KR940010769B1 - Au alloy and making method thereof - Google Patents
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Abstract
Description
제 1a, b 도는 각각 황동모재와 스테인레스강모재에 대하여 본 발명의 이온도금법에 의하여 얻어진 금합금층과 하지층의 단면도.1a, b are cross-sectional views of the gold alloy layer and the base layer obtained by the ion plating method of the present invention for the brass base material and stainless steel base material, respectively.
제 2 도는 금과 크롬의 상평형도("Binary Alloy Phase Diagrams" 2nd e.. Ed. : thaddeus B.Massalski, Vol. 1, p.356)Figure 2 shows the phase equilibrium of gold and chromium ("Binary Alloy Phase Diagrams" 2nd e .. Ed .: thaddeus B. Massalski, Vol. 1, p.356)
제 3 도는 금, 동 및 크롬의 분광반사특성도(松永正久등 : 表面改質技術〈日刊工業新聞社,1988〉, p288)Figure 3 shows the spectroscopic reflection characteristics of gold, copper and chromium (松 永 正 久, etc .: 表面 改 質 技術 〈日刊 工業 新聞 社, 1988〉, p288)
제 4 도는 금-동계에 있어서 금 중량비에 따른 색상의 변화도.4 is a change in color according to the weight ratio of gold to gold-winter.
본 발명은 이온도금용 금합금과 그 제조방법에 관한 것으로, 특히 금색상을 얻기위한 피도금 물질에 대한 이온도금층의 밀착성과 내마모성이 우수한 이온도금용 금합금과 이러한 금합금층의 제조방법에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a gold alloy for ion plating and a method of manufacturing the same, and more particularly, to an ion plating gold alloy excellent in adhesion and abrasion resistance of an ion plating layer to a material to be plated to obtain a gold color, and a method of manufacturing such a gold alloy layer.
종래 각종 금속제 장신구등을 도금하여 금색상의 표면 장식을 얻는 것에 있어서는 하지도금처리된 피도금물질에 습식방법으로 금 또는 금합금을 도금하거나 이온도금방법으로 TiN을 이온도금하고 있다.Conventionally, in order to obtain a gold-colored surface decoration by plating various kinds of metal ornaments and the like, gold or gold alloy is plated by a wet method or ion-plated TiN by an ion plating method.
습식방법으로 금 도금을 하는 경우 금색상의 표현에는 적합하나 과다한 금 소비량, 열등한 도금층의 밀착성과 내마모성, 환경오염 문제등의 결점이 있었다. 또한 이온도금방법으로 TiN을 도금하는 경우, 밀착성과 내마모성이 우수한 반면에 금 색상의 표현이 열등하고 균일한 색상생산이 어렵다는 문제점등이 있었다.Gold plating by the wet method is suitable for the expression of gold color, but there are disadvantages such as excessive gold consumption, inferior plating layer adhesion and abrasion resistance, and environmental pollution. In addition, when TiN is plated by ion plating, the adhesion and abrasion resistance are excellent, but there is a problem that the color expression is inferior and uniform color production is difficult.
본 발명자는 피도금 물질표면위에 TiN층을 제조한 후 Ar 기체분위기(압력 : 5×10-4Torr∼10-1Torr)하에서 금 또는 금합금을 증발시켜 음극전압(50V∼100V)이 가해진 피도금 물질의 TiN층 위에 금 또는 금합금층을 제조하였다(제 1 도 참조).The present inventors fabricated a TiN layer on the surface of the material to be plated, and then plated the negative voltage (50 V to 100 V) by evaporating gold or a gold alloy under an Ar gas atmosphere (pressure: 5 × 10 -4 Torr to 10 -1 Torr). A gold or gold alloy layer was prepared on the TiN layer of material (see FIG. 1).
순금박막의 열등한 기계적 성질을 향상시키기 위해서 본 발명에서는 순금에 소량의 크롬을 첨가하였다. 고용 경화와 석출경화(α"상-Au4Cr-의 석출, 제 2 도 참조)의 메카니즘을 통하여 소량의 크롬첨가로도 순금의 열등한 기계적 성질을 크게 향상시킬 수 있었다. 그러나, 크롬의 중량%가 증가함에 따라, 가시광선영역내에서 노란색상과 붉은색상의 파장의 빛을 선택적으로 반사하고 그외의 파장을 가진 빛들을 선택적으로 흡수하는 순금고유의 분광반사특성(제 3 도 참조)에서 벗어나기 시작하여 목적하는 색상을 얻을 수가 없었다. 이를 보완하기 위하여 가시광선 영역내에서 선택적 반사를 하는 또다른 금속, 동을 위 합금에 첨가하였다.In order to improve the inferior mechanical properties of the pure gold thin film, a small amount of chromium was added to the pure gold in the present invention. Through the mechanism of solid solution hardening and precipitation hardening (precipitation of α "phase -Au 4 Cr-, see FIG. 2), the addition of a small amount of chromium significantly improved the inferior mechanical properties of pure gold. However, the weight percentage of chromium As is increased, it starts to deviate from the pure spectral reflection characteristic (see FIG. 3) that selectively reflects light of yellow and red wavelengths in the visible ray region and selectively absorbs light with other wavelengths. To compensate for this, another metal, copper, was added to the alloy, with selective reflection in the visible range.
