KR20140118065A - Antibiotic thin layer comprising metal oxid - Google Patents
Antibiotic thin layer comprising metal oxid Download PDFInfo
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- KR20140118065A KR20140118065A KR1020130033302A KR20130033302A KR20140118065A KR 20140118065 A KR20140118065 A KR 20140118065A KR 1020130033302 A KR1020130033302 A KR 1020130033302A KR 20130033302 A KR20130033302 A KR 20130033302A KR 20140118065 A KR20140118065 A KR 20140118065A
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- oxide
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- zinc oxide
- calcium oxide
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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
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
- C23C2/06—Zinc or cadmium or alloys based thereon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
Abstract
Description
본 발명은 금속산화물 즉, 산화아연 및/또는 산화칼슘을 이용한 항균 박막 및 그의 제조방법에 관한 것이다. 더 상세히는 합성수지제의 평판, 예컨대, 안경 렌즈, 휴대전화 디스플레이, 식품 용기, 의료용기 등의 평판의 외부를 금속산화물, 즉 산화아연, 산화칼슘으로 이루어진 군에서 선택된 1종 또는 2종으로 진공 코팅하여 이루어진 항균 박막 및 그의 제조방법에 관한 것이다.
The present invention relates to an antibacterial thin film using metal oxide, that is, zinc oxide and / or calcium oxide, and a method for producing the same. More specifically, a flat plate made of a synthetic resin, such as a spectacle lens, a cell phone display, a food container, a medical container, or the like, is vacuum-coated with one or two kinds of metal oxides selected from the group consisting of zinc oxide and calcium oxide And a method for producing the same.
현재까지 알려진 항균성을 나타내는 물질로서는 은, 구리, 목초액, 유기약품, 항생제 등이 알려져 있다. 그러나 이러한 물질을 합성수지제의 평판에 이를 이용하는 것은 가능하지 않고, 또한 광촉매활성을 나타내는 산화티타늄 또는 이를 포함하는 금속산화물 복합체 등이 광촉매 활성을 나타내어 항균, 탈취 등의 목적으로 사용할 수 있음이 다수 알려져 있다(예, 특허문헌 1 등). 그러나 이러한 광촉매활성 물질은 광(hμ)에 의해 활성되기 때문에 그에 따른 제약이 많고, 또한 산화티타늄이 가격이 높아 범용적으로 사용하기 적합하지 않다. As a substance showing antimicrobial properties known to date, silver, copper, wood vinegar, organic chemicals, antibiotics and the like are known. However, it is not possible to use such a material for a plate made of a synthetic resin, and titanium oxide or a metal oxide complex containing the same exhibiting photocatalytic activity exhibits photocatalytic activity, and many of them can be used for antibacterial and deodorization purposes (For example, Patent Document 1, etc.). However, since such a photocatalytic active material is activated by light (hμ), there are many restrictions thereon, and titanium oxide is not suitable for general use due to its high price.
또한 산화아연이 ITO(인듐/주석산화물)의 대체물로서 사용하고 자 하는 시도(비특허문헌 1)가 있었으나, 산화아연 자체를 항균물질로서 이용하려는 어떠한 시도나 기재도 없었다. There has also been an attempt to use zinc oxide as a substitute for ITO (indium / tin oxide) (Non-Patent Document 1), but there has been no attempt to use zinc oxide itself as an antimicrobial substance.
또한 산화칼슘은 식용 등으로 이용되고 있으며, 특히 면류, 두부, 기타 식품에서의 저장성을 연장시킨다는 보고(비특허문헌 2 등)이 알려져 있으나, 이러한 산화칼슘이 항균성을 갖는다는 연구나, 이를 이용한 항균성 제품이 알려진 바 없다.
In addition, calcium oxide is used for edible purposes and the like, and it is reported that prolonging shelf life in noodles, tofu and other foods (Non-Patent Document 2) is known. However, researches that calcium oxide has antimicrobial activity, The product is not known.
합성수지 제품은 유리제품에 비하여 오염되기 쉽고, 오염원인 세균 등을 단순한 세정에 의해서는 제거되지 않고, 끓는 물에 소독하는 것은 합성수지의 변형이 오며, 근년에 전화기의 송수신기에 세균 오염이 심각함이 보고되어 있다(참조, 상지대학교 논문집 제12집(1991.9) pp 67-81). Synthetic resin products are more likely to be contaminated than glass products. Bacteria, which are pollution sources, are not removed by simple cleaning. Disinfecting in boiling water causes deformation of synthetic resin. In recent years, bacterial contamination of telephone transceiver has been reported (See, Sangji University Journal, Vol. 12 (1991.9) pp 67-81).
