KR101389020B1 - METHOD OF ETCHING A Ti-Nb-X BASED TITANIUM ALLOY - Google Patents

METHOD OF ETCHING A Ti-Nb-X BASED TITANIUM ALLOY Download PDF

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KR101389020B1
KR101389020B1 KR1020110089606A KR20110089606A KR101389020B1 KR 101389020 B1 KR101389020 B1 KR 101389020B1 KR 1020110089606 A KR1020110089606 A KR 1020110089606A KR 20110089606 A KR20110089606 A KR 20110089606A KR 101389020 B1 KR101389020 B1 KR 101389020B1
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etching
weight
titanium alloy
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KR20130026159A (en
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이동근
이지혜
이용태
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한국기계연구원
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23FNON-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
    • C23F1/00Etching metallic material by chemical means
    • C23F1/44Compositions for etching metallic material from a metallic material substrate of different composition
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K13/00Etching, surface-brightening or pickling compositions
    • C09K13/04Etching, surface-brightening or pickling compositions containing an inorganic acid
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23FNON-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
    • C23F1/00Etching metallic material by chemical means
    • C23F1/10Etching compositions
    • C23F1/14Aqueous compositions
    • C23F1/16Acidic compositions
    • C23F1/26Acidic compositions for etching refractory metals

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Abstract

본 발명은 에칭이 어려워 조직관찰이 용이하지 않았던 고내식성의 Ti-Nb-X계 타이타늄 합금 소재를 에칭하는 방법에 관한 것이다.
본 발명에 따른 방법은, 열처리된 Ti-Nb-X계 타이타늄 합금을 질산(HNO3) 2 ~ 15 중량%, 불산(HF) 1 ~ 20 중량%, 및 나머지 물(H02)을 포함하는 에칭액을 교반하거나 상기 합금을 흔들면서 2초 ∼ 15초로 침지하는 공정을 복수 회 반복하여 에칭시키며, 상기 침지 공정의 사이에는 수세 공정을 통해 앞의 침지 공정에서 부착되는 에칭액을 완전히 제거하도록 하는 것을 특징으로 한다.
The present invention relates to a method of etching a highly corrosion-resistant Ti-Nb-X-based titanium alloy material, which was difficult to etch, and thus the structure was not easily observed.
The method according to the invention, the heat treatment of the Ti-Nb-X-based titanium alloy etching solution comprising 2 to 15% by weight of nitric acid (HNO 3 ), 1 to 20% by weight of hydrofluoric acid (HF), and the remaining water (H0 2 ) Etching a plurality of times to immerse in 2 seconds to 15 seconds while stirring or shaking the alloy repeatedly, and the etching solution attached in the previous immersion process through the water washing process between the immersion process, characterized in that to completely remove do.

Description

Ti-Nb-X계 타이타늄 합금의 에칭방법 {METHOD OF ETCHING A Ti-Nb-X BASED TITANIUM ALLOY}Etching Method of Ti-NB-Titanium Alloy {METHOD OF ETCHING A Ti-Nb-X BASED TITANIUM ALLOY}

본 발명은 고내식성을 갖는 Ti-Nb-X계(여기서, X는 기타 성분임) 합금소재의 마이크로 에칭기술에 관한 것으로, 보다 구체적으로는 열처리 유무 등을 고려한 에칭액의 조성과 침지 방법을 달리 적용함으로써, 에칭이 어려워 조직관찰이 용이하지 않았던 Ti-Nb-X계 타이타늄 합금의 에칭 방법에 관한 것이다.The present invention relates to a micro-etching technology of a Ti-Nb-X-based alloy material having high corrosion resistance (where X is another component), and more specifically, applying a composition and an immersion method of an etching solution in consideration of the presence or absence of heat treatment. The present invention relates to a method for etching a Ti-Nb-X-based titanium alloy in which etching is difficult and structure observation is not easy.

타이타늄과 그 합금은 비강도가 우수하고, 타 금속재료에 비해 내식성이 우수하며, 화학적 안정성이 탁월하여 군수용이나 항공우주산업에서부터 민수용 소재로도 많이 이용되고 있을 뿐만 아니라, 생체 적합성이 우수하여 치과용 임플란트와 같은 생체 재료에도 많이 쓰이고 있다.Titanium and its alloys have excellent specific strength, excellent corrosion resistance compared to other metal materials, and excellent chemical stability, making them widely used in military and aerospace industries as well as civilian materials. It is also widely used in biomaterials such as implants.

