KR20130049507A - Etching solution composition for a titanium nitride layer and method for etching the titanium nitride layer using the same - Google Patents

Etching solution composition for a titanium nitride layer and method for etching the titanium nitride layer using the same Download PDF

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KR20130049507A
KR20130049507A KR1020110114584A KR20110114584A KR20130049507A KR 20130049507 A KR20130049507 A KR 20130049507A KR 1020110114584 A KR1020110114584 A KR 1020110114584A KR 20110114584 A KR20110114584 A KR 20110114584A KR 20130049507 A KR20130049507 A KR 20130049507A
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acid
titanium nitride
nitride film
etching
composition
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KR1020110114584A
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Korean (ko)
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명중재
권기진
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동우 화인켐 주식회사
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K13/00—Etching, surface-brightening or pickling compositions
    • C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
    • C09K13/06—Etching, surface-brightening or pickling compositions containing an inorganic acid with organic material
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K13/00—Etching, surface-brightening or pickling compositions
    • C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
    • C09K13/08—Etching, surface-brightening or pickling compositions containing an inorganic acid containing a fluorine compound
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K13/00—Etching, surface-brightening or pickling compositions
    • C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
    • C09K13/10—Etching, surface-brightening or pickling compositions containing an inorganic acid containing a boron compound
    • 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
    • C23F1/16—Acidic compositions
    • C23F1/26—Acidic compositions for etching refractory metals

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Weting (AREA)
  • ing And Chemical Polishing (AREA)
  • Internal Circuitry In Semiconductor Integrated Circuit Devices (AREA)

Abstract

The present invention relates to a titanium nitride film etchant composition comprising (a) nitric acid, (b) fluoroboric acid, (c) oxidizing agent, (d) organic acid, and (e) deionized water.

Description

Titanium nitride film etchant composition and method for etching titanium nitride film using the same {ETCHING SOLUTION COMPOSITION FOR A TITANIUM NITRIDE LAYER AND METHOD FOR ETCHING THE TITANIUM NITRIDE LAYER USING THE SAME}

The present invention relates to a titanium nitride film etching liquid composition and an etching method of a titanium nitride film using the same. In particular, the present invention relates to an etching liquid composition having excellent selective etching ability of titanium nitride and titanium nitride-based metal and an etching method of a titanium nitride film using the same.

Titanium nitride (TiN), a titanium-based metal, is used for semiconductor devices, liquid crystal displays, MEMS (Micro Electro Mechanical Systems) devices, printed wiring boards, and the like as a base layer and a cap layer of precious metals, aluminum (Al), and copper (Cu) wiring. Moreover, in a semiconductor device, it may be used as a barrier metal and a gate metal.

Along with the titanium nitride or titanium nitride-based metal, tungsten or tungsten-based metals are used for liquid crystal displays, gate electrodes of thin film transistors of semiconductor devices, wiring, barrier layers, contact holes, via holes, and the like. It is also used as a tungsten heater in the field of MEMS (Micro Electro Mechanical Systems).

In particular, a nitride film such as TiN serves to prevent etching of the lower material by inhibiting etching from the etchant composition as a barrier layer. Therefore, as a known etchant, it is difficult to etch a nitride film such as TiN. Thus, a method of removing the etchant using a chemical mechanical polishing (CMP) method that adds the chemical properties of the etchant and the physical effects of polishing is generally used.

In the case of CMP, the process is complicated, there is a limitation in the application of the process, there are many sources of other pollution, and the cost is inefficient because it is higher than the general wet process.

Accordingly, the development of an etchant composition capable of removing TiN through a wet treatment method is required. When the etchant composition of the present invention is used, the titanium nitride film is efficiently removed while controlling the etching amount of tungsten used in a process such as a via hole. It can be effectively used in device manufacturing processes such as semiconductors.

There is a Korean Patent Publication No. 10-2009-0049366 as a conventional etching solution for the wet etching. The etchant is a nitride film etching liquid composition comprising a hydroxycarboxylic acid compound, a fluorine-based compound, an oxidizing agent, and water, an etching solution composition for selectively etching SiON, SiN-based nitride film with respect to the polysilicon film, or selective etching function for titanium nitride There is a problem that does not represent.

In addition, the Republic of Korea Patent Publication No. 10-2010-0080761 provides an etchant comprising a fluorine compound, an oxidizing agent (nitric acid), water, an additional oxidizing agent, the etchant is titanium (Ti) or aluminum (Al) and alloys thereof (Al -Ti) as a batch etching solution does not have an etching function for tartan nitride, there is a problem that does not exhibit a selective etching function for this.

