JPWO2022014568A5 - - Google Patents
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- JPWO2022014568A5 JPWO2022014568A5 JP2022536372A JP2022536372A JPWO2022014568A5 JP WO2022014568 A5 JPWO2022014568 A5 JP WO2022014568A5 JP 2022536372 A JP2022536372 A JP 2022536372A JP 2022536372 A JP2022536372 A JP 2022536372A JP WO2022014568 A5 JPWO2022014568 A5 JP WO2022014568A5
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- layer
- antifouling layer
- contact angle
- water contact
- sliding
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- 230000003373 anti-fouling effect Effects 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000012788 optical film Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 5
- 230000003746 surface roughness Effects 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 2
- 239000010410 layer Substances 0.000 claims 27
- 239000010419 fine particle Substances 0.000 claims 2
- 239000000463 material Substances 0.000 claims 2
- 229910044991 metal oxide Inorganic materials 0.000 claims 2
- 150000004706 metal oxides Chemical class 0.000 claims 2
- 230000003287 optical effect Effects 0.000 claims 2
- 239000002346 layers by function Substances 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 14
- 239000010408 film Substances 0.000 description 11
- 229920002284 Cellulose triacetate Polymers 0.000 description 7
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 230000006866 deterioration Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000009832 plasma treatment Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- HEFNNWSXXWATRW-UHFFFAOYSA-N Ibuprofen Chemical compound CC(C)CC1=CC=C(C(C)C(O)=O)C=C1 HEFNNWSXXWATRW-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910021647 smectite Inorganic materials 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Description
比較例３
（第１工程）
透明な樹脂フィルムとしてのトリアセチルセルロース（ＴＡＣ）フィルム（厚さ８０μｍ）の片面に、ハードコート層を形成した。本工程では、まず、紫外線硬化型のアクリルモノマー（商品名「ＧＲＡＮＤＩＣ ＰＣ－１０７０」、ＤＩＣ社製）１００質量部と、粒子としてのナノシリカ粒子を含有するオルガノシリカゾル（商品名「ＭＥＫ－ＳＴ－Ｌ」、ナノシリカ粒子の平均一次粒子径は５０ｎｍ、固形分濃度３０質量％、日産化学社製）２５質量部（ナノシリカ粒子換算量）と、チキソトロピー付与剤（商品名「ルーセンタイトＳＡＮ」、有機粘土である合成スメクタイト、コープケミカル社製）１.５質量部と、光重合開始剤（商品名「ＯＭＮＩＲＡＤ９０７」、ＢＡＳＦ社製）３質量部と、レベリング剤（商品名「ＬＥ３０３」、共栄社化学社製）０.１５質量部とを混合して、固形分濃度５５質量％の組成物（ワニス）を調製した。混合には、超音波分散機を使用した。次に、上記ＴＡＣフィルムの片面に組成物を塗布して塗膜を形成した。次に、この塗膜を、紫外線照射により硬化させた後、加熱により乾燥させた。紫外線照射では、光源として高圧水銀ランプを使用し、波長３６５ｎｍの紫外線を用い、積算照射光量を２００ｍＪ／ｃｍ２とした。また、加熱の時間は８０℃とし、加熱の温度は３分間とした。これにより、ＴＡＣフィルム上に厚さ６μｍのハードコート層（第２のＨＣ層）を形成した。これにより、基材層（ＨＣ層付きＴＡＣフィルム）を得た。
Comparative example 3
(First step)
A hard coat layer was formed on one side of a triacetyl cellulose (TAC) film (80 μm thick) as a transparent resin film. In this step, first, 100 parts by mass of an ultraviolet curable acrylic monomer (trade name “GRANDIC PC-1070”, manufactured by DIC) and an organosilica sol (trade name “MEK-ST-L”) containing nanosilica particles as particles. ”, The average primary particle diameter of the nanosilica particles is 50 nm, the solid content concentration is 30% by mass, manufactured by Nissan Chemical Co., Ltd.) 25 parts by mass (in terms of nanosilica particles), and a thixotropy imparting agent (trade name “Lucentite SAN”, organic clay A certain synthetic smectite, Co-op Chemical Co., Ltd.) 1.5 parts by mass, a photopolymerization initiator (trade name "OMNIRAD907", manufactured by BASF) 3 parts by mass, and a leveling agent (trade name "LE303", manufactured by Kyoeisha Chemical Co., Ltd.) 0.15 parts by mass of these ingredients were mixed to prepare a composition (varnish) having a solid content concentration of 55% by mass. An ultrasonic disperser was used for mixing. Next, the composition was applied to one side of the TAC film to form a coating film. Next, this coating film was cured by ultraviolet irradiation and then dried by heating. In the ultraviolet irradiation, a high-pressure mercury lamp was used as a light source, ultraviolet rays with a wavelength of 365 nm were used, and the cumulative irradiation light amount was 200 mJ/cm 2 . The heating time was 80° C. and the heating temperature was 3 minutes. As a result, a hard coat layer (second HC layer) having a thickness of 6 μm was formed on the TAC film. Thus, a substrate layer (TAC film with HC layer) was obtained.
