JPH04371569A - Vacuum vapor deposition method and device - Google Patents

Abstract

PURPOSE:To deposit a raw material for vapor deposition by evaporation on a substrate with good utilization efficiency by maintaining a high-temp. inert gaseous atmosphere in a vapor deposition chamber at the time of vapor depositing the film of a metal, semimetals, dielectrics or the like on the substrate. CONSTITUTION:The inside of a vessel contg. the substrate and an Ag vapor deposition source is evacuated to a high vacuum of 10<-4> to 10<-2> Pa by a vacuum pump and thereafter an inert gas, such as Ar, is heated to >=373K by a heater and is supplied into the vessel at the time of depositing the Ag film by evaporation on the surface of the single crystal substrate consisting of, for example, NaCl. After the pressure in the vessel is regulated to 0.1 to 10Pa, the Ag evaporating source is heated to evaporate to form the vapor deposited Ag film on the substrate. The Ag as the raw material for vapor deposition is deposited by evaporation on the NaCl substrate with the high vapor deposition efficiency.

Description

[Detailed description of the invention]

0001

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a vapor deposition method and apparatus for efficiently forming metal, semiconductor, dielectric, or other films on a substrate.

0002

2. Description of the Related Art Conventionally, a method is known in which an evaporation source and a substrate are disposed facing each other in a vacuum evaporation apparatus to form a vapor deposited film on the substrate under high vacuum. However, in the above-mentioned normal vapor deposition method, since the vapor of the vapor deposition raw material flows out into the vacuum system, most of the vapor deposition raw material is wasted, and a vapor deposition film cannot be effectively formed.

0003

SUMMARY OF THE INVENTION The present invention aims to solve the above-mentioned drawbacks and to provide a vapor deposition method and a vapor deposition apparatus that can effectively utilize vapor deposition raw materials to form a good vapor deposited film. be.

0004

[Means for Solving the Problems] The present invention provides that after drawing the inside of a vacuum evaporation apparatus to a high vacuum of 10-4 to 10-2 Pa,
0 by introducing an inert gas heated to a high temperature of 3 K or higher.
．． 1 to 10 Pa, and then evaporating the evaporation raw material to form a deposited film on the substrate, and a means for heating the evaporation raw material; A vacuum evaporation apparatus having a substrate, an inert gas inlet pipe, and an exhaust pipe connected to a vacuum pump, characterized in that a heater is disposed around the inert gas inlet pipe or in the inert gas inlet. This is a vapor deposition device.

[0005]

[Effect] In conventional vapor deposition methods, most of the vapor deposition raw material flows out into the vacuum system because it is performed under high vacuum, making it impossible to form a film effectively on the substrate. A small amount often results in a discontinuous thin film, and
Even if a continuous film could be produced, it had drawbacks such as the occurrence of many lattice defects within or at the grain boundaries of the crystal grains that make up the film. Therefore, as a result of examining various vapor deposition conditions, the present inventor found that
It has been found that by introducing a heated inert gas into a vapor deposition apparatus and performing vacuum vapor deposition, vapor deposition efficiency can be significantly improved and a high-quality vapor deposited film can be formed. In particular, the effect was remarkable when an inert gas heated to a high temperature of 373 K or higher was introduced and vacuum deposition was performed under a pressure of 0.1 to 10 Pa. The heating temperature of the inert gas is particularly preferably 800 to 900K. 373K
If it is less than 20%, the above-mentioned drawbacks similar to those of conventional vapor deposition methods cannot be overcome. Also, the pressure of the inert gas is 0.1
If it is less than 10 Pa, no significant effect will be observed compared to the conventional vacuum evaporation method, and if it exceeds 10 Pa, the deposition rate will decrease, making it uneconomical.

[0006] The inert gas used here is H
In addition to rare gases such as e, Ne, Ar, and Kr, N2 gas can be used, and CO2 gas can also be used depending on the purpose. In addition, as the base substrate, mica, S
Examples include cleavage planes of single crystals such as i, NaCl, KCl, etc., clean glass surfaces, carbon evaporated films, and oxide films formed on the surfaces of Al plates.Furthermore, MgO single crystal surfaces, Ge
An oxide film formed on the surface of a single crystal, a deposited SiO film, a deposited MgO film, a Ge plate, etc. can also be used.

FIG. 1 is a conceptual diagram of a vacuum evaporation apparatus which is a specific example of the present invention. In this device, a base substrate is supported by a holder in the center of a chamber connected to a vacuum pump, and a membrane material evaporation source surrounded by a partition plate with an opening at a position opposite to this is placed. An inert gas introduction pipe having an opening was placed nearby, and a gas heater was provided around the introduction pipe and within the introduction part. Although two gas heaters are provided in FIG. 1, one may be omitted if necessary.

