US20110089044A1 - Copper electrolytic plating bath and copper electrolytic plating method - Google Patents

Copper electrolytic plating bath and copper electrolytic plating method Download PDF

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Publication number
US20110089044A1
US20110089044A1 US12/903,555 US90355510A US2011089044A1 US 20110089044 A1 US20110089044 A1 US 20110089044A1 US 90355510 A US90355510 A US 90355510A US 2011089044 A1 US2011089044 A1 US 2011089044A1
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electrolytic plating
copper
copper electrolytic
plating
liter
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Abandoned
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US12/903,555
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English (en)
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Toshihisa Isono
Shinji Tachibana
Naoyuki Omura
Shunsaku HOSHI
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C Uyemura and Co Ltd
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C Uyemura and Co Ltd
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Assigned to C. UYEMURA & CO., LTD. reassignment C. UYEMURA & CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HOSHI, SHUNSAKU, ISONO, TOSHIHISA, OMURA, NAOYUKI, TACHIBANA, SHINJI
Publication of US20110089044A1 publication Critical patent/US20110089044A1/en
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/38—Electroplating: Baths therefor from solutions of copper
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/40—Forming printed elements for providing electric connections to or between printed circuits
    • H05K3/42—Plated through-holes or plated via connections
    • H05K3/423—Plated through-holes or plated via connections characterised by electroplating method

