DE3907902A1 - METHOD FOR CHEMICALLY METALLIZING CERAMIC BODIES - Google Patents
METHOD FOR CHEMICALLY METALLIZING CERAMIC BODIESInfo
- Publication number
- DE3907902A1 DE3907902A1 DE19893907902 DE3907902A DE3907902A1 DE 3907902 A1 DE3907902 A1 DE 3907902A1 DE 19893907902 DE19893907902 DE 19893907902 DE 3907902 A DE3907902 A DE 3907902A DE 3907902 A1 DE3907902 A1 DE 3907902A1
- Authority
- DE
- Germany
- Prior art keywords
- acid
- etching
- fluoroboric acid
- piezoceramic
- added
- 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.)
- Withdrawn
Links
- 238000000034 method Methods 0.000 title claims description 16
- 239000000919 ceramic Substances 0.000 title claims description 7
- RILZRCJGXSFXNE-UHFFFAOYSA-N 2-[4-(trifluoromethoxy)phenyl]ethanol Chemical compound OCCC1=CC=C(OC(F)(F)F)C=C1 RILZRCJGXSFXNE-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000005530 etching Methods 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 7
- LDDQLRUQCUTJBB-UHFFFAOYSA-O azanium;hydrofluoride Chemical compound [NH4+].F LDDQLRUQCUTJBB-UHFFFAOYSA-O 0.000 claims abstract description 4
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001465 metallisation Methods 0.000 claims abstract description 4
- 239000004327 boric acid Substances 0.000 claims abstract description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 abstract description 5
- 230000001070 adhesive effect Effects 0.000 abstract description 5
- 239000000654 additive Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- GHPYJLCQYMAXGG-WCCKRBBISA-N (2R)-2-amino-3-(2-boronoethylsulfanyl)propanoic acid hydrochloride Chemical compound Cl.N[C@@H](CSCCB(O)O)C(O)=O GHPYJLCQYMAXGG-WCCKRBBISA-N 0.000 description 1
- 229910017855 NH 4 F Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 238000007747 plating 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
- C04B41/53—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone involving the removal of at least part of the materials of the treated article, e.g. etching, drying of hardened concrete
- C04B41/5338—Etching
- C04B41/5353—Wet etching, e.g. with etchants dissolved in organic solvents
-
- 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
- C04B41/91—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics involving the removal of part of the materials of the treated articles, e.g. etching
-
- 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
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1886—Multistep pretreatment
- C23C18/1893—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
- H10N30/06—Forming electrodes or interconnections, e.g. leads or terminals
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- ing And Chemical Polishing (AREA)
Abstract
Description
Die Erfindung bezieht sich auf ein Verfahren zum chemischen Metallisieren von Keramikkörpern, bei dem der Keramikkörper zu nächst geätzt, danach mit einer Palladium-Lösung aktiviert und anschließend chemisch metallisiert wird.The invention relates to a method for chemical Metallizing ceramic bodies, in which the ceramic body too next etched, then activated with a palladium solution and is then chemically metallized.
Es ist ein Verfahren zum chemischen Metallisieren von Aluminiumoxidkeramiken bekannt (Zeitschrift "Plating and Surface Finishing", September 1987, Seiten 62 bis 67), bei dem mehrere chemische Substanzen zum Ätzen verwendet werden können, von denen einzelne den Vorzug haben, daß sie zu einer verhältnis mäßig haftfesten Metallschicht auf dem behandelten Aluminiumoxid- Keramikkörper führen. Versucht man die beim Ätzen von Aluminium oxid-Keramikkörpern bewährten Substanzen auch zum Ätzen von piezokeramischen Körpern einzusetzen, dann stellt man in Versuchen fest, daß in derartiger Weise vor dem eigentlichen chemischen Metallisieren vorbehandelte Piezokeramikkörper hinsichtlich der Haftfestigkeit der Metallschicht den gestell ten Anforderungen nicht gerecht werden.It is a process for the chemical metallization of Alumina ceramics known (magazine "Plating and Surface Finishing ", September 1987, pages 62 to 67), in which several chemical substances for etching can be used by which individuals prefer to have a relationship moderately adhesive metal layer on the treated aluminum oxide Guide ceramic body. If you try to etch aluminum oxide ceramic bodies also proven substances for etching use piezoceramic bodies, then you put in Try stating that in such a way before the actual chemical metallizing pretreated piezoceramic bodies the frame with regard to the adhesive strength of the metal layer do not meet the requirements.
Gemäß der Erfindung wird daher bei einem Verfahren der eingangs angegebenen Art erfindungsgemäß bei einem Piezokeramikkörper das Ätzen mit Fluoroborsäure vorgenommen. Insbesondere bei Körpern aus Blei-Zirkonat-Titanat sowie aus Zinn-Zirkonat-Titanat als piezokeramischer Werkstoff konnten sehr gut haftende Metallschichten erzielt werden.According to the invention, therefore, in a method of the beginning specified type according to the invention in a piezoceramic body etching with fluoroboric acid. Especially at Bodies made of lead zirconate titanate and tin zirconate titanate as a piezoceramic material could adhere very well Metal layers can be achieved.
