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CN116103655B - Metal alkaline etching solution for integrated circuit and preparation method thereof - Google Patents

Metal alkaline etching solution for integrated circuit and preparation method thereof Download PDF

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Publication number
CN116103655B
CN116103655B CN202211669648.9A CN202211669648A CN116103655B CN 116103655 B CN116103655 B CN 116103655B CN 202211669648 A CN202211669648 A CN 202211669648A CN 116103655 B CN116103655 B CN 116103655B
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etching
etching solution
solution
ethanolamine
copper
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CN116103655A (en
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戈烨铭
何珂
郑武
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Jiangsu Zhongde Electronic Material Technology Co ltd
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Jiangsu Zhongde Electronic Material Technology Co ltd
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    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/32—Alkaline compositions
    • C23F1/34—Alkaline compositions for etching copper or alloys thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
    • H01L21/321—After treatment
    • H01L21/3213—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer
    • H01L21/32133—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer by chemical means only
    • H01L21/32134—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer by chemical means only by liquid etching only

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Computer Hardware Design (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • ing And Chemical Polishing (AREA)
  • Manufacturing Of Printed Circuit Boards (AREA)

Abstract

The invention relates to an alkaline etching solution for etching copper for an integrated circuit, which comprises copper chloride, ethanolamine and water; more particularly, it relates to an alkaline etching solution for etching copper for integrated circuits, comprising copper chloride, ethanolamine, beta-alanine and water, wherein the ratio of ethanolamine to beta-alanine in the alkaline etching solution is 12:1 to 8:1, preferably 10:1.

