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WO2016132562A1 - Film hydrofuge à haute dureté, moule et procédé de fabrication de film hydrofuge à haute dureté - Google Patents

Film hydrofuge à haute dureté, moule et procédé de fabrication de film hydrofuge à haute dureté Download PDF

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Publication number
WO2016132562A1
WO2016132562A1 PCT/JP2015/055309 JP2015055309W WO2016132562A1 WO 2016132562 A1 WO2016132562 A1 WO 2016132562A1 JP 2015055309 W JP2015055309 W JP 2015055309W WO 2016132562 A1 WO2016132562 A1 WO 2016132562A1
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Prior art keywords
film
fluorine
dlc film
mold
water
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Ceased
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PCT/JP2015/055309
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English (en)
Japanese (ja)
Inventor
本多　祐二
浩平 奥平
阿部　浩二
有希子 遠藤
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Youtec Co Ltd
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Youtec Co Ltd
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Priority to PCT/JP2015/055309 priority Critical patent/WO2016132562A1/fr
Priority to JP2017500268A priority patent/JP6653816B2/ja
Priority to TW105102705A priority patent/TWI699447B/zh
Publication of WO2016132562A1 publication Critical patent/WO2016132562A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C23C16/27—Diamond only
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30

Definitions

  • the present invention relates to a water repellent high hardness film having a fluorine-containing DLC (Diamond Like Carbon) film, a mold, and a method for producing a water repellent high hardness film.
  • a fluorine-containing DLC Diamond Like Carbon
  • a resin softened by heating is pressed into a mold by applying an injection pressure, and the mold is filled and molded.
  • resin seizure may occur in a part 102 of the mold 101.
  • the seized resin must be cleaned, which requires a lot of time and labor for cleaning, and the life of the mold is shortened. Therefore, it is conceivable to form a high-hardness DLC film on the surface of the mold as a method for suppressing the seizure of the resin.
  • the water contact angle of the conventional DLC film is about 60 ° to 72 °, if a resin having high adhesiveness (for example, acrylic resin, polyacetic acid resin, phenol resin, etc.) is used as the molding resin, the mold It is not possible to sufficiently suppress the seizure of the resin in the part 102 of the resin. Further, the conventional DLC film does not have a DLC film having a large water contact angle and high hardness in order to suppress the seizure of the resin and make the mold difficult to be scratched.
  • a resin having high adhesiveness for example, acrylic resin, polyacetic acid resin, phenol resin, etc.
  • One embodiment of the present invention is to manufacture a water-repellent high-hardness film having a water contact angle of 80 ° or more and high hardness, or a mold having the water-repellent high-hardness film formed on the surface or a water-repellent high-hardness film. It is an object to provide a method.
  • a fluorine-containing DLC film containing 3 atomic% or more of fluorine has a water contact angle of 80 ° or more and a Knoop hardness of 1050 Hk or more.
  • the upper limit content of fluorine in the fluorine-containing DLC film is preferably 17 atomic percent or less, and more preferably 10 atomic percent or less.
  • an amorphous carbon film containing carbon, hydrogen, silicon, and nitrogen [2] an amorphous carbon film containing carbon, hydrogen, silicon, and nitrogen; A DLC film formed on the amorphous carbon film; A laminated film having a fluorine-containing DLC film containing 3 atomic% or more of fluorine formed on the DLC film;
  • the fluorine-containing DLC film has a water contact angle of 80 ° or more (preferably 90 ° or more) and a Knoop hardness of 1050 Hk or more.
  • the upper limit content of fluorine in the fluorine-containing DLC film is preferably 17 atomic percent or less, and more preferably 10 atomic percent or less.
  • a water repellent high hardness film characterized in that a film thickness ratio of the amorphous carbon film, the DLC film, and the fluorine-containing DLC film satisfies the following formula 1.
  • (Amorphous carbon film): (DLC film): (Fluorine-containing DLC film) (2.5 to 7.5): (1.5 to 4.5): (1 to 3)
  • Formula 2 [4]
  • the fluorine-containing DLC film is a film formed by a plasma CVD method using a raw material gas having a hydrocarbon-based gas and a fluorocarbon-based gas and a high-frequency power having a frequency of 10 to 500 kHz.
