JP3190386B2 - Vacuum film forming equipment - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an insulating film, a passivation film, and a soft error of a semiconductor device or an electrostatic chuck.
The present invention relates to a thin vacuum film forming apparatus used for a film, a dielectric of a plastic capacitor, and the like.

[0002]

2. Description of the Related Art Conventionally, as a method of forming a synthetic resin film, a "wet method" in which a raw material monomer of a synthetic resin is dissolved in an appropriate solvent, applied to a substrate, and polymerized on the substrate, is used. There are known a "polymer vapor deposition method" for vapor deposition on a substrate and a "plasma polymerization method" in which a raw material monomer of a synthetic resin is converted into a plasma state and polymerized in plasma.

[0003]

However, in such a conventional method of forming a synthetic resin film, it is difficult to obtain an extremely thin film in the case of the "wet method", and the adhesion of the synthetic resin to the substrate is insufficient. In addition, impurities such as mixing of the coating liquid and removal (drying) and recovery of the solvent are included, so that impurities are likely to be mixed. In the case of the "polymer vapor deposition method", decomposition and the like occur together with depolymerization, and the degree of polymerization is not sufficient.In the case of the "plasma polymerization method", it is difficult to control the molecular structure due to decomposition of the raw material monomer itself. There were challenges.

Therefore, as disclosed in Japanese Patent Application Laid-Open No. 61-78463, for example, 4,4'-diphenylmethane
An aromatic diisocyanate such as diisocyanate;
For example, a method is known in which an aromatic diamine such as 4,4'-diamino diphenyl ether is used to evaporate both monomers in a vacuum and polymerize the monomer on a substrate to form a urea resin film. Proposed. However, when the shutter is closed in a normal metal vapor deposition or the like, the evaporant does not adhere to the substrate, but when the raw material monomer is evaporated in a vacuum and vapor deposition is performed on the substrate as described above, the shutter is not used. −
The monomer adheres to the substrate even in the closed state.
In the case of a small thin film capacitor or the like, the monomer adhered on the substrate reduces the adhesive force between the substrate and the protective film layer and significantly deteriorates the sealing property.

[0005] The present invention is intended to solve such problems, extra monomer onto a substrate - shall be the object of the invention to provide a vacuum film forming apparatus which can reduce the adhesion of.

[0006]

In order to achieve this object, the present invention provides a vacuum exhaust system 1, a vacuum chamber 2 evacuated by the vacuum exhaust system 1, and evaporating raw material monomers in the vacuum chamber 2. The evaporation source container 5 and the evaporated monomer are steamed on the surface.
And a shutter 7 provided between the base body 3 to wear and the evaporation source container 5 and the substrate 3, to polymerize the motor <br/> Nomar was deposited on the surface of the base body 3 to form a synthetic resin film Melting point of the lowest melting point among monomers in vacuum film forming equipment
The cooling shield plate 6 cooled below the temperature is placed around the evaporation source container 5.
It is installed so as to cover the surroundings, and the shutter 7 is cooled and blocked.
It is characterized by being arranged between the shielding plate 6 and the evaporation source container 5 .

[0007]

According to the conventional method of forming a synthetic resin film, when the substrate is set in a vacuum chamber for 10 minutes while the shutter provided at a position 30 mm above the evaporation port is kept closed, the adherence on the substrate becomes zero. It was confirmed that it adhered with a thickness of 0.2 μm. That is, since the raw material monomer-evaporation source is in a heated state,
The raw material monomer is constantly evaporating from the evaporating port, but since the amount of evaporation is larger than the amount of evacuation, the shutter
A part of the raw material monomer leaked from the surface adheres to the wall surface of the vacuum chamber, but most of the monomer remains in the vacuum chamber. It became clear that this residual monomer also adhered to the substrate transported in the vacuum chamber. In order to prevent the residual monomer from adhering to the base, a shutter is provided by installing a cooled shielding plate that covers the periphery of the raw material evaporation source and the shutter.
The monomer vapor generated in a closed state is blocked from traveling on the substrate by the shielding plate. At the same time, the vaporized monomer is trapped on the cooled shielding plate, so that it is possible to prevent the monomer from adhering to the substrate. The temperature of the cooling shielding plate at this time may be lower than the lowest melting point among the melting points of the raw material monomers used.

[0008]

DESCRIPTION OF THE PREFERRED EMBODIMENTS A vacuum film forming apparatus according to one embodiment of the present invention will be described below .
It will be described with reference to the drawings together with a method of forming a synthetic resin film using the same .

FIG. 1 shows the configuration of a synthetic resin film forming apparatus according to this embodiment. As shown in the figure, a vacuum chamber 2 connected to an evacuation system 1 has a substrate 3 for forming a synthetic resin film.
Are held downward by the base holder-4. An evaporation source 5 for evaporating the raw material monomer is provided below the vacuum chamber 2, and the amount of the raw material monomer evaporated by a heater (not shown) and a thermocouple (not shown). The temperature is controlled so as to be constant. The cooling shield plate 6 is installed so as to cover the periphery of the evaporation source 5, and is exhausted by the vacuum exhaust system 1. A shutter 7 is provided between the cooling shielding plate 6 and the evaporation source 5, and the thickness of the film formed on the base 3 is adjusted by opening and closing the shutter.