동은 금의 경우보다 더 높은 파장을 가진 붉은 빛만 선택적으로 반사하므로(제 3 도 참조), 크롬의 첨가로 합금의 색상이 흰색계통으로 변색되는 현상을 효과적으로 보완할 수 있었다. 그러나, 동의 함량이 늘어남에 따라 합금의 색상은 붉은 색을 거쳐 동의 25중량% 이상에서는 동 특유의 붉은 색을 띄게 되는 것이 밝혀졌다(제 4 도 참조).Since copper selectively reflects only red light with a higher wavelength than gold (see Figure 3), the addition of chromium could effectively compensate for the discoloration of the alloy into a white system. However, it was found that as the content of copper increases, the color of the alloy becomes red, and the color of the alloy becomes red at 25 wt% or more of copper (see FIG. 4).
위의 실험결과를 토대로 70∼99.8중량%의 금, 0.1∼5중량%의 크롬과, 0.1∼25%의 동의 조성으로 특징되어지는 본 발명의 금합금 조성이 결정되었다.Based on the above experimental results, the gold alloy composition of the present invention, which is characterized by a composition of 70 to 99.9% by weight of gold, 0.1 to 5% by weight of chromium, and 0.1 to 25% of copper, was determined.
본 발명을 이후 실시예를 참고로 상세히 설명한다.The invention is described in detail with reference to the following examples.
[실시예]EXAMPLE
A. 피도금재료 :A. Plated Material:
시계케이스 : Ni(6㎛)/Cr(0.5㎛)층이 습식도금방식으로 입혀진 황동모재Watch case: Brass base material with Ni (6㎛) / Cr (0.5㎛) layer coated by wet plating method
시계밴드 : 스테인레스강(SUS 304)Watch band: Stainless steel (SUS 304)
B. 피도금재료의 표면세정 공정 :B. Surface cleaning process of plated material:
(1) 알칼리 용액조 내에서 초음파 세척(1) Ultrasonic Cleaning in Alkaline Solution Tank
(2) 유산 용액조내 세척(2) washing in lactic acid solution tank
(3) 물 세척(3) water washing
(4) 습기제거(4) moisture removal
(5) 60∼80℃의 트리클로로에틸렌(TCE) 용액조 내에서 초음파 세척(5) Ultrasonic cleaning in a trichloroethylene (TCE) solution bath at 60 to 80 ° C
C. 도금방법 :C. Plating Method:
(1) 금합금 증발원 제작 :(1) Production of gold alloy evaporation source:
i) 크롬을 미세한 크기로 분활화 한다(0.83mm).i) Split the chromium into fines (0.83 mm).
ii) 용융방식으로 합금제작시, 첨가원소들과 대기중의 기체원자들간의 반응을 극소화 시키기 위하여 금과 동 및 크롬분말을 중량비에 따라 석영판에 넣고 10-2Torr 이하까지 관내의 압력을 낮추어준 후 석영판을 봉인한다.ii) When manufacturing alloy by melting method, put gold, copper and chromium powder in the quartz plate according to the weight ratio in order to minimize the reaction between additive elements and gas atoms in the atmosphere and lower the pressure in the pipe to 10 -2 Torr or less. After sealing, seal the quartz plate.
