WO2017057906A1 - Cmp slurry composition for polishing organic film and polishing method using same - Google Patents
Cmp slurry composition for polishing organic film and polishing method using same Download PDFInfo
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- WO2017057906A1 WO2017057906A1 PCT/KR2016/010874 KR2016010874W WO2017057906A1 WO 2017057906 A1 WO2017057906 A1 WO 2017057906A1 KR 2016010874 W KR2016010874 W KR 2016010874W WO 2017057906 A1 WO2017057906 A1 WO 2017057906A1
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- Prior art keywords
- polishing
- slurry composition
- cmp slurry
- organic film
- film
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Classifications
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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
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
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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
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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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
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
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- 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
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
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- 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
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30625—With simultaneous mechanical treatment, e.g. mechanico-chemical polishing
Definitions
- the present invention relates to an organic film polishing CMP slurry composition and a polishing method using the same.
- the CMP process is an oxide CMP process, a metal CMP process, a poly-Si CMP process, and an organic film CMP process depending on the material to be polished. It may be classified as such.
- the polishing rate and the degree of planarization are known to be greatly influenced by the surface modification reaction of the polished film.
- the CMP slurry may further include a pH adjusting agent such as an oxidizing agent, a high molecular compound, an inhibitor, a chelating agent, an acid or an alkali, in addition to the abrasive particles.
- a pH adjusting agent such as an oxidizing agent, a high molecular compound, an inhibitor, a chelating agent, an acid or an alkali, in addition to the abrasive particles.
- Fe, Mn, Cr has a problem that is likely to cause a leakage current problem in the shallow trench isolation (STI) process or the gate (burying) process.
- STI shallow trench isolation
- Ce 3+ trivalent cerium ions
- polishing characteristics such as polishing rate are variable.
- the problem to be solved by the present invention is to provide a CMP slurry composition capable of stabilizing tetravalent cerium ions (Ce 4 + ) even at pH 1 or more.
- Another problem to be solved by the present invention is to provide a CMP slurry composition excellent in the polishing effect on the organic film.
- Another object of the present invention is to provide a method of polishing an organic film using a CMP slurry composition excellent in polishing effect on the organic film.
- One aspect of the present invention is ultrapure water, abrasives, cerium salt containing tetravalent cerium ions; And an oxidant, wherein the oxidant has an oxidation potential of about 1.72 eV or more in an acidic region, and relates to an organic film polishing CMP slurry composition having a pH value of about 1 to about 7.
- the cerium salt is present as trivalent cerium ions and tetravalent cerium ions in the CMP slurry composition, and the concentration of the tetravalent cerium ions may be about 10 times or more than the concentration of the trivalent cerium ions.
- the oxidant may comprise one or more of hydrogen peroxide, potassium persulfate, sodium persulfate and ammonium persulfate.
- the abrasive may comprise colloidal silica, comprised from about 0.01 to about 20 weight percent of the CMP slurry composition, with an average particle diameter of about 10 kPa to about 100 nm.
- the organic film may be a carbon-based film containing a carbon-hydrogen bond.
- the carbon-based film may be a C-SOH film, an amorphous carbon layer (ACL), or an NCP film.
- the CMP slurry composition may further include at least one of a pH adjuster and an organic acid.
- the slurry composition may have a polishing amount of about 1,000 m 3 / min or more for the organic layer.
- Another aspect of the invention relates to a polishing method comprising polishing an organic film using the CMP slurry composition.
- the method includes forming an inorganic film having a negative pattern formed on the base layer; Forming an inorganic film on the surface of the inorganic film so as to fill the intaglio pattern;
- the surface of the organic layer on which the intaglio pattern is not formed may include removing the organic layer polishing CMP slurry composition.
- the organic layer may be a resist layer formed by a self-aligned double patterning technology (SaDPT).
- SaDPT self-aligned double patterning technology
- the CMP slurry composition of the present invention can stably maintain the concentration of tetravalent cerium ions (Ce 4+ ) even at a pH of 1 or higher, and has an excellent polishing effect on the organic film.
- organic film polishing can be easily performed in an organic film polishing process, in particular, a self-aligned double pattern process.
- the CMP slurry composition of the present invention can stabilize tetravalent cerium ions (Ce 4+ ) even at a pH of 1 or higher, and selectively has excellent abrasiveness with respect to the organic film.
- the CMP slurry composition for polishing an organic film may include a cerium salt including ultrapure water, an abrasive, and tetravalent cerium ions; And oxidants.
- the polishing target of the CMP slurry composition is an organic film.
- the organic film is a carbon-based film containing a carbon-hydrogen bond, and may include a spin on hardmask (C-SOH) film, an amorphous carbon layer (ACL), or an NCP film, and the C-SOH film has a selective polishing effect on the organic film. It is more preferable as the grinding
- the C-SOH film generally means a carbon-based hard mask film, but in the present invention, a resist film formed by a self-aligned double patterning technology (SADPT), an inorganic material such as a silica film deposited on a patterned wafer, and the like.
- a carbon-based film having a resist function such as a gap-filling or an anti-etching film that fills the via-hole of the film is generally referred to.
- the abrasive one or more metal oxides selected from silica, alumina, ceria, and titania may be used. Among them, when silica is used, the dispersion stability is excellent and the scratches are small, so that the CMP process may have many advantages.
- the abrasive may use colloidal silica.
- the average particle diameter of the colloidal silica may be about 10 nm to about 100 nm, and there is an advantage of obtaining a sufficient polishing rate in the above range.
- the abrasive may be included in an amount of about 0.1 wt% to about 20 wt%, preferably about 0.1 wt% to about 15 wt%, based on the total CMP slurry composition. If the abrasive is added in excess of the above range, it may have a problem such as poor dispersion stability, scratching during polishing, oxide erosion (oxide erosion), etc., if added in a smaller amount than the above range in the semiconductor process It is difficult to obtain the required polishing rate.