Description

Metal alkaline etching solution for integrated circuit and preparation method thereof
Technical Field
The invention belongs to the technical field of etching solutions, and particularly relates to a metal alkaline etching solution for an integrated circuit and a preparation method thereof.
Background
An integrated circuit is a microelectronic device commonly used in flat panel display devices. The conductive line is made of metal materials such as aluminum, copper, and titanium. In order to reduce the impedance of the wires and to increase the signal transmission speed, copper with low resistivity is often used as the material of the conductive lines instead of aluminum. The preparation process of the conductive circuit involves a series of steps such as sputtering a long film, coating photoresist, exposing, developing, etching, and the like. A critical step in the fabrication process of integrated circuits is the etching of the conductive lines. The etching process of the conductive circuit comprises spraying an etching solution on the developed copper material, and etching away the copper in the non-circuit part by utilizing the oxidation-reduction reaction of the etching solution and the copper.
The etching liquid systems widely used in the industry at present are two kinds of acid copper chloride etching liquid and alkaline copper chloride etching liquid. The alkaline etching solution is mainly an ammonia etching solution, which uses a buffer solution composed of ammonia and ammonium salt as main components, and contains trace components to improve the speed or prevent side etching, and the operation temperature is 45-50 ℃ and the pH value is 8-9. The ammonia etching solution has the following problems: 1) The etched plate surface is easy to form sediment such as basic copper chloride and the like to obstruct the etching and enlarge side etching; 2) The ammonia consumption is very large, more than 50kg of ammonia escapes from each ton of etching solution in the etching process, the ammonia and ammonium salt of the waste etching solution after etching reach more than 100kg/t, a large amount of ammonia escapes from the production preparation, transportation, use and treatment processes after use, the negative effects on production workshops and the surrounding environment are very remarkable, a series of problems of volatile ammonia still cannot be eradicated even if the waste etching solution is treated by adopting a 3R (recovery, regeneration and circulation) technology, and the environment-friendly alkaline etching solution without waste gas emission is very necessary to be researched; 3) The ammonia etching liquid has a higher etching speed, so that side etching is easy to generate in the current finer line etching process, and the requirement of fine etching is difficult to meet.
Disclosure of Invention
The invention solves the technical problem of the discharge of the ammonia gas by adopting the ethanolamine to replace ammonia as the main component of the alkaline etching solution. Experiments show that the etching performance of the ethanolamine alkaline etching solution is equivalent to that of the ammonia etching solution. In order to solve the problem that side etching is easy to occur at a higher etching speed, the invention also solves the technical problem by adding beta-alanine as an auxiliary component of the alkaline etching solution.
The reaction mechanism of the present invention is as follows.
For ethanolamine, when an etching solution is initially prepared, a complexing reaction of copper chloride and ethanolamine occurs, wherein EA represents H 2NCH2CH2O-:
CuCl2+2EA→Cu(EA)2Cl2+2H2O
the chemical reaction of the alkaline etching process is:
Cu+Cu(EA)2Cl2+2EA→2Cu(EA)2Cl
The regeneration reaction is
2Cu(EA)2Cl+1/2O2+2H++2Cl-→2Cu(EA)2Cl2+H2O
For beta-alanine, the complexing reaction of cupric chloride and ethanolamine occurs when the etching solution is initially prepared, wherein beta Ala represents H 2NCH2CH2COO-:
CuCl2+2βAla→Cu(βAla)2Cl2+2H2O
the chemical reaction of the alkaline etching process is:
Cu+Cu(βAla)2Cl2+2βAla→2Cu(βAla)2Cl
The regeneration reaction is
2Cu(βAla)2Cl+1/2O2+2H++2Cl-→2Cu(EA)2Cl2+H2O
Specifically, the invention provides an alkaline etching solution for etching copper for an integrated circuit, which comprises copper chloride, ethanolamine and water.
The invention also provides an alkaline etching solution for etching copper for an integrated circuit, which comprises copper chloride, ethanolamine, beta-alanine and water, wherein the ratio of the ethanolamine to the beta-alanine in the alkaline etching solution is 12:1 to 8:1.
In a preferred embodiment, the ratio of ethanolamine to beta-alanine in alkaline etching solution is 10:1.
In a specific embodiment, the alkaline etching solution has a pH of 8.5 to 11.
In a preferred embodiment, the alkaline etching solution has a pH of 9.0.
In a specific embodiment, the alkaline etching solution further comprises a pH adjuster to adjust the pH of the alkaline etching solution to a desired pH.
The pH adjustor can be any suitable agent. In a preferred embodiment, the pH adjusting agent is selected from the group consisting of hydrochloric acid and sodium hydroxide.
In a specific embodiment, the concentration of copper chloride in the alkaline etching solution is 150g/L to 220g/L.
In a preferred embodiment, the concentration of copper chloride in the alkaline etching solution is 200g/L.
In a specific embodiment, the concentration of ethanolamine in the alkaline etching solution is 3mol/L to 6mol/L.
In a preferred embodiment, the concentration of ethanolamine in the alkaline etching solution is 4.545mol/L.
In a preferred embodiment, the concentration of beta-alanine in the alkaline etching solution is 0.455mol/L.
The invention also provides a method for preparing an alkaline etching solution for etching copper for an integrated circuit, which comprises
1) Dissolving ethanolamine in water;
2) Dissolving copper chloride in the solution of step 1);
3) The pH of the solution is adjusted to 8.5-11 using a pH adjuster.
The invention also provides a method for preparing an alkaline etching solution for etching copper for an integrated circuit, which comprises
1) Dissolving ethanolamine and beta-alanine in water, wherein the ratio of ethanolamine to beta-alanine is from 12:1 to 8:1;
2) Dissolving copper chloride in the solution of step 1);
3) The pH of the solution is adjusted to 8.5-11 using a pH adjuster.
In a preferred embodiment, the ratio of ethanolamine to beta-alanine is 10:1.
In a preferred embodiment, the solution pH is adjusted to 9.0 using a pH adjuster.
In a specific embodiment, the concentration of copper chloride is 150g/L to 220g/L.
In a preferred embodiment, the concentration of copper chloride is 200g/L.
In a specific embodiment, the concentration of ethanolamine is from 3mol/L to 6mol/L.
In a preferred embodiment, the concentration of ethanolamine is 4.545mol/L.
In a preferred embodiment, the concentration of beta-alanine is 0.455mol/L.
In a specific embodiment, the pH adjuster is selected from hydrochloric acid and sodium hydroxide.
The beneficial effects of the invention are that
The invention perfectly solves the problem of environmental pollution of the ammonia etching solution by using the ethanolamine with low volatility to replace ammonia as the complexing agent of copper ions, and almost does not lose the etching rate at the same time, thereby being capable of replacing the traditional ammonia etching solution for industrial application.
