• 한국표면공학회지
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• 제49권5호
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• pp.401-407
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• 2016

In this work, effect of zincate treatment of AZ91 Mg alloy on the following electrodeposition of copper was examined in a non-cyanide bath containing pyrophosphate ions in view of surface morphology and adhesion of the electrodeposited copper layer. Without zincate treatment, the electrodeposited copper layer showed very porous structure and poor adhesion. On the other hand, the copper layer electrodeposited on the zincate-treated surface showed dense structure and good adhesion. The dissolution rate of AZ91 Mg alloy after the zincate treatment appeared to decrease about 40 times in the copper pyrophosphate bath, as compared to that of the surface without zincate treatment. The porous morphology and poor adhesion of a copper layer on the AZ91 Mg alloy surface without zincate treatment were attributed to small number of nucleation sites of copper because of rapid dissolution of the magnesium substrate in the pyrophosphate bath. Based on the experimental results, it is concluded that the zincate treatment to form a conducting and protecting layer on the AZ91 Mg alloy surface is essential for successful electrodeposition of a copper layer on AZ91 Mg alloy with good adhesion and dense structure in the copper pyrophosphate bath.

• 한국표면공학회지
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• 제49권3호
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• pp.238-244
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• 2016

Copper electrodeposition on AZ91 Mg alloy was studied in views of preferential deposition on ${\alpha}$- or ${\beta}$- phases and how to achieve uniform deposition over the entire surface on ${\alpha}$- and ${\beta}$-phases in a cyanide solution. The inhomogeneous microstructure of AZ91 Mg alloy, particularly ${\alpha}$- and ${\beta}$-phases, was found to result in non-uniform deposition of zincate layer, preferential deposition of zincate on ${\beta}$-phases, which leads to non-uniform growth of copper layer during the following electrodeposition process. The preferential depositions of zincate can be attributed to higher cathodic polarizations on the ${\beta}$-phases. Pin-hole defects in the copper electrodeposit were observed at the center of large size ${\beta}$-phase particles which is ascribed to gas bubbles formed at the ${\beta}$-phases. The activation of AZ91 Mg alloy in hydrofluoric acid solution was used to obtain uniform growth of zincate layer on both the ${\alpha}$- and ${\beta}$-phases. By choosing an optimum activation time, a uniform zincate layer was obtained on the AZ91 Mg alloy surface and thereby uniform growth of copper was obtained in a cyanide copper electroplating solution.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2016년도 추계학술대회 논문집
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• pp.124.1-124.1
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• 2016

In this work, uniform thickness and good adhesion of electrodeposited copper layer were achieved on AZ91 Mg alloy in alkaline noncyanide copper solution containing pyrophosphate ion by employing appropriate zincate pretreatment. Without zincate pretreatment, the electrodeposited copper layer on AZ91 Mg alloy was porous and showed poor adhesion which was explained by small number of nucleation sites of copper due to rapid dissolution of the magnesium substrate in the pyrophosphate solution. The zincate pretreatment was found as one of the most important steps that can form a conducting layer to cover AZ91 surface which decreased the dissolution rate of AZ91 Mg alloy about 40 times in the copper pyrophosphate solution. Electrodeposited copper layer on AZ91 Mg alloy after an appropriate zincate pretreatment showed good adhesion and uniform thickness with bright surface appearance, independent of the deposition time but the surface roughness of the electrodeposited copper layer increased with increasing Cu deposition time.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2016년도 추계학술대회 논문집
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• pp.194.1-194.1
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• 2016

The present study investigated the effect of zincate treatment time on the dissolution behavior and the deposition of copper by immersion process and electroplating process on AZ31 Mg alloy substrate in a copper pyrophosphate bath. Without zincate pretreatment, the AZ31 Mg substrate quickly dissolved in the copper pyrophosphate solution although an external cathodic current was applied. The copper layers deposited on non-zincate treated AZ31 Mg alloy substrate by both immersion and electroplating processes showed very porous structure and very poor adhesion. With increasing zincate treatment time up to 2 min, the dissolution of AZ31 substrate in pyrophosphate solution rapidly decreased and the deposited copper layer was less porous and exhibited stronger adhesion. The immersion of AZ31 Mg sample in zincate solution for 5 min was found as a critical time for producing a non-porous and adherent electrodeposited copper layer on AZ31 Mg alloy. The optimum zincating time can be determined by observing the open circuit potential (OCP) of AZ31 Mg alloy samples in a copper pyrophosphate electroplating bath. The OCP reached a stable value of about -0.10 V (vs. SCE) after 5 min of immersion in the copper pyrophosphate electroplating solution.

• 한국표면공학회지
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• 제44권6호
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• pp.239-245
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• 2011

Magnesium alloys is the lightest by structural metals, but it is not good corrosion resistant because of pit, void. Particularly, AZ31B magnesium alloy sheets that have slag, scratch by rolling process indicate some defects. The objective of this research is to perform uniform plating on AZ31B by studying etching and zincate process. Especially, zincate treatment by zinc salt and pyrophosphate is the most important in the decoration plating. Dissolution of magnesium is reduced by the formation of uniform zinc conversion layer during strick and post process, which decreases defects for plating process.

• 한국재료학회지
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• 제9권11호
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• pp.1095-1101
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• 1999

무전해 니켈 도금을 이용하여 플립칩 공정에 응용하기 위한 범프와 UBM층을 형성하고 특성을 조사하였다. 도금전 zincate 처리를 해석하고 도금 변수인 온도, pH 등에 따른 도금층의 특성 변화, 공정 후의 열처리 효과들을 관찰하였다. 이를 통해 각 변수들이 도금층의 특성에 미치는 영향과 전자패키지 응용시 요구되는 무전해 니켈 도금 조건을 제시하였다. 도금직후의 니켈은 P가 10wt% 포함되며, $60\mu\Omega$-cm의 비저항, 500HV의 경도의 비정질 결정구조를 갖으며 열처리후 결정질 변태와 동시에 경도가 증가한다. 무전해 범프를 실제 테스트 칩에 형성한 후, ACF 플립칩 접속하여 무전해 니켈 범프의 장점과 미세 전자 패키징응용의 가능성을 확인하였다.