Definitions

  • This invention relates to a copper electrolytic plating bath and method, which enable high-speed plating to articles to be plated, especially particles having through-holes, blind via holes, or posts.
  • plating has been conducted while ensuring the throwing power and the physical properties of the deposit within allowable ranges by increasing the agitation if the plating temperatures is lower than 30° C. and the cathode current density is less than 5 A/dm 2 .
  • the cathode current density is less than 5 A/dm 2 .
  • it is necessary to elevate the plating temperature since there is a limit for the power-up of agitation.
  • the elevation of the temperature has presented a problem in that the conventional organic additives used for plating a substrate having through-holes and blind via holes lose their effect.
  • the resist film has a low height and large-sized individual openings (i.e. a small aspect ratio), as in the case of blind via holes, the throwing power and the physical properties of the deposit can be ensured with the conventional electrolytic plating baths so long as agitation is strengthened.
  • the aspect ratio becomes large, good plating is not expected even if strong agitation is conducted. Even if plating is performed at high speed by strengthening agitation and increasing a plating temperature, a problem is involved in that the deposit cannot be flattened.
  • plating on a post (bump) having a large aspect ratio is carried out at high speed, it is necessary to increase the plating temperature.
  • additives suited for high temperature plating should have been needed.
  • the invention has been made under these circumstances in the art and it is an object of the invention to provide a copper electrolytic plating bath which enables high-speed plating on a substrate having through-holes, blind via holes, posts or the like formed therein while keeping good throwing power and ensuring physical properties of the deposit.
  • the advantages of the high-speed plating include shortage of plating time and the possibility of increasing a quantity of output per unit time.
  • the quantity of output increases if a takt time can be shortened.
  • a plating equipment can be saved in space and the size of a plating equipment can be made smaller for the same quantity of output (e.g. the numbers of lines and plating equipment can be reduced). For instance, if a cathode current density can be doubled, any of a line length, the number of plating tanks, an amount of plating bath and a plating time can be reduced substantially to half. The speeding up of plating is thus important from the standpoint of the reduction of plating costs.
  • a compound usable as a leveler of high-speed copper electrolytic plating baths studies have been made in order to obtain, as an effective additive, a compound (i) that is able to keep an effect as a leveler when agitation is made strong and a plating temperature is elevated, i.e. a compound that shows high throwing power relative to through-holes and blind via holes and is capable of forming a plated film whose physical properties are good, or a compound capable of flat post (bump) plating.
  • the polymer compound used as the nitrogen atom-containing organic compound is obtained by a two-stage reaction comprising reacting one mole of morpholine with two moles of epichlorohydrin in an acidic aqueous solution to obtain a reaction product and further reacting one to two moles, relative to one mole of the morpholine, of imidazole with the reaction product.
  • This polymer compound effectively functions as a leveler, especially, in the copper electrolytic plating bath at a temperature as high as 35° C. or over.
  • high-speed copper electrolytic plating can be carried out on substrates having through-holes, blind via holes, posts or the like formed therein while keeping a throwing powder and ensuring the physical properties of the deposit.
  • the invention provides the following copper electrolytic plating bath and method.
  • R 1 , R 2 and R 3 independently represent an alkyl group having 1 to 5 carbon atoms
  • M represents a hydrogen atom or an alkali metal
  • a is an integer of 1 to 8
  • b, c and d are, respectively, 0 or 1.
  • the nitrogen atom-containing polymer compound used as an organic additive and serving as a leveler does not change in quality when a plating temperature is elevated and is able to keep a good balance between the promoter effect and the inhibitor effect ascribed to the organic additive present in the plating bath under temperature-elevated conditions.
  • the copper electrolytic plating bath of the invention allows a throwing power relative to through-holes or blind via holes and physical properties of the deposit to be kept when the plating temperature is elevated.
  • high-speed plating can be performed even under weak agitation, such as air agitation, which is milder than jet flow.
  • high-speed plating has been hitherto carried out by application of plating temperature and cathode current density conditions essentially requiring vigorous agitation such as of jet flow.
  • FIGS. 1(A) and 1(B) are, respectively, a sectional view of part of a substrate illustrating a portion at which a thickness of the deposit is measured for evaluating a throwing power in Examples and Comparative Examples wherein FIG. 1(A) is a sectional view of a through-hole and FIG. 1(B) is a sectional view of a blind via hole; and