그러나 대다수의 일반인은 합성수지 제품이 오염되었는지도 인지하지도 못하고 있는 실정이다.However, most of the general public do not know whether or not synthetic resin products are contaminated.
최근 안경 착용자가 급격히 증가하여 전 인구의 약 1/3에 달하고, 또한 휴대전화기 소지자가 우리나라 총인구의 약 70% 이상을 점하고 있으나, 이러한 안경이나 휴대전화의 오염에 대한 취급이나 대책은 전무한 실정이다. Recently, eye wearers have increased rapidly, reaching about one third of the total population, and cell phone holders account for more than 70% of the total population in Korea. However, there is no treatment or countermeasures against such glasses or mobile phone pollution .
이러한 상황 하에서 안경이나 휴대전화의 디스플레이와 같은 판상 합성수지제의 오염을 방지하는 것이 본 발명의 해결하고자 하는 과제이다.
Under such circumstances, it is an object of the present invention to prevent contamination of a plate-like synthetic resin such as a glass or a display of a cellular phone.
본 발명자는 상기 문제점을 해결하기 위하여 예의 연구한 결과, 산화금속, 즉 산화아연 및/또는 산화칼슘을 합성수지제의 안경렌즈나 휴대폰 디스플레이부에 박막을 형성하여 본 결과, 의외로 항균성이 높음을 발견하고 본 발명을 완성하게 되었다. As a result of intensive studies to solve the above problems, the present inventors have found that a metal oxide, that is, zinc oxide and / or calcium oxide, is formed into a spectacle lens made of synthetic resin or a thin film on a cellular phone display part, Thereby completing the present invention.
그러나, 이러한 금속산화물로 박막을 형성하면 그의 두께에 따라 투과도가 떨어져 안경렌즈나 휴대전화 디스플레이로서 기능을 하지 못하는 단점이 있다. 이에 더 연구를 진행한 바, 박막의 두께를 30nm 이하, 바람직하기로는 20nm 이하로 하면, 투과도에 영향을 주지 않고, 또한 우수한 항균작용을 나타내며, 그의 항균작용의 효과도 장기간 유지됨을 발견하고 본 발명을 완성하게 되었다.
However, when a thin film is formed with such a metal oxide, the transmittance is decreased according to its thickness, and thus it has a disadvantage that it can not function as a spectacle lens or a mobile phone display. As a result of further studies, it has been found that when the thickness of the thin film is 30 nm or less, preferably 20 nm or less, the antimicrobial activity of the present invention is maintained for a long period of time without affecting the permeability, .
본 발명에 따르면, 안경렌즈, 휴대폰 디스플레이 등과 같은 평판 합성수지 제품의 항균성을 향상시키고, 내스크랫치성도 향상되어 산업상 유용하다.
INDUSTRIAL APPLICABILITY According to the present invention, antimicrobial properties of flat synthetic resin products such as spectacle lenses, mobile phone displays and the like are improved, and scratch resistance is improved, which is industrially useful.
도 1은 산화아연 및 산화칼슘을 1:1로 혼합하여 성막한 경우, 스타필로코쿠스 아우레우수 및 에세리아의 콜라이의 식균상태(도면의 좌측 Blank 표시)와 염색후의 상태(도면의 우측 Sample 표시)를 나타내는 도이다.
도 2는 산화칼슘을 이용하여 성막을 형성한 경우, 스타필로코쿠스 아우레우수 및 에세리아의 콜라이의 식균상태(도면의 좌측 Blank 표시)와 염색후의 상태 (도면의 우측 Sample 표시)를 나타내는 도이다.
도 3은 산화아연을 이용하여 성막을 형성한 경우, 스타필로코쿠스 아우레우수 및 에세리아의 콜라이의 식균상태(도면의 좌측 Blank 표시)와 염색후의 상태 (도면의 우측 Sample 표시)를 나타내는 도이다. Fig. 1 shows the state of staphylococcus aurel and Escherichia coli strains (left blank display in the figure) and the state after dyeing (in the right sample of the drawing) when zinc oxide and calcium oxide were mixed at a ratio of 1: FIG.
Fig. 2 is a graph showing the state of staphylococcus aurel and Escherichia coli (blank display on the left side in the drawing) and the state after staining (on the right side in the drawing) when a film is formed using calcium oxide to be.