Der wesentliche Vorteil des erfindungsgemäßen Verfahrens besteht darin, daß bei einem Ätzen von Piezokeramikkörpern mit Fluoroborsäure in dem ersten von mehreren Vorbehandlungsschritten vor dem eigentlichen chemischen Metallisieren das Aufbringen einer Metallschicht ermöglicht wird, die sich durch eine hohe Haftfestigkeit auf dem Piezokeramikkörper auszeichnet.The main advantage of the method according to the invention is that when etching piezoceramic bodies with Fluoroboric acid in the first of several pretreatment steps before the actual chemical metallization a metal layer that is characterized by a high Adhesion strength on the piezoceramic body.
Es hat sich bei dem erfindungsgemäßen Verfahren im Hinblick auf eine möglichst hohe Haftfestigkeit der Metallschicht auf Piezokeramikkörpern als besonders vorteilhaft erwiesen, wenn das Ätzen der Piezokeramikkörper mit Fluoroborsäure mit einer Konzentration von 30 bis 50% bei 20 bis 60°C für eine Zeit dauer zwischen 0,5 bis 5 Minuten vorgenommen wird.It has with regard to the method according to the invention the highest possible adhesive strength of the metal layer Piezoceramic bodies have proven to be particularly advantageous if etching the piezoceramic bodies with fluoroboric acid with a Concentration of 30 to 50% at 20 to 60 ° C for a time duration between 0.5 and 5 minutes.
Unter anderem dann, wenn mit dem erfindungsgemäßen Verfahren Piezokeramikkörper mit relativ engen Bohrungen auch im Bereich dieser Bohrungen chemisch metallisiert werden sollen, ist es vorteilhaft, wenn das Ätzen der Piezokeramikkörper unter Ultra schall-Beaufschlagung erfolgt.Among other things, when using the method according to the invention Piezoceramic body with relatively narrow holes in the area of these holes are to be chemically metallized, it is advantageous if the etching of the piezoceramic body under Ultra sound is applied.
Eine besonders hohe Haftfestigkeit von Metallschichten auf Piezokeramikkörpern läßt sich dann erzielen, wenn gemäß einer weiteren Ausgestaltung des erfindungsgemäßen Verfahrens der Fluoroborsäure 0,2 bis 35 g/1 Borsäure (H3BO3) zugesetzt werden. Anstelle des Zusatzes von Borsäure haben sich auch weitere Zusätze als sehr vorteilhaft herausgestellt. Dabei handelt es sich um Ammoniumhydrogenfluorid (NH4HF2), das mit 0,2 bis 50 g/l zuzusetzen ist, oder um Ammoniumfluorid (NH4F), das als Zusatz 0,2 bis 50 g/l ausmachen kann; auch ein Zusatz von 40%iger Flußsäure (HF) mit 0,5 bis 100 ml/l ist vorteilhaft.A particularly high adhesive strength of metal layers on piezoceramic bodies can be achieved if, according to a further embodiment of the process according to the invention, 0.2 to 35 g / 1 boric acid (H 3 BO 3 ) is added to the fluoroboric acid. Instead of adding boric acid, other additives have also proven to be very advantageous. These are ammonium hydrogen fluoride (NH 4 HF 2 ), which is to be added at 0.2 to 50 g / l, or ammonium fluoride (NH 4 F), which can make up 0.2 to 50 g / l as an additive; It is also advantageous to add 40% hydrofluoric acid (HF) at 0.5 to 100 ml / l.
Zur Erläuterung der Erfindung wird im folgenden ein besonders vorteilhafter Ätzvorgang beschrieben:In order to explain the invention, a special is given below advantageous etching process described:
Das Ätzen des Piezokeramikkörpers erfolgt mit einer 50%igen Fluoroborsäure (HBF4), der 1 g/l Ammoniumhydrogenfluorid (NH4HF2) zugesetzt worden ist. Die zu ätzenden Piezokeramik körper werden bei Raumtemperatur 1 Minute der Ätzflüssigkeit ausgesetzt, wobei während dieser Zeit eine Ultraschall-Beauf schlagung erfolgt.The piezoceramic body is etched with a 50% fluoroboric acid (HBF 4 ) to which 1 g / l ammonium hydrogen fluoride (NH 4 HF 2 ) has been added. The piezoceramic bodies to be etched are exposed to the etching liquid at room temperature for 1 minute, during which time ultrasound is applied.
Claims (8)
- a) der Keramikkörper zunächst geätzt,
- b) danach mit einer Palladium-Lösung aktiviert und
- c) anschließend chemisch metallisiert wird,
- a) the ceramic body is first etched,
- b) then activated with a palladium solution and
- c) is then chemically metallized,
- d) bei einem Piezokeramikkörper das Ätzen mit Fluoroborsäure vorgenommen wird.