The present invention has also surprisingly found that by adding a weaker copper ion complexing agent, beta-alanine, as an auxiliary ingredient, the ratio of beta-alanine to ethanolamine in the etching solution can be adjusted to significantly reduce undercut with little loss of etching rate. This is unexpected because, as shown in the examples, when β -alanine alone is used for etching, the etch rate is significantly lower, whereas when β -alanine is used with ethanolamine, the overall etch rate should theoretically be reduced, but the inventors demonstrate that the addition of β -alanine does not affect the overall etch rate at a particular ratio by using a range of ratios of β -alanine to ethanolamine, while also unexpectedly significantly reducing undercut. Without being bound by theory, the inventors believe that the reduction in undercut may be due to the combined effect of the slower etching of the β -alanine-copper complex and the faster etching of the ethanolamine-copper complex on the copper material surface, such that the edge etch rate is significantly lower than that of the ethanolamine-copper complex alone, while the etch rate is almost unaffected as a whole. The inventors have also found that this effect is characteristic of beta-alanine, since no such effect is observed for L-alanine.
Examples
The present invention is further illustrated below with reference to specific examples, which are not intended to limit the invention in any way. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art.
Example 1:
Preparation of alkaline etching solution for etching copper-containing metal layer:
1) Dissolving 5mol/L ethanolamine in water;
2) Dissolving 200g/L copper chloride in the solution of step 1);
3) The solution pH was adjusted to 9.0 using hydrochloric acid.
The process method for etching operation by using the etching liquid of the embodiment comprises the following process steps:
1) Pouring etching liquid into an etching cylinder, setting the temperature of the etching cylinder to 55 ℃, setting the pressure of an etching liquid nozzle of an etching machine to 2kg/cm 2, and starting etching operation; the automatic detection and feeding control machine automatically feeds and supplements all components in the balanced etching solution so as to keep the specific gravity at a specified value;
2) Etching factor test circuit boards with a size of 620×540mm, copper thickness of 1oz, and developed line width spacing of 50.8 μm and pure copper etching rate test boards with a size of 500×300mm×1.5mm were placed in an etcher for spray etching test, and etching rates and etching factors K were calculated using methods well known in the industry, and the results are shown in table 1.
Example 2:
Preparation of alkaline etching solution for etching copper-containing metal layer:
1) 4.762mol/L of ethanolamine and 0.238mol/L of beta-alanine (20:1) are dissolved in water;
2) Dissolving 200g/L copper chloride in the solution of step 1);
3) The solution pH was adjusted to 9.0 using hydrochloric acid.
As described in example 1, the etching process was performed using the etching solution of this example, and the etching rate and etching factor K were calculated, and the results are shown in table 1.
Example 3:
Preparation of alkaline etching solution for etching copper-containing metal layer:
1) 4.687mol/L of ethanolamine and 0.313mol/L of beta-alanine (15:1) are dissolved in water;
2) Dissolving 200g/L copper chloride in the solution of step 1);
3) The solution pH was adjusted to 9.0 using hydrochloric acid.
As described in example 1, the etching process was performed using the etching solution of this example, and the etching rate and etching factor K were calculated, and the results are shown in table 1.
Example 4:
Preparation of alkaline etching solution for etching copper-containing metal layer:
1) Dissolving 4.615mol/L ethanolamine and 0.385mol/L beta-alanine (12:1) in water;
2) Dissolving 200g/L copper chloride in the solution of step 1);
3) The solution pH was adjusted to 9.0 using hydrochloric acid.
As described in example 1, the etching process was performed using the etching solution of this example, and the etching rate and etching factor K were calculated, and the results are shown in table 1.
Example 5:
Preparation of alkaline etching solution for etching copper-containing metal layer:
1) 4.545mol/L of ethanolamine and 0.455mol/L of beta-alanine (10:1) are dissolved in water;
2) Dissolving 200g/L copper chloride in the solution of step 1);
3) The solution pH was adjusted to 9.0 using hydrochloric acid.
As described in example 1, the etching process was performed using the etching solution of this example, and the etching rate and etching factor K were calculated, and the results are shown in table 1.
Example 6:
Preparation of alkaline etching solution for etching copper-containing metal layer:
1) 4.444mol/L of ethanolamine and 0.556mol/L of beta-alanine (8:1) are dissolved in water;
2) Dissolving 200g/L copper chloride in the solution of step 1);
3) The solution pH was adjusted to 9.0 using hydrochloric acid.
As described in example 1, the etching process was performed using the etching solution of this example, and the etching rate and etching factor K were calculated, and the results are shown in table 1.
Example 7:
Preparation of alkaline etching solution for etching copper-containing metal layer:
1) 4.167mol/L of ethanolamine and 0.833mol/L of beta-alanine (5:1) are dissolved in water;
2) Dissolving 200g/L copper chloride in the solution of step 1);
3) The solution pH was adjusted to 9.0 using hydrochloric acid.
As described in example 1, the etching process was performed using the etching solution of this example, and the etching rate and etching factor K were calculated, and the results are shown in table 1.
Example 8:
Preparation of alkaline etching solution for etching copper-containing metal layer:
1) 2.5mol/L of ethanolamine and 2.5mol/L of beta-alanine (1:1) are dissolved in water;
2) Dissolving 200g/L copper chloride in the solution of step 1);
3) The solution pH was adjusted to 9.0 using hydrochloric acid and sodium hydroxide.
As described in example 1, the etching process was performed using the etching solution of this example, and the etching rate and etching factor K were calculated, and the results are shown in table 1.
Example 9
Preparation of alkaline etching solution for etching copper-containing metal layer:
1) Dissolving 5mol/L beta-alanine in water;
2) Dissolving 200g/L copper chloride in the solution of step 1);
3) The solution pH was adjusted to 9.0 using sodium hydroxide.
As described in example 1, the etching process was performed using the etching solution of this example, and the etching rate and etching factor K were calculated, and the results are shown in table 1.
Comparative example 1
Preparation of alkaline etching solution for etching copper-containing metal layer:
1) 4.545mol/L of ethanolamine and 0.455mol/L of L-alanine (10:1) were dissolved in water;
2) Dissolving 200g/L copper chloride in the solution of step 1);
3) The solution pH was adjusted to 9.0 using hydrochloric acid.
As described in example 1, the etching process was performed using the etching solution of this example, and the etching rate and etching factor K were calculated, and the results are shown in table 1.
Comparative example 2
A conventional ammonia alkaline etching solution was prepared using 200g/L of copper chloride, 300g/LNH 4 Cl, 20% ammonia water and water, as in example 1, and the etching process was performed using the etching solution of this example, and the etching rate and etching factor K were calculated, and the results are shown in table 1.
TABLE 1
From the above results, it can be seen that the etching solution containing ethanolamine as the main component has an etching rate comparable to that of the conventional ammonia-based alkaline etching solution.
In general, as the amount of β -alanine increases, the etching rate decreases to a different extent, and the etching factor (the higher the value, the smaller the degree of undercut) increases and then decreases. The undercut is significantly reduced and the etch rate is almost unchanged when the ratio of ethanolamine to beta-alanine is 12:1 to 8:1, with best results when the ratio is 10:1. When L-alanine was used (comparative example), no improvement in etching factor was observed.
In the description of the specification, reference to the term "one embodiment," "a particular embodiment," "an example," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or by similar arrangements, by those skilled in the art, without departing from the scope of the invention or beyond the scope of the appended claims.