타이타늄 합금의 미세 조직을 광학현미경으로 살펴보기 위해서는, 통상 기계연마(polishing)를 통해 거울 면을 형성한 후 타이타늄 합금 에칭액으로 가장 많이 사용되고 있는 크롤(Kroll) 용액을 활용하여 연마면을 수 초 혹은 수 분간 에칭하며, 이러한 에칭공정에 의해 결정립계, 상경계, 상의 종류, 결정방향 등이 부식의 정도가 서로 다르기 때문에 광학을 통해 미세 조직을 관찰할 수 있게 된다.In order to examine the microstructure of the titanium alloy with an optical microscope, the mirror surface is usually formed by mechanical polishing, and then the polished surface is polished for several seconds or several times using a Kroll solution, which is most commonly used as a titanium alloy etching solution. The etching process is performed for a minute, and since the degree of corrosion of the grain boundary, phase boundary, phase type, crystal direction, and the like are different from each other, the microstructure can be observed through optical.

하지만 Ti-Nb-X계와 같은 조성이나, 이 조성의 합금을 열처리하거나 가공한 방법에 따라 종래의 방법에 따라 에칭을 하게 될 경우, 결정립계와 결정 내부의 에너지의 차가 커서 에너지가 높은 결정립계에서 먼저 에칭액과 반응하여 부식하거나, 열처리 및 가공 중 생긴 침입형 원소나 불순물 등에 의해 고르게 부식되지 않아 과에칭되거나 부식이 많이 진행된 일부 조직은 파괴되어 미세 조직을 관찰하기 어려운 상태가 되기 쉽다.However, when etching according to the conventional method according to the same composition as the Ti-Nb-X system or the method of heat-treating or processing the alloy of this composition, the difference between the grain boundary and the energy inside the crystal is large, so the energy boundary is first determined. Some tissues, which are not etched evenly by intrusion-type elements or impurities generated during the heat treatment and processing due to reaction with the etching solution, or are excessively etched or highly corroded, are easily destroyed and difficult to observe the microstructure.

그러므로, Ti-Nb를 주로 하는 타이타늄 합금과 이 조성의 합금의 열처리 이력에 맞는 에칭액 혼합 및 에칭기술이 개발되어야 하며, 이러한 에칭기술이 개발되어야만 Ti-Nb-X계 타이타늄 합금의 여러 가지 파괴/비파괴 거동, 표면 부식거동, 미세조직학적 특성분석, 재료의 특성 요인분석 등이 가능해지게 된다.
Therefore, an etching solution mixing and etching technique suitable for the heat treatment history of a titanium alloy mainly composed of Ti-Nb and an alloy of this composition has to be developed, and such etching techniques have to be developed for various breakdown / non-destructive properties of Ti-Nb-X-based titanium alloys. Behavior, surface corrosion behavior, microstructural characterization, and material characteristic factors can be analyzed.

본 발명은 전술한 종래기술의 문제점을 해결하기 위해 안출된 것으로서, 고내식 Ti-Nb-X계 타이타늄 합금소재의 표면의 미세조직을 용이하게 관찰할 수 있게 하는 에칭방법을 제공하는데 그 목적이 있다.
The present invention has been made to solve the above problems of the prior art, an object of the present invention is to provide an etching method for easily observing the microstructure of the surface of a high corrosion-resistant Ti-Nb-X-based titanium alloy material. .

상기 목적을 달성하기 위한 수단으로 본 발명은, 열처리된 Ti-Nb-X계 타이타늄 합금의 에칭 방법으로서, 질산(HNO3) 2 ~ 15 중량%, 불산(HF) 1 ~ 20 중량%, 및 나머지 물(H02)을 포함하는 에칭액을 교반하거나 상기 합금을 흔들면서 2초 ∼ 15초로 침지하는 공정을 복수 회 반복하여 에칭시키며, 상기 침지 공정의 사이에는 수세 공정을 통해 앞의 침지 공정에서 부착되는 에칭액을 완전히 제거하도록 하는 것을 특징으로 한다.As a means for achieving the above object, the present invention provides an etching method of heat-treated Ti-Nb-X-based titanium alloy, nitric acid (HNO 3 ) 2-15% by weight, hydrofluoric acid (HF) 1-20% by weight, and the rest Etching the etching solution containing the water (H0 2 ) or immersed in a second to 15 seconds while stirring the alloy is repeatedly etched a plurality of times, between the immersion process is attached to the previous immersion process through the washing process It is characterized by removing the etching liquid completely.

