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EP0283681B1 - Apparatus for bump-plating chips - Google Patents

Apparatus for bump-plating chips Download PDF

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Publication number
EP0283681B1
EP0283681B1 EP88101499A EP88101499A EP0283681B1 EP 0283681 B1 EP0283681 B1 EP 0283681B1 EP 88101499 A EP88101499 A EP 88101499A EP 88101499 A EP88101499 A EP 88101499A EP 0283681 B1 EP0283681 B1 EP 0283681B1
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EP
European Patent Office
Prior art keywords
electroplating
anode
electroplating apparatus
wafer holder
leveller
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.)
Expired - Lifetime
Application number
EP88101499A
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German (de)
French (fr)
Other versions
EP0283681A1 (en
Inventor
Ernst Ing. Andrascek
Hans Ing. Grad. Hadersbeck
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Siemens AG
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Siemens AG
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Publication of EP0283681A1 publication Critical patent/EP0283681A1/en
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00Electroplating characterised by the article coated
    • C25D7/12Semiconductors
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/001Apparatus specially adapted for electrolytic coating of wafers, e.g. semiconductors or solar cells

Definitions

  • the invention relates to a galvanizing device with a galvanic bath, which contains, among other things, a leveler, and the galvanizing device further comprises activated carbon filtering.
  • This device is used to produce finely structured, thick metal deposits on semiconductor wafers.
  • the hump is generally square in shape, with the side edges being 140 ⁇ m, 100 ⁇ m and less in length. Despite the unfavorable starting point, in the middle area of the cusps there are recesses of a maximum of 8 ⁇ m up to the connection pad, the cusp surface should be almost flat.
  • the geometric properties of the system which determine the primary current distribution, should be mentioned first among the factors that determine the scatterability. They include the geometric formulas of the anode, cathode and electrolyte container as well as the arrangement of the electrodes in the electrolyte container and their distance from the vessel walls.
  • the electroplating device for producing finely structured, thick metal deposits on semiconductor wafers must also ensure a reproducible, uniformly good metal deposit for months. In addition, prevent that degradation products that interfere with good metal deposition can accumulate.
  • the invention is based on the object of designing the galvanizing device described at the outset which fulfills the extreme requirements mentioned. All known electroplating devices require at least a flat surface for this.
  • the electroplating device With the electroplating device according to the invention it is possible to produce bumps with an almost flat surface and to achieve a uniform metallization thickness over the entire area of a semiconductor wafer. In addition, this device ensures reproducible, uniformly good metal deposition for months.
  • FIG. 1 denotes an electrolyte container, shown in section, in which a galvanizing cell 2 hangs.
  • An electrolyte container can also hold several electroplating cells.
  • An insulated arrangement feeder has the reference symbol 3, a disk holder 4 and an anode 5. Outside the electrolyte container there is a continuous circulation filter 6, an activated carbon intake container 7 and an activated carbon filter pump unit 8. The power supply is provided by a current / voltage constant 9.
  • the electroplating cell is open at the top and shown with the jacket partially cut open. With 10 an aperture is designated, which is also indicated by dashed lines in Figure 1.
  • Shielding screens or porous disks can be used in the space between the anode and the disk holder, for example for uniform deposition or filtering.
  • anode 11 In the middle of the expanded metal anode 11 there is a dome-shaped elevation 12. In the jacket of the cell, openings 13 are provided at the cathode height for the electrolyte exchange (flow).
  • the disc holder 4 the body of which is identified by 14 in FIG. 3, serves as the upper end of the electroplating cell shown in FIG.
  • the disks 15 are held in the disk holder with two contacting tips 16. 17 denotes the cathode connection and 18 the aperture ring.
  • FIG. 1 comprises the essential elements of the electroplating device, namely the electroplating cell 1, the circulation filter 6 for removing impurities and an activated carbon filter 7/8 that can be activated at any time.
  • the electroplating cell consists of a plastic tube. To generate a good current distribution (macro scattering), the anode surface is designed identically to the lower opening in the plastic tube.
  • the wafer holder 4/14 with the semiconductor wafer 15 and a galvanizing ring aperture 18 covers the upper opening.
  • the ring diaphragm 18 is covered with an insulating varnish as required, whereby the macro scattering can still be optimized.
  • the insoluble titanium expanded metal anode was given the shape shown in FIG. 1 to support good current distribution, for example.
  • the required soluble anode is filled into the expanded metal anode in the form of copper granules or pallets.
  • the electrolyte is continuously pumped through a candle filter (mesh size ⁇ 10 ⁇ m) as a continuous circulation filter. In order to the necessary movement of the electrolyte in the direction of the arrow is guaranteed. However, removal of the degradation products is of greater importance for good metal deposition.
  • a special activated carbon filtering 7/8 is provided for this.
  • Special activated carbon filtering is to be understood to mean that this filtering is carried out using a paper or candle filter impregnated with activated carbon, which adsorbs in particular the low molecular weight constituents.
  • the breakdown products and the leveler are worked out.
  • the wetting agent is retained in the bathroom if the activated carbon filter is selected correctly.
  • the optimization relates to the choice of the right ratio of the daily breakdown products and leveling in relation to the area of the activated carbon filter. For example, 1 liter of electrolyte should be pumped 12 times through a filter area of 1 dm2.
  • the activated carbon filtering is carried out first on each working day, with the degradation products being removed with the leveler.
  • the renewed addition of approx. 0.1 to 0.5 ml / l leveler after the activated carbon filtering in the electrolyte cleaned of degradation products and used levelers is of particular importance for the quality of the metal deposition.
  • the newly added leveler has a very strong effect over a period of about one day. After that the leveling effect diminishes significantly.
  • the specified depressions then form again on the cusp surface in a concave shape ( ⁇ 4 ⁇ m).
  • leveling agent without the special activated carbon filtering no longer brings the strong leveling effect, but completely changes the separation characteristics, so that the opposite effect of leveling occurs.
  • the invention is not restricted to the exemplary embodiment described and illustrated.
  • glossers alone or leveling and glossing can be used Find.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Electrodes Of Semiconductors (AREA)

