KR20010094136A - A process for the preparation of polycarbonate transparent plane with improved abrasion resistance - Google Patents
A process for the preparation of polycarbonate transparent plane with improved abrasion resistanceInfo
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- KR20010094136A KR20010094136A KR1020000017612A KR20000017612A KR20010094136A KR 20010094136 A KR20010094136 A KR 20010094136A KR 1020000017612 A KR1020000017612 A KR 1020000017612A KR 20000017612 A KR20000017612 A KR 20000017612A KR 20010094136 A KR20010094136 A KR 20010094136A
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- hmdso
- plasma
- thin film
- feed speed
- oxygen
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
- B29C59/14—Surface shaping of articles, e.g. embossing; Apparatus therefor by plasma treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2069/00—Use of PC, i.e. polycarbonates or derivatives thereof, as moulding material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
- B29K2995/0018—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds having particular optical properties, e.g. fluorescent or phosphorescent
- B29K2995/0026—Transparent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2007/00—Flat articles, e.g. films or sheets
- B29L2007/002—Panels; Plates; Sheets
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- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Laminated Bodies (AREA)
- Coating Of Shaped Articles Made Of Macromolecular Substances (AREA)
- Polyesters Or Polycarbonates (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
Description
본 발명은 내마모성이 향상된 폴리카보네이트 투명판의 제조방법에 관한 것이다. 더욱 상세하게는 플라즈마 발생장치와 헥사메틸다이실록산(HMDSO : hexamethyl disiloxane), 산소, 아르곤가스를 이용하여 폴리카보네이트 표면에 내마모막을 형성하며, 이때 생성되는 박막이 플라즈마 내의 이온과 충돌할 수 있도록 폴리카보네이트 투명판을 플라즈마 발생장치와 연결된 전극 위에 놓고 처리하는 것을 특징으로 하는 내마모성이 향상된 폴리카보네이트 투명판을 제조하는 방법에 관한 것이다.The present invention relates to a method for producing a polycarbonate transparent plate with improved wear resistance. More specifically, a wear resistant film is formed on the surface of the polycarbonate using a plasma generator, hexamethyl disiloxane (HMDSO), oxygen, and argon gas, and the thin film is formed so that the thin film can collide with the ions in the plasma. The present invention relates to a method for producing a polycarbonate transparent plate having improved wear resistance, characterized in that the carbonate transparent plate placed on the electrode connected to the plasma generator.
폴리카보네이트 수지는 우수한 기계적, 화학적 특성을 가지고 있어 다양한 분야에 범용적으로 사용되고 있다. 특히 유리에 비해 적은 중량과 높은 투명성, 강한 내충격성을 가지고 있어 유리 소재를 대체하여 자동차 전조등, 투명 방음벽 등에 많이 사용되고 있다. 그러나 유리에 비해 마모가 쉽게 발생하여 응용 범위가 제한된다. 이와 같은 폴리카보네이트의 낮은 내마모성 문제를 극복하기 위하여 다양한 방법들이 고안되고 연구되고 있다. 일례로, 폴리카보네이트 수지 위에 유기물이나 무기물을 코팅하여 내마모성을 증대시키는 방법이 있다.Polycarbonate resins have excellent mechanical and chemical properties and are widely used in various fields. In particular, it has a low weight, high transparency, and strong impact resistance compared to glass, so it is widely used in automobile headlights and transparent soundproof walls in place of glass materials. However, wear occurs more easily than glass, which limits the scope of application. Various methods have been devised and studied to overcome the problem of low wear resistance of such polycarbonate. For example, there is a method of increasing the wear resistance by coating an organic material or an inorganic material on a polycarbonate resin.
범용적으로 많이 사용되는 방법은 폴리카보네이트 수지 위에 가교화 될 수 있는 유기물을 코팅한 후 열 또는 자외선에 의해 가교화하여 내마모성을 향상시키고 있으나, 내마모성의 향상이 유리에 비해 매우 나빠 유리를 대체할 수 있는 분야가 매우 한정된다.The widely used method is to improve the wear resistance by coating the organic material which can be crosslinked on the polycarbonate resin and then crosslinking by heat or ultraviolet rays, but the wear resistance is very poor compared to the glass, which can replace the glass. There is a very limited field.