Next, an example of a method for forming a urea resin film by a polyaddition reaction using the above apparatus will be described. 4,4 ′ methylene dianiline (melting point 91 ° C.,
Hereinafter, referred to as MDA), 4 is added to the other evaporation source container 5,
4 'diphenyl methane diisocyanate (melting point 39
C., hereinafter referred to as MDI), and the system is evacuated by the vacuum evacuation system 1 until the total pressure of the atmosphere gas in the vacuum chamber 2 becomes 1 × 10 ⁻³ Pa or less with the shutter closed. Then, the heater of the evaporation source container 5 is controlled to set the MDA at 110 ± 1 ° C.
The MDI is heated to 80 ± 1 ° C. At that time, the cooling shielding plate 6 was cooled to a surface temperature of 20 ° C. At this time, the total pressure of the atmosphere gas in the vacuum chamber 2 was 4 × 10 ⁻³ Pa. Next, the substrate 3 was inserted with the shutter 7 closed, left for 20 minutes, and then the substrate 3 was taken out to obtain the deposit A on the substrate.

FIG. 2 shows, as a comparative example, the configuration of a film forming apparatus without a cooling shield plate. Using this device,
Other conditions were exactly the same as those of the film forming equipment of the above-mentioned example, and the deposit B was obtained on the substrate.

[0012] The examples give et a deposit A was not be measured by the thickness step meter of stylus type. Further, the presence or absence of the attached matter could not be confirmed by optical microscope observation. When the film thickness of the deposit B obtained in the comparative example was measured in the same manner, it was 0.5 μm.

Further, a thin film capacitor element having a protective film layer was prepared by the method of forming a synthetic resin film used in the above Examples and Comparative Examples, and subjected to a humidity resistance test (temperature: 60 ° C., humidity:
95%, time: 500 h). FIG. 3 shows the capacitance change, and FIG. 4 shows the dielectric loss. As can be seen from the figure, the device prepared by the method of the example could maintain the characteristics (capacitance, dielectric loss, insulation resistance) before the test, but the method of the comparative example corroded the internal electrode layer in 100 hours. Occurred, and the dielectric loss deteriorated. After a further elapse of time, the corrosion progressed to the element facing portion, and an open defect occurred. From the above results, it was found that, unless the cooling shield plate was provided, extra monomer adhered to the substrate, the adhesion strength between the protective layer for securing the sealing property and the substrate was weakened, and the moisture resistance could not be secured. .

As described above, according to this embodiment, by providing a cooled shielding plate for covering the periphery of the raw material monomer-evaporating source and the shutter, extra monomer can be added to the substrate.
Can be reduced. In this example, the case where a urea resin was used as the synthetic resin was described, but the same effect was obtained even when a polyimide resin was used as the synthetic resin.

[0015]

According to apparent the present invention from the above description of the embodiments according to the present invention, synthetic resin raw material monomers in a vacuum - is evaporated, forming a synthetic resin film by polymerizing the monomer on the substrate In a vacuum film forming apparatus, an unnecessary monomer is prevented from adhering to a substrate by forming a synthetic resin film with a film forming apparatus provided with a cooled shielding plate covering the periphery of a raw material monomer evaporation source. An excellent vacuum film forming apparatus capable of performing the above can be realized.

[Brief description of the drawings]

FIG. 1 is a configuration diagram of a film forming apparatus used in a method of forming a synthetic resin film according to one embodiment of the present invention.

FIG. 2 is a configuration diagram of a film forming apparatus used in a conventional method of forming a synthetic resin film.

FIG. 3 is a diagram showing the results of a humidity resistance test of the capacities of the thin film capacitor elements of Examples and Comparative Examples of the present invention.

FIG. 4 is a view showing a result of a humidity resistance test of dielectric loss of the thin film capacitor element.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Vacuum exhaust system 2 Vacuum tank 3 Substrate 4 Substrate holder 5 Evaporation source container 6 Cooling shielding plate 7 Shutter

 ──────────────────────────────────────────────────続 き Continuing from the front page (72) Inventor Masayuki Iijima 2500 Hagizono, Hagizono, Chigasaki, Kanagawa Prefecture, Japan Inside (72) Inventor Yoshikazu Takahashi 2500, Hagizono, Hagizono, Chigasaki, Kanagawa, Japan (56) References JP-A-63-125655 (JP, A) JP-A-1-263263 (JP, A) JP-A-58-35920 (JP, A) JP-A-3-6363 (JP, A)

Claims (3)

(57) [Claims] An evacuation system (1) and a vacuum chamber (2) evacuated by the evacuation system (1)
And evaporating the raw material monomer in the vacuum chamber (2).Evaporation source
A container (5), on the surface of which the evaporated monomer isEvaporationGroupbody
(3) and the aboveEvaporation sourceBetween the container (5) and the base (3)
And a shutter (7) provided in the base.body
(3)Deposited on the surface ofPolymerize the monomerSynthesisresin
A vacuum film forming apparatus for forming a film, wherein the monomerThe melting point of the lowest melting point
The cooling shielding plate (6) cooled to a predetermined temperature is connected to the evaporation source container (5).
To cover the surrounding area, The shutter (7) is connected to the cooling shield plate (6) and the steam
Placed between the source container (5) Characterized by the fact that
Empty film forming equipment. 2. The vacuum film forming apparatus according to claim 1, wherein said synthetic resin film is a urea resin formed by a polyaddition reaction of diisocyanate and diamine. 3. The vacuum film forming apparatus according to claim 1, wherein the synthetic resin film is a polyimide resin formed by a heat polymerization reaction of a diamine and an acid dianhydride.