Description

Die Erfindung betrifft eine Galvanisiereinrichtung mit einem galvanischen Bad, das unter anderem einen Einebner enthält, und die Galvanisiereinrichtung ferner eine Aktivkohlefilterung aufweist. Diese Einrichtung dient zum Erzeugen feinstrukturierter, dicker Metallabscheidungen auf Halbleiterscheiben.The invention relates to a galvanizing device with a galvanic bath, which contains, among other things, a leveler, and the galvanizing device further comprises activated carbon filtering. This device is used to produce finely structured, thick metal deposits on semiconductor wafers.

Für die Mikropack-Technik, einer Bauform für integrierte Schaltungen, sind auf den Chip-Bauelementen aufgalvanisierte Höcker erforderlich, die etwa 18 µm über die Chip-Oberfläche herausragen. In der Draufsicht besitzt der Höcker im allgemeinen eine quadratische Form, wobei die Seitenkanten eine Länge von 140 µm, 100 µm und kleiner aufweisen. Trotz der ungünstigen Ausgangsbasis, im Mittelbereich der Höcker sind Vertiefungen von maximal 8 µm bis zum Anschluß-Pad vorgegeben, soll die Höckeroberfläche nahezu plan sein.For the micropack technology, a design for integrated circuits, bumps electroplated on the chip components are required, which protrude about 18 µm above the chip surface. In plan view, the hump is generally square in shape, with the side edges being 140 µm, 100 µm and less in length. Despite the unfavorable starting point, in the middle area of the cusps there are recesses of a maximum of 8 µm up to the connection pad, the cusp surface should be almost flat.

Aus der US-Patentschrift US 4,170,959 ist ein Gerät zur Galvanisierung von Höckern auf einer Oberfläche eines Halbleiterwafers bekannt. Der Wafer wird dabei durch eine Vielzahl von Halterungen horizontal arretiert, wobei dessen Unterseite in Kontakt mit einer Galvanisierflüssigkeit kommt. Eine ähnliche Apparatur wird in der US-Patentschrift US 4,137,867 beschrieben.From US Pat. No. 4,170,959, a device for galvanizing bumps on a surface of a semiconductor wafer is known. The wafer is locked horizontally by a plurality of holders, the underside of which comes into contact with an electroplating liquid. A similar apparatus is described in US Pat. No. 4,137,867.