폴리카보네이트 수지의 내마모성을 더욱 향상시키기 위하여 진공에서 플라즈마를 이용하여 내마모성 박막을 제조하는 방법이 활발히 연구되고 있다. 이러한 예가 미국 특허 제 5,320,875호에 게재되어 있다. 이 특허에서는 전력 밀도(Power density)가 106~108J/kg에서 실리콘, 산소, 탄소 그리고 수소로 이루어진 고분자 코팅을 폴리카보네이트 수지 위에 플라즈마 중합시켜서 제조하고 있다. 이 특허에서 기술한 방법으로 폴리카보네이트 수지 위에 고분자 코팅을 제조할 경우, 장치에 공급되는 가스의 분압이 변화되어도 같은 전력 밀도을 가질 수 있게 되어 단순히 전력밀도 값으로만 제조 조건을 설정했기 때문에 투입한 가스와 단량체 공급량에 대해 동일한 특성의 고분자 코팅을 제조하기 힘들다는 문제점이 있으며, 또한 얻어지는 내마모성도 유기물 코팅에 비해 높지만 유리에 비하면 여전히 낮은 값을 나타낸다.In order to further improve the wear resistance of polycarbonate resins, a method of manufacturing a wear resistant thin film using plasma in a vacuum has been actively studied. Such an example is disclosed in US Pat. No. 5,320,875. In this patent, a polymer coating made of silicon, oxygen, carbon and hydrogen is plasma polymerized on a polycarbonate resin at a power density of 10 6 to 10 8 J / kg. When manufacturing a polymer coating on a polycarbonate resin by the method described in this patent, even if the partial pressure of the gas supplied to the device is changed, the same power density can be obtained, and the gas is simply added because the manufacturing conditions are set only at the power density value. There is a problem in that it is difficult to prepare a polymer coating of the same properties for the monomer and the amount supplied, and the wear resistance obtained is also higher than that of the organic coating, but still shows a low value compared to the glass.
폴리카보네이트 수지의 내마모성을 유리 수준으로 향상시키기 위하여 플라즈마 발생 방식을 조절하여 수지 위에 제조되는 내마모성 박막의 특성을 조절하는연구가 진행되고 있다. 그 예가 미국 특허 제 5,618,619호에 게재되어 있다. 이 특허에서는 실리콘, 산소, 탄소 그리고 수소로 이루어진 내마모성 박막을 폴리카보네이트 수지 위에 플라즈마 중합으로 제조할 때, 플라즈마 발생장치와 연결된 전극 위에 폴리카보네이트 수지를 위치시켜서 플라즈마 내에서 발생하는 이온들이 증착되는 내마모성 박막에 충돌하도록 함으로써 내마모성이 유리와 유사한 박막을 제조하는 것을 특징으로 하고 있고, 또한 이렇게 만들어지는 내마모성 박막은 나노인덴테이션(nanoindentation) 경도가 2 내지 5 기가파스칼(GPa)범위, 마이크로 클랙킹(microcracking)이 발생하는 신율은 2 내지 3% 를 갖는 것을 특징으로 한다.In order to improve the abrasion resistance of the polycarbonate resin to the glass level, a study for adjusting the characteristics of the wear-resistant thin film prepared on the resin by adjusting the plasma generation method is in progress. An example is disclosed in US Pat. No. 5,618,619. In this patent, when a wear resistant thin film made of silicon, oxygen, carbon, and hydrogen is prepared by plasma polymerization on a polycarbonate resin, the wear resistant thin film is deposited by placing polycarbonate resin on an electrode connected to a plasma generator to deposit ions generated in the plasma. It is characterized by producing a thin film similar to wear resistance by impinging on the wear resistant thin film. The wear resistant thin film thus produced has a nanoindentation hardness in the range of 2 to 5 gigapascals (GPa) and microcracking. ) Elongation is generated is characterized by having 2 to 3%.
이 특허에서 기술한 방법에서는 내마모성 박막 제조에 필요한 인자인 단량체 공급속도, 산소의 공급속도, 사용되는 전력 밀도에 대한 연구가 되어 있지 않아 박리현상이나 크랙이 발생하지 않는 내마모 코팅 조건을 얻기 힘든 단점이 있다.In the method described in this patent, it is difficult to obtain abrasion-resistant coating conditions that do not cause peeling or cracking because there is no study on the monomer supply rate, oxygen supply rate, and power density used for manufacturing the wear resistant thin film. There is this.
