JPH03183757A - Formation of deposited film - Google Patents

Abstract

PURPOSE:To improve the quality of a deposited film and to shorten the length of tact time bay applying deaerating treatment to a base material to regulate the amount of released gas to a specific value and then forming a deposited film. CONSTITUTION:At the time of forming a deposited film on a base material, deaerating treatment is applied, prior to the formation of the deposited film, to the base material to regulate the amount of released gas from this base material at 25 deg.C to <=5X10<-7> Torr.l/sec.cm<3>. At the time of the above deaerating treatment, the amount of released gas can be precisely controlled by means of an equation Q=S(P2-P1)/A (where Q means the amount of released gas, S means pumping speed, P2 means pressure at the time when the deaeration of the base material is completed, P1 means ultimate pressure in the absence of the base material, and A means the surface area of the base material). By this method, the influence of the gas adsorbed by the base material before film formation can be removed, and the improvement of the quality of the deposited film and the shortening of the tact time can be attained with certainty. The above method can be effectively used when the base material to be coated with the deposited film is a base material composed of resin or a resin-coated base material, in particular.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for forming a deposited film in vacuum, for example, on a resin substrate or a resin-coated substrate.

[Prior Art] Resins and resin-coated substrates are often used as substrates for forming functional deposited films on optical disks, magneto-optical disks, etc., but gases adsorbed on the substrate before film formation can cause the deposited film to is known to affect the film quality of

Therefore, conventionally, the film was formed after deaeration was performed to remove the gas adsorbed on the substrate.

[all the invention tries to solve! ] However, until now, it has not been elucidated at all how much degassing is required to obtain good film quality, and it has also not been elucidated at all what factors should be used to control the amount of gas removed. There wasn't.

In other words, Conventional Technology C lacks quantitative properties, and it was not possible to determine whether or not the removal of gas from the substrate was sufficient. As a result, there is a problem of deterioration in the quality of the deposited film due to insufficient gas removal, or a long processing time due to more degassing than necessary. However, there was a problem of poor productivity.

[Means for Solving the Problems] The deposited film forming method of the present invention includes two steps before forming the deposited film.
The amount of gas released from the substrate at 5°C is 5 x 10'' To
It is characterized by performing toothpick degassing treatment to reduce the temperature to rr-11/5ec-c- or less.

[Function] The inventor of the present invention has diligently researched the criteria for determining whether gas removal from the substrate is sufficient, and has found that it can be determined whether gas removal is sufficient by using the amount of gas released from the substrate as a guide. As a result of various experiments, we found that the amount of gas released from the substrate at 25°C was 5 x 10-' Torr.
The inventors have discovered that good film quality can be obtained by setting r-u/sec-Cm2 or less, which led to the present invention.

Furthermore, we searched for a means to accurately and easily determine the amount of released gas from the substrate, and found that the amount of released gas is related to temperature, and furthermore, at a constant temperature, Q=S (P2 P1
)/A was found to hold true. However, Q: amount of released gas, S: pumping speed, P2: pressure at completion of degassing of the two substrates, Pl: arrival pressure when no substrate is present, A: surface area of the substrate. Therefore, when the temperature is 25°C, in the above equation, s, p,.

If A and P are managed, the amount of released gas Q can be reduced to 5X10-'To
It is possible to accurately ascertain whether the deaeration has been completed until rr[/5ee-c1 or less], and it becomes possible to improve the M-purity of the deposited film or shorten the takt time.

Note that deaeration in the present invention may be performed using, for example, an apparatus as shown in FIG.

In FIG. 1, 1 is a degassing chamber which is a vacuum container, 2 is a film forming chamber which is a vacuum container, 7 is a substrate on which a film is to be formed, 3 is a holder for fixing the substrate 7, and 4 is a degassing chamber 1. A cryopump for vacuum evacuation, 5 a gate valve between the degassing chamber 1 and the film forming chamber 2,
Reference numeral 6 denotes a main exhaust valve of the cryo bomb 4 in the film forming chamber 1.

In the above equation, the amount of gas released from the substrate at 25°C Q
5 x 10-' Torr-n/sec-Cm
By degassing until the temperature is 2 or less, the quality of the deposited film can be improved or the tact time can be shortened.

[Example code] The present invention will be explained in detail below.

FIG. 1 is a diagram showing an outline of an apparatus for carrying out the present invention, which is a high-frequency magnetron double-sided sputtering apparatus.

In the above configuration, there are six holders 3 that can mount 16 polycarbonate substrates 7 on both sides, which are substrates for functional deposited films of φ5.25-inch magneto-optical disks, for a total of 96 substrates to be simultaneously degassed in the degassing chamber 1. After the Qi treatment, Seiri
In chamber 2, sputter deposition was performed for each holder. The deposited film is S
i3N4, and the film thickness was 1000 people.