Mit den bekannten Galvanisiereinrichtungen ist es aufgrund der Makrostreufähigkeit nicht möglich, über die Fläche einer zum Beispiel 100 mm-Halbleiterscheibe, mit Ausnahme eines schmalen Randbereiches, eine Gleichmäßigkeit für die Höckerhöhe von ± 1,0 µm zu erreichen. Unter den die Streufähigkeit bestimmenden Faktoren sind die geometrischen Eigenschaften des Systems, die die primäre Stromverteilung bestimmen, an erster Stelle zu nennen. Zu ihnen gehören die geometrischen Formeln von Anode, Kathode und Elektrolytbehälter sowie die Anordnung der Elektroden im Elektrolytbehälter und ihr Abstand von den Gefäßwandungen.With the known electroplating devices, it is not possible due to the macro scattering ability, for the area of a 100 mm semiconductor wafer, for example, with the exception of a narrow edge area, to achieve a uniformity for the bump height of To achieve ± 1.0 µm. The geometric properties of the system, which determine the primary current distribution, should be mentioned first among the factors that determine the scatterability. They include the geometric formulas of the anode, cathode and electrolyte container as well as the arrangement of the electrodes in the electrolyte container and their distance from the vessel walls.

Die Galvanisiereinrichtung zum Erzeugen feinstrukturierter, dicker Metallabscheidungen auf Halbleiterscheiben muß außerdem über Monate hinweg eine reproduzierbare, gleichmäßig gute Metallabscheidung gewährleisten. Darüber hinaus ist zu verhindern, daß sich Abbauprodukte, die eine gute Metallabscheidung stören, ansammeln können.The electroplating device for producing finely structured, thick metal deposits on semiconductor wafers must also ensure a reproducible, uniformly good metal deposit for months. In addition, prevent that degradation products that interfere with good metal deposition can accumulate.

Der Erfindung liegt die Aufgabe zugrunde, die eingangs beschriebene Galvanisiereinrichtung zu konzipieren, die die erwähnten, extremen Anforderungen erfüllt. Alle bekannten Galvanisiereinrichtungen setzen hierzu wenigstens einen planen Untergrund voraus.The invention is based on the object of designing the galvanizing device described at the outset which fulfills the extreme requirements mentioned. All known electroplating devices require at least a flat surface for this.

Diese Aufgabe wird erfindungsgemäß durch die Merkmale des kennzeichnenden Teils des Anspruchs 1 gelöst. Vorteilhafte Ausführungsformen und Weiterbildungen der Erfindung sind in den Unteransprüchen angegeben.This object is achieved by the features of the characterizing part of claim 1. Advantageous embodiments and developments of the invention are specified in the subclaims.

Mit der Galvanisiereinrichtung nach der Erfindung ist es möglich, Höcker mit nahezu planer Oberfläche zu erzeugen und über den gesamten Bereich einer Halbleiterscheibe eine gleichmäßige Metallisierungsdicke zu erreichen. Außerdem gewährleistet diese Einrichtung auch über Monate hinweg eine reproduzierbare, gleichmäßig gute Metallabscheidung.With the electroplating device according to the invention it is possible to produce bumps with an almost flat surface and to achieve a uniform metallization thickness over the entire area of a semiconductor wafer. In addition, this device ensures reproducible, uniformly good metal deposition for months.

Die Erfindung wird anhand der Figuren erläutert. Es zeigen:

Figur 1
eine schematische Darstellung einer Galvanisiereinrichtung nach der Erfindung,
Figur 2
eine Galvanisierzelle und
Figur 3
einen Scheibenhalter von oben und unten gesehen.
The invention is explained on the basis of the figures. Show it:
Figure 1
1 shows a schematic representation of a galvanizing device according to the invention,
Figure 2
a galvanizing cell and
Figure 3
seen a disc holder from above and below.