Accordingly, in the manufacturing process of the semiconductor device, the liquid crystal display device, and the MEMS device, when etching titanium nitride, development of an etchant composition capable of selective eating without a etching function for tungsten or tungsten alloy is required.

KR 10-2009-0049366 A KR 10-2010-0080761 A

Disclosure of Invention The present invention is to solve the problems of the prior art as described above. A titanium nitride film etchant having an excellent etching force with respect to a titanium nitride metal at the time of etching a semiconductor device and an etching inhibiting power with respect to a tungsten metal An object of the present invention is to provide a composition and an etching method of a titanium nitride film using the same.

The present invention provides a titanium nitride film etchant composition comprising (a) nitric acid, (b) fluoroboric acid, (c) oxidizing agent, (d) organic acid and (e) residual deionized water.

In addition, the present invention provides a method for manufacturing an electronic device, comprising the step of etching the titanium nitride-based metal by the titanium nitride film etching liquid composition.

        The titanium nitride film etchant composition comprising (a) nitric acid, (b) fluoroboric acid, (c) oxidizing agent, (d) organic acid, and (e) residual deionized water of the present invention has excellent etching ability of titanium nitride-based metals. In addition, since the etching of the tungsten-based metal can be suppressed, it can be selectively etched depending on the metal at the time of manufacturing the semiconductor device.

1 is a photograph of a process of etching a titanium nitride film and a tungsten film using the etchant composition of the present invention.

The titanium nitride film etchant composition of the present invention may include (a) nitric acid, (b) fluoroboric acid, (c) oxidizing agent, (d) organic acid, and (e) residual deionized water. Each component is demonstrated below.

 (a) nitric acid

The nitric acid (a) has the effect of oxidizing the titanium nitride and etching the oxidized titanium nitride by the properties of the oxidant and the acidic properties. By adding to the titanium nitride film etchant composition in the present invention it was confirmed that the etching effect of the titanium nitride film can be implemented.

The (a) nitric acid contained in the composition is not particularly limited, and the (a) nitric acid is preferably included in an amount of 0.5 wt% to 3 wt% based on the total amount of the composition. If the amount is less than 0.5 wt%, the etching ability of the titanium nitride film is decreased, and if it is more than 3% by weight, the etching amount of the tungsten film is increased, thereby decreasing the function of selective etching.

(b) fluoroboric acid

(B) Fluoroboric acid is a strong acid represented by HBF 4 , and serves to remove the oxidized nitride film surface layer by contact between the oxidant and the nitride film. In addition, it serves to remove contaminants on the substrate, that is, fine dust. By adding to the titanium nitride film etching composition in the present invention it was confirmed that the etching effect of the titanium nitride film can be implemented.

(B) fluoroboric acid contained in the composition is not particularly limited, and may be increased or decreased depending on the object to be removed and the removal conditions, and (b) fluoroboric acid may be present in an amount of 1% by weight to 5% by weight based on the total weight of the composition. It is preferable to include. In the case of less than 1% by weight, the etching ability of the titanium nitride film is reduced, and in the case of more than 5% by weight, the additional effect is not large due to the increase in the amount added, and may cause an increase in corrosion of the polysilicon film.

(c) oxidizing agent

The (c) oxidant has an effect of increasing the amount of etching with respect to titanium nitride. By adding to the titanium nitride film etchant composition in the present invention it was confirmed that the etching effect of the titanium nitride film can be implemented.

Examples of the oxidizing agent included in the composition include hydrogen peroxide, persulfate compounds, and metal salt compounds. Examples of the persulfate compounds include ammonium persulfate, sodium persulfate, potassium persulfate, and the like. These can be mentioned, These can be used individually or in mixture of 2 or more types.

The oxidizing agent (c) preferably comprises 0.005 wt% to 2 wt% based on the total weight of the composition. If the amount is less than 0.005% by weight, the etching performance of the titanium nitride film may be degraded. If the amount is more than 2% by weight, the oxidizing power may be increased, thereby making it difficult to obtain a desirable etching selectivity by changing the etching amount of the nitride film.

