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EP0146732B1 - Procédé et dispositif pour déposer par exemple du cuivre à partir d'un électrolyte liquide introduit dans un électrolyeur pluricellulaire - Google Patents

Procédé et dispositif pour déposer par exemple du cuivre à partir d'un électrolyte liquide introduit dans un électrolyeur pluricellulaire Download PDF

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Publication number
EP0146732B1
EP0146732B1 EP84113215A EP84113215A EP0146732B1 EP 0146732 B1 EP0146732 B1 EP 0146732B1 EP 84113215 A EP84113215 A EP 84113215A EP 84113215 A EP84113215 A EP 84113215A EP 0146732 B1 EP0146732 B1 EP 0146732B1
Authority
EP
European Patent Office
Prior art keywords
liquid
electrolysis
inlet
etchant
container
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
Application number
EP84113215A
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German (de)
English (en)
Other versions
EP0146732A1 (fr
Inventor
Walter Senator H.C. Dr.H.C.Ing. Holzer
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from DE19833340360 external-priority patent/DE3340360C2/de
Priority claimed from DE19843422276 external-priority patent/DE3422276A1/de
Application filed by Individual filed Critical Individual
Priority to AT84113215T priority Critical patent/ATE32358T1/de
Publication of EP0146732A1 publication Critical patent/EP0146732A1/fr
Application granted granted Critical
Publication of EP0146732B1 publication Critical patent/EP0146732B1/fr
Expired legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/06—Operating or servicing
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells

Definitions

  • the invention relates to a working method for the deposition of copper from a liquid electrolyte serving as etching liquid by guiding the liquid flow metered through an inlet into a multi-cell electrolysis container, from which it emerges after deposition of the copper from an outlet, the liquid flow in front of one under the Liquid level of the electrolysis container lying inlet passes through a liquid template formed by the liquid flow in a liquid buffer container in order to flow through the individual cells of the electrolysis container with a uniform distribution.
  • the invention further relates to a device for the deposition of copper from a liquid electrolyte serving as an etching liquid using a multi-cell electrolysis container with an inlet below the liquid level to be formed in the electrolysis container for the entry of the liquid electrolyte and outlet for the discharge of the electrolyte as well as an inlet located in front of the inlet Buffer container which is formed by an intermediate wall arranged parallel to the inlet side of the electrolysis container, the lower edge and side edges of which are connected in a liquid-tight manner to the electrolysis container in the manner of a partition, the intermediate wall possibly being provided with inlet openings.
  • a sensor was in the etching liquid, which is continuously circulated. Even if the sensor is brought into flow-reduced places in the etching container, the measurement result is still so imprecise that the purpose of the invention, namely to obtain an optimal etching speed, is not achieved. Dipping printed circuit boards into the etching liquid changes their physical and chemical composition. It has been found that certain parameters of the chemical and / or physical nature of the etching liquid must be present in order to have an optimal etching speed.
  • the present method is an environmentally friendly etching, i.e. the etching liquid is continuously circulated. It is not replaced, as in known methods, when it is used up, but is regenerated or also contains additives which ensure that an optimal etching rate is always present.
  • the object of the invention is, based on an absolutely uniform distribution of the liquid electrolyte among the electrodes, to direct the working process and to design the device such that the liquid electrolyte serving as the etching liquid is optimally adjusted with regard to its chemical properties.
  • a sensor for adjusting the etching liquid in a bypass to a circulation line the etching liquid is arranged between an etching container and the electrolysis cell, which is connected at adjustable, time intervals via a valve to the circulation line, with a switching phase of the sensor when the valve is closed, i.e. when the etching liquid is at rest.
  • the liquid electrolyte enters the container via a liquid reservoir.
  • This liquid charge ensures that the electrodes are acted upon by the liquid electrolyte in a very uniform manner. Since the speed of the liquid flow from the inlet to the outlet is very low, it is important at these low flow speeds to carry out the supply of the liquid flow very evenly on the inlet side and, analogously, also to discharge the liquid flow evenly on the outlet side, so that every square millimeter of the plates - and these are usually very many in such a container - is evenly acted upon by the liquid flow or then a very uniform precipitation occurs.
  • the exact flow-independent measurement and setting of the etching liquid is carried out by a sensor, which is arranged in a bypass for the circulation of the etching liquid between the etching container and the electrolysis cell and is connected to the circulation line at adjustable, time intervals via a valve, the switching phase of the sensor when the valve is closed , ie in the bypass when the etching liquid is at rest.
  • An embodiment according to the invention is that the sensor is a known float with an inductive or capacitive tap.
  • the senor prefferably located in an overflow vessel arranged in the bypass line.
  • This overflow vessel ensures that the amount of sample liquid always remains exactly constant.
  • valve in the inlet to the overflow vessel.
  • valve In order to ensure automatic operation, it is important that the valve is an electromagnetic valve, the open and closed position of which is program-controlled.
  • the sensor e.g. B. via an amplifier, the power supply to the electrolytic cell switches.
  • the electrolysis cell is used for copper deposition, and depending on a set value, one is then able to assign a certain specific weight to the etching liquid according to a certain copper content.
  • the senor for. B. via a valve and an amplifier that controls the fluid supply to the electrolytic cell.
  • a working method for etching printed circuit boards results from the fact that the etching liquid in the etching container is continuously monitored;
  • the teaching of the invention then consists in that, depending on the number of etchings, additives are added to the etching liquid at intervals until an optimal etching rate is reached.
  • the working method can only be carried out precisely by a sensor monitoring the condition of the etching liquid in a control vessel, the filling of which takes place at selectable, time intervals, and the measuring phase of the sensor being moved to the stationary phase of the measuring liquid in the control vessel.
  • a preferably used device for uniform distribution of the liquid electrolyte provides a liquid buffer container which is formed by an intermediate wall arranged parallel to the inlet side of the electrolysis container, the upper edge of which is below the liquid level of the electrolytic container, while the lower edge and the side edges of this intermediate wall are also liquid-tight the electrolysis container are connected in the manner of a partition.
