JPH0723533B2 - Method for producing resin body coated with silicon oxide - Google Patents

Description

TECHNICAL FIELD The present invention relates to a method for producing a silicon oxide-coated resin body.

[Prior Art] It is conventionally known to form a silicon oxide thin film by a vacuum deposition method or an ion plating method. For example, in JP-A-49-60369, 1 × 10 ^-5 Torr to 8 × 10 ⁵
A method of vacuum-depositing silicon dioxide on plastic by heating silicon monoxide in an oxygen atmosphere of ^-4 Torr is described in VACUUM Vol. 14, 385-392 (1964) and Journal of Ap.
Plied Physics Vol.34, 347-351 (1962) describes forming a silicon monoxide film by vacuum vapor deposition.

A resin body in which a silicon oxide thin film is laminated is used for optical applications such as insulators and glasses, and it is required to thicken the thin film in order to harden the thin film.

However, since silicon monoxide has high reactivity with oxygen and water vapor, the stress of the silicon monoxide thin film changes with time, and if the film thickness is made thicker, the residual stress becomes larger and it becomes easier to remove the film. It cannot be transformed. Further, silicon dioxide has a smaller chemical activity than silicon monoxide and has poor adhesiveness to the resin body, and therefore, if the film thickness is increased, the film can be easily removed.

[Problems to be solved by the invention]

In view of the above drawbacks, an object of the present invention is to provide a method for producing a resin body in which a silicon oxide film having a thickness of 3 μm or more is firmly adhered.

[Means for solving problems]

Hereinafter, a method for producing a silicon oxide-coated resin body of the present invention will be described with reference to the drawings.

FIG. 1 is a schematic view showing an example of an apparatus used in the manufacturing method of the present invention. In the figure, reference numeral 1 denotes a vacuum chamber, which is evacuated to a high vacuum by an exhaust device (not shown) connected to an exhaust port 2. Inside the vacuum chamber 1, copper hearths 3 and 31 with heating and cooling devices, to which substances to be evaporated 4 and 41 are supplied, are arranged. The positions of the copper hearths 3 and 31 can be arbitrarily exchanged. An ionization electrode 5 connected to the electrode is installed above the copper hearth 3 so that the evaporated substance can be ionized. Further, a substrate 6 for fixing a resin body 7 made of polyether sulfone is provided above the ionization electrode 5, and the substrate 6
Are connected to the electrodes. In addition, 8 is a gas inlet.

In the present invention, when the vacuum degree of the vacuum chamber 1 is small, when the silicon monoxide is vacuum-deposited or ion-plated, the residual oxygen changes the silicon monoxide into silicon dioxide, and the ratio of silicon dioxide in the coating layer is high. Since the adhesion is reduced, the pressure is reduced to 5 × 10 ^-4 Torr or less. It should be noted that nitrogen or water vapor may be injected into the tank 1 as long as it is within this reduced pressure range. Then, silicon monoxide is supplied to the copper hearth 3 as the substance 4 to be evaporated, and the copper hearth 3 is heated to evaporate the silicon monoxide to a thickness of 0.05 to 3 μm on the resin body 7.
To form a coating layer. At this time, for coating by the ion plating method, a DC voltage may be applied to the ionization electrode to generate arc discharge and ionize a part of the evaporated silicon monoxide.
Alternatively, a negative DC voltage may be applied. Since the applied voltage causes the temperature of the substrate 6 to rise, it is appropriately determined by the heat resistance of the resin of the resin body 7.

Next, the positions of the copper hearth 31 and the copper hearth 3 supplied with silicon dioxide as the substance to be evaporated 41 are changed, and the copper hearth 31 is heated to evaporate the silicon dioxide and form a silicon dioxide layer on the coating layer. . Since the coating layer is mainly composed of silicon monoxide, it is easily oxidized when it comes into contact with oxygen. Therefore, after forming the coating layer, the vacuum chamber 1
It is preferable to maintain the reduced pressure state of, and subsequently to form the silicon dioxide layer.