• 대한용접접합학회:학술대회논문집
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• 대한용접접합학회 2002년도 Proceedings of the International Welding/Joining Conference-Korea
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• pp.456-462
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• 2002

In the present work, a low cost and fine pitch bumping process by electroless Ni/immersion Au UBM (under bump metallurgy) and stencil printing for the solder bump on the Al pad is discussed. The Chip used this experimental had an array of pad 14x14 and zincate catalyst treatment is applied as the pretreatment of Al bond pad, it was shown that the second zincating process produced a dense continuous zincating layer compared to first zincating. Ni UBM was analyzed using Scanning electron microscopy, Energy dispersive x-ray, Atomic force microscopy, and X-ray diffractometer. The electroless Ni-P had amorphous structures in as-plated condition. and crystallized at 321 C to Ni and Ni$_3$P. Solder bumps are formed on without bridge or missing bump by stencil print solder bump process.

• 한국재료학회지
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• 제6권7호
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• pp.700-708
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• 1996

Flip chip bonding에 무전해도금기술을 적용하여 solder bumper형성의 최적 조건을 규명하였다. 시편은 AI 패턴된 4 inch Si 웨이퍼를 사용하고, 활성화 처리시 zincate 용액을 사용하였으며, 무전해 도금은 Ni-P 도금액고 Au immersion 용액을 사용하였다. 활성화 물질의 AI 침식정도 및 Zn 석출 정도를 알아보기 위하여 EDS측정을 하였고, 각 공전에서의 표면형상을 알아보기 위해 SEM 분석을 하였다. 열처리 후 금도금층의 주 결정성장 방향은 XRD를 이용하여 측정하였다. 산처리에서 질산과 황산 중 질산에 의한 산화막제거 정도가 더 우수하게 나타났다. 활성화 처리시 zincate 용액을 희석시킬수록 입자 크기가 미세해 지고, 활성화 물질은 pH 13-13.5, 상온, 농도 15-25%의조건에서 크기가 작은 Zn 활성화 물질이 균일하게 분포하였다. Ni과 Auan전해도금 속도는 온도와 pH가 증가할수록 증가하였다. Ni 무전해 도금 조건은 pH 4.5, 온도 $90^{\circ}C$, 시간 20분이며, Au 무전해 도금조건은 pH7, 온도 $80^{\circ}C$, 시간 10분이었다. 상온에서 $400^{\circ}C$까지 30분동안 열처리 한 후 금도금막의 결정 방향은 pH 7, 온도 $80^{\circ}C$, 시간 10분이었다. 상온에서 $400^{\circ}C$까지 30분 동안 열처리 한 후 금도금막의 결정 방향은 pH 7에서 (111), pH 9에서는 (200)과 (111)이 주 peak로 나타났으며, 열처리에 의한 결정 방향의 변화는 없었다. 전체 공정에서 최종적인 표면 형상에 영향을 주는 단계는 활성화 처리로서 flip chip의 bonding layer형성에 가장 중요한 요소임을 알 수 있었다.보다 자생지(自生地)에서 높은 함량(含量)을 보였다. 5. 무기성분함양(無機成分含量)의 차이(差異)는 K의 경우(境遇) 자생지(自生地)에서 보다 재배지(栽培地)에서 평균적(平均的)으로 10배이상(倍以上) 정도(程度) 높은 함량(含量)의 차이(差異)를 보였으나 Mn, Zn, Na, Cu 등(等)은 일정(一定)한 경향(傾向)을 보이지 않는 것으로 나타났다. 6. 유리(遊離) 아미노산(酸)의 함량(含量)은 자생지(自生地은)보다 재배지(栽培地)에서 전반적(全般的)으로 높은 함량(含量)을 나타내었고, 특(特)히 Arginine은 다른 성분(成分)들과 비교(比較)해 볼 때 가장 높은 조성(組成)의 차이(差異)를 나타내었다. 7. 야생(野生)더덕과 재배(栽培)더덕의 정유성분수율(精油成分收率)은 자생지재배(自生地栽培)에서는 모두 0.004% 였고 재배지(栽培地)에서는 야생(野生)더덕이 0.005%였다. 8. 더덕의 재배장소(栽培場所)에 따른 향기성분(香氣成分)은 총(總) 21종(種)이었으며 自生地(自生地)에서 야생(野生)더덕은 16종(種), 재배(栽培)더덕은 18종(種)이었고, 재배지(栽培地)에서 야생(野生) 더덕은 14종(種), 재배(栽培)더덕은 20(種)이었다. 9. Trans-2-hexanol은 야생(野生)더덕의 자생지(自生地) 재배(栽培)에서 피이크 면적(面積) 당(當) 50.3%, 재배지(栽培地)에서 피이크 면적(面積) 당(當) 43.3%를 보였으며 amylalcohol, furfuryl acetate, 2-methoxy-4-vinyl phenol(MVP)는 재배(栽培)더덕에서만 확인(確認)되었다.는 KI, BMI와 유의적인 양의 상관관계를 보였고 (p<0.01), HCL-C은 비체중, BMI, LBM, TBM와 유의적인 음의 상관관계를 보였으며, (p<0.01), KI, SBP와도 음의 상관관계를 보였다. (p<0.05), LCL-C는 KI와 유의적이인 양의