  • the DLC film is a water-repellent high-hardness film characterized by being formed by a plasma CVD method using a source gas having a hydrocarbon gas and a high-frequency power having a frequency of 10 to 500 kHz.
  • the water-repellent high hardness film, wherein the fluorine-containing DLC film is formed on the surface of a mold.
  • the amorphous carbon film is formed on the surface of a mold.
  • the mold is made of die steel or high-speed steel.
  • a mold in which a fluorine-containing DLC film containing 3 atomic% or more of fluorine is formed on the surface The fluorine-containing DLC film has a water contact angle of 80 ° or more, and a Knoop hardness is equal to or higher than the Knoop hardness of the mold.
  • the upper limit content of fluorine in the fluorine-containing DLC film is preferably 17 atomic percent or less, and more preferably 10 atomic percent or less.
  • a mold having a laminated film formed on the surface, The laminated film includes an amorphous carbon film containing carbon, hydrogen, silicon, and nitrogen, a DLC film formed on the amorphous carbon film, and 3 atomic% of fluorine formed on the DLC film.
  • the fluorine-containing DLC film has a water contact angle of 80 ° or more (preferably 90 ° or more), and a Knoop hardness is equal to or higher than the Knoop hardness of the die.
  • the upper limit content of fluorine in the fluorine-containing DLC film is preferably 17 atomic percent or less, and more preferably 10 atomic percent or less.
  • a water-repellent and high hardness characterized by forming a fluorine-containing DLC film by a plasma CVD method using a source gas having a hydrocarbon-based gas and a fluorocarbon-based gas and a high-frequency power having a frequency of 10 to 500 kHz A method for producing a membrane.
  • An amorphous carbon film is formed by a plasma CVD method using a source gas containing carbon, hydrogen, silicon, and nitrogen
  • a DLC film is formed by a plasma CVD method using a raw material gas having a hydrocarbon-based gas and a high-frequency power having a frequency of 10 to 500 kHz
  • a fluorine-containing DLC film is formed on the DLC film by a plasma CVD method using a source gas having a hydrocarbon-based gas and a fluorocarbon-based gas and a high-frequency power having a frequency of 10 to 500 kHz.
  • the manufacturing method of can be provided.
  • FIG. 1 is a cross-sectional view illustrating a method for producing a water-repellent high hardness film according to one embodiment of the present invention.
  • FIG. 2 is a cross-sectional view illustrating a method for manufacturing a water-repellent high hardness film according to one embodiment of the present invention.
  • FIG. 3 shows the water contact angle of the fluorine-containing DLC film of Sample 1-1 of Example 1, the water contact angle of the fluorine-containing DLC film of Comparative Sample 1-2, and the DLC film of the Comparative Sample. It is a figure which shows the result of having measured the contact angle of water.
  • FIG. 1 is a cross-sectional view illustrating a method for producing a water-repellent high hardness film according to one embodiment of the present invention.
  • FIG. 2 is a cross-sectional view illustrating a method for manufacturing a water-repellent high hardness film according to one embodiment of the present invention.
  • FIG. 3 shows the water contact angle of the fluorine-containing DLC
  • FIG. 4 shows the Knoop hardness of the fluorine-containing DLC film of Sample 1-1 of Example 1, the Knoop hardness of the fluorine-containing DLC film of Sample 1-2 of the comparative example, and the Knoop hardness of the DLC film of the sample of the comparative example. It is a figure which shows the result.
  • FIG. 5 is a diagram showing the results of measuring the water contact angle of the fluorine-containing DLC film of each of Sample 2-1 and Sample 2-2 of Example 2 and the water contact angle of the DLC film of the sample of the comparative example. is there.
  • FIG. 5 is a diagram showing the results of measuring the water contact angle of the fluorine-containing DLC film of each of Sample 2-1 and Sample 2-2 of Example 2 and the water contact angle of the DLC film of the sample of the comparative example. is there.
  • FIG. 6 is a diagram showing the results of measuring the Knoop hardness of the fluorine-containing DLC film of Sample 2-1 and Sample 2-2 of Example 2 and the Knoop hardness of the DLC film of the Comparative Example sample.
  • FIG. 7 is a photograph of Sample 2-1 of Example 2.
  • FIG. 8 is a diagram showing the results of XPS analysis performed on the fluorine-containing DLC films of Sample 2-1 and Sample 2-2 of Example 2.