After the film was formed, it was returned to the degassing chamber to complete one patch. This was done for 6 holders, and 6 holders constituted one cycle.

Films were formed while varying the amount of released gas from the substrate 7 to the values shown in Table 1, and changes in film quality due to the released gas were observed.

A: 26815cm” P: 7.5X 1
0-'TorrS: 9300j2/S was substituted into the above equation, the value of P2 was determined, and deaeration processing was performed.

(Evaluation of Example I) After film formation, the substrate was cut with a sharp knife at 11111 intervals, 6 in each length and width.
Draw a line perpendicular to this line to make 25 square cells of 11 Im on each side.
After forming a film onto the substrate and pasting adhesive tape on it to ensure sufficient adhesion, the adhesive tape was peeled off and the degree of adhesion of the film to the substrate was measured by the number of squares attached to the tape (crosshatch test). ), that is, if the number of peeled pieces (number of peeled pieces) attached to the tape is 0 (0/25), the adhesion of the film is good.

Table-x&: Shows M fruits. As can be seen from the table, the amount of released gas Q is 5 x 10-' Torri / 5ec-c
When it was 1 or less, it was rated O, and the adhesion of the film was good. Also, Q wealth 5 x 10-' Tor+”n/5e
The time T1 required to degas to below c-c1 was 90 m.
1 n, which was a sufficient &: short takt time.

(Example 2) In Example f111, only one holder 3 was used, the substrate 7 was made of polymethyl methacrylate instead of polycarbonate, and a total of 16 substrates were subjected to degassing treatment and then film-formed. The amount of gas released from the base is 5×10-' Torr-1/
When the film was formed by degassing until it became 5ee-c1 or less,
No insufficient adhesion of the membrane due to insufficient deaeration was observed.

(Example 3) In the same manner as in Example 2, when the deaeration chamber 1 and the film formation chamber 2 are in the same vacuum vessel and the deaeration process is performed in the formation IIi chamber 2 and then the film formation is performed, the release of the substrate 7 Gas volume is 5x 10-'T
When a film was formed by degassing the film to a value of less than ori/sec-cm, no insufficient adhesion of the film due to insufficient degassing was observed.

(Example 4) In the same manner as in Example 2, when a so-called glass 2P substrate in which glass is coated with a photocurable resin is used as the substrate 7, the amount of gas released from the substrate 7 is 5 x 10-' Torr-f.
/sec-cm'' or less, and when the film was formed, no insufficient adhesion of the film due to insufficient degassing was observed.

(Example 5) In the same manner as in Example 2, a film was formed on a polymethyl methacrylate substrate by vapor deposition instead of sputter vapor deposition, and similarly good results were obtained.

[Effects of the Invention] As explained above, when a deposited film is formed on, for example, a fat substrate or a resin-coated substrate in a vacuum container, the amount of gas released from the substrate before film formation is 5 x 10-'T.
By setting orri/5ee-c1 or less, high quality deposited films can be mass-produced on a regular basis.

In addition, in any deaeration processing equipment, the amount of released gas is quantitatively determined by controlling the pressure by temperature and pumping speed, and by degassing to below that value and forming a film,
It is possible to improve the quality of the deposited film and shorten the takt time. This is effective in steadily mass producing high quality deposited films.

[Brief explanation of drawings]

Figure N1 is a conceptual diagram of a deposited film forming apparatus used in an embodiment of the present invention. FIG. 2 is a diagram showing only the holder of FIG. 1. (Takeyo t!'1 eel area) 1... Deaeration chamber, 2... Film forming chamber, 3... Holder
4... Cryopump, 5... Gate valve, 6... Main exhaust valve, 7... Base. Figure Figure

Claims (3)

[Claims] (1) Before forming the deposited film, reduce the amount of gas released from the substrate at 25°C to 5 x 10^-^7 Torr・l/sec・c
A method for forming a deposited film, characterized by performing deaeration treatment so that the value becomes less than m^2. (2) The method for forming a deposited film according to claim 1, wherein the substrate on which the deposited film is formed is a resin substrate or a resin-coated substrate. (3) The deposited film forming method according to claim 1 or 2, characterized in that during the degassing process, the amount of released gas is controlled by the following equation. Q=S(P_2-P_1)/A However, Q: Released gas amount, S: Pumping speed, P_2: Pressure at the completion of degassing of the substrate, P_1: Arrival pressure when no substrate exists, A: Substrate surface area