  • FIG. 2 is a schematic view showing a shape and a size of a test piece used for measurement of physical properties of the deposit in Examples and Comparative Examples.
  • the copper electrolytic plating bath of the invention contains copper sulfate, sulfuric acid and chloride ions.
  • Copper sulfate is contained as copper sulfate pentahydrate in an amount of 50 to 250 g/liter, preferably 100 to 200 g/liter
  • sulfuric acid is contained in an amount of 20 to 200 g/liter, preferably 50 to 200 g/liter
  • the chloride ion is contained in an amount of 20 to 150 mg/liter, preferably 30 to 100 mg/liter.
  • the copper electrolytic plating bath of the invention further contains a sulfur atom-containing organic compound and a nitrogen atom-containing organic compound.
  • the sulfur atom-containing organic compounds may be known sulfur atom-containing organic compounds ordinarily used for copper electrolytic plating of through-holes or blind via holes. More particularly, there can be used sulfur atom-containing organic compounds of the following formulas (1) to (4):
  • R 1 , R 2 and R 3 independently represent an alkyl group having 1 to 5 carbon atoms
  • M represents a hydrogen atom or an alkali metal
  • a is an integer of 1 to 8
  • b, c and d are, respectively, 0 or 1.
  • the concentration of the compound in the copper electrolytic plating bath is generally at 0.001 to 100 mg/liter.
  • the nitrogen atom-containing organic compound used in the copper plating bath of the invention is a polymer compound, which is obtained by a two-stage reaction including reacting one mole of morpholine with two moles of epichlorohydrin in an acidic aqueous solution to obtain a reaction product and further reacting one to two moles, relative to one mole of the morpholine, of imidazole with the reaction product.
  • This nitrogen-containing polymer compound serves as a so-called leveler and does not undergo quality change when the plating temperature is elevated, for example, to 30° C. or over, particularly, to 35 to 50° C.
  • the polymer compound Under high temperature conditions, the polymer compound is able to keep a good balance between the promoter effect and the inhibitor effect ascribed to the organic additives contained in the plating bath.
  • the nitrogen-containing polymer compound serves as an effective leveler capable of keeping a throwing power and physical properties of the deposit as they are when the plating temperature is elevated.
  • This nitrogen atom-containing polymer compound is known as CAS No. 109882-76-0 and is considered to be a polymer compound having a polyether structure.
  • This polymer compound is one obtained by the two-stage reaction including a first stage of reaction between one mole of morpholine and two moles of epichlorohydrin and a second stage of reaction wherein one to two moles, preferably about two moles and more preferably 1.8 to two moles of imidazole is added to the reaction product of the first stage to provide a polymer compound.
  • one mole of morpholine is dissolved in about 375 ml of distilled water, which is adjusted in pH to 5.5 by means of HCl.
  • Two moles of epichlorohydrin are dropped in the solution at a reaction temperature of about 50° C., followed by keeping at 40° C. to 50° C. until free epichlorohydrin is not detected (first stage).
  • one mole of imidazole is added to the reaction product obtained in the first stage, to which 50 g of NaOH dissolved in 125 ml of water is added, followed by reaction at 55° C. to 60° C. for 6 hours (second stage).
  • the water is further added to the obtained solution, whereby the resultant solution of which the total amount is one litter can be used.
  • Ralu registered trademark
  • Plate MOME made by Raschig GmbH
  • the concentration of the nitrogen atom-containing polymer compound in the copper electrolytic plating bath is at 1 to 1,000 mg/liter, preferably 10 to 500 mg/liter.
  • the copper electrolytic plating bath of the invention may further comprise oxygen-containing organic compounds including polyether organic additives such as polyethylene glycol used in copper electrolytic plating of through-holes or blind via holes.
  • concentration of the oxygen-containing organic compound in the copper electrolytic plating bath is preferably at 0.001 to 5,000 mg/liter.
  • polyethylene glycol useful in the invention is one having a molecular weight of 200 to 200,000. The molecular weight in this case is measured according to a method described in Japanese Pharmacopoeia.
  • the conventional plating conditions are applicable. Especially, when employing a plating temperature of not lower than 35° C., preferably 35° C. to 50° C. and a cathode current density of not less than 5 A/dm 2 , preferably 5 to 20 A/dm 2 , a more stable throwing power and better characteristics of deposit than those obtained in the conventional copper electrolytic plating can be attained.
  • the anode used is preferably an insoluble anode.
  • an anode wherein platinum, iridium oxide or the like is coated on titanium.
  • agitation created by known agitation means may be used including, for example, jet flow agitation or circulation agitation made by a pump, air agitation made by an air pump, and mechanical agitation made by a paddle, cathode locking means or the like.
  • the copper electrolytic plating using the copper electrolytic plating bath of the invention is particularly suited for copper electrolytic plating of articles to be plated such as printed boards having a non-flat portion formed on or in a substrate such as through-holes or blind via holes, or a non-flat portion formed by a resist film upon formation of posts (bumps) or the like.