次に、プラズマ処理後のＨＣ層付きＴＡＣフィルムのＨＣ層上に、密着層と反射防止層とを順次に形成した。具体的には、ロールトゥロール方式のスパッタ成膜装置により、プラズマ処理後のＨＣ層付きＴＡＣフィルムのＨＣ層上に、密着層としての厚さ１.５ｎｍのインジウムスズ酸化物（ＩＴＯ）層と、第１高屈折率層としての厚さ１２ｎｍのＮｂ２Ｏ５層と、第１低屈折率層としての厚さ２８ｎｍのＳｉＯ２層と、第２高屈折率層としての厚さ１００ｎｍのＮｂ２Ｏ５層と、第２低屈折率層としての厚さ８５ｎｍのＳｉＯ２層とを、順次に形成した。密着層の形成では、ＩＴＯターゲットを用い、不活性ガスとしてのアルゴンガスと、アルゴンガス１００体積部に対して１０体積部の反応性ガスとしての酸素ガスとを用い、放電電圧を４００Ｖとし、成膜室内の気圧（成膜気圧）を０.２Ｐａとし、ＭＦＡＣスパッタリングによってＩＴＯ層を成膜した。比較例３における第１高屈折率層、第１低屈折率層、第２高屈折率層、および第２低屈折率層の形成条件は、比較例１における第１高屈折率層、第１低屈折率層、第２高屈折率層、および第２低屈折率層の上記の形成条件と同じである。 Next, an adhesion layer and an antireflection layer were sequentially formed on the HC layer of the TAC film with the HC layer after the plasma treatment. Specifically, an indium tin oxide (ITO) layer having a thickness of 1.5 nm as an adhesion layer was formed on the HC layer of the TAC film with the HC layer after the plasma treatment using a roll-to-roll type sputtering deposition apparatus. , a 12 nm thick Nb 2 O 5 layer as the first high refractive index layer, a 28 nm thick SiO 2 layer as the first low refractive index layer and a 100 nm thick Nb layer as the second high refractive index layer. A 2 O 5 layer and an SiO 2 layer with a thickness of 85 nm as a second low refractive index layer were sequentially formed. In forming the adhesion layer, an ITO target was used, argon gas was used as an inert gas, oxygen gas was used as a reactive gas in an amount of 10 parts by volume with respect to 100 parts by volume of the argon gas, and the discharge voltage was set to 400 V. The pressure in the film chamber (film formation pressure) was set to 0.2 Pa, and the ITO layer was formed by MFAC sputtering. The conditions for forming the first high refractive index layer, the first low refractive index layer, the second high refractive index layer, and the second low refractive index layer in Comparative Example 3 were the same as those for the first high refractive index layer, the first The conditions for forming the low refractive index layer, the second high refractive index layer, and the second low refractive index layer are the same as those described above.
実施例３
比較例３と同様にして、防汚層付き光学フィルムを製造した。
Example 3
An optical film with an antifouling layer was produced in the same manner as in Comparative Example 3 .
比較例４
比較例３と同様にして、防汚層付き光学フィルムを製造した。
Comparative example 4
An optical film with an antifouling layer was produced in the same manner as in Comparative Example 3 .