- d) in the case of a piezoceramic body, the etching is carried out with fluoroboric acid.
- e) das Ätzen mit Fluoroborsäure mit einer Konzentration von 30 bis 50% bei 20 bis 60°C für eine Zeitdauer zwischen 0,5 bis 5 Minuten vorgenommen wird.
- e) the etching with fluoroboric acid is carried out at a concentration of 30 to 50% at 20 to 60 ° C for a period of between 0.5 to 5 minutes.
- f) das Ätzen der Piezokeramikkörper unter Ultraschall-Beaufschlagung erfolgt.
- f) the etching of the piezoceramic body is carried out under ultrasound.
- g) der Fluoroborsäure 0,2 bis 35 g/l Borsäure zugesetzt wird.
- g) 0.2 to 35 g / l boric acid is added to the fluoroboric acid.
- h) der Fluoroborsäure 0,2 bis 50 g/l Ammoniumhydrogenfluorid zugesetzt wird.
- h) 0.2 to 50 g / l of ammonium hydrogen fluoride is added to the fluoroboric acid.
- i) der Fluoroborsäure 0,2 bis 50 g/l Ammoniumfluorid zugesetzt wird.
- i) 0.2 to 50 g / l of ammonium fluoride is added to the fluoroboric acid.
- j) der Fluoroborsäure 0,5 bis 100 ml/l 40%ige Flußsäure zugesetzt wird.
- j) 0.5 to 100 ml / l of 40% hydrofluoric acid is added to the fluoroboric acid.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19893907902 DE3907902A1 (en) | 1989-03-08 | 1989-03-08 | METHOD FOR CHEMICALLY METALLIZING CERAMIC BODIES |
| PCT/DE1990/000176 WO1990010609A1 (en) | 1989-03-08 | 1990-03-07 | Process for chemical metallization of ceramic bodies |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19893907902 DE3907902A1 (en) | 1989-03-08 | 1989-03-08 | METHOD FOR CHEMICALLY METALLIZING CERAMIC BODIES |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE3907902A1 true DE3907902A1 (en) | 1990-09-13 |
Family
ID=6376082
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE19893907902 Withdrawn DE3907902A1 (en) | 1989-03-08 | 1989-03-08 | METHOD FOR CHEMICALLY METALLIZING CERAMIC BODIES |
Country Status (2)
| Country | Link |
|---|---|
| DE (1) | DE3907902A1 (en) |
| WO (1) | WO1990010609A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19945267C1 (en) * | 1999-09-21 | 2001-04-19 | Bosch Gmbh Robert | Method for applying flat external electrodes on a piezoceramic multilayer actuator |
| CN113088289A (en) * | 2021-03-30 | 2021-07-09 | 华中科技大学 | Etching solution, application thereof and preparation method of high-bonding-strength metal layer on ceramic surface |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5045007A (en) * | 1990-11-19 | 1991-09-03 | Thomson Consumer Electronics, Inc. | Method of salvaging a color selection electrode for a CRT |
| DE69210910T2 (en) * | 1991-07-05 | 1996-12-05 | Murata Manufacturing Co | Piezoelectric element |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1515566A (en) * | 1967-03-23 | 1968-03-01 | Slip Pruf Service Corp | Process for increasing the slip resistance of glazed surfaces and concrete |
| DE1690054A1 (en) * | 1967-09-26 | 1971-04-22 | Siemens Ag | Electrical component, in particular polarized piezoelectric element with solderable assignments and method for producing the assignments |
| US4428986A (en) * | 1982-11-18 | 1984-01-31 | Eaton Corporation | Method of preparing a beryllia substrate for subsequent autocatalytic deposition of a metallized film directly thereon |
| DE3523956A1 (en) * | 1985-07-04 | 1987-01-08 | Licentia Gmbh | METHOD FOR CHEMICALLY METALLIZING AN ELECTRICALLY POOR CONDUCTING BODY FROM AN INORGANIC MATERIAL |
| DE3731167A1 (en) * | 1987-09-14 | 1989-05-11 | Schering Ag | METHOD FOR ADHESIVE METALIZATION OF EMAILS |
-
1989
- 1989-03-08 DE DE19893907902 patent/DE3907902A1/en not_active Withdrawn
-
1990
- 1990-03-07 WO PCT/DE1990/000176 patent/WO1990010609A1/en unknown
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19945267C1 (en) * | 1999-09-21 | 2001-04-19 | Bosch Gmbh Robert | Method for applying flat external electrodes on a piezoceramic multilayer actuator |
| CN113088289A (en) * | 2021-03-30 | 2021-07-09 | 华中科技大学 | Etching solution, application thereof and preparation method of high-bonding-strength metal layer on ceramic surface |
Also Published As
| Publication number | Publication date |
|---|---|
| WO1990010609A1 (en) | 1990-09-20 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| 8139 | Disposal/non-payment of the annual fee |