ浴と、その後において、酸性浴、例え
ば５−１０％ＨＣｅ水溶液が、通常使用される。これに
よって異物及び油脂弁が除去される。In practice, it may be necessary to clean gold-plated ceramic components after metal coating. This component can be cleaned - for example, while being exposed to ultrasound in a rotating drum containing an aqueous bath. An alkaline bath followed by an acidic bath, such as a 5-10% aqueous HCe solution, is usually used. This removes foreign objects and grease valves.
弗化水素２７ Ｈ，，５ｉＦ６（Ｌによる処理は、存在
していることのある珪酸塩ガラス及びＳｉＯ２による金
属被覆の粒子の被膜を確実に除去する。好ましくは、Ｉ
−ＩＰ２Ｃ）−４０重量饅、１Ｊ２ＳｉＦ’６ １−５
重量φの濃度とする。この処理は室温で１分間以上持続
させる。Treatment with hydrogen fluoride 27H,,5iF6(L) reliably removes any coating of particles of silicate glass and metallization with SiO2 that may be present.
-IP2C)-40 weight rice cake, 1J2SiF'6 1-5
Let the concentration be the weight φ. This treatment lasts for at least 1 minute at room temperature.
金めつきの前に使用される水性アルカリ浴及び水性酸浴
の組成及び濃度は、ｐＨ値１０以上３以下が保たれてい
れば、臨界では／、（い。アルカリ浴としては、１−５
重量袈の濃度の水酸化ナトリウム水溶液を例えば使用す
ることができる。The composition and concentration of the aqueous alkaline bath and aqueous acid bath used before gold plating are critical if the pH value is maintained between 10 and 3.
For example, an aqueous solution of sodium hydroxide having a concentration of about 100 g can be used.
酸化タングステン（Ｖｉ）は、この浴中に容易に溶解す
る。４０°Ｃ」Ｊ、上の温度で処理することが望ましい
。Tungsten (Vi) oxide dissolves easily in this bath. It is desirable to process at temperatures above 40°C.
５−２０重量多の濃度の希硫酸を例えば水性酸浴のため
に使用することができる。タングステンの表面が新たに
酸化を受けないようにするためには、硫酸の濃度が高い
ほどその温度を低くすべき（７）
である。従って酸溶液は、酸化作用を示すべきではない
。従って１ｉＮｏ３７ｆｌＦの混合物も使用すべきでは
ない。しかし２０重量φを含有する硫酸は、４０’Ｃに
おいて満足に使用することができる。どちらの浴におい
ても、処理時間は、１分以下どすべきでば／よい。Dilute sulfuric acid at a concentration of 5-20% by weight can be used, for example, for the aqueous acid bath. In order to prevent the surface of tungsten from undergoing further oxidation, the higher the concentration of sulfuric acid, the lower the temperature should be (7). The acid solution should therefore not exhibit oxidizing effects. Therefore mixtures of 1iNo37flF should also not be used. However, sulfuric acid containing 20 wt φ can be used satisfactorily at 40'C. In either bath, the treatment time should/should be less than 1 minute.
次に、例えば米国特許第３９９３８０８号に記載された
高温のアルカリ性金浴中において、無電解金めつきを実
施する。この工程では、０．０５１μｍ１好ましくは０
．１−０．８μｍの層厚に金めっきする。これよりも層
厚が大きくなると剥落の」６それを生ずる。Electroless gold plating is then carried out in a hot alkaline gold bath as described, for example, in US Pat. No. 3,993,808. In this step, 0.051 μm1 preferably 0
．． Gold plated to a layer thickness of 1-0.8 μm. If the layer thickness is greater than this, flaking will occur.
前記の各工程の間に注意深く水洗を実施ずろことが好ま
しい。特に酸処理浴とアルカリ処理浴どの間に適切は水
洗を行うべきである。注意深い水洗工程は、金めつき工
程の後にも行うが、この水洗工程においては、１μシー
メンス／ ｃｙｎよ’）少／：ｒい導電度の水を好まし
くは使用する。還元雰囲気中においての金属″＄、覆セ
ラミックコンポーネントの熱処理は不要である。Preferably, careful water washing is not performed between each of the above steps. In particular, washing with water should be carried out appropriately between the acid treatment bath and the alkaline treatment bath. A careful water rinsing step is also carried out after the gold plating step, in which water with a conductivity as low as 1 μSiemens/cyn is preferably used. Heat treatment of metal-covered ceramic components in a reducing atmosphere is not required.
