CN103924269A - Application of non-pigmentary leveling agent - Google Patents
Application of non-pigmentary leveling agent Download PDFInfo
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- leveling agent
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Abstract
The invention discloses an application of a non-pigmentary leveling agent. The molecular structural formula of the leveling agent is shown in the specification. In the formula, an anion X is Cl<-> or Br<->; R1 is O or S or N, and R2, R3 and R4 can be one of H, alkyl groups, alkenyl groups, aralkyl groups, heteroarylalkyl groups, substituted alkyl groups, substituted alkenyl groups, substituted aralkyl groups or substituted heteroarylalkyl groups. The leveling agent is used in an acid copper plating technology. Molecules having special functional groups and having different structure and attributes from previous traditional leveling agents are searched and designed on the basis of the full understanding of the molecular characteristics of the acid copper plating leveling agent. The leveling agent molecules in the invention have the advantages of good water solubility, colorlessness, non-toxicity, harmlessness to human bodies, wide operating range and the like, avoid and overcome the defects of traditional pigment leveling agents, and promote the development of the non-pigmentary acid copper technology.
Description
Technical field
The present invention relates to the advanced function electronic chemical product field in semiconductor core blade technolgy, be specifically related to the application that a kind of non-dyestuff is leveling agent.
Background technology
Along with semiconductor core blade technolgy is to high-density, high function, high integrated and future development cheaply, when dwindling, electroplate technology is had higher requirement.Plating highlighted, high-flatness need to have the additive of specific function and benefit.Therefore selection and the quality evaluation of additive are most important for semicon industry.In acid copper-plating, additive system is mainly divided into organic dye system and non-dyestuff system at present, and it is main in industry member, being still at present with dyestuff.Organic dye representative as 210,510 series of Atotech (Atotech), without dyestuff cording representational be the EPI series (producing for the wheel hub of Ford Motor at present) that AM General company releases.What domestic market application was relatively wide is MN series additive without dye system.
Although it is with a long history as sour copper leveling agent that organic dye is molecule, there is obvious shortcoming in it: (1) is contaminated equipment easily; (2) plating solution is unstable when high temperature, and component is easily decomposed; (3) coating internal stress is poor etc.On market, having at present applied non-dyestuff is that additive system (as the MN series of China's exploitation) is because bright range is narrow, bright dipping is slow, leveling property (especially low current density district) is poor, the defects such as covering power deficiency, can only be for low grade products, cannot meet semicon industry for the high request of quality of coating and additive molecule, even if the EPI series of the U.S. also has no the report for semicon industry.
Summary of the invention
The Novel leveling agent of electroplating as sour copper by exploring the molecule of non-dye class, environmental friendliness and stable chemical nature, the non-dyestuff the invention provides in a kind of sour copper plating is leveling agent, object is to evade or overcome the defect that conventional dyes is leveling agent, thereby promotes that non-dyestuff is the development of sour process for copper.
For realizing above-mentioned technical purpose, reach above-mentioned technique effect, the present invention is achieved through the following technical solutions:
Non-dyestuff is an application for leveling agent, and the molecular structural formula of described leveling agent is
Wherein, negatively charged ion X=Cl
-or Br
-; R1=O or S or N; R2, R3, R4=H, alkyl, thiazolinyl, aralkyl, heteroaralkyl, substituted alkyl, substituted alkenyl, substituted aralkyl or replace a kind of in heteroaralkyl, described leveling agent is applied to sour copper electroplating technology.
Preferably, described leveling agent is L113, and its molecular structural formula is
The invention has the beneficial effects as follows:
The present invention is fully understanding on the basis of acid copper-plating leveling agent molecular characterization and the mechanism of action, seeks and designed to have specific functional groups, the molecule of traditional leveling agent different from the past on molecular structure and attribute.The advantages such as this class leveling agent molecule has good water solubility, colourless nontoxic, harmless, and operating restraint is wider.Evading and having overcome conventional dyes is the defect of leveling agent, has promoted that non-dyestuff is the development of sour process for copper.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand technique means of the present invention, and can be implemented according to the content of specification sheets, below with preferred embodiment of the present invention and coordinate accompanying drawing to describe in detail.The specific embodiment of the present invention is provided in detail by following examples and accompanying drawing thereof.