FIG. 3 is a graph showing the state of staphylococcus aurel and Escherichia coli in a state of blank (left blank display in the drawing) and a state after staining (right sample display in the drawing) when a film is formed using zinc oxide to be.
본 발명은 다양한 변경을 가할 수 있고 여러 가지 실시예를 가질 수 있는 바, 이하에서는 본 발명의 바람직한 형태의 구조를 예시하고 이에 기하여 본 발명을 상세하게 설명하고자 한다. 그러나 이는 본 발명을 예시된 형태만으로 한정하려는 것이 아니며, 본 발명의 사상 및 기술 범위는 예시된 형태의 통상적인 변경이나 균등물 내지 대체물까지 포함한다.
While the present invention has been described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. It should be understood, however, that there is no intention to limit the invention to the form just described, and the spirit and scope of the present invention encompasses the ordinary variations, equivalents, and alternatives of the illustrated forms.
이하, 본 발명의 실시예를 보인 도면을 참조하여 본 발명을 더욱 상세하게 설명한다.Hereinafter, the present invention will be described in detail with reference to the drawings showing embodiments of the present invention.
본 발명에서 사용하는 금속산화물이란 전술한 바와 같이 산화아연 및 산화칼슘을 의미한다. 산화아연은 아연화라고 불리는 무정형의 백색분말로 밀도 5.47g/㎤인 것과 6방정계 결정으로 밀도 5.78g/㎤인 것이 존재한다. 또한 탄산아연이나 탄산수산화아연을 하소시켜 순수한 산화아연을 얻을 수 있다. 본 발명에서는 시판의 결정형 산화아연을 사용한다. 또한 산화칼슘은 융점이 2572℃로 탄산칼슘을 하소하여 고순도의 것을 얻든가 또는 질산칼슘과 탄산암모늄 용액으로부터 탄산칼슘을 만들고, 이것을 전기로에서 강열하여 아산화탄소탄화칼슘으로 하고, 공기중의 이산화탄소를 흡수하여 탄산칼슘을 얻기도 한다. 본 발명에서는 탄산칼슘을 하소하여 얻은 산화칼슘을 사용하였다. 이러한 산화칼슘은 도기, 의료용으로 이용되고, 토양개량제로서 이용되기도 하나, 합성수지제의 표면의 코팅재료로 사용된 적은 없다. The metal oxide used in the present invention means zinc oxide and calcium oxide as described above. Zinc oxide is an amorphous white powder called zincation, which has a density of 5.47 g / cm 3 and a hexagonal crystal with a density of 5.78 g / cm 3. In addition, pure zinc oxide can be obtained by calcining zinc carbonate or bicarbonate water. In the present invention, commercially available crystalline zinc oxide is used. Further, calcium oxide is calcined at a melting point of 2572 DEG C to obtain high purity calcium carbonate or calcium carbonate from calcium nitrate and ammonium carbonate solution, which is heat treated in an electric furnace to form calcium diboronoxide and absorbs carbon dioxide Calcium carbonate may also be obtained. In the present invention, calcium oxide obtained by calcination of calcium carbonate was used. Such calcium oxide is used for pottery, medical use, and is used as a soil improving agent, but has never been used as a coating material on the surface of a synthetic resin.
이러한 금속산화물을 이용하여 항균층을 형성하는 것은 통상 안경렌즈의 진공증착, 소위 멀티코팅이라고 불리는 방법을 그대로 이용한다. The formation of the antimicrobial layer using such a metal oxide generally uses a method called vacuum deposition of a spectacle lens, so-called multi-coating.
즉, 광학 제품의 표면에서 고굴절물질과 저굴절물질이 교번하여 복수 개의 층을 이룬 멀티코팅층과, 상기 멀티코팅층 상에 적층된 베이스층과, 상기 베이스층 상에 적층된 항균층 및 상기 항균층 상에 적층된 보호층을 포함하는 층간 항균층이 구비된 멀티코팅에 있어서, 상기 항균층을 전술한 산화아연 및/또는 산화칼슘을 이용하여 형성하는 것이다. That is, a multi-coating layer having a plurality of layers alternating high-refractive-index material and low-refractive material on the surface of an optical product, a base layer laminated on the multi-coating layer, an antimicrobial layer laminated on the base layer, In which the antimicrobial layer is formed by using zinc oxide and / or calcium oxide as described above.