（８）
タングステン又はモリブテンの表面上に金めつきを施こ
されるセラミック本体の組成は臨界ではない。酸化アル
□ニウムからできて（・る部材特にＡｌ）２０．を９０
重重量板上含有するセラミック本体が好ましい。(8) The composition of the ceramic body to be gold plated on a tungsten or molybdenum surface is not critical. Made of aluminum oxide (particularly Al)20. 90
A ceramic body containing a heavy weight plate is preferred.
次に本発明を、表に示した例によって一層詳細に説明す
る。この例では、スクリーンプリンティング及び焼成に
よって薄り・幾何学的／、〔タングステン構造を被覆（
−たセラミックＡｌ、、０２基体の金めつきが記述され
る。The invention will now be explained in more detail by means of examples shown in the table. In this example, the tungsten structure is covered by screen printing and firing.
-Gold plating of ceramic Al,.02 substrates is described.
１０−４０秒 ０％塩酸水溶液 ２０°０１３０秒 水 洗 ２０℃、 １０−４０秒 ２７５％ＩＩ Ｆ及び２５％ Ｈ２，’；□Ｆ６水溶液 ２０’Ｃ１ ］２０秒 純水による水洗 ２０’Ｃ１ １Ｏ−４０秒 ３％ ＮａＯＨ水溶液 ９０℃、 １８０秒 純水による水洗 ９０’Ｃ。10-40 seconds 0% hydrochloric acid aqueous solution 20°0130 seconds water wash 20℃, 10-40 seconds 275% II F and 25% H2,’;□F6 aqueous solution 20’C1 ]20 seconds Washing with pure water 20’C1 1O-40 seconds 3% NaOH aqueous solution 90℃, 180 seconds Washing with pure water 90'C.
］５秒 ２０％ｌｌ２Ｓｏ、水溶液 ４０’Ｃ。]5 seconds 20%ll2So, aqueous solution 40'C.
１２０秒 純水による水洗 ２０℃、 １５秒 シアン化金（１１力リ０５％及び ｐＨ１３，５までの水酸化ナト リウムを含有する無電解金浴 ９５°Ｃ 純水による水洗 ６５秒 乾燥120 seconds Washing with pure water 20℃, 15 seconds Gold cyanide (11 strength 05% and Sodium hydroxide up to pH 13.5 Electroless gold bath containing lithium 95°C Washing with pure water 65 seconds drying
Claims (5)
いタングステン又はモリブデンの表面に無電解金めつき
を施こす方法において、ＨＦ及びＨ＿２ＳｉＦ＿６の水
溶液によつて該表面をひと先ず処理した後、ｐＲが１０
以上の水性アルカリ浴中及びｐＨが３以下の水性酸浴中
において該表面を次々に処理し、このように処理した該
表面を水性の金含有浴によつて金めつきすることから成
る金めつき方法。1. In a method for electroless gold plating of a thin tungsten or molybdenum surface deposited on a ceramic body by metallization, after the surface has been first treated with an aqueous solution of HF and H_2SiF_6, a pR of 10
A gold plating method comprising sequentially treating the surface in an aqueous alkaline bath as described above and an aqueous acid bath having a pH of 3 or less, and gold plating the thus treated surface in an aqueous gold-containing bath. How to attach.
Ｈ＿２ＳｉＦ＿６によつて処理する前に酸化物の被膜そ
の他の汚染物をアルカリ浴及び酸浴中の処理によつて最
初に除去する請求項１記載の金めつき方法。2. The surface of the tungsten or molybdenum coating is HF/
2. The method of gold plating according to claim 1, wherein oxide coatings and other contaminants are first removed by treatment in alkaline and acid baths before treatment with H_2SiF_6.
にセラミツク本体を水酸化アルカリの水性浴中において
処理する請求項１記載の金めつき方法。3. 2. The method of gold plating according to claim 1, wherein the ceramic body is treated in an aqueous alkali hydroxide bath after the treatment with HF/H_2SiF_6 and before gold plating.
に希硫酸から成る浴中においてセラミツク本体を処理す
る請求項１記載の金めつき方法。4. 2. The method of claim 1, wherein the ceramic body is treated in a bath of dilute sulfuric acid after the treatment with HF/H_2SiF_6 and before gold plating.