[0008]

【Example】

(Example 1) Using the vacuum evaporation apparatus shown in FIG. 1, a surface area of 4
An Ag film was formed on a ×4 mm 2 NaCl single crystal substrate. First, the inside of the device was evacuated to 10-4 Pa with a vacuum pump, then Ar gas heated with a heater set to 800 K was supplied at a flow rate of 25 ml/min, and the pressure inside the device was adjusted to 1 Pa. , Ag evaporation raw material 1300
Evaporation was started by heating to K 2 and deposition was carried out for 1 minute. The obtained Ag film had an average thickness of 13 nm and was found to be a pseudo-single crystal thin film grown parallel to the substrate crystal or oriented at 45 degrees.

(Comparative Example 1) In Example 1, when the inert gas heater was stopped, the temperature of the introduced Ar gas was set to 300K, and other conditions were the same as in Example 1, Ag was deposited. The resulting film had a thickness of 12 nm and was a quasi-single crystal thin film similar to that in Example 1, but contained many lattice defects within the crystal grains and many subgrain boundaries and twin boundaries were observed. . Furthermore, when Ag was deposited in the same manner by setting the Ar gas temperature to 280K, the resulting Ag film had a thickness of 12
nm, but it was found to be a polycrystalline thin film with orientation comparable to that of a film obtained by a conventional vapor deposition method that does not use an inert gas.

(Example 2) In Example 1, introduced Ar
Ag was evaporated for 5 minutes with the gas temperature set at 373K and other conditions the same as in Example 1. Obtained Ag
The film has a thickness of 60 nm and is a continuous single crystal film oriented parallel to the substrate crystal, and a continuous single crystal film grows on the sharp rising surface of the cleavage step existing on the substrate surface as well as on the top surface of the step. I found out that it was.

(Comparative Example 2) In Example 2, introduced Ar
Set the gas temperature to 500K and the pressure inside the device to 0.0
The pressure was adjusted to 1 Pa, and other conditions were the same as in Example 2, and Ag was deposited for 5 minutes. The resulting film has a thickness of 40n
m, and it was found that the polycrystalline thin film had an orientation comparable to that of a film obtained by a conventional vapor deposition method that does not use an inert gas. Furthermore, in this case, it was found that the Ag film did not grow on the sharp rising surfaces of the cleavage steps existing on the substrate surface.

(Example 3) In Example 1, the surface area 2
Area 2 x 40 mm on a 5 x 80 mm2 glass substrate
2 elongated Ag films were formed. Set the temperature of the gas heater to 3
The temperature was set at 73K, and other conditions were the same as in Example 1, and Ag was deposited for 10 minutes. The thickness of the obtained Ag film is
It was found that the film had a thickness of 120 nm and was a polycrystalline film with no orientation. Also, the electrical resistivity of this Ag film is 3×10
-8 Ωm, and it was found that the change in electrical resistance over time was a stable monotonous decrease.

(Comparative Example 3) In Example 3, the introduction of Ar gas was stopped and the pressure inside the apparatus was adjusted to 10-3 Pa, and Ag was evaporated for 13 minutes under the same conditions as in Example 3. . The resulting film had a thickness of 120 nm,
It turned out to be a polycrystalline thin film with no orientation. Also,
The electrical resistivity of this Ag film was 4×10 −8 Ωm, and unlike in Example 3, the electrical resistance changed over time in an unstable manner, and during the change, the electrical resistance suddenly increased twice and then decreased again.

[0014]

[Effects of the Invention] By adopting the above structure, the present invention makes it possible to effectively utilize vapor deposition raw materials and form a high quality vapor deposited film at a high vapor deposition rate.

[Brief explanation of the drawing]

FIG. 1 is a conceptual diagram of a vacuum evaporation apparatus that is an embodiment of the present invention.

Claims (2)

[Claims] Claim 1: The inside of the vacuum evaporation apparatus is 10-4 to 10-2.
After drawing a high vacuum of Pa, inert gas heated to a high temperature of 373 K or higher was introduced to adjust the pressure to 0.1 to 10 Pa.
A vapor deposition method characterized in that the vapor deposition raw material is then evaporated to form a vapor deposited film on the substrate. 2. A vacuum evaporation apparatus comprising: means for heating a vapor deposition raw material; a substrate disposed opposite to the heating means; an inert gas introduction pipe; and an exhaust pipe connected to a vacuum pump. A vapor deposition apparatus characterized in that a heater is arranged around an introduction pipe or within an inert gas introduction part.