KR920002707B1 - Platinum-aluminide coating method of a super alloy - Google Patents

Platinum-aluminide coating method of a super alloy Download PDF

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KR920002707B1
KR920002707B1 KR1019880012339A KR880012339A KR920002707B1 KR 920002707 B1 KR920002707 B1 KR 920002707B1 KR 1019880012339 A KR1019880012339 A KR 1019880012339A KR 880012339 A KR880012339 A KR 880012339A KR 920002707 B1 KR920002707 B1 KR 920002707B1
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platinum
layer
resistant
heat
coating method
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KR900004961A (en
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신세균
강황진
장성기
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삼성항공산업 주식회사
송세창
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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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D

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Abstract

In methods for coating Pt-aliuminide films on Ni-base super alloy, it is characterized by following processes; (1) after polishing and cleaning the surface of substrate, electro-plating platimum film on it; (2) enhancing cohesion between platinum and Ni-base super alloy by diffusing Ni into platinum layer with heat treatments (diffuse-out process); (3) diffusing metal powder of aluminum and yttrium into Ni diffused platinum layer for making binary phase mixed structure (diffuse-in process). In this method, the diffuse-out process is consisting of calcining Ni diffused layer at 250 deg.C for 2 hrs and at 400 deg.C 3 hrs and diffusing Ni element in platinum layer at 800-1100 deg.C for 1-4 hrs in vacuum furnace. In the above method, the diffuse-in process is consisting of making binary phase mixed structure of Pt-Al-Y compound layer and Al-Ni compound layer.

Description

초내열 Ni기 합금의 백금-알루미나이드 코팅방법Platinum-aluminate coating method of super heat-resistant Ni-based alloy

제1도는 본 발명에 의한 백금 도금 공정 후 확산 열처리 이전(A)과 이후(B)의 코팅층 상태를 비교한 조직사진.1 is a tissue photograph comparing the state of the coating layer before (A) and after (B) diffusion heat treatment after the platinum plating process according to the present invention.

제2도는 본 발명의 금속확산 침투공정 후 코팅층의 형성상태를 나타낸 조직사진.Figure 2 is a tissue photograph showing the formation state of the coating layer after the metal diffusion penetration process of the present invention.

제3도는 본 발명에 의해 내열내식 코팅된 초내열 합금의 산화시험 결과 그래프.3 is a graph of the oxidation test results of the superheat-resistant alloy coated with a heat-resistant corrosion resistance by the present invention.

* 도면의 주요부분에 대한 부호의 설명* Explanation of symbols for main parts of the drawings

100 : 모재(母材) 101 : 공백(空白)100: base material 101: blank

110 : 백금층 120 : 확산층110: platinum layer 120: diffusion layer

130 : NiAl층 140 : PtAl2+NiAl+Y층130: NiAl layer 140: PtAl 2 + NiAl + Y layer

본 발명은 항공기 제트엔진(Jet Engine)이나 선박 및 산업용 터보(Turbo)엔진에 사용되는 블레이드(Blade)의 고온 내열내식 코팅(Coating)방법에 관한 것으로, 특히 제트엔진의 작동온도를 높이고 블레이드의 고온 내산화 내식성을 증진시켜 엔진의 작동효율 향상 및 사용수명을 연장시킬 수 있도록 한 초내열 Ni기 합금의 백금 알루미나이드 코팅방법에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a method for coating a high temperature and heat resistant coating of a blade used in an aircraft jet engine or a marine and industrial turbo engine, and in particular, increases the operating temperature of the jet engine and the high temperature of the blade. The present invention relates to a platinum aluminide coating method of a super heat-resistant Ni-based alloy capable of improving oxidation resistance and improving engine operation efficiency and extending service life.