  • FIG. 9 is a diagram showing the results of XPS analysis performed on the fluorine-containing DLC films of Sample 2-1 and Sample 2-2 of Example 2.
  • FIG. 10 is a cross-sectional view schematically showing a conventional mold for an injection molding machine.
  • FIG. 10 is a cross-sectional view schematically showing a conventional mold for an injection molding machine.
  • FIG. 11A is a diagram showing a film thickness measurement result by HAADF of sample 2-2 in Example 2
  • FIG. 11B is a diagram showing a film thickness measurement result by HAADF of sample 2-1 in Example 2. is there.
  • FIG. 12 is a diagram showing a depth-profile of XPS analysis of sample 2-1 of Example 2.
  • FIG. 13 is a diagram illustrating a depth-profile of XPS analysis of Sample 2-2 of Example 2.
  • FIG. 1 is a cross-sectional view illustrating a method for producing a water-repellent high hardness film according to one embodiment of the present invention.
  • a mold 11 formed of die steel or high speed steel is prepared.
  • die 11 is used, it is not limited to a metal mold
  • a gas mixture of hydrocarbon gas and fluorocarbon gas is used as a raw material gas on the surface of the mold 11, and the frequency is 10 to 500 kHz (preferably under a pressure of 1.5 to 5 Pa).
  • the fluorine-containing DLC film 12 is formed by plasma CVD under the condition of supplying high-frequency power of 100 to 400 kHz to the mold 11 or an electrode (not shown) opposed to the mold 11.
  • the temperature condition at this time is preferably about room temperature to about 100 ° C.
  • This fluorine-containing DLC film 12 contains 3 atomic% or more of fluorine, has a water contact angle of 80 ° or more, and Knoop hardness of 1050 Hk or more. Further, the upper limit content of fluorine in the fluorine-containing DLC film 12 is preferably 17 atomic% or less, and more preferably 10 atomic% or less. The fluorine-containing DLC film 12 may contain 5 atomic% or less of nitrogen.
  • a plasma CVD apparatus used for forming the fluorine-containing DLC film 12 for example, a parallel plate type plasma CVD apparatus can be used.
  • the “fluorocarbon-based gas” means an organic compound-based gas having a bond of carbon and fluorine.
  • the fluorine-containing DLC film 12 since the fluorine-containing DLC film 12 is formed by the plasma CVD method under the above film formation conditions, the fluorine-containing DLC film 12 has a water contact angle of 80 ° or more and a Knoop hardness of 1050 Hk or more. A certain water-repellent high hardness film can be obtained. Specifically, since the fluorine-containing DLC film 12 contains 3 atomic% or more of fluorine, the water contact angle of the fluorine-containing DLC film 12 can be 80 ° or more. The reason why the lower limit of the fluorine content is 3 atomic% is that the fluorine content needs to be at least 3 atomic% in order to make the contact angle of water 80 ° or more.
  • the preferable upper limit of the fluorine content is set to 17 atomic% is that if it contains more than 17 atomic%, the Knoop hardness of 1050 Hk cannot be maintained.
  • the surface of the mold 11 is made water-repellent with a water contact angle of 80 ° or more, thereby separating the mold 11 from the resin.
  • the moldability can be improved, and as a result, it is possible to suppress the occurrence of resin seizure in a part of the mold 11. Therefore, the frequency of cleaning the burned-in resin can be suppressed, the time and labor required for the cleaning can be reduced, and the life of the mold can be extended.
  • the fluorine-containing DLC film 12 has high hardness, it is possible to suppress the mold and the fluorine-containing DLC film 12 from being scratched. Further, the reason why the fluorine-containing DLC film 12 can obtain a high hardness is that the DLC film containing a large amount of sp3 called a diamond structure has a main structure. By substituting a part of carbon constituting DLC with fluorine, a fluorine-containing DLC film having both high hardness and water repellency can be obtained. On the other hand, a simple carbon film has many sp2 called an amorphous structure, and it is impossible to obtain strength structurally.
  • FIG. 2 is a cross-sectional view illustrating a method for manufacturing a water-repellent high hardness film according to one embodiment of the present invention. First, a mold 11 similar to that of the first embodiment is prepared.
  • a raw material gas containing carbon, hydrogen, silicon, and nitrogen (for example, a raw gas having HMDS-N) is used on the surface of the mold 11 at a frequency of 10 at a pressure of 1.5 to 5 Pa.
  • the amorphous carbon film 13 is formed by plasma CVD under the condition that high-frequency power of ⁇ 500 kHz (preferably 100 to 400 kHz) is supplied to the mold 11 or an electrode (not shown) facing the mold 11.