본 발명은 상술한 문제들의 해결을 위한 것으로, 폴리카보네이트 표면 위에 내마모성 박막을 제조할 때 내마모성 박막의 특성을 결정하는 다양한 인자의 범위를 조절하는 것에 의해 박리나 크랙(crack)이 발생하지 않는 내마모성 박막을 제조하는 것을 과제로 한다.The present invention is to solve the above-mentioned problems, wear-resistant thin film that does not occur peeling or crack (crack) by adjusting the range of various factors that determine the characteristics of the wear-resistant thin film when manufacturing the wear-resistant thin film on the polycarbonate surface Let it be a subject to manufacture.
본 발명은 내마모성이 향상된 폴리카보네이트 투명판의 제조방법을 제공하는 것을 그 목적으로 한다.It is an object of the present invention to provide a method for producing a polycarbonate transparent plate having improved wear resistance.
본 발명은 폴리카보네이트 표면을 플라즈마 처리함에 있어서, 폴리카보네이트 수지를 플라즈마 발생장치와 연결된 전극 위에 위치시키고 헥사메틸다이실록산(HMDSO)과 아르곤의 혼합 가스와 산소를 투입하여 플라즈마 도움 화학 증착법으로 내마모막을 형성하되 이때 공급되는 에너지와 헥사메틸다이실록산의 공급속도는 전력밀도(W/FM)가 107내지 109(J/Kg)의 범위를 가지는 범위를 갖고, 산소의 투입량은 헥사메틸다이실록산(HMDSO)의 공급속도의 12 내지 18배의 범위를 갖게 하고, 아르곤 가스의 공급속도는 헥사메틸다이실록산(HMDSO) 공급속도의 0.1 내지 2배 범위로 실시함으로써 상기 목적을 달성하게 된다.In the present invention, in the plasma treatment of the surface of the polycarbonate, the polycarbonate resin is placed on an electrode connected to the plasma generator, and a mixed gas of hexamethyldisiloxane (HMDSO) and argon and oxygen are added to the wear-resistant film by plasma assisted chemical vapor deposition. At this time, the energy supplied and the supply rate of hexamethyldisiloxane have a range in which the power density (W / FM) is in the range of 10 7 to 10 9 (J / Kg), and the amount of oxygen is hexamethyldisiloxane ( The above object is achieved by making the feed rate of HMDSO) range from 12 to 18 times and the feed rate of argon gas from 0.1 to 2 times the hexamethyldisiloxane (HMDSO) feed rate.
이하, 본 발명을 더욱 상세히 설명한다.Hereinafter, the present invention will be described in more detail.
플라스틱 중에서도 내충격성이 가장 우수하고 투명성에서도 우수한 폴리카보네이트가 유리를 대체하여 사용되기 위해서는 무엇보다도 내마모성을 향상시켜야 한다.Among the plastics, polycarbonate, which has the highest impact resistance and excellent transparency, needs to improve wear resistance, among other things, in order to replace glass.
내마모성을 향상시키기 위해 본 발명에서는 폴리카보네이트 표면 위에 플라즈마 도움 화학 증착법으로 헥사메틸다이실록산(HMDSO)을 원료로 하는 내마모막을 입히는 방법을 사용한다.In order to improve the wear resistance, the present invention uses a method of coating a wear resistant film made of hexamethyldisiloxane (HMDSO) on the polycarbonate surface by plasma assisted chemical vapor deposition.
구체적으로, 폴리카보네이트 표면에 직접 플라즈마 도움 화학 증착법으로 헥사메틸다이실록산(HMDSO)을 원료로 하는 내마모막을 입히는 방법은 진공상태에서 플라즈마 발생 장치와 연결된 전극 위에 위치한 폴리카보네이트 기판 주변에 플라즈마를 형성한 후 헥사메틸다이실록산(HMDSO)과 산소가스를 투입하면 플라즈마의 에너지에 의해 분해되고 폴리카보네이트 투명판에 SiO2와 유사한 성분의 물질이 증착된다. 그와 동시에 플라즈마 발생장치와 연결된 전극에 의해 발생하는 전압 강하(Self-Bias)에 의해 플라즈마 내의 이온들이 막과 충돌하여 내마모성이 우수한 박막이 생성된다.Specifically, a method of coating a wear resistant film made of hexamethyldisiloxane (HMDSO) as a raw material by plasma assisted chemical vapor deposition on a polycarbonate surface is to form a plasma around a polycarbonate substrate located on an electrode connected to a plasma generator in a vacuum state. Then, when hexamethyldisiloxane (HMDSO) and oxygen gas are added, it is decomposed by the energy of plasma and a material of SiO 2 similar component is deposited on the polycarbonate transparent plate. At the same time, ions in the plasma collide with the film due to the voltage drop generated by the electrode connected to the plasma generator to produce a thin film having excellent wear resistance.