  • the design of the buffer container or the partition walls can be different.
  • One possibility is that the upper edge of the intermediate wall projects above the liquid level of the electrolysis container and inlet openings are arranged in the intermediate wall below the liquid level.
  • the inlet openings arranged approximately in the middle of the liquid level, to conduct the liquid flow evenly between the electrodes.
  • outlet side also has one or more intermediate walls and that the discharge below the liquid level takes place through individual openings and / or slits comparable to that at the inlet.
  • a wide variety of designs can be combined on the inlet side with the outlet side.
  • two partitions could be used on the inlet side and only one partition on the outlet side, or the same distribution devices for the liquid flow could be used on the inlet and outlet sides.
  • FIG. 1 the direction of the arrow 1 schematically shows the liquid flow of the liquid electrolyte through the electrolysis container 3.
  • the liquid flow enters on the inlet side 6 and leaves the container on the outlet side 18.
  • Electrodes 16 are connected in series as anodes or cathodes. The uniform supply or flow through the individual cells is of the utmost importance.
  • FIG. 2 which shows an electrolysis container 3 used in the device according to the invention
  • the liquid flow in the direction of the arrow 1 is fed from above by a feed 14.
  • the liquid buffer container 5 is formed in a manner known per se from an intermediate wall 7, the side edges 10, 11, such as. B. Fig. 3 shows, and the lower edge 9 are liquid-tightly connected to the container 3 so that they form a partition.
  • inlet openings 4 are then arranged. These inlet openings can either be arranged above, in the middle or in some way distributed.
  • a lower inlet 12 can also be provided instead of the upper inlet or the upper feed 14. In this case, the upstream buffer container 13 would then be omitted.
  • Fig. 4 is shown again in perspective, such as. B. inlet openings 4 can be arranged below the liquid level 2 in the upper region within the intermediate wall 7.
  • the outlet side 18 can also be designed accordingly, it being possible to combine individual elements on the inlet side with other elements on the outlet side, but these elements are in themselves the same.
  • 20 processes 21 are arranged in an intermediate wall. These processes can in turn be circular, slit-shaped or otherwise adapted to the flow.
  • the liquid flow arriving in the direction of the arrow 25 then enters in the direction of the arrow 27 into the buffer container 28 on the outlet side, which can be designed analogously to the buffer container 5 on the inlet side.
  • An overflow 22 is provided there, that is to say the liquid which now flows out is released in free fall. This overflow automatically ensures that the liquid level 2 remains constant.
  • FIG. 5 which shows an exemplary embodiment of the entire device of the invention, schematically shows printed circuit boards 31, which are immersed in the etching container 32 by dipping in the direction of the arrow 43 in a manner known per se for producing electrical circuits.
  • the etching container 32 is connected to an electrolysis cell 33 which, according to the above statements, has a buffer container (not shown).
  • a sensor 34 which in the exemplary embodiment (FIG. 6) has a float 35, is arranged in the bypass 36 of a circulation line 37.
  • the valve 38 which controls the inflow to an overflow vessel 40 in which the float 35 is located, can be actuated by a program control 42.
  • the float has a known inductive tap 39, i.e. the measurement order switches on or off via their contact connections 44 when the contact 39 attached to the float 35, e.g. B. a reed contact from the magnetic field of the excitation coils 45 in the fixed part.
  • FIGS. 5 and 6 The mode of operation can be seen from FIGS. 5 and 6 as follows:
  • the etching liquid 46 is drawn in by the pump 48 in the direction of the arrow 47 and thus reaches the circulation line 37.
  • there is also a water jet pump 49 in the circulation line which draws in partial quantities of regenerated etching liquid from the electrolysis cell 33 in the direction of the arrow 50.
  • the pump then conveys the partially regenerated etching liquid back into the etching tank 32 in the direction of the arrow 51.
  • the feed to the electrolysis cell 33 takes place via a branch 52 when the valve 53 is open. At intervals, e.g. B. by a program control 42, the valve 38 is opened.
  • a sample amount is taken from the etching liquid located in the circulation line 37 and is fed into an overflow vessel 40 in the direction of arrow 54 (cf. FIG. 6).
  • the overflow 55 in this vessel ensures that the amount to be measured in the measuring container 56 remains the same. If this measuring container 56 is filled, the excess sample quantity runs again in the direction of arrow 57 into the etching container 32.
  • the float 35 now moves in the direction of arrow 58, so that the contacts 45 z. B. switch off the power supply of the electrolytic cell 33, not shown, if the copper content in the etching liquid becomes too high, or switch it on again if it becomes too low.
  • valves 59, 60 can be switched, which feed additives into the etching container 32 via lines 61, 62 into the etching container 32.
  • additives for this in order to bring the etching speed to an optimal level.