(d) organic acids

The (d) organic acid is generally an acid having a carboxylic acid group (-COOH) or a sulfonic acid group (-SO3H) and the like, to form a complex with a metal by an unshared electron pair in oxygen such as the carboxylic acid group or the sulfonic acid group. There is an easy property. Due to the nature of the non-covalent electron pairs in these organic acids, the effect of complexing with tungsten can be expected, and when the organic acid forms a complex with tungsten, it exhibits steric hindrance from the effects of oxidizing agent and nitric acid. Can reduce the amount of tungsten, thereby suppressing the etching amount of tungsten.

The organic acid included in the composition may be classified into an organic acid having a carboxylic acid group and an organic acid having a sulfonic acid group, and the organic acid having a carboxylic acid may be citric acid, maleic acid, malonic acid, succinic acid, glycolic acid, gluconic acid, tartaric acid, malic acid, Lactic acid, lactic acid, formic acid, acetic acid, oxalic acid, and the like, and polyacids containing carboxylic acid groups. Examples of polyacids include polyacrylic acid and polyacrylic maleic acid. Organic acids having sulfonic acid groups include methanesulfonic acid, ethanesulfonic acid, propanesulfonic acid, minomethanesulfonic acid, benzenesulfonic acid, toluene sulfonic acid (4-methylbenzenesulfonic acid) sodium toluenesulfonic acid, phenolsulfonic acid, pyridinesulfonic acid, dodecylbenzene sulfonic acid, 0-cresolsulfonic acid (2-methylphenol sulfonic acid), cresol sulfonic acid (methylphenol sulfonic acid), etc. can be mentioned, These can be used individually or in mixture of 2 or more types.

The content of the organic acid (d) is not particularly limited, but preferably 0.1 to 5% by weight, more preferably 0.5 to 3% by weight based on the total weight of the composition. Less than 0.1% by weight of the tungsten may reduce the etching amount of the effect may not appear, when 5% by weight or more in proportion to the amount added is not expected to greatly reduce the etching amount of the tungsten.

(e) deionized water

The (e) deionized water contained in the tungsten film removal composition of the present invention is used as a solvent of the above (a) nitric acid, (b) fluoroboric acid, (c) oxidizing agent and (d) organic acid. The deionized water (e) is preferably included in the remaining amount relative to the total weight of the composition.

The titanium nitride film etching method mentioned above may be performed by a method commonly known in the art. For example, deposition, spraying, or a method using deposition and spraying may be used, in which case, as a visual condition, the temperature is usually 30 to 80 ° C, preferably 50 to 70 ° C, and deposition, spraying, or deposition and spraying The time is usually 30 seconds to 10 minutes, preferably 1 minute to 5 minutes. However, these conditions are not strictly applied and can be selected as easy or suitable conditions by those skilled in the art.

Hereinafter, the present invention will be described in more detail using examples, comparative examples, and experimental examples. However, the following Examples, Comparative Examples and Experimental Examples are for illustrating the present invention, the present invention is not limited to the following Examples, Comparative Examples and Experimental Examples can be variously modified and changed.

Examples 1-13 and Comparative Examples 1-3: Preparation of titanium nitride film etching liquid composition

The titanium nitride film etchant composition was prepared by mixing the components and contents shown in Table 1 below. All of the units of content in Table 1 are by weight.

nitric acid FBA APS Organic acid water Example-1 2 4.5 0.1 Citric acid 0.1 Balance Example-2 2 4.5 0.5 Citric acid One Balance Example-3 2 One 0.5 Maleic acid 0.5 Balance Example-4 One 4.5 0.5 Maleic acid 5 Balance Example 5 0.5 4 2 Glycolic Acid 2 Balance Example-6 0.5 2 0.5 Glycolic Acid 5 Balance Example-7 One 3 0.5 Gluconic acid 2 Balance Example-8 2.5 2 0.5 Gluconic acid 4 Balance Example-9 One 4 0.5 p-TSA 2 Balance Example-10 2 4 0.5 p-TSA 2 Balance Example-11 2 4 0.5 PAA One Balance Example-12 2 4 0.5 PAA 3 Balance Example-13 One 4.5 0.5 PAA One Balance Comparative Example 1 2 4.5 0.5 Citric acid 0.05 Balance Comparative Example 2 2 4.5 0.1 Balance Comparative Example 3 One 4 0.5 Balance

FBA: fluoroboric acid

APS: Ammonium Persulfate

PAA: polyacrylic acid

p-TSA: p-toluenesulfonic acid

Experimental Example 1 Evaluation of Titanium Nitride and Tungsten Membrane Etching Ability

The etching ability evaluation of the titanium nitride film etching liquid composition on the titanium nitride film, as shown in FIG. , Using a substrate laminated at 500 mm 3. First, the substrate was deposited at 60 ° C. for 2 minutes on the titanium nitride film etching liquid composition prepared in Examples 1 to 13 and Comparative Examples 1 to 3 on the substrate on which the titanium nitride film and tungsten were laminated, and then washed and dried. The substrate was etched. The thickness of the titanium nitride film and tungsten film etched from the substrate was measured using a 4-point probe device (Changmin Tech CMT series). The results are shown in Table 2 below.