In der Figur 1 ist mit 1 ein im Schnitt dargestellter Elektrolytbehälter bezeichnet, in dem eine Galvanisierzelle 2 hängt. Ein Elektrolytbehälter kann aber auch mehrere Galvanisierzellen aufnehmen. Eine isolierte Anordenzuführung hat das Bezugszeichen 3, ein Scheibenhalter 4 und eine Anode 5. Außerhalb des Elektrolytbehälters befinden sich eine Dauerumlauffilterung 6, ein Aktivkohle-Einfahrbehälter 7 und ein Aktivkohle-Filterpumpenaggregat 8. Die Stromversorgung erfolgt über einen Strom-/Spannungskonstanter 9.In FIG. 1, 1 denotes an electrolyte container, shown in section, in which a galvanizing cell 2 hangs. An electrolyte container can also hold several electroplating cells. An insulated arrangement feeder has the reference symbol 3, a disk holder 4 and an anode 5. Outside the electrolyte container there is a continuous circulation filter 6, an activated carbon intake container 7 and an activated carbon filter pump unit 8. The power supply is provided by a current / voltage constant 9.

In der Figur 2 ist die Galvanisierzelle oben offen und mit teilweise aufgeschnittenem Mantel gezeigt. Mit 10 ist eine Blende bezeichnet, die auch gestrichelt in der Figur 1 angedeutet ist. Im Raum zwischen Anode und Scheibenhalter können Abschirmblenden bzw. poröse Scheiben (Diaphragma) zum Beispiel zur gleichmäßigen Abscheidung bzw. Filterung eingesetzt sein.In FIG. 2, the electroplating cell is open at the top and shown with the jacket partially cut open. With 10 an aperture is designated, which is also indicated by dashed lines in Figure 1. Shielding screens or porous disks (diaphragm) can be used in the space between the anode and the disk holder, for example for uniform deposition or filtering.

In der Streckmetallanode 11 ist in der Mitte eine kalottenförmige Erhöhung 12. Im Mantel der Zelle sind in Kathodenhöhe Öffnungen 13 für den Elektrolytaustausch (Durchströmung) vorgesehen.In the middle of the expanded metal anode 11 there is a dome-shaped elevation 12. In the jacket of the cell, openings 13 are provided at the cathode height for the electrolyte exchange (flow).

Als oberer Abschluß der in der Figur 2 dargestellten Galvanisierzelle dient der Scheibenhalter 4, dessen Körper in der Figur 3 mit 14 gekennzeichnet ist. Im Scheibenhalter werden die Scheiben 15 mit zwei Kontaktierspitzen 16 gehalten. Mit 17 sind der Kathodenanschluß und mit 18 der Blendring bezeichnet.The disc holder 4, the body of which is identified by 14 in FIG. 3, serves as the upper end of the electroplating cell shown in FIG. The disks 15 are held in the disk holder with two contacting tips 16. 17 denotes the cathode connection and 18 the aperture ring.

Die Figur 1 umfaßt die wesentlichen Elemente der Galvanisiereinrichtung, und zwar die Galvanisierzelle 1, die Umlauffilterung 6 zur Beseitigung von Verunreinigungen und eine jederzeit zuschaltbare Aktivkohlefilterung 7/8. Die Galvanisierzelle besteht aus einem Kunststoffrohr. Zur Erzeugung einer guten Stromverteilung (Makrostreuung) ist die Anodenfläche identisch mit der unteren Öffnung im Kunststoffrohr ausgelegt. Der Scheibenhalter 4/14 mit der Halbleiterscheibe 15 und einer Galvanisier-Ringblende 18 überdeckt die obere Öffnung.FIG. 1 comprises the essential elements of the electroplating device, namely the electroplating cell 1, the circulation filter 6 for removing impurities and an activated carbon filter 7/8 that can be activated at any time. The electroplating cell consists of a plastic tube. To generate a good current distribution (macro scattering), the anode surface is designed identically to the lower opening in the plastic tube. The wafer holder 4/14 with the semiconductor wafer 15 and a galvanizing ring aperture 18 covers the upper opening.