Accompanying drawing explanation
Accompanying drawing described herein is used to provide a further understanding of the present invention, forms the application's a part, and schematic description and description of the present invention is used for explaining the present invention, does not form inappropriate limitation of the present invention.In the accompanying drawings:
Fig. 1 is molecular structural formula of the present invention;
Fig. 2 is the molecular structural formula of an embodiment of the present invention L113;
Fig. 3 is the Hull groove test electroplating effect comparison diagram that L113 add-on of the present invention regulates experiment;
Fig. 4 is fixing L113 concentration of the present invention, carries out Hull groove test electroplating effect comparison diagram after adding conventional additive L26;
Fig. 5 a-5e is unchangable traditions additive L26 concentration, adds the effect contrast figure who carries out Hull groove test plating after L113 of the present invention;
Fig. 6 is continuous current electroplating effect comparison diagram.
Embodiment
Below with reference to the accompanying drawings and in conjunction with the embodiments, describe the present invention in detail.
Shown in Figure 1, a kind of non-dyestuff is leveling agent, is applied to sour copper electroplating technology, and its molecular structural formula is
Wherein, negatively charged ion X=Cl
-or Br
-; R1=O or S or N; R2, R3, R4=H, alkyl, thiazolinyl, aralkyl, heteroaralkyl, substituted alkyl, substituted alkenyl, substituted aralkyl or replace a kind of in heteroaralkyl.
Preferably, described leveling agent is L113, its molecular structure be for
The present invention passes through great many of experiments, explored and there is the molecule of above-mentioned feature as the feasibility of novel sour copper leveling agent, studied its in sour copper plating system with other components (as inhibitor, brightening agent etc.) impact of composite chemical ratios on quality of coating such as, with and composite in the impact on sour copper electroplating quality with traditional leveling agent.Its specific experiment flow process is as follows:
(1) preparation of electroplating chemical solution system
1, preparing sour copper, to electroplate required electroplating chemical solution be mother liquor system
The component of mother liquor comprises that concentration is the CuSO of 200g/L
45H
2the H that O, concentration are 100g/L
2sO
4and the concentration chlorion that is 0-120ppm;
By the above-mentioned CuSO of calculated amount
45H
2o fully dissolves by deionized water and stirring, slowly adds the above-mentioned H of calculated amount
2sO
4and HCl, after filtration, be diluted to 1L, get 250ml to standby in the groove of Hull;
2, prepare sour copper and electroplate required additive
The component of additive comprises the outstanding glossy dark green B(L26 of inhibitor polyoxyethylene glycol (PEG), conventional dyes type leveling agent) and/or non-dyestuff be leveling agent L113 and brightening agent sodium polydithio-dipropyl sulfonate (SPS);
By the pressed powder of PEG, L113 and/or L26 and SPS respectively with deionized water dissolving and be diluted in 50ml volumetric flask, take PEG, the L113 of calculated amount and/or the aqueous solution of L26 and SPS adds in the Hull groove at mother liquor place successively, and more than making full use of pneumatic blending 10min;
(2) plating condition and method (groove test in Hull is electroplated with continuous current)
1, galvanic anode: carry out in advance the plough groove type phosphorus-copper anode of pre-film (Anode filming), be placed in respectively both sides, negative plate front and back;
2, electroplating cathode: negative electrode sheet brass;
3, negative plate pre-treatment: negative electrode sheet brass washed with de-ionized water, then for electroplating;
(3) choose the leveling agent that L113 electroplates as sour copper and carry out testing research
1, the impact experiment of chlorine ion concentration on leveling agent L113 molecule leveling performance
From upper table, can see, when chlorine ion concentration is 80ppm left and right, Hull slotted vane integral body is light comparatively, and the flaws such as burr, pin hole are less.Under condition at this quasi-molecule as leveling agent, adjustable chlorine ion concentration scope is 70-90ppm.In follow-up study, employing chlorine ion concentration is 80ppm.