比較例２
比較例３と同様にして、防汚層付き光学フィルムを製造した。
Comparative example 2
An optical film with an antifouling layer was produced in the same manner as in Comparative Example 3 .
実施例５
比較例３と同様にして、防汚層付き光学フィルムを製造した。
Example 5
An optical film with an antifouling layer was produced in the same manner as in Comparative Example 3 .
３．考察
防汚層の表面粗さＲａが、１０ｎｍ以下である実施例１、比較例３、実施例３、比較例４および実施例５は、防汚層の表面粗さＲａが、１７．７ｎｍである比較例１に比べて、水接触角の変化量が小さい。このことから、防汚層の表面粗さＲａが、１０ｎｍ以下であれば、防汚層に付着した汚れを拭き取った後でも、防汚層の防汚性の低下を抑制できるとわかる。具体的には、数十回程度の拭き取り（摺動）に対して、防汚性の低下を抑制できる品質を有しているとわかる。
3. Consideration In Example 1 , Comparative Example 3, Example 3, Comparative Example 4, and Example 5 in which the surface roughness Ra of the antifouling layer was 10 nm or less, the surface roughness Ra of the antifouling layer was 17.7 nm. Compared with Comparative Example 1, the amount of change in water contact angle is small. From this, it can be seen that when the surface roughness Ra of the antifouling layer is 10 nm or less, deterioration of the antifouling property of the antifouling layer can be suppressed even after wiping off the stains adhering to the antifouling layer. Specifically, it can be seen that it has a quality capable of suppressing deterioration of the antifouling property against wiping (sliding) several tens of times.
摺動後の水接触角が、８３°以上であり、防汚層の厚み方向一方面の水接触角（第１接触角）が、１１０°以上である実施例１、比較例３、実施例３、比較例４および実施例５は、摺動後の水接触角が、８０°であり、防汚層の厚み方向一方面の水接触角（第１接触角）が、１０９．４°である比較例２に比べて、防汚性に優れる。このことから、防汚層の摺動後の水接触角が、８３°以上、かつ、防汚層の厚み方向一方面の水接触角（第１接触角）が、１１０°以上であれば、防汚層に付着した汚れを拭き取った後でも、防汚層の防汚性の低下を抑制できるとわかる。具体的には、数千回程度の拭き取り（摺動）に対して、実用レベルの防汚性を維持できる実用性を確保することができるとわかる。 Example 1 , Comparative Example 3, and Examples in which the water contact angle after sliding is 83° or more, and the water contact angle (first contact angle) of one surface of the antifouling layer in the thickness direction is 110° or more. 3. In Comparative Example 4 and Example 5, the water contact angle after sliding was 80°, and the water contact angle (first contact angle) on one side in the thickness direction of the antifouling layer was 109.4°. Compared with a certain comparative example 2, it is excellent in antifouling property. From this, if the water contact angle of the antifouling layer after sliding is 83° or more and the water contact angle (first contact angle) of one surface in the thickness direction of the antifouling layer is 110° or more, It can be seen that deterioration of the antifouling property of the antifouling layer can be suppressed even after the stain adhering to the antifouling layer is wiped off. Specifically, it can be seen that the practicability of maintaining a practical level of antifouling property against wiping (sliding) about several thousand times can be ensured.
Claims (6)
前記基材層が、基材と、ハードコート層とを厚み方向一方側に向かって順に備え、
前記防汚層の表面粗さＲａが、５．０１ｎｍ以下であり、
前記ハードコート層の厚み方向一方面の表面粗さＲａが、１．２ｎｍ以上５．０ｎｍ以下であり、
前記防汚層の厚み方向一方面の水接触角が、１１０°以上であり、
第１耐久性試験により求められる防汚層の水接触角が、８３°以上である、防汚層付き光学フィルム。
第１耐久性試験：防汚層について、以下の条件に基づき、第１消しゴム摺動試験を実施する。第１消しゴム摺動試験を実施した後、防汚層の純水に対する水接触角を測定する。
＜第１消しゴム摺動試験＞
Ｍｉｎｏａｎ社製の消しゴム（Φ６ｍｍ）
摺動距離：片道１００ｍｍ
摺動速度：１００ｍｍ／秒
荷重：１ｋｇ／６ｍｍΦ
摺動回数：３０００回 A substrate layer, an optical function layer made of an inorganic layer, and an antifouling layer are provided in order toward one side in the thickness direction,
The base material layer includes a base material and a hard coat layer in order toward one side in the thickness direction,
The antifouling layer has a surface roughness Ra of 5.01 nm or less,
The surface roughness Ra of one surface in the thickness direction of the hard coat layer is 1.2 nm or more and 5.0 nm or less ,
The water contact angle of one surface in the thickness direction of the antifouling layer is 110° or more,
An optical film with an antifouling layer, wherein the antifouling layer has a water contact angle of 83° or more as determined by the first durability test.