일반적으로 제트엔진이나 블레이드는 니켈(Ni)이나 코발트(Co)기 초내열 합금으로서 고온강도 유지 및 가혹분위기 가스에 대한 저항성이 요구되므로 이를 위해 초내열 합금은 ＂고온에서 강도가 높은 니켈-알루미늄(Ni3Al)＂화합물을 많이 생성시켜야 하지만 고온 강도를 위해 알루미늄(Al)이나 티타늄(Ti)등의 원소가 다량 첨가되면 오히려 고온내식성을 저하시키는 경향이 있기 때문에 고온 내식성을 증가시킬 수 있는 초내열 합금의 코팅처리가 필요하고 제트엔진 및 터보엔진의 작동온도 상승과 내구성 향상을 위한 초내열 합금의 터어빈 블레이드 코팅은 고온 내식 및 내열에 대한 저항성은 물론 정밀도, 열충격에 견딜 수 있어야 한다.In general, jet engines or blades are nickel (Ni) or cobalt (C) -based superheat-resistant alloys that require high temperature strength and resistance to harsh atmosphere gases. Therefore, superheat-resistant alloys have high strength at high temperatures. Ni3Al) ＂compounds should be produced a lot, but when a large amount of elements such as aluminum (Al) or titanium (Ti) are added for high strength, they tend to lower high temperature corrosion resistance. Turbine blade coatings of super heat-resistant alloys that require coating and increase the operating temperature and durability of jet and turbo engines must be able to withstand high temperature corrosion and heat resistance, as well as precision and thermal shock.

따라서 종래에는 고온에서 사용되는 코팅방법으로서 알루미나이드(Aluminide) 코팅방법과 플라즈마(Plasma)용사법등이 있는데 상기 알루미나이드 코팅에 의한 코팅층은 장시간 사용할 경우 코팅층의 원소들이 모재속으로 확산됨과 아울러 모재의 주원소인 Ni 및 Co가 코팅층으로 확산되므로 표면에서 고온 부식이 발생되어 사용수명이 감소되는 결점이 있고 상기 플라즈마 용사에 의한 코팅층은 정밀도를 요구하는 블레이드의 크기를 변화시키고 결합력이 약해 열충격이 약해 열충격이 가해지면 코팅층이 박리되는 결점이 있다.Therefore, conventionally, a coating method used at high temperature includes an aluminide coating method and a plasma spraying method. The coating layer by the aluminide coating is used for a long time and the elements of the coating layer diffuse into the base material and the main material of the base material. Since Ni and Co, which are elements, are diffused into the coating layer, a high temperature corrosion occurs on the surface, and thus the service life is reduced.The coating layer by plasma spraying changes the size of the blade requiring precision and the thermal shock is weak due to the weak bonding force. There is a drawback that the coating layer is peeled off when applied.

본 발명은 이러한 결점들을 해결하기 위하여 블레이드에 내식성이 강한 백금(Pt)을 피복한 다음 Al을 확산 침투시켜 2상 혼합구조의 내식성이 강한 코팅층을 형성하되 이들 코팅층의 안정성 및 조직을 개선시키고 부착력을 향상시킬 수 있도록 이트륨(Yttrim : Y)을 첨가함으로써 고온 내식성 및 내산화성 등 내구성이 좋은 코팅특성을 갖도록 창안한 것으로, 이하 본 발명의 내열내식 코팅방법을 상세히 설명하면 다음과 같다.In order to solve these drawbacks, the present invention coats the blade with high corrosion resistance platinum (Pt) and diffuses and infiltrates the Al to form a corrosion resistant coating layer of a two-phase mixed structure, but improves the stability and structure of these coating layers and improves adhesion. By adding yttrium (Y) to improve the present invention, the invention has been developed to have excellent coating properties such as high temperature corrosion resistance and oxidation resistance. Hereinafter, the heat resistant corrosion coating method of the present invention will be described in detail.

본 발명의 코팅공정은 코팅층을 형성하기 전에 블레이드의 표면을 깨끗하게 하기 위해서 표면연마, 세척 및 여러 가지 오물제거 등의 공정을 실시하는 백금도금 전처리 공정과 내식성 증가를 위해 백금을 도금하는 백금도금 공정, 도금층과 모재의 결합력을 강화시키기 위해 소둔(Annealing)처리 및 열처리하는 확산 열처리 공정과 코팅층의 접착성 및 조직개선을 위해 이트륨을 함유한 금속분말을 확산 침투코팅시키는 금속 확산침투공정, 모재의 조직개선을 위해 열처리를 행하는 모재 열처리 공정과 확신 침투 피복층의 인성부여 및 모재의 응력제거를 위해 시효처리를 행하는 시효열처리공정 등으로 구분되며 각각의 공정에서 요구되는 조건들에 따라 코팅층의 특성이 달라지는데 상기와 같은 구성의 본 발명 내열내식 코팅방법을 첨부된 도면을 참조하여 보다 상세히 설명하면 다음과 같다.The coating process of the present invention is a platinum plating pretreatment process for performing a surface polishing, cleaning and various dirt removal processes to clean the surface of the blade before forming the coating layer, and a platinum plating process for plating the platinum for increased corrosion resistance, Diffusion heat treatment process for annealing and heat treatment to reinforce the bonding strength between the plating layer and the base material, metal diffusion penetration process for diffusion penetration coating of yttrium-containing metal powder for adhesion and structure improvement of the coating layer, and tissue improvement of the base material It is divided into the heat treatment process of the base material which performs heat treatment for treatment and the aging heat treatment process which performs the aging treatment to remove the stress of the base material and the toughening of the infiltrating coating layer. The characteristics of the coating layer vary according to the conditions required in each process. Refer to the accompanying drawings of the present invention heat-resistant coating method of the same configuration When described in more detail over the following:

먼저 첫번째 공정은 블레이드의 표면을 깨끗하게 함과 아울러 다음 공정인 도금처리가 원할하게 되도록 하기 위한 백금 도금 전처리 공정으로써 습식 블레스트(Blast)로 상기 블레이드 표면을 연마한 다음 세척한 후 다시 알칼리 탈지처리를 하고 다시 세척한 다음 40%의 황산(H2SO4용액에서 산세처리를 한 후 세척하여 스므트(Smut) 제거 처리를 하는데 상기 블레이드를 10%의 불산(HF)과 70%의 질산(HNO3)에 30∼60초동안 담구어 표면의 오물이나 얼룩을 제거한 뒤 다시 세척하여 스트라이크 처리를 하되 상기 스트라이크는 백금용액에서 10A/dm2의 음극으로 60초간 처리하여 상기 스트라이크 처리 후 블레이드를 세척하여 다음 공정을 수행할 수 있도록 한다.First, the first process is a platinum plating pretreatment process to clean the surface of the blade and to make the plating process smooth. And then washed again, followed by pickling in 40% sulfuric acid (H 2 SO 4 solution, followed by smut removal). The blades were treated with 10% hydrofluoric acid (HF) and 70% nitric acid (HNO 3). Immerse for 30 to 60 seconds, remove dirt or stain on the surface, and wash again to treat the strike, but the strike is treated with a cathode of 10 A / dm 2 for 60 seconds in a platinum solution to wash the blade after the strike. Allow the process to be carried out.

두번째 공정은 백금도금 공정으로써 K2Pt(NO2)3Cl계 백금용액을 사용하는데 이때 상기 용액온도는 40∼60℃, 전류밀도는 1.5-1A/dm2, 음극 대 양극 면적비는 1 : 1로 하고 도금두께는 도금시간으로 조정하되 적어도 2-10㎛ 두께를 유지하도록 하며 상기와 같은 백금도금 공정 후 도금층은 제1a도에서 도시한 바와 같이 모재(100)위에 백금층(110)이 형성된 구조가 된다.The second process is a platinum plating process using a K 2 Pt (NO 2 ) 3 Cl-based platinum solution, wherein the solution temperature is 40 ~ 60 ℃, the current density is 1.5-1A / dm 2 , the area ratio of cathode to anode is 1: 1 The plating thickness is adjusted to the plating time, but at least 2-10㎛ to maintain the thickness and the plating layer after the platinum plating process as described above is a structure in which the platinum layer 110 is formed on the base material 100 as shown in Figure 1a Becomes

미설명부호 101은 공백을 의미한다.Reference numeral 101 denotes a space.

세번째 공정은 외부확산열처리공정으로써 상기 백금도금시 음극에서 발생한 도금층내 합류된 수소가스를 제거하고 백금층(110)에 인성을 부여하기 위해서 상기 백금도금한 블레이드를 260℃에서 2시간, 400℃에서 3시간 동안 소둔 처리한 후 상기 백금층(110)과 모재(100)의 결합력을 강하시키기 위해 진공로에서 1040℃의 온도로 2시간 동안 열처리하여 제1b도에서 도시한 것처럼 모재(100)의 니켈원소가 백금층(110)으로 외부 확산되도록 한다.The third process is an external diffusion heat treatment process in which the platinum-plated blade is removed at 260 ° C. for 2 hours at 400 ° C. to remove hydrogen gas joined in the plating layer generated at the cathode during platinum plating and to give toughness to the platinum layer 110. After annealing for 3 hours, the nickel layer of the base material 100 was heat treated at a temperature of 1040 ° C. for 2 hours in a vacuum furnace to lower the bonding strength of the platinum layer 110 and the base material 100, as shown in FIG. 1b. The element is allowed to diffuse out of the platinum layer 110.