이러한 항균층의 두께는 50nm를 초과하면 렌즈나 휴대전화 디스플레이의 투과도가 떨어져 바람직하지 않다. 바람직한 두께는 10~30nm, 더 바람직하기로는 5~20nm이다. If the thickness of the antimicrobial layer exceeds 50 nm, the transmittance of the lens or the cellular phone display is low, which is undesirable. The preferred thickness is 10 to 30 nm, more preferably 5 to 20 nm.
이러한 항균층의 형성은 산화아연 또는 산화칼슘에서 선택된 1종 만을 이용하여 성막하고, 항균성을 살펴보면 양자 모두 항균성을 나타내며, 산화아연과 산화칼슘의 혼합물을 사용하여 성막하여도 항균성을 나타내었다. 본 발명자가 항균시험을 외부에 의뢰한 바, 상기 화합물들을 단독으로 하였을 때보다, 이들을 혼합하여 성막하였을 때, 특히 산화아연과 산화칼슘을 1:1로 혼합한 것을 이용하여 성막하고, 황색 포도상 구균 ATCC 6538p 및 대장균 ATCC 8739로 식균하고 항균시험을 측정한 바, 가장 우수한 항균효과를 나타냈다. These antimicrobial layers were formed using only one selected from zinc oxide or calcium oxide. Both antimicrobial activities exhibited antimicrobial activity, and antimicrobial activity was exhibited even when a mixture of zinc oxide and calcium oxide was used. The inventors of the present invention commissioned an antibacterial test and found out that when the above compounds were mixed and formed into a film by mixing with zinc oxide and calcium oxide in a ratio of 1: ATCC 6538p and Escherichia coli ATCC 8739, and the antibacterial test was carried out.
산화아연과 산화칼슘의 혼합물을 사용할 때, 이들의 비는 7: 3 내지 1:1인 경우가 바람직하다.
When a mixture of zinc oxide and calcium oxide is used, the ratio thereof is preferably from 7: 3 to 1: 1.
실시예 Example
산화아연, 산화칼슘 및 산화아연과 산화칼슘의 1:1 혼합물을 이용하여 20nm의 두께를 갖는 항균층을 형성하였다. A 1: 1 mixture of zinc oxide, calcium oxide, and zinc oxide and calcium oxide was used to form an antimicrobial layer having a thickness of 20 nm.
이러한 항균층이 형성된 렌즈를 하기 시험방법에 따라 항균시험을 측정하였다. The antibacterial layer-formed lens was subjected to the antibacterial test according to the following test method.
시험예Test Example
시험방법Test Methods
하기 조건으로 JIS 2801을 준용하여 시험하였다.The test was conducted in accordance with JIS 2801 under the following conditions.
사용공시균주Used disclosure strain
균주 1: 황색 포도상 구균(Staphylococcus aureus) ATCC 6538p, Strain 1: Staphylococcus aureus ATCC 6538p,
균주 2: 대장균(Escherichia coli) ATCC 8739.Strain 2: Escherichia coli ATCC 8739.
표준 피복필름: Stomacher 400® POLY-BAGStandard Coating Film: Stomacher 400 ® POLY-BAG
시험조건: 시험균액을 35±1℃Test conditions: The test strain was incubated at 35 ± 1 ° C
시료 표면적: 25㎠Sample surface area: 25 cm 2
항균활성치(S): log(Mb/Mc), 감소율 (%): [(Mb-Mc)/Mb]×100Antibacterial hwalseongchi (S): log (M b / M c), reduction ratio (%): [(Mb- Mc) / Mb] × 100
증식치(F): log(Mb/Mc)(1.5 이상)Growth value (F): log (M b / M c ) (1.5 or more)
Ma: 표준시료의 시험균 접종직후의 생균수의 평균(3검체)Ma: Average number of viable cells immediately after inoculation of the test sample of the standard sample (3 samples)
Mb: 표준시료의 일정시간(24시간) 배양 후 생균수의 평균(3검체)Mb: Average number of viable cells (3 samples) after a certain time (24 hours)
Mc: 항균가공시료의 일정시간(24시간) 배향후 생균수의 평균(3검체)
Mc: a certain time (24 hours) of the antimicrobial processed sample The average number of living bacteria in the future (3 samples)
상기 시험방법에 따라 항균시험한 결과, 산화아연:산화칼슘=1:1의 혼합물을 상기 균주를 접증, 증식하였을 때는 항균활성치가 99.9%이었고, 산화아연 단독의 항균층을 형성한 경우는 항균활성치가 99.8%이었으며, 산화칼슘 단독의 항균층을 형성한 경우는 항균활성치가 99.6~99.7%이었다. 이 결과의 성적서 및 접촉시의 사진 및 접종 24시간 후의 염색하였을 때의 생존하는 균의 상태를 촬영한 사진을 각각 도 1, 도 2 및 도 3으로 나타낸다.