2, L113 add-on regulates experiment
Hull groove test plating condition:
（1）2A,5min
(2) Cl-concentration: 80ppm
（3）T=24.0℃,Bath?T=24.0℃,H(humidity)=50.0%
Shown in Figure 3
L113 test-results: in the situation that keeping other conditions constant, suitably regulate the latten(-tin) after add-on is electroplated to improve a lot than the blank copper sheet luminance brightness that does not add leveling agent, compare with traditional leveling agent, also have by improving processing condition and further optimizing the methods such as molecular structure and improve the space that it fills and leads up performance.
(4) take L113 as basic binary leveling agent performance study
Known by above-mentioned experiment, using L113 molecular structure as the feasibility of basic molecule as Novel leveling agent.Carry out next step experiment, research impact on quality of coating when composite by L113 and traditional leveling agent molecule L 26 simultaneously.
1, fixed L 113 concentration, add the outstanding glossy dark green B(L26 of conventional additive)
Hull groove test plating condition:
（1）2A,5min
（2）T=24.0℃,Bath?T=24.0℃,H(humidity)=50.0%
Shown in Figure 4
2, unchangable traditions additive L26 concentration, adds new additive agent L113
Hull groove test plating condition:
（1）2A,5min
（2）T=24.0℃,Bath?T=24.0℃,H(humidity)=50.0%
A. additive: L260.5mL, L1130mL, Cl-80ppm
Phenomenon: shown in Fig. 5 a, integral body is brightless.
B. additive: L260.5mL, L1130.25mL, Cl-80ppm
Phenomenon: shown in Fig. 5 b, whole more little than changing with a, low district 1cm slightly brightens.
C. additive: L260.5mL, L1130.5mL, Cl-80ppm
Phenomenon: shown in Fig. 5 c, integral body starts to brighten, but crystallization is thin not, and brightness is inadequate.
D. additive: L260.5mL, L1131mL, Cl
-80ppm
Phenomenon: shown in Fig. 5 d, luminance factor c brightens, but there is no the best fashion of L26 but crystallization very carefully leveling property is fine, low district 2cm atomization.
E. additive: L260.5mL, L1131.5mL, Cl
-80ppm
Phenomenon: shown in Fig. 5 e, high district 3-4cm crystallization is coarse, and Zhong Di district is smooth,
Low district adularescent striped.
Conclusion: the amount that fixed L 26 increases L113 gradually for 0.5mL can find out that although very bright, crystallization is careful between 10ASD-4ASD when L113 amount is during for 1mL.
From above experiment, reach a conclusion, suitably regulate the ratio that L26 and L113 add can obtain different electroplating effects.
(5) continuous current is electroplated
Current density: 5asd
Thickness of coating: 5 m
Electroplating time: 4.5min
By Faraday's law, calculate, the electroplating efficiency that the L113 molecule of take is leveling agent can reach 99.7%
Shown in Figure 6, from test piece quality of coating, surface-brightening, planarization is better.From electroplating result, see that but 2ASD and the brighter brightness of 12ASD do not have 5ASD good, current density operating restraint can be at 2ASD within 12ASD.
By the selected and condition optimizing to molecular structure, test, we have verified that types of molecules described in the invention is as the possibility of sour copper electroplating technology leveling agent, and related system is electroplated to the assessment of having carried out electroplating performance by the experiment of Hull groove and continuous current.
Above-described embodiment is just to allow one of ordinary skilled in the art can understand content of the present invention and implement according to this for technical conceive of the present invention and feature being described, its objective is, can not limit the scope of the invention with this.Every equivalent variation or modification that according to the present invention, the essence of content has been done, all should be encompassed in protection scope of the present invention.
Claims (2)
1. non-dyestuff is an application for leveling agent, and the molecular structural formula of described leveling agent is
Wherein, negatively charged ion X=Cl
-or Br
-; R1=O or S or N; R2, R3, R4=H, alkyl, thiazolinyl, aralkyl, heteroaralkyl, substituted alkyl, substituted alkenyl, substituted aralkyl or replace a kind of in heteroaralkyl, is characterized in that: described leveling agent is applied to sour copper electroplating technology.