Etching amount of titanium nitride film (화 / min) Etching amount of tungsten
(Å / min) TiN / W etching selectivity Example-1 45 9 5 Example-2 51 6 8.5 Example-3 40 5 8 Example-4 42 7 6 Example 5 52 6 8.7 Example-6 43 5 8.6 Example-7 43 7 6.1 Example-8 40 8 5 Example-9 44 6 7.3 Example-10 39 5 7.8 Example-11 39 7 5.6 Example-12 37 5 7.4 Example-13 43 6 7.1 Comparative Example 1 49 15 3.3 Comparative Example 2 46 18 2.6 Comparative Example 3 42 14 3

As confirmed in Table 2, with respect to the total weight of the composition, 0.1 to 3% by weight of nitric acid, 1 to 5% by weight of fluoroboric acid, 0.005% by weight of ammonium persulfate The titanium nitride film etching composition of Examples 1 to 13 containing 2 wt% to 2 wt% and an organic acid of 0.1 wt% to 5 wt% maintains the etching amount of the tungsten film while maintaining excellent etching performance with respect to the titanium nitride film. It was shown that the suppression, as a result shows that the etching selectivity of the TiN / W is excellent, while Comparative Examples 1 to 3 that do not satisfy the above range, the etching amount of the tungsten film is high, indicating a poor etching selectivity.

From these results, the titanium nitride film etchant composition of the present invention not only has excellent etching ability of the titanium nitride film, but also has excellent ability in the corrosion resistance of the tungsten film, and it can be confirmed that the selective etching performance of the tungsten film and the titanium nitride film is excellent. .

Claims (12)