또한, 본 발명에 따른 타이타늄 합금 에칭방법에 있어서, 상기 질산은 3 ~ 10 중량%, 불산은 1 ~ 10 중량% 및 나머지 물을 포함하는 에칭액에 침지하여 에칭시킬 수 있다.In addition, in the titanium alloy etching method according to the present invention, the nitric acid may be etched by immersion in an etching solution containing 3 to 10% by weight, hydrofluoric acid 1 to 10% by weight and the remaining water.

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또한, 본 발명에 따른 타이타늄 합금 에칭방법에 있어서, 상기 X는 Zr, Ge, Si, V, Ta 및 Sn 중에서 선택된 1종 이상일 수 있다.
In addition, in the titanium alloy etching method according to the present invention, X may be at least one selected from Zr, Ge, Si, V, Ta and Sn.

본 발명에 따른 고내식 Ti-Nb-X계 합금의 에칭방법을 사용할 경우, 종래의 에칭방법에 비해 결정립계를 선명하게 관찰할 수 있게 에칭이 가능하며, 특히 시효 열처리된 시편을 에칭할 때 나타나는 과에칭 현상을 줄여 결정립계를 보다 명확하게 관찰할 수 있다.
When the etching method of the high corrosion resistance Ti-Nb-X-based alloy according to the present invention is used, the etching is possible to clearly observe the grain boundary compared to the conventional etching method, especially when etching the aging heat-treated specimens By reducing the etching phenomenon, the grain boundary can be observed more clearly.

도 1은 본 발명의 실시예 1에 따라 Ti-Nb-Zr계 합금을 에칭한 후의 미세조직 사진이다.
도 2는 본 발명의 실시예 1에 따라 용체화처리후 시효처리한 Ti-Nb-Zr계 합금을 에칭한 후의 미세조직 사진이다.
도 3은 본 발명의 실시예 1에 따라 Ti-Nb-Ge계 합금을 에칭한 후의 미세조직 사진이다.
도 4는 발명의 실시예 2에 따라 용체화처리후 시효처리한 Ti-Nb-Zr계 합금을 에칭한 후의 미세조직 사진이다.
1 is a microstructure photograph after etching a Ti-Nb-Zr based alloy according to Example 1 of the present invention.
Figure 2 is a microstructure photograph after etching the Ti-Nb-Zr alloy after aging treatment according to Example 1 of the present invention.
3 is a microstructure photograph after etching a Ti-Nb-Ge-based alloy according to Example 1 of the present invention.
Figure 4 is a microstructure photograph after etching the Ti-Nb-Zr alloy aging after solution treatment in accordance with Example 2 of the invention.

이하, 본 발명을 하기의 실시예에 의거하여 좀 더 상세히 설명하고자 한다. 단, 하기 실시예는 여러 가지 다른 형태로 변형될 수 있으며, 본 발명을 예시하기 위한 것일 뿐 한정하지는 않는다.Hereinafter, the present invention will be described in more detail based on the following examples. However, the following examples may be modified in many different forms and are not intended to limit the invention.

본 발명의 실시예는 고내식용으로 개발된 타이타늄 합금인 Ti-Nb-Zr계 합금과 Ti-Nb-Ge계 합금의 표면을 에칭하는 에칭액 조성물 및 이를 이용한 에칭방법을 제시할 것이다.An embodiment of the present invention will propose an etching solution composition for etching a surface of a Ti-Nb-Zr alloy and a Ti-Nb-Ge alloy, which is a titanium alloy developed for high corrosion resistance, and an etching method using the same.