2. the application that non-dyestuff according to claim 1 is leveling agent, is characterized in that: described leveling agent is L113, and its structural formula formula is
。
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310731859.5A CN103924269B (en) | 2013-12-26 | 2013-12-26 | The application of a kind of non-dyestuff system leveling agent |
| PCT/CN2014/076807 WO2015096347A1 (en) | 2013-12-26 | 2014-05-05 | Leveling composition and method for electrodeposition of metals in microelectronics |
| CN201480000564.3A CN105026385B (en) | 2013-12-26 | 2014-05-05 | A kind of method applied to the leveling agent composition of microelectronics and its for metal electrodeposition |
| US13/261,924 US9551081B2 (en) | 2013-12-26 | 2014-05-05 | Leveling composition and method for electrodeposition of metals in microelectronics |
| US15/388,927 US9920023B2 (en) | 2013-12-26 | 2016-12-22 | Leveling composition and method for electrodeposition of metals in microelectronics |
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| CN201310731859.5A CN103924269B (en) | 2013-12-26 | 2013-12-26 | The application of a kind of non-dyestuff system leveling agent |
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| CN103924269B CN103924269B (en) | 2016-04-13 |
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| CN105026385A (en) * | 2013-12-26 | 2015-11-04 | 苏州昕皓新材料科技有限公司 | Leveling composition and method for electrodeposition of metals in microelectronics |
| WO2016106543A1 (en) * | 2014-12-30 | 2016-07-07 | Suzhou Shinhao Materials Llc | Leveler, leveling composition and method for electrodeposition of metals in microelectronics |
| WO2018095133A1 (en) * | 2016-11-23 | 2018-05-31 | Suzhou Shinhao Materials Llc | Method for preparing electroplating copper layer with preferred growth orientation |
| KR20180071256A (en) * | 2016-11-23 | 2018-06-27 | 쑤저우 신하오 머티리얼즈 엘엘씨 | Copper crystal grains having high preferential orientation and method for producing the same |
| CN108396344A (en) * | 2018-03-19 | 2018-08-14 | 苏州昕皓新材料科技有限公司 | With the electrolytic copper foil and preparation method thereof for distorting band-like unordered winding microstructure |
| CN109112580A (en) * | 2018-09-18 | 2019-01-01 | 苏州昕皓新材料科技有限公司 | One kind having anisotropic metal material of thermodynamics and preparation method thereof |
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| US9551081B2 (en) | 2013-12-26 | 2017-01-24 | Shinhao Materials LLC | Leveling composition and method for electrodeposition of metals in microelectronics |
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| US10683275B2 (en) | 2014-12-30 | 2020-06-16 | Shinhao Materials LLC | Leveler, leveler composition and method for electrodeposition of metals in microelectronics |
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| KR20180071257A (en) * | 2016-11-23 | 2018-06-27 | 쑤저우 신하오 머티리얼즈 엘엘씨 | First, a method of manufacturing an electroplated copper layer having a growth orientation |
| KR20180071256A (en) * | 2016-11-23 | 2018-06-27 | 쑤저우 신하오 머티리얼즈 엘엘씨 | Copper crystal grains having high preferential orientation and method for producing the same |
| WO2018095133A1 (en) * | 2016-11-23 | 2018-05-31 | Suzhou Shinhao Materials Llc | Method for preparing electroplating copper layer with preferred growth orientation |
| CN108396344A (en) * | 2018-03-19 | 2018-08-14 | 苏州昕皓新材料科技有限公司 | With the electrolytic copper foil and preparation method thereof for distorting band-like unordered winding microstructure |
| CN109112580A (en) * | 2018-09-18 | 2019-01-01 | 苏州昕皓新材料科技有限公司 | One kind having anisotropic metal material of thermodynamics and preparation method thereof |
| WO2020057060A1 (en) * | 2018-09-18 | 2020-03-26 | Suzhou Shinhao Materials Llc | A metal material with thermodynamic anisotropy and a method of preparing the same |
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Address after: 215000 East Side of Chang'an Road, Wujiang Economic and Technological Development Zone, Suzhou City, Jiangsu Province (Science and Technology Pioneering Park) Patentee after: Meiyouke (Suzhou) Semiconductor Materials Co.,Ltd. Country or region after: China Address before: 215000 East Side of Chang'an Road, Wujiang Economic and Technological Development Zone, Suzhou City, Jiangsu Province (Science and Technology Pioneering Park) Patentee before: SUZHOU SHINHAO MATERIALS LLC Country or region before: China |