Die Ringblende 18 wird je nach Erfordernis mit einem Isolierlack bedeckt, wodurch sich die Makrostreuung noch optimieren läßt. Bei der insbesondere für die Kupferabscheidung gestalteten Galvanisierzelle erhielt die unlösliche Titan-Streckmetallanode zur Unterstützung einer guten Stromverteilung zum Beispiel die aus der Figur 1 ersichtliche Form. Die erforderliche lösliche Anode ist in Form von Kupfer-Granalien oder Pallets in die Streckmetallanode eingefüllt.The ring diaphragm 18 is covered with an insulating varnish as required, whereby the macro scattering can still be optimized. In the electroplating cell designed in particular for copper deposition, the insoluble titanium expanded metal anode was given the shape shown in FIG. 1 to support good current distribution, for example. The required soluble anode is filled into the expanded metal anode in the form of copper granules or pallets.

Um die bei der Metallabscheidung störenden Verunreinigungen zu vermeiden, wird der Elektrolyt ständig durch ein Kerzen-Filter (Maschenweite ≦ 10 µm) als Dauerumlauffilterung gepumpt. Damit ist die notwendige Bewegung des Elektrolyts in Pfeilrichtung gewährleistet. Von größerer Bedeutung für eine gute Metallabscheidung ist jedoch die Entfernung der Abbauprodukte.In order to avoid the impurities that get in the way of metal deposition, the electrolyte is continuously pumped through a candle filter (mesh size ≦ 10 µm) as a continuous circulation filter. In order to the necessary movement of the electrolyte in the direction of the arrow is guaranteed. However, removal of the degradation products is of greater importance for good metal deposition.

Erfindungsgemäß ist hierfür eine besondere Aktivkohlefilterung 7/8 vorgesehen. Unter besondere Aktivkohlefilterung ist zu verstehen, daß diese Filterung unter Verwendung eines Aktivkohle getränkten Papier- bzw. Kerzenfilters erfolgt, das im besonderen die niedermolekularen Bestandteile adsorbiert. Bei einer täglichen, zeitoptimierten Aktivkohle-Filterung werden die Abbauprodukte und der Einebner ausgearbeitet. Das Netzmittel bleibt be richtiger Wahl der Aktivkohlefilter im Bad erhalten. Die Optimierung bezieht sich auf die Wahl des richtigen Verhältnisses der täglich anfallenden Abbauprodukte und Einebner in bezug auf die Fläche des Aktivkohlefilters. So soll zum Beispiel 1 Liter Elektrolyt 12 mal durch eine Filterfläche von 1 dm² durchgepumpt werden.According to the invention, a special activated carbon filtering 7/8 is provided for this. Special activated carbon filtering is to be understood to mean that this filtering is carried out using a paper or candle filter impregnated with activated carbon, which adsorbs in particular the low molecular weight constituents. In the case of daily, time-optimized activated carbon filtering, the breakdown products and the leveler are worked out. The wetting agent is retained in the bathroom if the activated carbon filter is selected correctly. The optimization relates to the choice of the right ratio of the daily breakdown products and leveling in relation to the area of the activated carbon filter. For example, 1 liter of electrolyte should be pumped 12 times through a filter area of 1 dm².

Vor Arbeitsbeginn wird jeweils an einem Arbeitstag zuerst die Aktivkohlefilterung durchgeführt, wobei die Abbauprodukte mit dem Einebner entfernt werden. Die erneute Zugabe von ca. 0,1 bis 0,5 ml/l Einebner nach der Aktivkohlefilterung in den von Abbauprodukten und benutzten Einebner gereinigten Elektrolyt hat eine besondere Bedeutung für die Qualität der Metallabscheidung. Der frisch zugegebene Einebner wirkt über den Zeitraum etwa eines Tages sehr stark. Danach läßt die einebnende Wirkung deutlich nach. Die vorgegebenen Vertiefungen bilden sich an der Höckeroberfläche dann wieder in konkaver Form (∼4 µm) ab.Before starting work, the activated carbon filtering is carried out first on each working day, with the degradation products being removed with the leveler. The renewed addition of approx. 0.1 to 0.5 ml / l leveler after the activated carbon filtering in the electrolyte cleaned of degradation products and used levelers is of particular importance for the quality of the metal deposition. The newly added leveler has a very strong effect over a period of about one day. After that the leveling effect diminishes significantly. The specified depressions then form again on the cusp surface in a concave shape (∼4 µm).