  • the copper electrolytic plating is especially effective for the case of forming the deposit on inner surfaces of blind via holes including a bottom face and side faces of the blind via holes (the case does not apply via filling plating where the blind via holes are filled by copper plating).
  • the invention is suited for copper electrolytic plating of substrates having through-holes or blind via holes having a large aspect ratio (AR).
  • the invention is effective for high-speed plating of through-holes having a diameter of 0.05 to 2.0 mm, preferably 0.1 to 1.0 mm, a sheet thickness (height) of 0.01 to 2.0 mm, preferably 0.05 to 1.6 mm, and an aspect ratio (AR), i.e. height/diameter, of 0.1 to 10, preferably 0.1 to 5.0, and also of blind via holes having a diameter of 20 to 300 ⁇ m, preferably 30 to 200 ⁇ m, a height (depth) of 20 to 150 ⁇ m, preferably 40 to 100 ⁇ m, and an aspect ratio (AR), i.e. height/diameter, of 0.2 to 1.5, preferably 0.4 to 1.0.
  • AR aspect ratio
  • posts (bumps) are formed by plating
  • two methods including a method wherein an electroplated copper layer is formed on the surface of an article on which posts (bumps) are to be formed and the post (bump)-formed portion is protected with an etching resist film, followed by etching the portion not covered with the resist film and thereafter removing the resist film, and a method wherein a plating resist pattern is formed by a resist film on the surface of an article so that posts (bumps) to be formed are opened, and copper plating is carried out on this opening portion, followed by removing the resist film.
  • speeding up of the copper plating is possible.
  • the copper electrolytic plating of the invention is effective for high-speed plating of posts (bumps) having a large aspect ratio (AE), e.g. a post (bump) having a diameter of 30 to 300 ⁇ m, preferably 50 to 200 ⁇ m, a height (resist film height) of 25 to 200 ⁇ m, preferably 30 to 150 ⁇ m, and an aspect ratio (AR) of 0.2 to 3, preferably 0.3 to 2.
  • AE aspect ratio
  • the plating is such that the deposit is filled in a recessed portion formed at an opening of the plating resist.
  • copper electrolytic plating baths of the following formulations were used to form electroplated copper layers in the through-holes or blind via holes under the following plating conditions. It will be noted that the copper electrolytic plating was carried out in such a way that a known pretreatment was conducted at a portion where the copper deposit is to be formed, on which an electroless copper film (with a thickness of 0.3 ⁇ m) was formed as an underlying layer, followed by copper electrolytic plating.
  • PAS-A-5 and JGB were, respectively, set from an additive concentration sufficient to give a gloss in the highest electric potential region when determined by Hull cell test.
  • the thickness of the copper layer at portions A to F indicated in FIG. 1(A) was measured, followed by evaluation in terms of a ratio (%) calculated according to the following equation. It should be noted that as to E and F, the thickness at the central portions of the through-hole indicated at E 1 and F 1 was measured for Examples 1 to 4 and Comparative Examples 1, 3 and the thickness at upper end portion of the through-hole indicated at E 2 , F 2 was measured for Comparative Example 2.
  • the thickness of the copper layer at portions A to C indicated in FIG. 1(B) was measured, followed by evaluating in terms of a ratio (%) calculated by the following equation.
  • FIGS. 1(A) and 1(B) indicated by 1 is a substrate (insulating layer), by 2 is laminated copper, by 3 is an electroless plated copper layer, by 4 is an electroplated copper layer, by t is a through-hole, and by v is a blind via hole.
  • the thickness of the copper layer was smallest at the corner portion of the opening side of the blind via hole, and except for this, the thickness of the copper layer was smallest at the corner portion of the bottom side.
  • the copper electrolytic plating baths of Examples 1 to 4 and Comparative Examples 1 to 3 were used to evaluate physical properties of the copper layers according to the following procedures.
  • a SUS sheet was subjected to the following pretreatment and an electroplated copper layer was formed on the SUS sheet by the use of the above copper electrolytic plating baths under the following plating conditions. Moreover, after subjecting to the following aftertreatment, a foil-shaped plated layer was peeled off from the SUS sheet. This plated film (layer) was subjected to evaluation of tensile strength and percentage elongation according to the following methods.
  • the copper film prepared above was punched out into a dumbbell-shaped test piece with the sizes indicated in FIG. 2 , and the percentage elongation and tensile strength before the film was broken down under conditions of a chuck distance of 40 mm and a pulling rate of 4 mm/minute were evaluated by calculation from the following equations.
  • T tensile strength
  • F maximum tensile stress
  • d film thickness at a central portion of test piece.
  • the upper face shape of the posts after copper electrolytic plating was evaluated in respect of the longitudinal section of the posts (i.e. a section along the height). The maximum and minimum values of the post height were measured and a difference therebetween was calculated. The results are shown in Table 4.