- cerium salt containing tetravalent cerium ions may be, for example, Ceric Ammonium Nitrate.
- the ceric ammonium nitrate oxidizes the organic layer surface layer with oxides or ions to facilitate removal of the organic layer surface layer, and evenly polishes the organic layer material in the pattern region when the polishing stop layer such as a silica layer is exposed. It serves to improve the surface roughness in the pattern.
- the residue of the organic film material present in the polishing stop film layer can be easily removed, there is an advantage to enable a more uniform polishing.
- the ceric ammonium nitrate may be present in the slurry composition in the form of an ionic compound or a chelate compound, and when used in this form, may provide a high polishing rate for the organic film.
- the ceric ammonium nitrate may be present in the slurry composition in the form of ammonium ions (NH 4 + ) and anions [Ce (NO 3 ) 6 ] 2 ⁇ which are cations as shown in Equation 1 below.
- the ceric ammonium nitrate may be included in an amount of about 0.01 to about 5% by weight based on the total slurry composition, preferably about 0.05 to about 3% by weight, and most preferably about 0.1 to about 3% by weight. Appropriate etching property with respect to an organic film can be maintained in the said range.
- the oxidizing agent is a compound having an oxidation potential of about 1.72 eV or more in the acidic region, and for example, hydrogen peroxide, potassium persulfate, sodium persulfate, ammonium persulfate, or the like may be used alone or in combination.
- the oxidizing agent is present in the cerium salt containing tetravalent cerium ions separated in an ionic state in the CMP slurry solution, the tetravalent cerium ions (Ce 4+ ) is reduced to trivalent cerium ions (Ce 3 + ). It is to prevent the stability of tetravalent cerium ions and to improve polishing characteristics such as polishing rate.
- the slurry composition of the present invention may further include an organic acid in order to suppress the polishing rate for the inorganic film.
- the organic acid is malic acid, citric acid, citric acid, formic acid, glutaric acid, glutaric acid, oxalic acid, phthalic acid, succinic acid, tartaric acid), maleic acid, and malonic acid may be one or more carboxylic acids selected from the group consisting of.
- the organic acid may be included in an amount of about 0.02 to about 0.1% by weight, preferably about 0.05 to about 0.1% by weight, based on the total CMP slurry composition in terms of polishing rate, dispersion stability of the slurry, and surface properties of the polished product. .
- the CMP slurry composition of the present invention may have a pH value of about 1 to about 7, and preferably may have a pH value of about 1 or more and less than about 3.
- a pH adjuster may be further included to adjust the pH value in the above range.
- the pH adjusting agent may be used potassium hydroxide, sodium hydroxide, ammonia water and the like.
- the CMP slurry composition may have a polishing amount of about 1,000 mW / min or more, preferably about 2,000 mW / min or more.
- the organic film polishing method of the present invention includes the step of polishing the organic film with the organic film polishing CMP slurry composition.
- the organic layer may be formed on one surface of the inorganic layer on which the intaglio pattern is formed.
- the method comprises forming an inorganic film having a negative pattern formed on the substrate layer; Forming an inorganic film on the surface of the inorganic film so as to fill the intaglio pattern; It may include the step of removing the organic film on the surface of the intaglio pattern is not formed with the organic film polishing CMP slurry composition.
- the organic film is a carbon-based film containing a carbon-hydrogen (C-H) bond
- the inorganic film may be a metal layer or a metal oxide layer.
- the organic film may be a C-SOH film
- the inorganic film may be a silica film.
- the organic layer may be a resist layer formed by a self-aligned double patterning technology (SADPT).
- SADPT self-aligned double patterning technology
- the CMP slurry composition of the present invention may be applied to a rotating polishing pad, and the polishing pad may be in contact with the surface of the organic layer to rub the organic layer in a predetermined pressure condition.
- the predetermined pressure conditions include pressure conditions generally accepted in the art of CMP polishing.
- Formation of an organic film A 5,000 ⁇ thick silica film was deposited on a pattern wafer having a negative pattern formed on the surface thereof, and a 2,650 S thick SOH film (SDI Co., Ltd.) was formed to fill the negative pattern formed on the surface of the silica film. The film was formed. The baking temperature at the time of film formation of the SOH film was 400 ° C.
- CMP Slurry Composition The CMP slurry composition was prepared by mixing each component having the following specifications in ultrapure water in the composition of Table 1 (% by weight relative to the total composition).
- the SOH film was polished under the following polishing conditions.
- Polishing conditions FUJIBO H800 CMP pad was used as a polishing pad. Using Applied Materials (AMAT) 200mm MIRRA equipment, polishing was performed for 1 minute at a lower pressure of 1.0 psi, a slurry flow rate of 200 mL / min, and a table and spindle speed of 90 rpm. The amount was measured and shown in Table 1 below.
- AMAT Applied Materials
- hydrochloric acid hydrochloric acid of Samjeon Pure Chemical Co., Ltd. was used (oxidation potential: 0.00 eV).
- Examples 1 to 5 to which the CMP slurry composition according to the present invention is applied are excellent in the organic film polishing effect, and the concentration ratio of tetravalent cerium ions: trivalent cerium ions is 10: 1 or more and tetravalent. The stability of cerium ions was secured.
- Comparative Example 1 which does not include an oxidizing agent, has a low organic film polishing effect, has a low concentration ratio of tetravalent cerium ions: trivalent cerium ions, and thus cannot stabilize the tetravalent cerium ions, and has an oxidation potential of less than 1.72 eV. Comparative Examples 2 to 5 also include a low polishing effect and could not stabilize the tetravalent cerium ions.
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Abstract
Description
본 발명은 유기막 연마용 ＣＭＰ 슬러리 조성물 및 이를 이용한 연마방법에 관한 것이다.The present invention relates to an organic film polishing CMP slurry composition and a polishing method using the same.