First Durability Test: The antifouling layer is subjected to the first eraser sliding test under the following conditions. After conducting the first eraser sliding test, the water contact angle of the antifouling layer with respect to pure water is measured.
<First eraser sliding test>
Minoan eraser (Φ6mm)
Sliding distance: 100 mm one way
Sliding speed: 100mm/sec Load: 1kg/6mmΦ
Sliding times: 3000 times
第２耐久性試験：防汚層の純水に対する第１水接触角を測定する。次いで、防汚層について、以下の条件に基づき、第２消しゴム摺動試験を実施する。第２消しゴム摺動試験を実施した後、防汚層の純水に対する第２水接触角を測定する。次いで、下記式（１）に基づき、水接触角の変化量を算出する。
水接触角の変化量＝第１水接触角－第２水接触角 （１）
＜第２消しゴム摺動試験＞
Ｍｉｎｏａｎ社製の消しゴム（Φ６ｍｍ）
摺動距離：片道１００ｍｍ
摺動速度：１００ｍｍ／秒
荷重：１ｋｇ／６ｍｍΦ
摺動回数：１０回 2. The optical film with an antifouling layer according to claim 1, wherein the amount of change in the water contact angle of the antifouling layer determined by the second durability test is 5[deg.] or less.
Second durability test: The first water contact angle of the antifouling layer to pure water is measured. Next, a second eraser sliding test is performed on the antifouling layer under the following conditions. After conducting the second eraser sliding test, the second water contact angle of the antifouling layer with respect to pure water is measured. Next, the amount of change in the water contact angle is calculated based on the following formula (1).
Change in water contact angle = 1st water contact angle - 2nd water contact angle (1)
<Second eraser sliding test>
Minoan eraser (Φ6mm)
Sliding distance: 100 mm one way
Sliding speed: 100mm/sec Load: 1kg/6mmΦ
Sliding times: 10 times
Applications Claiming Priority (7)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2020120131 | 2020-07-13 | ||
| JP2020120131 | 2020-07-13 | ||
| JP2020146144 | 2020-08-31 | ||
| JP2020146144 | 2020-08-31 | ||
| JP2020166844 | 2020-10-01 | ||
| JP2020166844 | 2020-10-01 | ||
| PCT/JP2021/026246 WO2022014568A1 (en) | 2020-07-13 | 2021-07-13 | Optical film with anti-fouling layer |
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| Publication Number | Publication Date |
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| JPWO2022014568A1 JPWO2022014568A1 (en) | 2022-01-20 |
| JPWO2022014568A5 true JPWO2022014568A5 (en) | 2022-08-12 |
| JP7130893B2 JP7130893B2 (en) | 2022-09-05 |
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| JP (1) | JP7130893B2 (en) |
| KR (1) | KR102518011B1 (en) |
| CN (1) | CN115803192B (en) |
| TW (1) | TWI811736B (en) |
| WO (1) | WO2022014568A1 (en) |
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| JP2023163654A (en) * | 2022-04-28 | 2023-11-10 | 日東電工株式会社 | Antireflection film and image display device |
| JP2024079169A (en) * | 2022-11-30 | 2024-06-11 | デクセリアルズ株式会社 | Antifouling coating composition, antifouling coating film, antifouling coating laminate, and methods for producing the same |
| JP2024079170A (en) * | 2022-11-30 | 2024-06-11 | デクセリアルズ株式会社 | Antifouling coating composition, antifouling coating film, antifouling coating laminate, and methods for producing the same |
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