본 발명에 의한 상기 에칭액 조성물은 질산 2 ~ 15중량%, 불산 1 ~ 20중량%, 나머지 물로 이루어지는 것이 바람직하다. 이때 질산은 2 중량% 미만일 경우 고내식성 Nb 및 Zr 등의 에칭이 되지 않을 수 있고, 15중량%를 초과하면 과에칭될 수 있어 표면이 까맣게 탈 수 있으므로, 2 ~ 15중량%가 바람직하다. 상기 불산은 1중량% 미만일 경우 고내식성 Nb 및 Zr 등의 에칭이 되지 않을 수 있고, 20중량%를 초과하면 강력한 에칭효과에 의해 표면이 까맣게 탈 수 있으며 또한 강력한 휘발성에 의해 공기 흡입시 인체에 치명적인 영향을 줄 수 있기도 하기 때문에 1 ~ 20중량%가 바람직하다.It is preferable that the said etching liquid composition by this invention consists of 2-15 weight% of nitric acid, 1-20 weight% of hydrofluoric acid, and remainder. At this time, nitric acid may not be etched such as high corrosion resistance Nb and Zr when less than 2% by weight, and may be overetched when it exceeds 15% by weight, so that the surface may burn black, 2 to 15% by weight is preferable. When the hydrofluoric acid is less than 1% by weight, it may not be etched such as high corrosion resistance Nb and Zr, and when it exceeds 20% by weight, the surface may be blackened by a strong etching effect and may be fatal to the human body when inhaling air due to strong volatility. 1-20 weight% is preferable because it may affect.

또한, 시효 열처리된 Ti-Nb-Zr계 합금의 경우, 질산 3 ~ 10 중량%, 불산 1 ~ 10 중량%와 나머지 물로 이루어진 혼합된 산성용액을 에칭액 조성물로 이용하는 것이 바람직하다. 이때 질산은 3중량% 미만일 경우 에칭이 충분히 이루어지지 않거나 에칭시간이 많이 소요되고, 10중량%를 초과할 경우 열처리의 열역학적 영향에 의해 시편의 표면이 과에칭되기 쉬으므로, 3 ~ 10중량%가 바람직하다. 상기 불산은 1중량% 미만일 경우 에칭이 충분히 이루어지지 않거나 에칭시간이 많이 소요되고, 10중량%를 초과하면 열처리의 열역학적 영향에 의해 시편의 표면이 과에칭되기 쉬으므로, 1 ~ 10중량%가 바람직하다.
In addition, in the case of the aging heat-treated Ti-Nb-Zr-based alloy, it is preferable to use a mixed acid solution consisting of 3 to 10% by weight of nitric acid, 1 to 10% by weight of hydrofluoric acid and the remaining water as the etching solution composition. At this time, the nitric acid is less than 3% by weight, the etching is not enough or takes a lot of etching time, if it exceeds 10% by weight, the surface of the specimen is easily overetched by the thermodynamic effect of the heat treatment, 3 ~ 10% by weight is preferred Do. When the hydrofluoric acid is less than 1% by weight, etching is not sufficiently performed or takes a long time for etching, and when it exceeds 10% by weight, the surface of the specimen is easily overetched due to the thermodynamic effect of heat treatment, so 1 to 10% by weight is preferable. Do.

[실시예 1]Example 1

고내식용 합금인 Ti-Nb-Zr계 합금(Nb:39중량%, Zr:6중량%, 나머지 Ti)의 미세조직을 정확하게 관찰할 수 있도록 마이크로 에칭하기 위하여, 본 발명의 실시예 1에서는 다음과 같은 방법으로 에칭을 하였다.In order to micro-etch to accurately observe the microstructure of the high corrosion-resistant alloy Ti-Nb-Zr-based alloy (Nb: 39% by weight, Zr: 6% by weight, the remaining Ti), in Example 1 of the present invention Etching was performed in the same manner.

먼저, 시편인 Ti-Nb-Zr계 합금의 단면을 기계연마한 후, 에칭 전에 기계연마한 시편을 초음파 세척기로 충분히 세척을 하고 표면을 깨끗하게 건조시킨다.First, after mechanically polishing the cross section of the Ti-Nb-Zr alloy, which is a specimen, the mechanically polished specimen is thoroughly cleaned with an ultrasonic cleaner before etching, and the surface is thoroughly dried.

그리고, 질산 5중량%, 불산 3중량%, 나머지 물로 이루어진 에칭용액을 준비한 후, 상기 건조한 시편을 집게를 이용하여 에칭액에 3초 ~ 8초 정도 담근 후 표면을 물로 깨끗이 세척하고 최종적으로 표면을 에탄올을 이용하여 빠르게 건조시킨다.In addition, after preparing an etching solution consisting of 5% by weight of nitric acid, 3% by weight of hydrofluoric acid, and the remaining water, immerse the dried specimen in an etchant for 3 seconds to 8 seconds using forceps, and then clean the surface with water and finally clean the surface with ethanol. Dry quickly using.