최근 반도체 소자의 고집적화 및 고성능화에 따라 배선 패턴의 선 폭은 더욱 미세해지고 구조는 점점 다층화되는 추세이다. 한편, 반도체 소자 제조 공정에서 사용되는 포토리소그래피(photolithography)의 정밀도 향상을 위해서 각 공정에서의 층간 평탄도가 매우 중요한 요소로 작용하고 있다. 이러한 평탄화 기술로서 현재 가장 각광받고 있는 것이 CMP 공정이며, CMP 공정은 연마 대상 물질에 따라 산화막(oxide) CMP 공정, 금속(metal) CMP 공정, 폴리실리콘(poly-Si) CMP공정, 유기막 CMP 공정 등으로 분류되기도 한다.In recent years, as the integration and performance of semiconductor devices become higher, line widths of wiring patterns become finer and structures become increasingly multilayered. Meanwhile, in order to improve the precision of photolithography used in a semiconductor device manufacturing process, interlayer flatness in each process is very important. The most popular spotlighting technology is the CMP process, and the CMP process is an oxide CMP process, a metal CMP process, a poly-Si CMP process, and an organic film CMP process depending on the material to be polished. It may be classified as such.
CMP 공정에서 연마 속도와 평탄화 정도는 피연마막의 표면 개질 반응에 큰 영향을 받는 것으로 알려져 있다. 표면 개질 반응을 향상시키기 위해, CMP 슬러리는 연마입자 이외에 산화제, 고분자 화합물, 인히비터, 킬레이팅제, 산 또는 알칼리 등의 pH 조절제를 더 포함할 수 있다. 연마 속도 및 평탄화 정도를 고려할 때, 금속막이나 유기막을 연마할 때에는 Fe, Mn, Cr, Ce 등의 전이금속을 포함하는 강한 산화제를 선택하여 사용하는 것이 바람직하다. 그러나, Fe, Mn, Cr은 STI(shallow trench isolation) 공정 또는 게이트(gate) 매립 공정시 누설전류(leakage current) 문제를 일으킬 가능성이 높다는 문제점이 있다. 세륨(Ce)의 경우, 누설전류 문제를 일으키지는 않으나, pH 1이상의 조건에서 4가 세륨이온(Ce4 +)이 3가 세륨이온(Ce3+)으로 변하게 되므로 산화제 자체의 안정성이 확보되기 어려우며, 4가 산화세륨 이온의 농도가 변화됨에 따라, 연마속도 등의 연마특성이 가변적이라는 문제점이 있다. 슬러리 용액의 pH를 낮게 하면, 4가 세륨이온(Ce4 +)이 3가 세륨이온(Ce3+)으로 변하는 것을 방지할 수 있으나, 이 경우, 연마포 표면을 정돈하는 Diamond Disk, CMP 장치의 부식을 일으킬 수 있다는 문제가 있으며, 또한, 일단 4가 세륨이온(Ce4 +)에서 3가 세륨이온(Ce3 +)으로 변하게 되면 단순히 pH를 낮춘다고 해서 다시 4가 세륨이온(Ce4 +)으로 돌아오지 않는다는 문제점이 있다. 따라서, pH 1이상인 조건에서도 4가 세륨이온(Ce4 +)을 안정화시킬 수 있는 CMP 슬러리 조성물의 개발이 요구되고 있다.In the CMP process, the polishing rate and the degree of planarization are known to be greatly influenced by the surface modification reaction of the polished film. In order to improve the surface modification reaction, the CMP slurry may further include a pH adjusting agent such as an oxidizing agent, a high molecular compound, an inhibitor, a chelating agent, an acid or an alkali, in addition to the abrasive particles. In consideration of the polishing rate and the degree of planarization, it is preferable to select and use a strong oxidant containing transition metals such as Fe, Mn, Cr, and Ce when polishing the metal film or the organic film. However, Fe, Mn, Cr has a problem that is likely to cause a leakage current problem in the shallow trench isolation (STI) process or the gate (burying) process. In the case of cerium (Ce), leakage current does not cause a problem, but since tetravalent cerium ions (Ce 4 + ) are changed to trivalent cerium ions (Ce 3+ ) at a pH of 1 or higher, it is difficult to secure stability of the oxidizing agent itself. As the concentration of the tetravalent cerium oxide ion is changed, there is a problem that polishing characteristics such as polishing rate are variable. Decreasing the pH of the slurry solution, tetravalent cerium ions (Ce + 4) trivalent cerium ion, but can be prevented from varying (Ce 3+), in this case, Diamond Disk, CMP apparatus to fix the polishing cloth surface There is a problem that can cause corrosion, and also, once it is changed from tetravalent cerium ions (Ce 4 + ) to trivalent cerium ions (Ce 3 + ), simply lowering the pH again makes the tetravalent cerium ions (Ce 4 + ) There is a problem that does not come back. Accordingly, there is a need for the development of a CMP slurry composition capable of stabilizing tetravalent cerium ions (Ce 4+ ) even at a pH of 1 or more.
본 발명이 해결하고자 하는 과제는 pH 1 이상에서도 4가 세륨이온(Ce4 +)을 안정화시킬 수 있는 CMP 슬러리 조성물을 제공하는 것이다.The problem to be solved by the present invention is to provide a CMP slurry composition capable of stabilizing tetravalent cerium ions (Ce 4 + ) even at pH 1 or more.
본 발명이 해결하고자 하는 다른 과제는 유기막에 대한 연마효과가 우수한 CMP 슬러리 조성물을 제공하는 것이다.Another problem to be solved by the present invention is to provide a CMP slurry composition excellent in the polishing effect on the organic film.
본 발명이 해결하고자 하는 또 다른 과제는 유기막에 대한 연마효과가 우수한 CMP 슬러리 조성물을 이용하여 유기막을 연마하는 방법을 제공하는 것이다.Another object of the present invention is to provide a method of polishing an organic film using a CMP slurry composition excellent in polishing effect on the organic film.