이때 사용되는 에너지와 헥사메틸다이실록산(HMDSO)의 공급속도의 비율, 산소가스 공급속도에 의해 막의 성분이 변하게 되어 박막의 특성이 크게 바뀌게 된다. 내마모성 박막 제조에 사용되는 에너지와 헥사메틸다이실록산(HMDSO)의 공급속도의 비율은 전력 밀도 (W/FM)로 정의할수 있다. 여기서 W는 플라즈마 발생기에서 공급하는 전력(W=J/sec), F는 헥사메틸다이실록산(HMDSO)의 공급 속도(mol/sec)그리고 M은 헥사메틸다이실록산(HMDSO)의 분자량(0.1624 Kg/mol)이다.At this time, the composition of the membrane is changed by the ratio of the energy used, the supply rate of hexamethyldisiloxane (HMDSO), and the oxygen gas supply rate, thereby greatly changing the characteristics of the thin film. The ratio of the energy used to manufacture the wear resistant thin film to the supply rate of hexamethyldisiloxane (HMDSO) can be defined as the power density (W / FM). Where W is the power supplied by the plasma generator (W = J / sec), F is the supply rate of hexamethyldisiloxane (HMDSO) (mol / sec) and M is the molecular weight of hexamethyldisiloxane (HMDSO) (0.1624 Kg / mol).
내마모성 박막 제조에 적당한 전력 밀도는 107내지 109J/kg이며, 만일 107J/kg 이하의 전력 밀도에서는 박막이 불투명하게 생성되고 109J/Kg 에서는 막에 박리가 발생하므로 상기 범위로 하는 것이 바람직하다.Suitable power density for the wear-resistant thin film is 10 7 to 10 9 J / kg, if the power density of 10 7 J / kg or less thin film is formed opaque and at 10 9 J / Kg film peeling occurs in the above range It is desirable to.
증착되는 물질의 성질 및 색상을 조절하기 위해 산소를 투입한다. 산소가 투입되면 생성되는 막의 색상이 투명해지지만 투입되는 양이 더 증가되면 박막에 크랙(crack) 및 박리가 발생하는 원인이 된다. 내마모성 박막 제조에 적당한 산소 공급속도는 헥사메틸다이실록산(HMDSO)의 공급 속도(mol/sec)의 12 내지 18배 정도이다.Oxygen is added to control the nature and color of the deposited material. When oxygen is added, the color of the formed film becomes transparent, but when the amount of the added film is further increased, cracks and peeling occur in the thin film. Suitable oxygen feed rates for the production of wear resistant thin films are on the order of 12 to 18 times the feed rate of hexamethyldisiloxane (HMDSO) (mol / sec).
플라즈마의 안정성을 향상시키기 위해 헥사메틸다이실록산(HMDSO) 기체와 아르곤 가스를 혼합하여 투입할 수 있다. 그러나, 너무 많은 양의 아르곤 가스를 공급하면 헥사메틸다이실록산(HMDSO)의 분압을 떨어뜨려 증착속도를 감소시킨다. 내마모성 박막 제조에 적당한 아르곤 가스의 공급속도는 헥사메틸다이실록산(HMDSO)의 공급 속도(mol/sec)의 0.1 내지 2배 정도이다.In order to improve the stability of the plasma, hexamethyldisiloxane (HMDSO) gas and argon gas may be mixed and added. However, supplying too much argon gas lowers the partial pressure of hexamethyldisiloxane (HMDSO) to reduce the deposition rate. The supply rate of argon gas suitable for the wear resistant thin film is about 0.1 to 2 times the supply rate of hexamethyldisiloxane (HMDSO) (mol / sec).