A titanium nitride film etchant composition comprising (a) nitric acid, (b) fluoroboric acid, (c) oxidizing agent, (d) organic acid, and (e) deionized water. The method according to claim 2,
In the total amount of the composition,
(A) 0.5 wt% to 3 wt% of nitric acid;
(B) 1% to 5% by weight of fluoroboric acid;
0.005% to 2% by weight of the oxidizing agent (c);
(D) 0.1 wt% to 5 wt% of an organic acid; And
The titanium nitride film etchant composition comprising the (e) deionized water in the remaining amount. The method according to claim 1 or 2,
The tungsten film etchant composition according to claim (c), wherein the oxidizing agent is hydrogen peroxide. The method according to claim 1 or 2,
(C) the oxidizing agent is a tungsten film etching solution composition, characterized in that the persulfate compound. The method of claim 4,
The persulfate compound is titanium nitride film etchant composition, characterized in that any one or a mixture thereof selected from the group consisting of ammonium persulfate, sodium persulfate, potassium persulfate. The method according to claim 1 or 2,
The tungsten film etchant composition according to claim (c), wherein the oxidizing agent is a metal salt compound. The method of claim 6,
The metal salt compound is a tungsten film etching solution composition, characterized in that any one or a mixture thereof selected from the group consisting of iron chloride and copper chloride. The method according to claim 1 or 2,
The (d) organic acid is a titanium nitride film etching liquid composition, characterized in that any one or a mixture thereof selected from the group consisting of an organic acid having a carboxylic acid group, an organic acid having a sulfonic acid group and a polyacid having a carboxylic acid group. The method according to claim 8,
The organic acid having a carboxylic acid group is citric acid, maleic acid, malonic acid, succinic acid, glycolic acid, gluconic acid, tartaric acid, malic acid, lactic acid, lactic acid, formic acid, acetic acid and oxalic acid, characterized in that any one or a mixture thereof Titanium nitride film etching liquid composition. The method according to claim 8,
The organic acid having the sulfonic acid group is methanesulfonic acid, ethanesulfonic acid, propanesulfonic acid, minomethanesulfonic acid, benzenesulfonic acid, toluene sulfonic acid (4-methylbenzenesulfonic acid) sodium toluenesulfonic acid, phenolsulfonic acid, pyridine sulfonic acid, dodecylbenzene sulfonic acid, 0-cresolsulfonic acid (2-methylphenolsulfonic acid) and cresolsulfonic acid (methylphenolsulfonic acid), the titanium nitride film etching liquid composition, characterized in that any one or a mixture thereof. The method according to claim 8,
The polyacid having a carboxylic acid group is a titanium nitride film etchant composition, characterized in that any one or a mixture of polyacrylic acid, polyacrylic maleic acid. A method of manufacturing an electronic device, comprising the step of etching a titanium nitride metal with the titanium nitride film etchant composition of claim 1.
KR1020110114584A 2011-11-04 2011-11-04 Etching solution composition for a titanium nitride layer and method for etching the titanium nitride layer using the same KR20130049507A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20160000388A (en) * 2014-06-23 2016-01-04 삼성전자주식회사 Metal etchant composition and method of fabricating a semiconductor device using the same
KR101587758B1 (en) * 2015-03-05 2016-01-21 동우 화인켐 주식회사 ETCHANT COMPOSITION FOR ETHCING TiN LAYER AND METHOD FOR FORMING METAL LINE USING THE SAME
EP3024016A1 (en) * 2014-07-24 2016-05-25 Air Products And Chemicals, Inc. Titanium nitride hard mask and etch residue removal
KR20170084600A (en) * 2016-01-12 2017-07-20 동우 화인켐 주식회사 ETCHANT COMPOSITION FOR ETHCING TiN LAYER AND METHOD FOR FORMING METAL LINE USING THE SAME
KR20190007636A (en) * 2017-07-13 2019-01-23 동우 화인켐 주식회사 Composition for removal of Ni and TiN
EP3540764A1 (en) * 2018-03-16 2019-09-18 Versum Materials US, LLC Etching solution for tungsten word line recess
US11427759B2 (en) 2019-10-17 2022-08-30 Samsung Electronics Co., Ltd. Etchant compositions for metal-containing films and methods of manufacturing integrated circuit devices using the etchant compositions
KR20220161184A (en) * 2021-05-28 2022-12-06 도쿄엘렉트론가부시키가이샤 Etching method and etching apparatus

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20160000388A (en) * 2014-06-23 2016-01-04 삼성전자주식회사 Metal etchant composition and method of fabricating a semiconductor device using the same
EP3024016A1 (en) * 2014-07-24 2016-05-25 Air Products And Chemicals, Inc. Titanium nitride hard mask and etch residue removal
KR101587758B1 (en) * 2015-03-05 2016-01-21 동우 화인켐 주식회사 ETCHANT COMPOSITION FOR ETHCING TiN LAYER AND METHOD FOR FORMING METAL LINE USING THE SAME
KR20170084600A (en) * 2016-01-12 2017-07-20 동우 화인켐 주식회사 ETCHANT COMPOSITION FOR ETHCING TiN LAYER AND METHOD FOR FORMING METAL LINE USING THE SAME
KR20190007636A (en) * 2017-07-13 2019-01-23 동우 화인켐 주식회사 Composition for removal of Ni and TiN
CN110272742A (en) * 2018-03-16 2019-09-24 弗萨姆材料美国有限责任公司 Etching solution for tungsten word line recess
EP3540764A1 (en) * 2018-03-16 2019-09-18 Versum Materials US, LLC Etching solution for tungsten word line recess
KR20190109317A (en) * 2018-03-16 2019-09-25 버슘머트리얼즈 유에스, 엘엘씨 Etching solution for tungsten word line recess
JP2019165225A (en) * 2018-03-16 2019-09-26 バーサム マテリアルズ ユーエス，リミティド ライアビリティ カンパニー Etching solution for tungsten word line recess
TWI706026B (en) * 2018-03-16 2020-10-01 美商慧盛材料美國責任有限公司 Etching solution for tungsten word line recess
US11499236B2 (en) 2018-03-16 2022-11-15 Versum Materials Us, Llc Etching solution for tungsten word line recess
US11427759B2 (en) 2019-10-17 2022-08-30 Samsung Electronics Co., Ltd. Etchant compositions for metal-containing films and methods of manufacturing integrated circuit devices using the etchant compositions
KR20220161184A (en) * 2021-05-28 2022-12-06 도쿄엘렉트론가부시키가이샤 Etching method and etching apparatus

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