본 발명의 일 관점은 초순수, 연마제, 4가 세륨 이온을 포함하는 세륨염; 및 산화제를 포함하고, 상기 산화제는 산성 영역에서 약 1.72eV 이상의 산화전위를 가지며, pH값이 약 1 내지 약 7인 유기막 연마용 CMP 슬러리 조성물에 관한 것이다.One aspect of the present invention is ultrapure water, abrasives, cerium salt containing tetravalent cerium ions; And an oxidant, wherein the oxidant has an oxidation potential of about 1.72 eV or more in an acidic region, and relates to an organic film polishing CMP slurry composition having a pH value of about 1 to about 7.
상기 세륨염은 상기 CMP 슬러리 조성물 내에서 3가 세륨이온 및 4가 세륨 이온으로 존재하고, 상기 4가 세륨이온의 농도는 상기 3가 세륨이온 농도의 약 10배 이상일 수 있다.The cerium salt is present as trivalent cerium ions and tetravalent cerium ions in the CMP slurry composition, and the concentration of the tetravalent cerium ions may be about 10 times or more than the concentration of the trivalent cerium ions.
상기 산화제는 과산화수소, 과황산칼륨, 과황산나트륨 및 과황산암모늄 중 하나 이상을 포함할 수 있다.The oxidant may comprise one or more of hydrogen peroxide, potassium persulfate, sodium persulfate and ammonium persulfate.
상기 연마제는 CMP 슬러리 조성물 중 약 0.01 내지 약 20 중량%로 포함되고, 평균 입경이 약 10 내지 약 100㎚인 콜로이달 실리카일 수 있다.The abrasive may comprise colloidal silica, comprised from about 0.01 to about 20 weight percent of the CMP slurry composition, with an average particle diameter of about 10 kPa to about 100 nm.
상기 유기막은 탄소-수소 결합을 함유하는 카본계막일 수 있다.The organic film may be a carbon-based film containing a carbon-hydrogen bond.
상기 카본계막은 C-SOH막, ACL(amorphous carbon layer) 또는 NCP막일 수 있다.The carbon-based film may be a C-SOH film, an amorphous carbon layer (ACL), or an NCP film.
상기 CMP 슬러리 조성물은 pH조절제와 유기산 중 하나 이상을 더 포함할 수 있다.The CMP slurry composition may further include at least one of a pH adjuster and an organic acid.
상기 슬러리 조성물은 유기막에 대한 연마량이 약 1,000Å/min 이상일 수 있다.The slurry composition may have a polishing amount of about 1,000 m 3 / min or more for the organic layer.
본 발명의 다른 관점은 상기 CMP 슬러리 조성물을 이용하여 유기막을 연마하는 것을 포함하는 연마방법에 관한 것이다.Another aspect of the invention relates to a polishing method comprising polishing an organic film using the CMP slurry composition.
상기 방법은 기재층 상에 음각 패턴이 형성된 무기막을 형성하고; 상기 음각패턴이 충진되도록 무기막 표면을 유기막으로 성막하고; 상기 음각 패턴이 형성되지 않은 표면의 유기막은 상기 유기막 연마용 CMP 슬러리 조성물로 제거하는 단계를 포함할 수 있다.The method includes forming an inorganic film having a negative pattern formed on the base layer; Forming an inorganic film on the surface of the inorganic film so as to fill the intaglio pattern; The surface of the organic layer on which the intaglio pattern is not formed may include removing the organic layer polishing CMP slurry composition.
상기 유기막은 자가정렬 이중 패턴 공정(self-aligned double patterning technology: SaDPT)에서 형성된 레지스트막일 수 있다.The organic layer may be a resist layer formed by a self-aligned double patterning technology (SaDPT).
본 발명의 CMP 슬러리 조성물은 pH 1이상에서도 4가 세륨이온(Ce4+)의 농도를 안정적으로 유지할 수 있어, 유기막에 대한 연마효과가 우수하다.The CMP slurry composition of the present invention can stably maintain the concentration of tetravalent cerium ions (Ce 4+ ) even at a pH of 1 or higher, and has an excellent polishing effect on the organic film.
또한, 상기 CMP 슬러리 조성물을 이용한 연마방법에 의하여 유기막 연마 공정, 특히, 자가정렬 이중 패턴 공정에서 유기막 연마가 용이하게 이루어질 수 있다.In addition, by the polishing method using the CMP slurry composition, organic film polishing can be easily performed in an organic film polishing process, in particular, a self-aligned double pattern process.
이하, 본 발명을 구체적으로 설명하기로 한다.Hereinafter, the present invention will be described in detail.
유기막Organic membrane 연마용 For polishing CMPCMP 슬러리 조성물 Slurry composition
먼저, 본 발명에 따른 CMP 슬러리 조성물에 대해 설명한다.First, the CMP slurry composition according to the present invention will be described.
본 발명의 CMP 슬러리 조성물은, pH 1이상에서도 4가 세륨이온(Ce4 +)을 안정화시킬 수 있으며, 유기막에 대하여 선택적으로 우수한 연마성을 갖는다.The CMP slurry composition of the present invention can stabilize tetravalent cerium ions (Ce 4+ ) even at a pH of 1 or higher, and selectively has excellent abrasiveness with respect to the organic film.
일 구체예로서, 상기 유기막 연마용 CMP 슬러리 조성물은 초순수, 연마제, 4가 세륨이온을 포함하는 세륨염; 및 산화제를 포함할 수 있다.In one embodiment, the CMP slurry composition for polishing an organic film may include a cerium salt including ultrapure water, an abrasive, and tetravalent cerium ions; And oxidants.