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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)
  • Electrolytic Production Of Metals (AREA)
  • ing And Chemical Polishing (AREA)
  • Manufacturing Of Printed Circuit Boards (AREA)

Claims (9)

1. Procédé pour déposer du cuivre à partir d'un électrolyte liquide servant d'agent décapant, par l'introduction dosée de l'électrolyte liquide dans . un électrolyseur pluricellulaire (3), qu'il quitte après avoir déposé le cuivre, le liquide (1) traversant, en amont d'une entrée d'admission située plus bas que le niveau dans la cellule, une réserve de cet électrolyte liquide se trouvant dans un compartiment-tampon (5), pour parvenir ensuite également réparti aux différentes cellules de l'électrolyseur (3), caractérisé en ce que le débit de l'électrolyte est contrôlé par un régulateur (34) monté dans une branche de dérivation (36) dirigée vers une canalisation de recirculation (37) entre la cuve d'électrolyte (32) et la cellule (33) de l'électrolyseur, le régulateur étant mis en communication par une vanne (38) avec la canalisation de recirculation (37), à des intervalles de temps réglables, ladite vanne (38) se fermant quand le débit d'électrolyte s'interrompt.
2. Dispositif pour déposer du cuivre à partir d'un électrolyte liquide servant d'agent décapant, utilisant un électrolyseur pluricellulaire (3) pourvu d'une entrée d'admission de l'électrolyte située plus bas que le niveau à atteindre dans l'électrolyseur et d'une sortie d'évacuation, ainsi que d'un compartiment-tampon (5) situé en amont de l'entrée d'admission, défini par une cloison intermédiaire (7) parallèle à la face (6) côté admission de l'électrolyseur (3) et dont le bord inférieur (9) et les bords latéraux (10, 11) sont reliés de manière étanche à l'électrolyseur (3) à la manière d'une paroi de compartimentage, cette cloison intermédiaire (7) pouvant être éventuellement pourvue d'ouvertures de passage (4), caractérisé en ce qu'un régulateur (34) contrôlant le débit de l'électrolyte est monté dans une branche de dérivation (36) de la canalisation de recirculation (37) entre le réservoir (32) et la cellule d'électrolyse (33), ledit régulateur (34) pouvant être mis en communication avec la canalisation de recirculation (37), à des intervalles de temps réglables, au moyen d'une vanne (38).
3. Dispositif suivant la revendication 2, caractérisé en ce que le bord supérieur (8) de la paroi (7) de l'électrolyseur (3) se trouve plus bas que le niveau à atteindre dans la cellule.
4. Dispositif suivant les revendications 2 ou 3, caractérisé en ce que l'entrée (12) dans le compartiment-tampon (5) se fait par le bas, sous la pression de l'électrolyte.
5. Dispositif suivant les revendications 2 à 4, caractérisé en ce que l'entrée dans le compartiment-tampon (5) s'effectue à travers un premier compartiment-tampon (13).
6. Dispositif suivant las revendications 2 à 5, caractérisé en ce que le régulateur (34) comporte un flotteur (39) inductif ou capacitif.
7. Dispositif suivant les revendications 2 à 6, caractérisé en ce que le régulateur (34) est logé dans une chambre de trop-plein (40) montée dans la branche de dérivation (36).
8. Dispositif suivant les revendications 2 à 7, caractérisé en ce que la vanne (38) est montée dans la canalisation (41) vers la chambre de trop- plain (40).
9. Dispositif suivant la revendication 8, caractérisé en ce que la vanne (38) est une vanne électromagnétique à ouverture/fermeture programmée (42).
EP84113215A 1983-11-08 1984-11-02 Procédé et dispositif pour déposer par exemple du cuivre à partir d'un électrolyte liquide introduit dans un électrolyeur pluricellulaire Expired EP0146732B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT84113215T ATE32358T1 (de) 1983-11-08 1984-11-02 Arbeitsverfahren und vorrichtung zur ausuebung des verfahrens zur abscheidung von z.b. kupfer aus fluessigen elektrolyten, der durch einen mehrzelligen elektrolysebehaelter gefuehrt wird.