Eine weitere Zugabe von Einebner ohne die besondere Aktivkohlefilterung bringt nicht mehr die starke einebnende Wirkung, sondern verändert völlig die Abscheidungscharakteristik, so daß ein gegenteiliger Effekt der Einebnung entsteht.A further addition of leveling agent without the special activated carbon filtering no longer brings the strong leveling effect, but completely changes the separation characteristics, so that the opposite effect of leveling occurs.

Die Erfindung ist nicht auf das beschriebene und dargestellte Ausführungsbeispiel beschränkt. So kann zum Beispiel statt Einebner allein Glänzer allein oder Einebner und Glänzer Verwendung finden.The invention is not restricted to the exemplary embodiment described and illustrated. For example, instead of leveling alone, glossers alone or leveling and glossing can be used Find.

Claims (9)

  1. Electroplating apparatus for producing finely structured, thick metal deposits, for example for producing bumps on semiconductor wafers (15), comprising an electroplating bath containing a leveller, and an active carbon filtering system, characterised in that an electroplating cell (2) equipped with anode (5), cathode (17) and diaphragm ring (18) is suspended in the electroplating bath and for its part receives the semiconductor wafer (15) in such a way that the latter is held and electrically contacted in a replaceable wafer holder (4/14) by means of contacting tips (16) and the electrically connected diaphragm ring (18) is sited in the electroplating cell (2) in such a way that no shadows are produced on the face of the semiconductor wafer (15).
  2. Electroplating apparatus according to Claim 1, characterised in that the electroplating cell (2) comprises an open plastic tube which is suspended in the electrolyte and whose lower opening is designed with a dome-shaped anode (5) extending over the entire tube opening and whose upper opening is covered by the wafer holder (4, 14) containing the semiconductor wafer (15).
  3. Electroplating apparatus according to Claim 2, characterised in that two contacting tips (16) and an electroplating ring diaphragm (18) whose area can be varied are provided on the wafer holder (4, 14).
  4. Electroplating apparatus according to Claim 2, characterised in that additional screening diaphragms or porous discs (membranes) are inserted in the space between anode (5) and wafer holder (4, 14).
  5. Electroplating apparatus according to Claim 3, characterised in that, depending on the requirement, the electroplating ring diaphragm (18) is covered with an insulating lacquer for the purpose of reducing its size.
  6. Electroplating apparatus according to Claim 3, characterised in that the electroplating ring diaphragm (18) is constructed so as to project beyond the area of the wafer holder (4, 14) for the purpose of increasing the area.
  7. Electroplating apparatus for fluoride-free baths according to Claim 2, characterised in that the anode area (5) is constructed in mesh form as an insoluble titanium expanded metal anode (11) and the soluble anode is loaded in contact with the dome.
  8. Electroplating apparatus according to Claim 1, characterised in that an active carbon filtering system (8) is used which preferably filters out the low-molecular-weight constituents of the bath, that is to say the remaining leveller and decomposition products, and leaves the high-molecular-weight wetting agent in the bath.
  9. Electroplating apparatus according to Claim 8, characterised in that a brightener or a leveller and brightener is used instead of a leveller.
EP88101499A 1987-02-23 1988-02-02 Apparatus for bump-plating chips Expired - Lifetime EP0283681B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3705727 1987-02-23
DE3705727 1987-02-23

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EP0283681B1 true EP0283681B1 (en) 1992-05-06

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EP (1) EP0283681B1 (en)
JP (1) JPS63216998A (en)
DE (1) DE3870685D1 (en)

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JPH044399B2 (en) 1992-01-28
JPS63216998A (en) 1988-09-09
EP0283681A1 (en) 1988-09-28
US4906346A (en) 1990-03-06
DE3870685D1 (en) 1992-06-11

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