상기 CMP 슬러리 조성물의 연마 대상은 유기막이다. 상기 유기막은 탄소-수소 결합을 함유하는 카본계막으로서, C-SOH(spin on hardmask)막, ACL(amorphous carbon layer) 또는 NCP막을 예시할 수 있으며, C-SOH막이 유기막에 대한 선택적인 연마 효과가 우수하다는 점에서 본 발명의 연마 대상으로 보다 바람직하다.The polishing target of the CMP slurry composition is an organic film. The organic film is a carbon-based film containing a carbon-hydrogen bond, and may include a spin on hardmask (C-SOH) film, an amorphous carbon layer (ACL), or an NCP film, and the C-SOH film has a selective polishing effect on the organic film. It is more preferable as the grinding | polishing object of this invention from the point which is excellent.
상기 C-SOH막은 일반적으로 카본계 하드마스크 막을 의미하나, 본 발명에서는 자가정렬 이중 패턴 공정(self-aligned double patterning technology: SaDPT)에서 형성된 레지스트막, 패턴화된 웨이퍼 위에 증착된 실리카막과 같은 무기막의 via-hole을 채워주는 갭-필링(gap-filling) 또는 에칭 방지막 등의 레지스트 기능을 가지는 카본계막을 총체적으로 의미한다.The C-SOH film generally means a carbon-based hard mask film, but in the present invention, a resist film formed by a self-aligned double patterning technology (SADPT), an inorganic material such as a silica film deposited on a patterned wafer, and the like. A carbon-based film having a resist function such as a gap-filling or an anti-etching film that fills the via-hole of the film is generally referred to.
상기 연마제로는 실리카, 알루미나, 세리아(ceria), 티타니아(titania)로부터 선택되는 1종 이상의 금속산화물을 사용할 수 있다. 이 중에서도 실리카를 사용할 때 분산 안정성이 우수하고 스크래치가 적어 CMP 공정에 적용시 많은 장점을 가질 수 있다. 일 구체예로서, 상기 연마제는 콜로이달 실리카를 사용할 수 있다. 상기 콜로이달 실리카의 평균 입경은 약 10nm 내지 약 100㎚일 수 있고, 상기 범위에서 충분한 연마속도를 얻을 수 있는 이점이 있다.As the abrasive, one or more metal oxides selected from silica, alumina, ceria, and titania may be used. Among them, when silica is used, the dispersion stability is excellent and the scratches are small, so that the CMP process may have many advantages. In one embodiment, the abrasive may use colloidal silica. The average particle diameter of the colloidal silica may be about 10 nm to about 100 nm, and there is an advantage of obtaining a sufficient polishing rate in the above range.
상기 연마제는 전체 CMP 슬러리 조성물에 대하여 약 0.1 중량% 내지 약 20 중량%로 포함될 수 있으며, 바람직하게는 약 0.1 중량% 내지 약 15 중량%로 포함될 수 있다. 연마제가 상기 범위보다 과량 첨가될 경우, 분산 안정성이 떨어지거나 연마 시에 스크래치가 발생하거나 산화물이 침식(oxide erosion)되는 등의 문제를 가질 수 있으며, 상기 범위보다 소량으로 첨가될 경우에는 반도체 공정에서 요구되는 연마속도를 얻기 어려워진다. The abrasive may be included in an amount of about 0.1 wt% to about 20 wt%, preferably about 0.1 wt% to about 15 wt%, based on the total CMP slurry composition. If the abrasive is added in excess of the above range, it may have a problem such as poor dispersion stability, scratching during polishing, oxide erosion (oxide erosion), etc., if added in a smaller amount than the above range in the semiconductor process It is difficult to obtain the required polishing rate.
한편, 상기 4가 세륨이온을 포함하는 세륨염은, 예를 들면, 세릭암모늄니트레이트(Ceric Ammonium Nitrate)일 수 있다.Meanwhile, the cerium salt containing tetravalent cerium ions may be, for example, Ceric Ammonium Nitrate.
상기 세릭암모늄니트레이트는 유기막 표면층을 산화물 또는 이온으로 산화시켜 유기막 표면층의 제거를 용이하게 하며, 실리카막 등의 연마 정지막(stop layer)이 드러날 때 패턴 영역의 유기막 물질을 고르게 연마하여 패턴 내 표면 거칠기(roughness)를 좋게 하는 작용을 한다. 또한, 연마 정지막층에 존재하는 유기막 물질의 잔류물(Residue)이 쉽게 제거될 수 있게 함으로써 보다 균일한 연마를 가능하게 하는 장점이 있다.The ceric ammonium nitrate oxidizes the organic layer surface layer with oxides or ions to facilitate removal of the organic layer surface layer, and evenly polishes the organic layer material in the pattern region when the polishing stop layer such as a silica layer is exposed. It serves to improve the surface roughness in the pattern. In addition, the residue of the organic film material present in the polishing stop film layer can be easily removed, there is an advantage to enable a more uniform polishing.
상기 세릭암모늄니트레이트는 이온 화합물 또는 킬레이트 화합물 형태로 슬러리 조성물 내 존재할 수 있으며, 상기 형태로 사용하는 경우 유기막에 대하여 높은 연마 속도를 제공할 수 있다. 일 구체예로서, 상기 세릭암모늄니트레이트는 슬러리 조성물 내에서 하기 식 1과 같이 양이온인 암모늄 이온(NH4 +)과 음이온[Ce(NO3)6]2 -형태로 존재할 수 있다.The ceric ammonium nitrate may be present in the slurry composition in the form of an ionic compound or a chelate compound, and when used in this form, may provide a high polishing rate for the organic film. In one embodiment, the ceric ammonium nitrate may be present in the slurry composition in the form of ammonium ions (NH 4 + ) and anions [Ce (NO 3 ) 6 ] 2 − which are cations as shown in Equation 1 below.