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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)
  • Manufacturing & Machinery (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Manufacturing Of Printed Wiring (AREA)
US12/903,555 2009-10-15 2010-10-13 Copper electrolytic plating bath and copper electrolytic plating method Abandoned US20110089044A1 (en)

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JP2009238460A JP5471276B2 (ja) 2009-10-15 2009-10-15 電気銅めっき浴及び電気銅めっき方法
JP2009-238460 2009-10-15

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US20170044682A1 (en) * 2014-04-25 2017-02-16 Jcu Corporation High-speed filling method for copper
JP2017222925A (ja) * 2016-03-29 2017-12-21 ローム アンド ハース エレクトロニック マテリアルズ エルエルシーＲｏｈｍ ａｎｄ Ｈａａｓ Ｅｌｅｃｔｒｏｎｉｃ Ｍａｔｅｒｉａｌｓ ＬＬＣ メガサイズのフォトレジスト画定フィーチャを電気めっきすることが可能な電気銅めっき浴及び電気めっき方法
US9932684B2 (en) 2015-08-06 2018-04-03 Rohm And Haas Electronic Materials Llc Method of electroplating photoresist defined features from copper electroplating baths containing reaction products of alpha amino acids and bisepoxides
US10006136B2 (en) 2015-08-06 2018-06-26 Dow Global Technologies Llc Method of electroplating photoresist defined features from copper electroplating baths containing reaction products of imidazole compounds, bisepoxides and halobenzyl compounds
US10104782B2 (en) 2015-08-06 2018-10-16 Dow Global Technologies Llc Method of electroplating photoresist defined features from copper electroplating baths containing reaction products of pyridyl alkylamines and bisepoxides
US10100421B2 (en) 2015-08-06 2018-10-16 Dow Global Technologies Llc Method of electroplating photoresist defined features from copper electroplating baths containing reaction products of imidazole and bisepoxide compounds
US20180305833A1 (en) * 2017-04-20 2018-10-25 C. Uyemura & Co., Ltd. Copper electrolytic plating bath and copper electrolytic plating film
CN114134544A (zh) * 2021-12-31 2022-03-04 三门峡毕昇制版科技股份有限公司 一种电子雕刻印刷凹版碱性镀铜添加剂

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US10154598B2 (en) * 2014-10-13 2018-12-11 Rohm And Haas Electronic Materials Llc Filling through-holes
JP2016132822A (ja) * 2015-01-22 2016-07-25 富士電機株式会社 電気銅メッキ浴及び電気銅メッキ装置、並びに電気銅メッキ方法
CN105887144B (zh) * 2016-06-21 2018-09-21 广东光华科技股份有限公司 电镀铜镀液及其电镀铜工艺
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CN108950614B (zh) * 2018-06-15 2021-11-26 惠州市荣安达化工有限公司 一种vcp高效镀铜光亮剂
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Cited By (9)

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Publication number Priority date Publication date Assignee Title
US20170044682A1 (en) * 2014-04-25 2017-02-16 Jcu Corporation High-speed filling method for copper
US9932684B2 (en) 2015-08-06 2018-04-03 Rohm And Haas Electronic Materials Llc Method of electroplating photoresist defined features from copper electroplating baths containing reaction products of alpha amino acids and bisepoxides
US10006136B2 (en) 2015-08-06 2018-06-26 Dow Global Technologies Llc Method of electroplating photoresist defined features from copper electroplating baths containing reaction products of imidazole compounds, bisepoxides and halobenzyl compounds
US10104782B2 (en) 2015-08-06 2018-10-16 Dow Global Technologies Llc Method of electroplating photoresist defined features from copper electroplating baths containing reaction products of pyridyl alkylamines and bisepoxides
US10100421B2 (en) 2015-08-06 2018-10-16 Dow Global Technologies Llc Method of electroplating photoresist defined features from copper electroplating baths containing reaction products of imidazole and bisepoxide compounds
JP2017222925A (ja) * 2016-03-29 2017-12-21 ローム アンド ハース エレクトロニック マテリアルズ エルエルシーＲｏｈｍ ａｎｄ Ｈａａｓ Ｅｌｅｃｔｒｏｎｉｃ Ｍａｔｅｒｉａｌｓ ＬＬＣ メガサイズのフォトレジスト画定フィーチャを電気めっきすることが可能な電気銅めっき浴及び電気めっき方法
US20180305833A1 (en) * 2017-04-20 2018-10-25 C. Uyemura & Co., Ltd. Copper electrolytic plating bath and copper electrolytic plating film
US11248305B2 (en) * 2017-04-20 2022-02-15 C. Uyemura & Co., Ltd. Copper electrolytic plating bath and copper electrolytic plating film
CN114134544A (zh) * 2021-12-31 2022-03-04 三门峡毕昇制版科技股份有限公司 一种电子雕刻印刷凹版碱性镀铜添加剂

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CN102071443B (zh) 2016-03-02
CN102071443A (zh) 2011-05-25
JP5471276B2 (ja) 2014-04-16
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TWI534304B (zh) 2016-05-21
JP2011084779A (ja) 2011-04-28
KR20190120132A (ko) 2019-10-23

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