상기 본 발명에 따른 내마모성이 향상된 폴리카보네이트 투명판의 제조방법에서, 폴리카보네이트 투명판의 표면을 세척하는데 사용하는 유기 용제는 폴리카보네이트가 녹지 않는, 예를 들면 에탄올이나 메탄올을 선택하여 사용할 수 있다.In the method for producing a polycarbonate transparent plate having improved wear resistance according to the present invention, the organic solvent used to clean the surface of the polycarbonate transparent plate may be selected, for example, ethanol or methanol in which the polycarbonate is not dissolved.
이하, 본 발명을 다음의 실시예를 들어 보다 구체적으로 설명하면 다음과 같다.Hereinafter, the present invention will be described in more detail with reference to the following examples.
실시예 1Example 1
표면이 매끄러운 폴리카보네이트 투명판을 준비하고 표면을 에탄올로 깨끗이 닦았다. 전극이 설치된 진공 챔버에 폴리카보네이트 투명판을 플라즈마 발생 장치와 연결된 전극 위에 설치하고 배기하여 챔버내 압력을 2.5 X 10-2토르(torr)로 낮추었다. 챔버에 산소 가스를 100sccm(7.44 X 10-5mol/sec) 을 투입하면서 전극에 50W의 RF 전압을 걸어 플라즈마를 형성하였다.A smooth polycarbonate transparent plate was prepared and the surface was cleaned with ethanol. The polycarbonate transparent plate was installed on the electrode connected to the plasma generator in the vacuum chamber in which the electrode was installed and exhausted to lower the pressure in the chamber to 2.5 × 10 −2 Torr. 100 sccm (7.44 × 10 −5 mol / sec) of oxygen gas was introduced into the chamber to form a plasma by applying an RF voltage of 50 W to the electrode.
플라즈마가 형성된 챔버에 액상인 헥사메틸다이실록산(HMDSO)을 3.6g/hr(6.16 X 10-6mol/sec) 속도로 공급하여 기화시킨후, 아르곤 가스를 10sccm(7.44 X 10-6mol/sec)의 속도로 투입해 폴리카보네이트 투명판 위에 내마모막을 40분간 증착시켰다. 증착시 챔버의 압력은 6 X 10-1토르(torr)로 유지하였다. 본 실험의 전력밀도(W/FM)를 구하면After supplying liquid hexamethyldisiloxane (HMDSO) at a rate of 3.6 g / hr (6.16 X 10 -6 mol / sec) to the chamber in which the plasma was formed, the gas was evaporated, followed by argon gas (10 sccm (7.44 X 10 -6 mol / sec). The wear resistant film was deposited for 40 minutes on a polycarbonate transparent plate at a rate of). During deposition, the pressure in the chamber was maintained at 6 × 10 −1 Torr. If we find the power density (W / FM) of this experiment
W/FM = 50(W=J/sec) /(6.16 X 10-6mol/sec X 0.1624 Kg/mol)W / FM = 50 (W = J / sec) / (6.16 X 10 -6 mol / sec X 0.1624 Kg / mol)
= 5 X 107J/sec 이다.= 5 X 10 7 J / sec.
전압을 끄고 기체 투입을 중단한 후 공기를 챔버에 불어넣어 압력을 대기상태로 높인 후 내마모막이 증착된 폴리카보네이트 투명판을 꺼내었다. 제조된 내마모 폴리카보네이트는 투명하고 박리가 발생하지 않았다.After the voltage was turned off and the gas was stopped, air was blown into the chamber to raise the pressure to the atmospheric state, and the polycarbonate transparent plate on which the wear-resistant film was deposited was taken out. The wear resistant polycarbonates produced were transparent and no delamination occurred.
이에 대한 물성을 표 1에 나타내었다.The physical properties thereof are shown in Table 1.
실시예 2Example 2
표면이 매끄러운 폴리카보네이트 투명판을 준비하고 표면을 에탄올로 깨끗이 닦았다. 전극이 설치된 진공 챔버에 폴리카보네이트 투명판을 플라즈마 발생장치와 연결된 전극 위에 설치하고 배기하여 챔버내 압력을 2.5 X 10-2토르(torr)로 낮추었다. 챔버에 산소 가스를 68sccm(5.06 X 10-5mol/sec)을 투입하면서 전극에 150W의 RF 전압을 걸어 플라즈마를 형성하였다.A smooth polycarbonate transparent plate was prepared and the surface was cleaned with ethanol. The polycarbonate transparent plate was installed on the electrode connected to the plasma generator in the vacuum chamber in which the electrode was installed and exhausted to lower the pressure in the chamber to 2.5 × 10 −2 Torr. 68 sccm (5.06 X 10 -5 mol / sec) of oxygen gas was introduced into the chamber to form a plasma by applying an RF voltage of 150 W to the electrode.