[식 1][Equation 1]
상기 세릭암모늄니트레이트는 전체 슬러리 조성물에 대하여 약 0.01 내지 약 5 중량%로 포함될 수 있고, 바람직하게는 약 0.05 내지 약 3 중량%, 가장 바람직하게는 약 0.1 내지 약 3 중량%로 포함될 수 있다. 상기 범위에서 유기막에 대한 적절한 에칭성을 유지할 수 있다.The ceric ammonium nitrate may be included in an amount of about 0.01 to about 5% by weight based on the total slurry composition, preferably about 0.05 to about 3% by weight, and most preferably about 0.1 to about 3% by weight. Appropriate etching property with respect to an organic film can be maintained in the said range.
다음으로, 상기 산화제는 산성 영역에서 약 1.72eV 이상의 산화전위를 가지는 화합물로서, 예를 들면, 과산화수소, 과황산칼륨, 과황산나트륨, 과황산암모늄 등을 단독 또는 혼합하여 사용할 수 있다. 상기 산화제는 4가 세륨 이온을 포함하는 세륨염이 CMP 슬러리 용액 내에서 이온 상태로 분리하여 존재하는 경우, 4가 세륨이온(Ce4+)이 3가 세륨이온(Ce3 +)으로 환원되는 것을 방지하여 4가 세륨이온의 안정성을 확보하고, 연마속도 등의 연마특성을 향상시키기 위한 것이다.Next, the oxidizing agent is a compound having an oxidation potential of about 1.72 eV or more in the acidic region, and for example, hydrogen peroxide, potassium persulfate, sodium persulfate, ammonium persulfate, or the like may be used alone or in combination. When the oxidizing agent is present in the cerium salt containing tetravalent cerium ions separated in an ionic state in the CMP slurry solution, the tetravalent cerium ions (Ce 4+ ) is reduced to trivalent cerium ions (Ce 3 + ). It is to prevent the stability of tetravalent cerium ions and to improve polishing characteristics such as polishing rate.
한편, 본 발명의 슬러리 조성물은 무기막에 대한 연마 속도를 억제하기 위하여 유기산을 더 포함할 수 있다. 상기 유기산은 말산(malic acid), 시트르산(citric acid), 개미산(formic acid), 글루타르산(glutaric acid), 옥살산(oxalic acid), 프탈산(phthalic acid), 숙신산(succinic acid), 타르타르산(tartaric acid), 말레산(maleic acid), 및 말론산(malonic acid)으로 이루어진 그룹에서 선택되는 1종 이상의 카르복시산일 수 있다.On the other hand, the slurry composition of the present invention may further include an organic acid in order to suppress the polishing rate for the inorganic film. The organic acid is malic acid, citric acid, citric acid, formic acid, glutaric acid, glutaric acid, oxalic acid, phthalic acid, succinic acid, tartaric acid), maleic acid, and malonic acid may be one or more carboxylic acids selected from the group consisting of.
상기 유기산은 연마 속도, 슬러리의 분산 안정성, 피연마물의 표면 특성 측면에서 전체 CMP 슬러리 조성물에 대하여 약 0.02 내지 약 0.1 중량%로 포함될 수 있고, 바람직하게는 약 0.05 내지 약 0.1 중량%로 포함될 수 있다.The organic acid may be included in an amount of about 0.02 to about 0.1% by weight, preferably about 0.05 to about 0.1% by weight, based on the total CMP slurry composition in terms of polishing rate, dispersion stability of the slurry, and surface properties of the polished product. .
본 발명의 CMP 슬러리 조성물은 약 1 내지 약 7의 pH값을 가질 수 있고, 바람직하게는 약 1 이상 약 3 미만의 pH값을 가질 수 있다. 상기 범위로 pH 값을 조절하기 위하여 pH 조절제가 더 포함될 수 있다. 상기 pH 조절제로는 수산화 칼륨, 수산화나트륨, 암모니아수 등을 사용할 수 있다. CMP 슬러리의 pH값이 상기 범위를 만족할 경우, 유기막에 대한 연마 특성을 보다 향상시킬 수 있다.The CMP slurry composition of the present invention may have a pH value of about 1 to about 7, and preferably may have a pH value of about 1 or more and less than about 3. A pH adjuster may be further included to adjust the pH value in the above range. The pH adjusting agent may be used potassium hydroxide, sodium hydroxide, ammonia water and the like. When the pH value of the CMP slurry satisfies the above range, the polishing characteristics for the organic film can be further improved.
상기 CMP슬러리 조성물은 유기막에 대한 연마량이 약 1,000Å/min 이상일 수 있고, 바람직하게는 약 2,000Å/min 이상일 수 있다.The CMP slurry composition may have a polishing amount of about 1,000 mW / min or more, preferably about 2,000 mW / min or more.
유기막Organic membrane 연마용 For polishing CMPCMP 슬러리 조성물을 이용한 연마방법 Polishing method using slurry composition
다음으로, 본 발명에 따른, 유기막 연마 방법에 대해 설명한다.Next, an organic film polishing method according to the present invention will be described.
본 발명의 유기막 연마 방법은 상기한 유기막 연마용 CMP 슬러리 조성물로 유기막을 연마하는 단계를 포함한다. 이때, 상기 유기막은 음각 패턴이 형성된 무기막 일면에 성막된 것일 수 있다.The organic film polishing method of the present invention includes the step of polishing the organic film with the organic film polishing CMP slurry composition. In this case, the organic layer may be formed on one surface of the inorganic layer on which the intaglio pattern is formed.
일 구체예로서, 상기 방법은 기재층 상에 음각 패턴이 형성된 무기막을 형성하고; 상기 음각패턴이 충진되도록 무기막 표면을 유기막으로 성막하고; 상기 음각 패턴이 형성되지 않은 표면의 유기막을 상기 유기막 연마용 CMP 슬러리 조성물로 제거하는 단계를 포함할 수 있다.In one embodiment, the method comprises forming an inorganic film having a negative pattern formed on the substrate layer; Forming an inorganic film on the surface of the inorganic film so as to fill the intaglio pattern; It may include the step of removing the organic film on the surface of the intaglio pattern is not formed with the organic film polishing CMP slurry composition.