Claims (5)

1. An alkaline etching solution for etching copper for an integrated circuit, comprising copper chloride, ethanolamine and water;
it also comprises beta-alanine, wherein the molar ratio of ethanolamine to beta-alanine in the alkaline etching solution is 12:1 to 8:1;
wherein the mass ratio of the ethanolamine to the beta-alanine in the alkaline etching solution is 10:1;
The concentration of copper chloride is 150g/L-220g/L, and the concentration of ethanolamine is 3mol/L-6mol/L.
2. The alkaline etching solution of claim 1, wherein the pH of the alkaline etching solution is 8.5 to 11.
3. The alkaline etching solution of claim 1, wherein the pH of the alkaline etching solution is 9.0.
4. The alkaline etching solution of claim 1, further comprising a pH adjuster to adjust the pH of the alkaline etching solution to a desired pH.
5. The alkaline etching solution of claim 1, wherein the concentration of copper chloride is 200g/L and the concentration of ethanolamine is 4.545mol/L.
CN202211669648.9A 2022-12-25 2022-12-25 Metal alkaline etching solution for integrated circuit and preparation method thereof Active CN116103655B (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103459672A (en) * 2011-03-08 2013-12-18 长濑化成株式会社 Etching liquid

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TWI288046B (en) * 2003-11-14 2007-10-11 Showa Denko Kk Polishing composition and polishing method
JP6101421B2 (en) * 2010-08-16 2017-03-22 インテグリス・インコーポレーテッド Etching solution for copper or copper alloy
CN103614726B (en) * 2011-03-04 2015-07-29 侯延辉 A kind of engraving method
JP5933950B2 (en) * 2011-09-30 2016-06-15 アドバンスド テクノロジー マテリアルズ，インコーポレイテッド Etching solution for copper or copper alloy
JP2013091820A (en) * 2011-10-24 2013-05-16 Kanto Chem Co Inc Etchant composition for metal film including copper layer and/or copper alloy layer, and etching method using the same
JP5866566B2 (en) * 2014-04-25 2016-02-17 パナソニックＩｐマネジメント株式会社 Etching solution, etching concentrate and etching method for multilayer film containing molybdenum and copper
TWI640656B (en) * 2016-03-24 2018-11-11 Daxin Materials Corporation Alkaline etchant composition and etching method using thereof
CN114231984A (en) * 2021-12-02 2022-03-25 江苏中德电子材料科技有限公司 Metal etching liquid for integrated circuit and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103459672A (en) * 2011-03-08 2013-12-18 长濑化成株式会社 Etching liquid

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