그리고 에칭 시에는 시편을 에칭액에 담글 때에는 시편을 좌우로 흔들어 침전물로 인해 부분 에칭이 되는 것을 방지하였다. 이때 에칭은 시편 상태에 따라서 원하는 선명도의 미세 조직이 나올 때까지 1회 이상 반복할 수 있다.When etching, when the specimen is immersed in the etching solution, the specimen was shaken from side to side to prevent partial etching due to the precipitate. At this time, the etching may be repeated one or more times until the microstructure of the desired sharpness comes out according to the specimen state.

도 1은 본 발명의 실시예 1에 따라 Ti-Nb-Zr계 합금을 에칭한 후의 미세조직 사진이며, 도 1에서 확인되는 바와 같이, 본 발명의 실시예 1에 따른 방법에 의하면, 종래 명확한 미세조직을 관찰하기 어려웠던 Ti-Nb-Zr계 합금의 미세조직을 명확하게 관찰할 수 있음을 알 수 있다.1 is a microstructure photograph after etching a Ti-Nb-Zr based alloy according to Example 1 of the present invention, and as shown in FIG. 1, according to the method according to Example 1 of the present invention, the conventional fine It can be seen that the microstructure of the Ti-Nb-Zr alloy that was difficult to observe the structure can be clearly observed.

도 2는 Ti-Nb-Zr계 합금을 용체화처리 후 시효 처리한 시편을 상기 에칭액으로 에칭한 미세조직의 사진이다. 시효 처리한 시편의 경우, 그렇지 않은 시편에 비해 결정립계를 따라 부식이 심하게 일어남을 확인할 수 있다. 이는 동일한 농도의 에칭액일지라도 시편의 상태에 따라서 부식 상태가 다르게 나타난다는 것을 알 수 있다. 따라서 용체화처리후 시효처리한 시편의 경우 실시예 1에서 사용한 에칭액을 적용하기 어렵다.FIG. 2 is a photograph of a microstructure in which a specimen obtained by aging treatment of a Ti-Nb-Zr alloy is etched with the etching solution. In the case of aging specimens, it can be seen that the corrosion occurs more severely along the grain boundaries than the specimens that are not. It can be seen that even if the etching solution of the same concentration, the corrosion state is different depending on the state of the specimen. Therefore, it is difficult to apply the etching solution used in Example 1 in the case of the aged specimen after the solution treatment.

도 3은 Ti-Nb-Ge계 합금(Nb:36중량%, Ge:1.3중량%, 나머지 Ti)을 실시예 1에 따른 방법으로 에칭한 후의 미세조직사진이다. 사진에서 확인되는 바와 같이, 미세조직 내부는 마르텐사이트 조직 형태임을 확인할 수 있으며, 결정립계는 흰색으로 명확하게 나타나, 미세조직을 관찰하는데 적절한 에칭이 이루어졌음을 알 수 있다. 3 is a microstructure photograph after etching a Ti-Nb-Ge-based alloy (Nb: 36% by weight, Ge: 1.3% by weight, remaining Ti) by the method according to Example 1. FIG. As confirmed in the photograph, it can be seen that the inside of the microstructure is a martensite structure, and the grain boundary is clearly shown in white, and it can be seen that the etching is appropriate for observing the microstructure.

즉, 본 발명의 실시예 1에 따른 에칭방법은 Ti-Nb-Zr계 합금은 물론 Ti-Nb-Ge계 합금도 명료하게 에칭이 가능함을 알 수 있다.
That is, the etching method according to the first embodiment of the present invention can be seen that the Ti-Nb-Zr-based alloy as well as the Ti-Nb-Ge-based alloy can be clearly etched.