플라즈마가 형성된 챔버에 헥사메틸다이실록산(HMDSO)을 3.6g/hr(6.16 X 10-6mol/sec) 속도로 공급하여 기화시킨 후, 아르곤 가스를 10sccm(7.44 X 10-6mol/sec)의 속도로 투입해 폴리카보네이트 투명판 위에 내마모막을 40분간 증착시켰다. 증착시 챔버의 압력은 6 X 10-1토르(torr)로 유지하였다. 전압을 끄고 기체투입을 중단한 후 공기를 챔버에 불어넣어 압력을 대기상태로 높인 후 내마모막이 증착된 폴리카보네이트 투명판을 꺼내었다. 제조된 내마모 폴리카보네이트는 투명하고 박리가 발생하지 않았다. 본 실험에서 사용한 전력밀도(W/FM)은 1.5 X 108J/sec 이다.Hexamethyldisiloxane (HMDSO) was supplied to the chamber where the plasma was formed at a rate of 3.6 g / hr (6.16 X 10 -6 mol / sec) to vaporize, followed by argon gas at 10 sccm (7.44 X 10 -6 mol / sec). Abrasion resistant film was deposited for 40 minutes on a polycarbonate transparent plate at a speed. During deposition, the pressure in the chamber was maintained at 6 × 10 −1 Torr. After turning off the voltage and stopping the gas injection, the air was blown into the chamber to raise the pressure to atmospheric state, and then the polycarbonate transparent plate on which the wear-resistant film was deposited was taken out. The wear resistant polycarbonates produced were transparent and no delamination occurred. The power density (W / FM) used in this experiment is 1.5 X 10 8 J / sec.
이에 대한 물성을 표 1에 나타내었다.The physical properties thereof are shown in Table 1.
비교예 1Comparative Example 1
표면이 매끄러운 폴리카보네이트 투명판을 준비하고 표면을 에탄올로 깨끗이 닦았다. 전극이 설치된 진공 챔버에 폴리카보네이트 투명판을 접지된 전극 위에 설치하고 배기하여 챔버내 압력을 2.5 X 10-2토르(torr)로 낮추었다. 챔버에 산소 가스를 100sccm(7.44 X 10-5mol/sec)을 투입하면서 전극에 400W의 RF 전압을 걸어 플라즈마를 형성하였다.A smooth polycarbonate transparent plate was prepared and the surface was cleaned with ethanol. The polycarbonate transparent plate was installed on the grounded electrode and evacuated in the vacuum chamber where the electrode was installed to lower the pressure in the chamber to 2.5 × 10 −2 torr. 100 sccm (7.44 × 10 −5 mol / sec) of oxygen gas was introduced into the chamber to form a plasma by applying an RF voltage of 400 W to the electrode.
플라즈마가 형성된 챔버에 헥사메틸다이실록산(HMDSO)을 2.4g/hr(4.11 X 10-6mol/sec) 속도로 공급하여 기화시킨 후, 아르곤 가스를 10sccm(7.44 X 10-6mol/sec)의 속도로 투입하여 폴리카보네이트 투명판 위에 내마모막을 40분간 증착시켰다. 증착시 챔버의 압력은 6 X 10-1토르(torr)로 유지하였다. 전압을 끄고 기체 투입을 중단한 후 공기를 챔버에 불어넣어 압력을 대기상태로 높인 후 내마모막이 증착된 폴리카보네이트 투명판을 꺼낸다. 제조된 내마모박막은 투명하지만표면에 많은 크랙이 발생하고 박리되는 것을 확인 할 수 있었다. 본 실험에서 사용한 전력밀도(W/FM)은 6 X 108J/sec 이다.Hexamethyldisiloxane (HMDSO) was supplied at a rate of 2.4 g / hr (4.11 X 10 -6 mol / sec) to the chamber where the plasma was formed, followed by vaporization, and then argon gas was added at 10 sccm (7.44 X 10 -6 mol / sec). Abrasion resistant film was deposited for 40 minutes on a polycarbonate transparent plate at a speed. During deposition, the pressure in the chamber was maintained at 6 × 10 −1 Torr. After the voltage was turned off and the gas was stopped, air was blown into the chamber to raise the pressure to atmospheric state, and the polycarbonate transparent plate on which the wear-resistant film was deposited was taken out. The wear-resistant thin film produced was transparent but many cracks were generated on the surface and it could be confirmed that it was peeled off. The power density (W / FM) used in this experiment is 6 X 10 8 J / sec.