네번째 공정은 내부확산 침투공정으로써 확산용 금속분말은 80∼150메쉬(mesh)의 알루미늄을 1-5%, Ti-Al-C 분말을 1-5% 혼합하고 소결방지제로 100mesh의 산화알루미늄(Al2O3)을 90-97%, 할로겐 화합물인 염화암모늄(NH4Cl)을 0.01%∼3%, 이트룸을 0.01%∼2% 첨가하여 혼합해 1050℃의 온도에서 2∼6시간 열처리 함으로써 확산침투시키되 815℃까지는 아르곤 가스 분위기로 가열하며 815℃ 이상에서 수소분위기 가스로 가열하도록 한다.The fourth process is the internal diffusion penetration process. Diffusion metal powder is mixed with 1-5% of 80-150 mesh aluminum and 1-5% of Ti-Al-C powder, and 100mesh aluminum oxide (Al) 90-97% of 2 O 3 ), 0.01% to 3% of ammonium chloride (NH 4 Cl) as a halogen compound, and 0.01% to 2% of yttrum are mixed and heat-treated at a temperature of 1050 ° C. for 2 to 6 hours. Diffusion permeation is carried out in an argon gas atmosphere up to 815 ° C. and at least 815 ° C. in a hydrogen atmosphere gas.

따라서 상기와 같은 확산침투공정후 코팅층은 제2도에서 도시한 바와 같이 모재(100) 위에 확산층(120)/NiAl층(130)/PtAl2_NiAl+Y층(140)이 순서대로 적층된 구조를 갖는다. 다섯번째 공정은 모재 열처리 공정으로써 모재의 조직을 개선시키기 위해 1050℃에서 2∼6시간 동안 불활성 가스나 진공 분위기에서 열처리를 하는데 모재의 조직은 열처리 후 냉각속도의 영향에 따라서도 좌우되므로 1050℃에서 650℃까지의 냉각 속도는 15∼60분으로 조절하도록 하며, 여섯번째 공정은 시효열처리 공정으로써 코팅층의 인성부여 및 모재의 응력을 제거시키기 위하여 843℃에서 4∼16시간 동안 열처리한다.Therefore, after the diffusion penetration process as described above, the coating layer has a structure in which the diffusion layer 120 / NiAl layer 130 / PtAl 2 _NiAl + Y layer 140 is sequentially stacked on the base material 100 as shown in FIG. Have The fifth process is the heat treatment of the base metal, and heat treatment is performed in an inert gas or vacuum atmosphere at 1050 ° C. for 2-6 hours to improve the structure of the base material. The structure of the base material also depends on the influence of the cooling rate after the heat treatment. The cooling rate up to 650 ℃ is controlled to 15 to 60 minutes, and the sixth process is an aging heat treatment process is heat-treated for 4 to 16 hours at 843 ℃ to remove the toughness of the coating layer and the stress of the base material.

제3도는 본 발명에 의해 확산침투 코팅시킨 초내열 합금의 산화시험(1120℃의 공기중에서)결과를 도시한 그래프로서 제3도에서 도시한 바와 같이 시간이 경과함에 따라 코팅되지 않은 초내열 합금의 그래프(1)에 비해 알루미늄을 코팅시킨 초내열 합금의 그래프(2)가 내열 내식성이 우수하고 상기 알루미늄을 코팅시킨 초내열 합금의 그래프(2)보다 본 발명에 의해 PtAl2+Y층을 코팅시킨 초내열 합금의 그래프(3)의 내열 내식성이 훨씬 우수하게 나타났다.FIG. 3 is a graph showing the results of oxidation test (in air at 1120 ° C.) of the superheat-resistant superalloy coated by the present invention. As shown in FIG. Compared to graph (1), the graph (2) of the super-heat-resistant alloy coated with aluminum is superior to the graph (2) of the super-heat-resistant alloy coated with aluminum and the PtAl 2 + Y layer is coated by the present invention. The heat resistance corrosion resistance of the graph (3) of the super heat resistant alloy was much better.

이상에서와 같이 본 발명의 코팅방법은 기존의 코팅방법에 비해 더욱 가혹한 분위기에서도 사용이 가능한 효과가 있고 작동온도를 더 높일 수 있고 내열 내식성이 우수하므로 블레이드의 사용수명을 향상시킬 수 있는 효과가 있으며, 이로인해 제트엔진과 터보엔진의 성능 및 효율을 향상시킬 수 있는 효과가 있는 것이다.As described above, the coating method of the present invention has an effect that can be used in a harsher environment than the conventional coating method, can increase the operating temperature and has excellent heat resistance and corrosion resistance, thereby improving the service life of the blade. This has the effect of improving the performance and efficiency of jet and turbo engines.