[실시예 2][Example 2]

본 발명의 실시예 2에 따른 에칭의 경우, 실시예 1과 달리, 질산 5중량%, 불산 1.5중량% 및 나머지 물로 이루어진 에칭액을 사용하였다. 즉, 실시예 1에 비해 에칭액에서 불산의 중량을 반으로 낮춘 것이다. 이후, 실시예 1과 동일하게 용체화처리후 시효처리한 Ti-Nb-Zr계 합금 시편을 준비한 후, 동일한 방법으로 에칭을 행하였다.In the case of etching according to Example 2 of the present invention, unlike Example 1, an etching solution consisting of 5% by weight of nitric acid, 1.5% by weight of hydrofluoric acid and the remaining water was used. That is, compared with Example 1, the weight of hydrofluoric acid was reduced by half in etching liquid. Thereafter, the Ti-Nb-Zr-based alloy specimens which had been aged after the solution treatment were aged in the same manner as in Example 1, and then etched in the same manner.

도 4는 본 발명의 실시예 2에 따른 에칭방법으로 용체화처리후 시효처리한 Ti-Nb-Zr계 합금을 에칭한 후의 미세조직사진이다. 도 4에서 확인되는 바와 같이 결정립계에서 부식이 심하게 진행된 도 2와 달리, 결정립계 경계면이 보다 명확해지고, 결정립계를 경계에서 조직 내부로 미세한 아결정립계가 형성되어 있는 것을 관찰할 수 있을 정도로 에칭이 선명도가 높아졌다.
Figure 4 is a microstructure photograph after etching the Ti-Nb-Zr alloy aging after the solution treatment by the etching method according to Example 2 of the present invention. As shown in FIG. 4, unlike in FIG. 2, where the corrosion is severely progressed at the grain boundary, the grain boundary becomes clearer, and the etching becomes clear enough to observe that fine grain boundaries are formed from the grain boundary into the tissue. .

Claims (5)

열처리된 Ti-Nb-X계 타이타늄 합금의 에칭 방법으로서,
질산(HNO3) 2 ~ 15 중량%, 불산(HF) 1 ~ 20 중량%, 및 나머지 물(H02)을 포함하는 에칭액을 교반하거나 상기 합금을 흔들면서 2초 ∼ 15초로 침지하는 공정을 복수 회 반복하여 에칭시키며, 상기 침지 공정의 사이에는 수세 공정을 통해 앞의 침지 공정에서 부착되는 에칭액을 완전히 제거하도록 하는 것을 특징으로 하는 Ti-Nb-X계 타이타늄 합금의 에칭 방법.
An etching method of heat-treated Ti-Nb-X-based titanium alloy,
A plurality of processes for immersing the etching solution containing 2 to 15% by weight of nitric acid (HNO 3 ), 1 to 20% by weight of hydrofluoric acid (HF), and the remaining water (H0 2 ) by stirring or shaking the alloy The etching method of the Ti-Nb-X-based titanium alloy, wherein the etching solution is repeatedly removed, and the etching solution adhered in the previous dipping step is completely removed between the dipping steps.
제 1 항에 있어서,
상기 질산이 3 ~ 10 중량%이고, 상기 불산이 1 ~ 10 중량%인 것을 특징으로 하는 Ti-Nb-X계 타이타늄 합금의 에칭방법.
The method according to claim 1,
The etching method of the Ti-Nb-X-based titanium alloy, characterized in that the nitric acid is 3 to 10% by weight, the hydrofluoric acid is 1 to 10% by weight.
삭제delete 삭제delete 제 1 항 또는 제 2 항에 있어서,
상기 X는 Zr, Ge, Si, V, Ta 및 Sn 중에서 선택된 1종 이상인 것을 특징으로 하는 Ti-Nb-X계 타이타늄 합금의 에칭방법.
3. The method according to claim 1 or 2,
X is an etching method of a Ti-Nb-X-based titanium alloy, characterized in that at least one selected from Zr, Ge, Si, V, Ta and Sn.
KR1020110089606A 2011-09-05 2011-09-05 METHOD OF ETCHING A Ti-Nb-X BASED TITANIUM ALLOY KR101389020B1 (en)

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JP2008174839A (en) 2007-01-17 2008-07-31 United Technol Corp <Utc> Method of surface treating metallic article, and solution system
KR20090123762A (en) * 2008-05-28 2009-12-02 한국기계연구원 Beta-based titanium alloy with low elastic modulus
KR20110064795A (en) * 2009-12-09 2011-06-15 신진볼텍주식회사 A manufacturing method for titanium alloy bolting of use production equipment of titanium alloy bolt

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