iii) 크롬이 완전히 용해된 균질의 합금액상 용액을 만들기 위하여 제 2 도에 보여지고 있는 상평형도에 의거 크롬의 각각의 첨가 조성에서의 액상선보다 높은 온도에서, 고주파 유도용해로를 이용, 석영관속의 혼합물을 열처리한다. 크롬분말이 완전히 용해되는데 소요되는 시간은 분말의 입자크기가 미세할수록 또 가열온도가 증가할수록 단축된다. 0.83mm 크기의 크롬분말 사용시 크롬의 중량비가 0.1∼5%일때의 액상선보다 100℃정도 높은 1170℃∼1260℃로 시편을 가할 때 크롬분말이 완전히 용해되는데는 약 10분 정도의 시간이 소요된다.iii) using a high frequency induction furnace at a temperature higher than the liquidus in each of the additive compositions of chromium according to the phase equilibrium shown in FIG. 2 to produce a homogeneous solution of chromium in which the chromium is completely dissolved. Heat the mixture. The time required for complete dissolution of the chromium powder is shortened as the particle size of the powder is fine and as the heating temperature is increased. When 0.83mm chromium powder is used, it takes about 10 minutes to completely dissolve the chromium powder when the specimen is added at 1170 ℃ ~ 1260 ℃, which is 100 ℃ higher than the liquid line when the weight ratio of chromium is 0.1-5%.
iv) 석영관속의 액상용액이 잘 혼합되도록 교반하여준 후 급냉시킨다.iv) After stirring the liquid solution in the quartz tube to mix well, quench it.
(2) 도금전 진공조내에서 피도금 재료 표면의 전처리 :(2) Pretreatment of the surface of the material to be plated in the vacuum chamber before plating:
4피도금 재료의 진공조내 장착 후 Ar 기체분위기(10-2Torr)하에서 피도금 재료들에 음극고전압을 가하여, 스퍼터링 효과를 통한 표면위의 잔존 불순물 제거 및 도금물질의 밀착력 향상을 위한 표면 결합층의 형성을 유도한다.The surface bonding layer for removing residual impurities on the surface through the sputtering effect and improving the adhesion of the plating material by applying a cathode high voltage to the material to be plated under Ar gas atmosphere (10 -2 Torr) after mounting in the vacuum chamber of the 4 plated material. Induces the formation of.
(3) Ti 질화물층(TiN) 형성 :(3) Ti nitride layer (TiN) formation:
질소 플라즈마 분위기 하에서 Ti를 증발시켜 피도금 재료 표면위에 Ti 질화물(TiN)층을 형성시킨다.Ti is evaporated under a nitrogen plasma atmosphere to form a Ti nitride (TiN) layer on the surface of the material to be plated.
(4) 이온도금방식을 통한 Au 합금층 제작 :(4) Au alloy layer production by ion plating method:
Ar 플라즈마 분위기 하에서(압력 : 5×10-4Torr∼10-1Torr) 전자총 가열방식, 전기저항 가열방식, 할로우 캐소우드(hollow cathode) 가열방식 또는 고주파 유도용해방식을 이용하여 금 또는 금합금을 증발시켜 음극전압이 가하여진(50∼1000) 피도금 물질 TiN층 위에 500∼10,000Å두께의 금합금층을 제작한다. 금 또는 금의 합금 원소들의 일부는 증발원으로부터 기판으로 가는 도중 전자와의 충돌로 인하여 이온화되고 이들은 Ar원소의 이온들과 함께 높은 에너지로 피도금 물질의 표면과 충돌하게 된다. 이로 인하여 밀도가 높고 밀착력이 우수한 균일한 금합금층이 TiN 표면위에 생성되게 된다.Evaporate gold or gold alloy under Ar plasma atmosphere (pressure: 5 × 10 -4 Torr to 10 -1 Torr) using electron gun heating, electric resistance heating, hollow cathode heating or high frequency induction melting A gold alloy layer having a thickness of 500 to 10,000 kPa is produced on the TiN layer to which the cathode voltage is applied (50 to 1000). Some of the gold or alloying elements of gold are ionized due to collision with electrons from the evaporation source to the substrate and they collide with the surface of the material to be plated with high energy together with the ions of the Ar element. As a result, a uniform gold alloy layer having a high density and excellent adhesion is formed on the TiN surface.
본 발명에 따르면 상기 언급된 바와같이 질화물(TiN)로 하지 도금된 피도금 물질에 상기 조성 비율, 즉 70∼99.8중량%의 금, 0.1∼5중량%의 크롬, 0.1∼25중량%의 동의 조성을 갖는 금합금층을 이온도금 방식으로 제작할 시, 금색상이 양호하고 밀착성과 내마모성이 뛰어난 장식용 금도금층을 습식 금도금 장식보다 횔씬 낮은 생산가로 제조 가능하다.According to the present invention, the above mentioned composition ratio, 70 to 99.9 wt% of gold, 0.1 to 5 wt% of chromium, and 0.1 to 25 wt% of copper, is applied to the plated material plated with nitride (TiN) as mentioned above. When manufacturing a gold alloy layer having an ion plating method, it is possible to produce a decorative gold plated layer with good gold color and excellent adhesion and wear resistance at a much lower production price than a wet gold plated ornament.
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