이때, 상기 유기막은 탄소-수소(C-H) 결합을 함유하는 카본계막이며, 상기 무기막은 금속층 또는 산화금속층일 수 있다.In this case, the organic film is a carbon-based film containing a carbon-hydrogen (C-H) bond, the inorganic film may be a metal layer or a metal oxide layer.
일 구체예로서, 상기 유기막은 C-SOH막일 수 있으며, 상기 무기막은 실리카막일 수 있다.In one embodiment, the organic film may be a C-SOH film, the inorganic film may be a silica film.
다른 구체예로서, 상기 유기막은 자가정렬 이중 패턴 공정(self-aligned double patterning technology: SaDPT)에서 형성된 레지스트막일 수 있다.In another embodiment, the organic layer may be a resist layer formed by a self-aligned double patterning technology (SADPT).
상기 연마 단계는 본 발명의 CMP 슬러리 조성물을 회전하는 연마용 패드에 도포하고, 상기 연마용 패드를 상기 유기막 표면에 접촉하여 소정의 압력 조건 하에서 마찰하며 유기막 일부를 연마할 수 있다. 상기 소정의 압력 조건은 CMP 연마의 기술분야에서 일반적으로 허용되는 압력조건을 포함한다.In the polishing step, the CMP slurry composition of the present invention may be applied to a rotating polishing pad, and the polishing pad may be in contact with the surface of the organic layer to rub the organic layer in a predetermined pressure condition. The predetermined pressure conditions include pressure conditions generally accepted in the art of CMP polishing.
이하 실시예를 들어 본 발명을 보다 구체적으로 설명하나 하기 실시예들은 단지 설명을 위한 것으로서 본 발명의 보호 범위를 제한하는 것은 아니다. 또한 하기 실시 예를 통해 상변화 물질을 평탄화시키는데 있어 바람직한 CMP 연마방법을 제공한다. Hereinafter, the present invention will be described in more detail with reference to the following examples, but the following examples are merely illustrative and are not intended to limit the protection scope of the present invention. In addition, the following examples provide a preferable CMP polishing method for planarizing the phase change material.
실시예Example
실시예Example 1 One
유기막의 성막: 표면에 음각 패턴이 형성된 패턴 웨이퍼 상에 연마 정지막으로 5,000Å 두께의 실리카막을 증착하고, 상기 실리카막 표면에 형성된 음각 패턴을 충진하기 위하여 2,650Å 두께의 SOH막(SDI社)을 성막하였다. 상기 SOH막의 성막시 베이킹 온도는 400℃였다. Formation of an organic film: A 5,000 Å thick silica film was deposited on a pattern wafer having a negative pattern formed on the surface thereof, and a 2,650 S thick SOH film (SDI Co., Ltd.) was formed to fill the negative pattern formed on the surface of the silica film. The film was formed. The baking temperature at the time of film formation of the SOH film was 400 ° C.
CMP 슬러리 조성물: CMP슬러리 조성물은 초순수에 하기 사양을 갖는 각 성분들을 표 1의 조성(전체 조성물 대비 중량%)으로 혼합하여 제조하였다. CMP Slurry Composition: The CMP slurry composition was prepared by mixing each component having the following specifications in ultrapure water in the composition of Table 1 (% by weight relative to the total composition).
제조된 CMP 슬러리 조성물을 이용하여, 하기 연마 조건으로 상기 SOH막을 연마하였다. Using the prepared CMP slurry composition, the SOH film was polished under the following polishing conditions.
연마 조건: 연마 패드로는 FUJIBO社의 H800 CMP 패드를 사용하였다. 어플라이드머티리얼(Applied Materials; AMAT)社의 200mm MIRRA 장비를 사용하여 하강압력 1.0psi, 슬러리 유속 200mL/분, 정반(table)과 스핀들(spindle) 속도를 모두 90rpm으로 하여 1분간 연마를 수행한 후 연마량을 측정하여 하기 표 1에 나타내었다.Polishing conditions: FUJIBO H800 CMP pad was used as a polishing pad. Using Applied Materials (AMAT) 200mm MIRRA equipment, polishing was performed for 1 minute at a lower pressure of 1.0 psi, a slurry flow rate of 200 mL / min, and a table and spindle speed of 90 rpm. The amount was measured and shown in Table 1 below.
실시예Example 2-5 및 2-5 and 비교예Comparative example 1-6 1-6
유기막의 성막은 실시예 1과 동일한 조건으로 성막하였으며, 하기 표 1의 조성을 갖는 CMP 슬러리 조성물을 제조한 후 상기 실시예 1과 동일한 방법으로 유기막을 연마하였다. 그런 다음, 연마량을 측정하여 하기 표 1에 나타내었다.Film formation of the organic film was carried out under the same conditions as in Example 1, after preparing a CMP slurry composition having a composition of Table 1 and then polishing the organic film in the same manner as in Example 1. Then, the polishing amount was measured and shown in Table 1 below.
CMPCMP 슬러리 조성물 각 성분의 사양 Specification of each composition of slurry composition
(A) 연마제: 평균입경이 35㎚인 콜로이달 실리카(Evonic社)를 사용하였다.(A) Abrasive: Colloidal silica (Evonic) having an average particle diameter of 35 nm was used.
(B) Ce4 +이온을 포함하는 세륨염: 삼전순약社의 세릭 암모늄 니트레이트를 사용하였다.(B) cerium salt containing Ce 4 + ions was used to serik ammonium nitrate Samchun sunyak社.
(C) 산화제 (C) oxidizing agent
(c1) 과산화수소: 동우화인켐社의 과산화수소를 사용하였다(산화전위: 1.77 eV).(c1) Hydrogen peroxide: Hydrogen peroxide from Dongwoo Finechem Co., Ltd. was used (oxidation potential: 1.77 eV).
(c2) 질산: 삼전순약社의 질산을 사용하였다(산화전위: 0.80 eV).(c2) Nitric acid: Nitric acid of Samjeon Pure Chemical Co., Ltd. was used (oxidation potential: 0.80 eV).