Claims (3)

초내열 Ni기 합금의 백금-알루미나이드 코팅방법에 있어서, 모재의 표면연마 및 세척후 백금을 도금하여 모재의 표면에 코팅층을 형성하는 백금도금공정과, 니켈원소를 상기 코팅층으로 확산시켜서 상기 코팅층과 모재의 결합력을 강화하는 외부확산 열처리공정과, 알루미늄 및 이트륨을 함유한 금속분말을 상기 니켈이 투입된 코팅층의 내부로 침투시켜서 2상 혼합구조를 형성하는 내부확산 침투공정 및, 열처리하는 공정으로 구성된 것을 특징으로 하는 초내열 Ni기 합금의 백금-알루미나이드 코팅방법.In the platinum-aluminate coating method of ultra-heat-resistant Ni-based alloy, a platinum plating process for forming a coating layer on the surface of the base material by plating platinum after surface polishing and washing of the base material, and spreading nickel element into the coating layer and It consists of an external diffusion heat treatment step of strengthening the bonding strength of the base material, an internal diffusion penetration step of forming a two-phase mixed structure by infiltrating the metal powder containing aluminum and yttrium into the coating layer into which nickel is added, and a heat treatment step. Platinum-aluminate coating method of super heat-resistant Ni-based alloy characterized in that. 제1항에 있어서, 상기 외부확산처리공정은 니켈이 함유된 코팅층을 260℃에서 2시간 동안 400℃에서 3시간 동안 소성처리한 후 진공로에서 800∼1100℃의 온도로 1∼4시간 동안 확산 열처리하도록 한 것을 특징으로 하는 초내열 Ni기 합금의 백금-알루미나이드 코팅방법.The method of claim 1, wherein the external diffusion treatment step is to bake the coating layer containing nickel for 3 hours at 400 ℃ for 2 hours at 260 ℃ for 1 to 4 hours in a vacuum furnace at a temperature of 800 ~ 1100 ℃ Platinum-aluminate coating method of super heat-resistant Ni-based alloy, characterized in that the heat treatment. 제1항에 있어서, 상기 내부확산 침투공정은 백금-알루미늄-이트륨화합물을 함유한 제1층과 알루미늄-니켈화합물을 함유한 제2층으로된 2상혼합구조를 갖도록 이트륨 및 알루미늄이 함유된 금속분말이 상기 도금층으로 침투되게 하는 것을 특징으로 하는 초내열 Ni기 합금의 백금-알루미나이드 코팅방법.2. The metal containing yttrium and aluminum according to claim 1, wherein the internal diffusion penetration process has a two-phase mixed structure consisting of a first layer containing a platinum-aluminum yttrium compound and a second layer containing an aluminum-nickel compound. Platinum-aluminate coating method of super heat-resistant Ni-based alloy, characterized in that the powder to penetrate the plating layer.
KR1019880012339A 1988-09-23 1988-09-23 Platinum-aluminide coating method of a super alloy KR920002707B1 (en)

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Publication number Priority date Publication date Assignee Title
FR2748494A1 (en) * 1996-02-26 1997-11-14 Gen Electric HIGH TEMPERATURE ALLOY PIECE HAVING AN ADDITIONAL PROTECTIVE COATING IN PLACES, AND MANUFACTURING METHOD THEREOF
FR2813318A1 (en) * 2000-08-28 2002-03-01 Snecma Moteurs FORMATION OF AN ALUMINIURE COATING INCORPORATING A REACTIVE ELEMENT ON A METAL SUBSTRATE

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KR101105457B1 (en) * 2010-04-19 2012-01-17 한양대학교 산학협력단 Method for manufacturing a heat resistence superalloy having anti-oxidation

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2748494A1 (en) * 1996-02-26 1997-11-14 Gen Electric HIGH TEMPERATURE ALLOY PIECE HAVING AN ADDITIONAL PROTECTIVE COATING IN PLACES, AND MANUFACTURING METHOD THEREOF
FR2813318A1 (en) * 2000-08-28 2002-03-01 Snecma Moteurs FORMATION OF AN ALUMINIURE COATING INCORPORATING A REACTIVE ELEMENT ON A METAL SUBSTRATE

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