  • the temperature condition at this time is preferably about room temperature to about 100 ° C.
  • the amorphous carbon film 13 is, for example, a C a H b Si c N d film.
  • a, b, c, and d are natural numbers.
  • HMDS-N is hexamethyldisilazane (C 6 H 19 NSi 2 ).
  • the frequency of the high-frequency power when forming the amorphous carbon film 13 is 10 to 500 kHz, but is not limited to this, and 13.56 MHz is set as the frequency of the high-frequency power. It may be used.
  • a raw material gas having a hydrocarbon gas for example, a raw material gas having C 7 H 8
  • the DLC film 14 is formed by plasma CVD under the condition of supplying high frequency power (preferably 100 to 400 kHz) to the mold 11 or an electrode (not shown) opposed to the mold 11.
  • the temperature condition at this time is preferably about room temperature to about 100 ° C.
  • a fluorine-containing DLC film 15 is formed on the DLC film 14 by a plasma CVD method under the same film formation conditions as in the first embodiment.
  • the fluorine-containing DLC film 15 contains 3 atomic% or more of fluorine, has a water contact angle of 80 ° or more (preferably 90 ° or more), and a Knoop hardness of 1050 Hk or more. Further, the upper limit content of fluorine in the fluorine-containing DLC film 15 is preferably 17 atomic% or less, and more preferably 10 atomic% or less. In this embodiment, the same effect as that of the first embodiment can be obtained. In addition, according to the present embodiment, since the amorphous carbon film 13 and the DLC film 14 are formed between the mold 11 and the fluorine-containing DLC film 15, compared with the fluorine-containing DLC film 12 of the first embodiment.
  • the contact angle of water can be increased even if high hardness is maintained. This will be described in detail below.
  • a part of the elements constituting the amorphous carbon film 13 diffuses into the DLC film 14, and by forming a diffusion layer, the mold 11 and the DLC film 14 are in close contact with each other. Can increase the sex.
  • a diffusion layer made of an element constituting the DLC film 15 is formed between the DLC film 14 and the fluorine-containing DLC film 15, and adhesion is enhanced. Further, by forming the DLC film 14, the hardness of the fluorine-containing DLC film 15 can be further increased.
  • the Si may be etched by fluorine of the fluorine-containing DLC film 15, but the etching of Si by the fluorine can be suppressed by the DLC film 14.
  • the film thickness ratio of the amorphous carbon film 13, the DLC film 14, and the fluorine-containing DLC film 15 is expressed by the following formula 1, and the following formula 2 is in the range of ⁇ 50% with the formula 1 as a central value. Preferably, it is in the range of ⁇ 30%, more preferably in the range of ⁇ 20%.
  • the DLC film 14 can withstand the impact. Furthermore, since the amorphous carbon film 13 has a function of improving the adhesion of the DLC film 14, the amorphous carbon film 13 can prevent the DLC film 14 from being peeled off. These effects can be sufficiently exerted by setting the film thickness ratio to satisfy the above formula 2.
  • the hardness of the amorphous carbon film 13 is about 900 Hk, for example, in the range of 800 to 1000 Hv.
  • the total film thickness of the amorphous carbon film 13, the DLC film 14, and the fluorine-containing DLC film 15 is not less than 0.3 ⁇ m and not more than 5 ⁇ m (preferably not less than 1 ⁇ m and not more than 3 ⁇ m).
  • the Knoop hardness of the fluorine-containing DLC film 15 is set to 1050 Hk or more.
  • the present invention is not limited to this, and the base (mold 11 or substrate) on which the fluorine-containing DLC film 15 is formed is not limited thereto. Any Knoop hardness or higher is acceptable.
  • FIG. 3 shows the water contact angle of the fluorine-containing DLC film of Sample 1-1 of Example 1, the water contact angle of the fluorine-containing DLC film of Comparative Sample 1-2, and the DLC film of the Comparative Sample. It is a figure which shows the result of having measured the contact angle of water.
  • the measurement result shown in FIG. 3 is obtained by measuring and averaging the contact angles of a plurality of points on the sample.
  • FIG. 4 shows the Knoop hardness of the fluorine-containing DLC film of Sample 1-1 of Example 1, the Knoop hardness of the fluorine-containing DLC film of Sample 1-2 of the comparative example, and the Knoop hardness of the DLC film of the sample of the comparative example. It is a figure which shows the result.