(c3) 과염소산: 삼전순약社의 과염소산을 사용하였다(산화전위: 0.17 eV).(c3) Perchloric acid: Perchloric acid of Samjeon Pure Chemical Company was used (oxidation potential: 0.17 eV).
(c4) 염산: 삼전순약社의 염산을 사용하였다(산화전위: 0.00eV).(c4) hydrochloric acid: hydrochloric acid of Samjeon Pure Chemical Co., Ltd. was used (oxidation potential: 0.00 eV).
(c5) 붕산: 삼전순약社의 붕산을 사용하였다(산화전위: -0.48 eV).(c5) Boric acid: Boric acid manufactured by Samjeon Pure Chemical Co., Ltd. (oxidation potential: -0.48 eV) was used.
(D) pH 조절제: 삼전순약社의 수산화칼륨을 사용하였다.(D) pH adjuster: Potassium hydroxide of Samjeon Pure Chemical Co., Ltd. was used.
상기 표 1에 나타난 바와 같이, 본 발명에 따른 CMP 슬러리 조성물을 적용한 실시예 1 내지 5는 유기막 연마효과가 우수하고, 4가 세륨이온 : 3가 세륨 이온의 농도비가 10 : 1 이상으로 4가 세륨 이온의 안정성을 확보할 수 있었다.As shown in Table 1, Examples 1 to 5 to which the CMP slurry composition according to the present invention is applied are excellent in the organic film polishing effect, and the concentration ratio of tetravalent cerium ions: trivalent cerium ions is 10: 1 or more and tetravalent. The stability of cerium ions was secured.
반면, 산화제를 포함하지 않는 비교예 1은 유기막 연마효과가 낮고, 4가 세륨이온 : 3가 세륨이온의 농도비가 낮아 4가 세륨이온을 안정화할 수 없었고, 1.72eV 미만의 산화전위를 갖는 산화제를 포함하는 비교예 2 내지 5 역시 연마효과가 낮고 4가 세륨이온을 안정화할 수 없었다.On the other hand, Comparative Example 1, which does not include an oxidizing agent, has a low organic film polishing effect, has a low concentration ratio of tetravalent cerium ions: trivalent cerium ions, and thus cannot stabilize the tetravalent cerium ions, and has an oxidation potential of less than 1.72 eV. Comparative Examples 2 to 5 also include a low polishing effect and could not stabilize the tetravalent cerium ions.
그리고, 슬러리 조성물의 pH가 1 미만인 비교예 6의 경우에도 유기막 연마효과가 낮은 것을 확인할 수 있었다.And also in the case of the comparative example 6 whose pH of a slurry composition is less than 1, it was confirmed that organic membrane polishing effect was low.
본 발명의 단순한 변형 내지 변경은 이 분야의 통상의 지식을 가진 자에 의하여 용이하게 실시될 수 있으며, 이러한 변형이나 변경은 모두 본 발명의 영역에 포함되는 것으로 볼 수 있다.Simple modifications or changes of the present invention can be easily carried out by those skilled in the art, and all such modifications or changes can be seen to be included in the scope of the present invention.
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| KR20210079573A (en) * | 2019-12-20 | 2021-06-30 | 주식회사 케이씨텍 | Slurry composition for organic film |
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| US5958288A (en) * | 1996-11-26 | 1999-09-28 | Cabot Corporation | Composition and slurry useful for metal CMP |
| US20030060135A1 (en) * | 2001-09-24 | 2003-03-27 | Cabot Microelectronics Corporation | Rare earth salt/oxidizer-based cmp method |
| KR20100080095A (en) * | 2008-12-31 | 2010-07-08 | 제일모직주식회사 | Cmp slurry composition for polishing metal wiring |
| KR20100080074A (en) * | 2008-12-31 | 2010-07-08 | 제일모직주식회사 | Cmp slurry composition for polishing metal wiring and polishing method using the same |
| KR20110013291A (en) * | 2009-07-30 | 2011-02-09 | 주식회사 동진쎄미켐 | Photoresist composition for self-aligned double pattern formation |
| KR20140125316A (en) * | 2013-04-17 | 2014-10-28 | 제일모직주식회사 | Cmp slurry composition for organic film and polishing method using the same |
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| TW200836002A (en) * | 2006-12-19 | 2008-09-01 | Cheil Ind Inc | Photosensitive resin composition and organic insulating film produced using the same |
| KR20150009914A (en) * | 2013-07-17 | 2015-01-27 | 삼성전자주식회사 | CMP composition for polishing an organic layer and method of forming a semiconductor device using the composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5958288A (en) * | 1996-11-26 | 1999-09-28 | Cabot Corporation | Composition and slurry useful for metal CMP |
| US20030060135A1 (en) * | 2001-09-24 | 2003-03-27 | Cabot Microelectronics Corporation | Rare earth salt/oxidizer-based cmp method |
| KR20100080095A (en) * | 2008-12-31 | 2010-07-08 | 제일모직주식회사 | Cmp slurry composition for polishing metal wiring |
| KR20100080074A (en) * | 2008-12-31 | 2010-07-08 | 제일모직주식회사 | Cmp slurry composition for polishing metal wiring and polishing method using the same |
| KR20110013291A (en) * | 2009-07-30 | 2011-02-09 | 주식회사 동진쎄미켐 | Photoresist composition for self-aligned double pattern formation |
| KR20140125316A (en) * | 2013-04-17 | 2014-10-28 | 제일모직주식회사 | Cmp slurry composition for organic film and polishing method using the same |
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| CN108138030A (en) | 2018-06-08 |
| TWI621673B (en) | 2018-04-21 |
| KR101882561B1 (en) | 2018-07-26 |
| KR20170040036A (en) | 2017-04-12 |
| TW201714994A (en) | 2017-05-01 |
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