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE3340360 1983-11-08
DE19833340360 DE3340360C2 (de) 1983-11-08 1983-11-08 Elektrolysebehälter
DE19843422276 DE3422276A1 (de) 1984-06-15 1984-06-15 Vorrichtung und arbeitsverfahren zum aetzen von leiterplatten
DE3422276 1984-06-15

Publications (2)

Publication Number Publication Date
EP0146732A1 EP0146732A1 (fr) 1985-07-03
EP0146732B1 true EP0146732B1 (fr) 1988-02-03

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EP84113215A Expired EP0146732B1 (fr) 1983-11-08 1984-11-02 Procédé et dispositif pour déposer par exemple du cuivre à partir d'un électrolyte liquide introduit dans un électrolyeur pluricellulaire

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US (1) US4581115A (fr)
EP (1) EP0146732B1 (fr)
JP (1) JPH0653946B2 (fr)
DE (1) DE3469190D1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109742175A (zh) * 2019-01-02 2019-05-10 北京工业大学 垂直耦合型波分复用光信号接收共面光电探测器

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JPH0389166U (fr) * 1989-12-25 1991-09-11
US5855756A (en) * 1995-11-28 1999-01-05 Bhp Copper Inc. Methods and apparatus for enhancing electrorefining intensity and efficiency
DE19841587A1 (de) * 1998-09-11 2000-03-16 Metallgesellschaft Ag Elektrolsysezelle zum elektrochemischen Abscheiden eines der Metalle Kupfer, Zink, Blei, Nickel oder Kobalt
RU2213165C2 (ru) * 2001-03-20 2003-09-27 Открытое акционерное общество "Уральский институт металлов" Электролизeр для электрохимического осаждения меди
DE10131982A1 (de) * 2001-07-02 2003-01-16 Voith Paper Patent Gmbh Verfahren und Vorrichtung zum Entgasen von Suspension, insbesondere Faserstoffsuspension
JP4802424B2 (ja) * 2001-09-04 2011-10-26 住友金属鉱山株式会社 電解液給液流量制御装置およびその装置を使用した種板製造方法
AT505700B1 (de) 2007-08-27 2009-12-15 Mettop Gmbh Verfahren zum betreiben von kupfer-elektrolysezellen
JP5632340B2 (ja) * 2011-08-05 2014-11-26 Jx日鉱日石金属株式会社 水酸化インジウム及び水酸化インジウムを含む化合物の電解製造装置及び製造方法
CN104512946B (zh) * 2013-09-29 2018-03-30 上海轻工业研究所有限公司 金属废水的在线电沉积方法和装置
JP6222071B2 (ja) * 2014-12-19 2017-11-01 住友金属鉱山株式会社 水酸化インジウム粉の電解装置、水酸化インジウム粉の製造方法、及びスパッタリングターゲットの製造方法
JP6222072B2 (ja) * 2014-12-19 2017-11-01 住友金属鉱山株式会社 水酸化インジウム粉又は水酸化スズ粉の電解装置、水酸化インジウム粉又は水酸化スズ粉の製造方法、及びスパッタリングターゲットの製造方法
CN105780051A (zh) * 2014-12-23 2016-07-20 重庆航凌电路板有限公司 印制电路板碱性蚀刻铜回收电解设备
JP7150769B2 (ja) * 2020-01-30 2022-10-11 Ｊｘ金属株式会社 電解装置及び電解方法
JP7150768B2 (ja) * 2020-01-30 2022-10-11 Ｊｘ金属株式会社 電解装置及び電解方法

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JPS5124537A (en) * 1974-08-26 1976-02-27 Hitachi Ltd Etsuchinguyokuno saiseihoho
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NL8005427A (nl) * 1980-09-30 1982-04-16 Veco Beheer Bv Werkwijze voor het vervaardigen van zeefmateriaal, verkregen zeefmateriaal alsmede inrichting voor het uitvoeren van de werkwijze.
JPS6053117B2 (ja) * 1981-01-29 1985-11-22 小名浜製錬株式会社 銅電解操業法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109742175A (zh) * 2019-01-02 2019-05-10 北京工业大学 垂直耦合型波分复用光信号接收共面光电探测器

Also Published As

Publication number Publication date
DE3469190D1 (en) 1988-03-10
JPS60121292A (ja) 1985-06-28
JPH0653946B2 (ja) 1994-07-20
US4581115A (en) 1986-04-08
EP0146732A1 (fr) 1985-07-03

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