又はモリブデンの表面を処理する請求項１記載の金めつ
き方法。5. 2. The gold plating method according to claim 1, wherein the surface of tungsten or molybdenum deposited on the aluminum oxide body is treated.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE3917867.6 | 1989-06-01 | ||
| DE19893917867 DE3917867A1 (en) | 1989-06-01 | 1989-06-01 | Electroless gold plating - of tungsten or molybdenum metallisations esp. on electronic ceramic components |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0336282A true JPH0336282A (en) | 1991-02-15 |
Family
ID=6381840
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14327490A Pending JPH0336282A (en) | 1989-06-01 | 1990-05-31 | Gold-plating |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JPH0336282A (en) |
| DE (1) | DE3917867A1 (en) |
| FR (1) | FR2647780B1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004143597A (en) * | 2002-10-21 | 2004-05-20 | General Electric Co <Ge> | Process for removing aluminosilicate material from substrate, and composition used therefor |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7457537B2 (en) * | 2020-03-06 | 2024-03-28 | 関東化学株式会社 | Composition for electroless gold plating |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1413507A (en) * | 1963-11-04 | 1965-10-08 | Thomson Houston Comp Francaise | Improvements to metallized semiconductor substrates |
| DE1621367A1 (en) * | 1967-10-18 | 1971-05-06 | Telefunken Patent | Method for activating a metallization layer |
| US3993808A (en) * | 1971-08-13 | 1976-11-23 | Hitachi, Ltd. | Method for electroless plating gold directly on tungsten or molybdenum |
| FR2294243A1 (en) * | 1974-12-11 | 1976-07-09 | Ceramic Systems | Plating refractory metals - using a non-electrolytic plating bath |
| US4093756A (en) * | 1976-10-04 | 1978-06-06 | General Electric Company | Process for electroless deposition of metals on zirconium materials |
| JPS63190177A (en) * | 1987-02-03 | 1988-08-05 | Nippon Mining Co Ltd | Pretreatment of copper paste before electroless plating |
-
1989
- 1989-06-01 DE DE19893917867 patent/DE3917867A1/en not_active Withdrawn
-
1990
- 1990-05-28 FR FR9006570A patent/FR2647780B1/en not_active Expired - Fee Related
- 1990-05-31 JP JP14327490A patent/JPH0336282A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004143597A (en) * | 2002-10-21 | 2004-05-20 | General Electric Co <Ge> | Process for removing aluminosilicate material from substrate, and composition used therefor |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2647780B1 (en) | 1992-09-04 |
| FR2647780A1 (en) | 1990-12-07 |
| DE3917867A1 (en) | 1990-12-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4811756B2 (en) | Method for manufacturing metal-ceramic bonding circuit board | |
| US5058799A (en) | Metallized ceramic substrate and method therefor | |
| US5100714A (en) | Metallized ceramic substrate and method therefor | |
| TWI552658B (en) | Plating method of circuit substrate, production method of plated circuit substrate, and silver etching liquid | |
| CN105887149B (en) | A kind of metallized ceramic electro-plating method | |
| US4832988A (en) | Process for chemically metallizing an inorganic substrate | |
| CN111627822A (en) | Etching solution and etching method for active metal layer of copper-clad ceramic substrate | |
| JP2014053619A (en) | Method for manufacturing metal-ceramic bonded circuit board | |
| WO1995014116A1 (en) | Preparation of alumina ceramic surfaces for electroless and electrochemical metal deposition | |
| JP3959044B2 (en) | Pretreatment method for plating aluminum and aluminum alloy | |
| JPH0336282A (en) | Gold-plating | |
| JPH0356310B2 (en) | ||
| WO2018121219A1 (en) | Heat dissipation substrate, preparation method and application thereof, and electronic component | |
| KR20010042625A (en) | Method for coating surfaces of copper or of a copper alloy with a tin or tin alloy layer | |
| JP2005518328A (en) | Method for metallizing titanate-based ceramics | |
| JPH05160551A (en) | Method of manufacturing electronic part mounting aluminum nitride board | |
| JP2011211217A (en) | Manufacturing method for metal-ceramic junction circuit board | |
| US4948674A (en) | Method of applying a metal layer of large adhesive strength on enamels | |
| US3862850A (en) | Electroless gold plating on refractory metals | |
| JPH07235750A (en) | Manufacture of circuit board | |
| EP0254201A1 (en) | Method of metallizing ceramic substrates | |
| CN108950471A (en) | A kind of metal product surface corrosion-resistance treatment technique | |
| KR101179118B1 (en) | Heating plate with AlN-hBN composite substrate and manufacturing method of the same | |
| JP3131029B2 (en) | Aluminum nitride substrate and method of manufacturing the same | |
| JP4556312B2 (en) | Ceramic multilayer electronic component and manufacturing method thereof |