  • the measurement result shown in FIG. 4 is obtained by measuring and averaging Knoop hardness at a plurality of points on the sample.
  • Sample 1-1 of Example 1 >> Sample 1-1 of Example 1 is obtained by forming a fluorine-containing DLC film on a substrate under the following film formation conditions.
  • the sample 1-1 of Example 1 has a water contact angle of 80 ° or more and a Knoop hardness of 1265 Hk, whereas the sample 1-2 of the comparative example has a contact angle of water. Although the Knoop hardness was significantly lower than 1050 Hk, the Knoop hardness was higher than 1050 Hk in the comparative sample (DLC), but the contact angle of water was considerably lower than 80 °.
  • FIG. 5 is a diagram showing the results of measuring the water contact angle of the fluorine-containing DLC film of each of Sample 2-1 and Sample 2-2 of Example 2 and the water contact angle of the DLC film of the sample of the comparative example. is there.
  • the measurement result shown in FIG. 5 is obtained by measuring and averaging the contact angles of a plurality of points on the sample.
  • FIG. 6 is a diagram showing the results of measuring the Knoop hardness of the fluorine-containing DLC film of Sample 2-1 and Sample 2-2 of Example 2 and the Knoop hardness of the DLC film of the Comparative Example sample. The measurement result shown in FIG.
  • FIG. 6 is obtained by measuring and averaging Knoop hardness at a plurality of points on the sample.
  • FIG. 7 is a photograph of Sample 2-1 of Example 2.
  • 8 and 9 are diagrams showing the results of XPS analysis performed on the fluorine-containing DLC films of Sample 2-1 and Sample 2-2 of Example 2, respectively.
  • XPS analysis is X-ray photoelectron spectroscopy (XPS).
  • Table 1 quantifies the contents of carbon C, fluorine F and nitrogen N in the fluorine-containing DLC films of Sample 2-1 and Sample 2-2 of Example 2 from the XPS analysis results.
  • FIG. 11A is a diagram showing a film thickness measurement result by HAADF of sample 2-2 of Example 2, and FIG.
  • FIG. 11B is a film thickness measurement result by HAADF of sample 2-1 of Example 2.
  • HAADF is one of the STEM dark field methods, and when a transmission electron scattered at a large angle is detected by an annular detector and imaged, a contrast proportional to the square of the atomic number (Z Contrast).
  • FIG. 12 is a diagram showing a depth-profile of XPS analysis of sample 2-1 of Example 2.
  • FIG. 13 is a diagram illustrating a depth-profile of XPS analysis of Sample 2-2 of Example 2. 12 and 13, the horizontal axis represents depth (nm), and the vertical axis represents content (atomic%).
  • Sample 2-1 of Example 2 An amorphous carbon film containing carbon, hydrogen, silicon, and nitrogen is formed on a substrate, a DLC film is formed on the amorphous silicon film, and the DLC film A fluorine-containing DLC film is formed thereon.
  • the film formation conditions of the amorphous carbon film, the DLC film, and the fluorine-containing DLC film are as follows.
  • the film formation conditions of the amorphous carbon film, the DLC film, and the fluorine-containing DLC film are as follows.
  • Base material the same as the condition of the amorphous carbon film of sample 2-1
  • Film forming apparatus the same as the condition of the amorphous carbon film of sample 2-1
  • Raw material gas conditions of the amorphous carbon film of sample 2-1
  • High-frequency output the same as the condition of the amorphous carbon film of the sample 2-1
  • Pressure the amorphous carbon film of the sample 2-1
  • Temperature Same as the condition of the amorphous carbon film of Sample 2-1
  • Film thickness Same as the condition of the amorphous carbon film of Sample 2-1
  • Film formation apparatus same as DLC film of sample 2-1
  • Source gas same as DLC film of sample 2-1
  • Frequency of high frequency power source same as D
  • the contact angle of water can be made larger than 90 °, but the Knoop hardness can be maintained higher than 1050 Hk, but it has been confirmed to be lower than 1250 Hk. (See Sample 2-2 in Example 2).
  • the contact angle can be increased, but the reason for the decrease in Knoop hardness is considered to be that sp3 in the fluorine-containing DLC film is decreased. According to FIG.
  • the film thickness of the amorphous carbon film of Sample 2-2 of Example 2 is 384.6 nm
  • the film thickness of the DLC film is 237.8 nm
  • the film thickness of the fluorine-containing DLC film is 86. 0.7 nm.
  • the film thickness of the amorphous carbon film of Sample 2-1 of Example 2 is 402.8 nm
  • the film thickness of the DLC film is 251.7 nm
  • the film thickness of the fluorine-containing DLC film. Was 167.8 nm. According to each of FIGS.