The coating layer is a layer formed of silicon monoxide containing a small amount of silicon dioxide, since silicon monoxide is a layer formed by vacuum deposition or ion plating under a reduced pressure of 5 × 10 ⁻⁴ Torr or less. Therefore, the thinner the coating layer, the higher the proportion of silicon dioxide and the lower the adhesion.
formed to a thickness of μm.

The thickness of the silicon dioxide layer may be determined so that the total thickness of the coating layer and the silicon dioxide layer is 3 μm or more, but it is preferably thicker than the thickness of the coating layer, more preferably 3 to 20 μm. is there.

〔The invention's effect〕

The configuration of the method for producing a silicon oxide-coated resin body of the present invention is as described above, and a resin body made of polyether sulfone coated with a thick film of silicon oxide having a thickness of 3 μm or more can be easily produced. The resulting resin body made of polyethersulfone has a high surface hardness and a silicon oxide layer with excellent scratch resistance firmly adheres to it, and plastic lenses, window glass, and other surface-hardened plastic products Can be suitably used as.

〔Example〕

 Next, examples of the present invention will be described.

Examples 1 to 4 and Comparative Examples 3 and 4 In the apparatus shown in FIG. 1, a polyether sulfone film was installed as the resin body 7, the pressure was reduced to the predetermined pressure shown in Table 1, and 50 V was applied to the ionization electrode 5. Then, the substrate 6 is grounded, and the copper hearth 3 to which silicon monoxide is supplied as the substance to be evaporated 4 is heated to form a coating layer of silicon monoxide by the ion plating method, and then ionized. The electrode 5 and the substrate 6 are grounded,
Copper hearth supplied with silicon dioxide as the substance to be evaporated 41
After replacing 31 with copper hearth 3, it was heated and a silicon dioxide layer was laminated on the coating layer by vacuum deposition. The thicknesses of the coating layer and the silicon dioxide layer were measured and are shown in Table 1. In addition, surface hardness test (Knoop hardness, load 25g) and heat cycle test (hold at -20 ℃ for 1 hour)
After maintaining at 100 ° C. for 1 hour 100 times, the surface condition was observed with an optical microscope) and the results are shown in Table 1. The Knoop hardness of the polyether sulfone film was 20 kg / mm ² .

Examples 5 to 8 As in Example 1, except that the pressure in the vacuum chamber was reduced to 1 × 10 ⁻⁵ Torr, and then the gas shown in Table 1 was injected to 2 × 10 ⁻⁴ Torr. A coating layer and a silicon dioxide layer were laminated, and the thickness of each tank is shown in Table 1. In addition, the surface hardness test and the heat cycle test were performed, and the result was the first
Shown in the table.

Comparative Example 1 When a 13 μm-thick silicon dioxide layer was laminated by a vacuum deposition method without forming a coating layer of silicon monoxide in Example 1, a part of the silicon dioxide layer was exfoliated.

Comparative Example 2 The pressure in the vacuum chamber was reduced to 1 × 10 ⁻⁵ Torr, nitrogen gas was introduced to 2 × 10 ⁻⁴ Torr, and a silicon monoxide coating layer having a thickness of 6 μm was obtained in the same manner as in Example 1. Was formed, the coating layer was partially peeled off.

[Brief description of drawings]

FIG. 1 is a schematic view showing an example of an apparatus used in the manufacturing method of the present invention. 1 ... Vacuum tank, 2 ... Exhaust port, 3,31 ... Copper hearth, 4,41
…… Evaporation material, 5 …… Ionization electrode, 6 …… Substrate, 7
...... Resin body

Claims (1)

[Claims] 1. A coating layer of 0.05 to 3 .mu.m is formed on the surface of a resin body made of polyethersulfone by heating and evaporating silicon monoxide under a reduced pressure of 5.times.10.sup.- ⁴ Torr or less and by a vacuum deposition method or an ion plating method. And then evaporating the silicon dioxide by heating to form a silicon dioxide layer by a vacuum deposition method or an ion plating method so that the total thickness of the coating layer and the silicon dioxide layer is 3 μm or more. A method for producing a silicon oxide-coated resin body.