이에 대한 물성을 표 1에 나타내었다.The physical properties thereof are shown in Table 1.
비교예 2Comparative Example 2
표면이 매끄러운 폴리카보네이트 투명판을 준비하고 표면을 에탄올로 깨끗이 닦았다. 전극이 설치된 진공 챔버에 폴리카보네이트 투명판을 접지된 전극 위에 설치하고 배기하여 챔버내 압력을 2.5 X 10-2토르(torr)로 낮추었다. 챔버에 산소 가스를 4 sccm(2.98 X 10-6mol/sec)을 투입하면서 전극에 400W의 RF 전압을 걸어 플라즈마를 형성하였다.A smooth polycarbonate transparent plate was prepared and the surface was cleaned with ethanol. The polycarbonate transparent plate was installed on the grounded electrode and evacuated in the vacuum chamber where the electrode was installed to lower the pressure in the chamber to 2.5 × 10 −2 torr. 4 sccm (2.98 × 10 −6 mol / sec) of oxygen gas was introduced into the chamber to form a plasma by applying an RF voltage of 400 W to the electrode.
플라즈마가 형성된 챔버에 헥사메틸다이실록산(HMDSO)을 2.4g/hr (4.11 X 10-6mol/sec) 속도로 공급하여 기화시킨 후, 아르곤 가스를 10sccm(7.44 X 10-6mol/sec)의 속도로 투입하여 폴리카보네이트 투명판 위에 내마모막을 40분간 증착시켰다. 증착시 챔버의 압력은 6 X 10-1토르(torr)로 유지하였다. 전압을 끄고 기체 투입을 중단한 후 공기를 챔버에 불어넣어 압력을 대기상태로 높인 후 내마모막이 증착된 폴리카보네이트 투명판을 꺼내었다. 제조된 내마모 박막은 뿌옇게 변해 투명도가 떨어지는 것을 확인 할 수 있었다. 본 실험에서 사용한 전력밀도(W/FM)은 6 X 108J/sec 이다.After supplying hexamethyldisiloxane (HMDSO) at a rate of 2.4 g / hr (4.11 X 10 -6 mol / sec) to the chamber in which the plasma was formed, the gas was evaporated, followed by argon gas of 10 sccm (7.44 X 10 -6 mol / sec). Abrasion resistant film was deposited for 40 minutes on a polycarbonate transparent plate at a speed. During deposition, the pressure in the chamber was maintained at 6 × 10 −1 Torr. After the voltage was turned off and the gas was stopped, air was blown into the chamber to raise the pressure to the atmospheric state, and the polycarbonate transparent plate on which the wear-resistant film was deposited was taken out. The produced wear-resistant thin film turned cloudy and could be confirmed that the transparency is poor. The power density (W / FM) used in this experiment is 6 X 10 8 J / sec.
이에 대한 물성을 표 1에 나타내었다.The physical properties thereof are shown in Table 1.
※ 내마모성 : ASTM D1044- 테이모 마모 시험과 ASTM D1003 헤이즈 (Haze) 측정법에 의거 측정하였다. (테이버 회전수:500회, 하중:500그램(g))※ Wear resistance: It measured according to ASTM D1044-Taemo abrasion test and ASTM D1003 Haze measurement method. (Tape rotation number: 500 times, load: 500 grams (g))
이와 같이 본 발명에 따른 제조된 내마모 폴리카보네이트 투명판은 투명하고 유리와 유사한 내마모성을 보유하면서 깨지기 않아 많은 분야에서에서 유리를 대체할 수 있다.As such, the wear-resistant polycarbonate transparent plate prepared according to the present invention is transparent and retains abrasion resistance similar to glass, and thus can be replaced in many fields.
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