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Abstract

Cette invention concerne un film hydrofuge à haute dureté présentant un angle de contact avec l'eau supérieur ou égal à 80° et une haute dureté. Selon un mode de réalisation, l'invention concerne un film hydrofuge à haute dureté à base de carbone sous forme de diamant amorphe contenant du fluor, contenant au moins 3 % de fluor en pourcentage atomique, ledit film à base de carbone sous forme de diamant amorphe contenant du fluor présentant un angle de contact avec l'eau supérieur ou égal à 80° et une dureté Knoop supérieure ou égale à 1050 Hk.
PCT/JP2015/055309 2015-02-18 2015-02-18 Film hydrofuge à haute dureté, moule et procédé de fabrication de film hydrofuge à haute dureté Ceased WO2016132562A1 (fr)

Priority Applications (3)

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PCT/JP2015/055309 WO2016132562A1 (fr) 2015-02-18 2015-02-18 Film hydrofuge à haute dureté, moule et procédé de fabrication de film hydrofuge à haute dureté
JP2017500268A JP6653816B2 (ja) 2015-02-18 2015-02-18 撥水性高硬度膜、金型及び撥水性高硬度膜の製造方法
TW105102705A TWI699447B (zh) 2015-02-18 2016-01-28 撥水性高硬度膜、鑄模及撥水性高硬度膜之製造方法

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PCT/JP2015/055309 WO2016132562A1 (fr) 2015-02-18 2015-02-18 Film hydrofuge à haute dureté, moule et procédé de fabrication de film hydrofuge à haute dureté

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WO2019117267A1 (fr) * 2017-12-15 2019-06-20 ニプロ株式会社 Récipient médical en verre et son procédé de fabrication
JP2019107445A (ja) * 2017-12-15 2019-07-04 ニプロ株式会社 医療用ガラス容器及びその製造方法
JP2020066797A (ja) * 2018-10-26 2020-04-30 アドバンストマテリアルテクノロジーズ株式会社 保護膜、保護膜付き容器、その製造方法及びプラズマｃｖｄ装置
US11157717B2 (en) * 2018-07-10 2021-10-26 Next Biometrics Group Asa Thermally conductive and protective coating for electronic device

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