As a result of the antibacterial test according to the above test method, the antibacterial activity value was 99.9% when the strain of zinc oxide: calcium oxide = 1: 1 was confined and proliferated, and when the antimicrobial layer of zinc oxide alone was formed, 99.8% and 99.6 ~ 99.7%, respectively, when the antibacterial layer of calcium oxide alone was formed. The results of the test and photographs taken at the time of contact and photographs of the state of the surviving bacteria when stained 24 hours after inoculation are shown in Fig. 1, Fig. 2 and Fig. 3, respectively.
시험 결과 (1)Test results (1)
산화아연:산화칼슘=1:1의 혼합물을 이용하여 항균층을 형성한 후, 그 위에 상기 균주를 접증, 증식하였을 때의 항균활성 시험 결과An antimicrobial layer was formed using a mixture of zinc oxide: calcium oxide = 1: 1, and the antimicrobial activity test result
주, 1) < = 미만, 2) CFU= Colony Forming Unit
Note 1) Less than <=, 2) CFU = Colony Forming Unit
시험 결과 (2)Test results (2)
산화칼슘 만을 이용하여 항균층을 형성한 후, 그 위에 상기 균주를 접증, 증식하였을 때의 항균활성 시험 결과After the antimicrobial layer was formed using only calcium oxide, the antimicrobial activity test result when the strain was folded and proliferated was observed
주 1) < = 미만, 2) CFU= Colony Forming Unit
Note 1) Less than <=, 2) CFU = Colony Forming Unit
시험 결과 (3)Test results (3)
산화아연 만을 이용하여 항균층을 형성한 후, 그 위에 상기 균주를 접증, 증식하였을 때의 항균활성 시험 결과After forming an antimicrobial layer using only zinc oxide, the antimicrobial activity test result when the strain was folded and propagated
주 1) < = 미만, 2) CFU= Colony Forming Unit
Note 1) Less than <=, 2) CFU = Colony Forming Unit
상기 결과로부터 산화아연 및 산화칼슘으로 이루어진 군에서 선택된 1종 또는 2종으로 항균층을 형성한 경우, 항균활성이 99.6~99.9% 감소함을 알 수 있다.
From the above results, it can be seen that when the antimicrobial layer is formed of one or two selected from the group consisting of zinc oxide and calcium oxide, the antibacterial activity is reduced by 99.6 to 99.9%.
Claims (5)
An antimicrobial layer composed of a metal oxide formed by vacuum deposition using one or two selected from the group consisting of zinc oxide and calcium oxide on the surface of a synthetic resin
상기 항균층이 산화아연 및 산화칼슘으로 이루어진 군에서 선택된 1종 또는 2종을 이용하여 진공 증착 형성된 금속산화물로 이루어진 항균층.
A multi-coating layer having a plurality of layers alternating high-refractive-index material and low-refractive material on the surface of the optical product; a base layer laminated on the multi-coating layer; an antimicrobial layer laminated on the base layer; In a multi-coating comprising an interlaminar anti-microbial layer comprising a protective layer,
Wherein the antimicrobial layer comprises a metal oxide formed by vacuum deposition using one or two selected from the group consisting of zinc oxide and calcium oxide.
The antimicrobial layer according to claim 1 or 2, wherein the antimicrobial layer is a mixture of zinc oxide and calcium oxide.
The antimicrobial layer according to claim 3, wherein the antimicrobial layer comprises a metal oxide formed by vacuum deposition using a mixture of zinc oxide and calcium oxide in a mixing ratio of 7: 3 to 5: 5.
The antibacterial layer according to claim 1 or 2, wherein the antimicrobial layer comprises a metal oxide having a thickness of 5 to 20 nm.
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| KR101939382B1 (en) | 2017-02-15 | 2019-01-16 | 충남대학교산학협력단 | Method for Antimicrobial Treatment Using Zinc Aluminate |
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| JP2023521612A (en) | 2020-04-09 | 2023-05-25 | エシロール アンテルナショナル | Optical article with antibacterial function |
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