JPH0382756A - Ion beam assisted vapor deposition device and method thereof - Google Patents

Abstract

PURPOSE:To efficiently produce uniform films having high quality by forming a guide pipe for supplying a metallic wire for vapor deposition to a specific shape and specifying the speed of vapor deposition of the metal and the value of the current density of an ion beam as well as the correlative relation thereof. CONSTITUTION:The guide pipe 24 is disposed in the direction crossing the liquid level of a crucible 28 near the crucible 28 and is bent in an opposite direction to constantly supply the metallic wire 21 for vapor deposition to a crucible 24. A faraday cup 53 which detects the quantity of the ion beam and an insulator 54 to insulate the vapor deposition device are made into stepped structure. The crossing angle of vapor flow and the ion beam is set within 25 deg.. The evaporation rate R of Ti near a base material is set at 2 to 5Angstrom /S and the current density (p) of the nitrogen ion beam at 30 to 2000muA/Cm<2>. The relation between both is set approximately at p=40R-50. The uniform evaporating metal flow in the ion beam assisted vapor deposition device is thus obtd. and the specified quality of the films, compsn., etc., is obtd.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to an ion beam assisted vapor deposition apparatus and method thereof.

[Prior Art] As a conventional ion beam assisted vapor deposition method, there is, for example, Japanese Unexamined Patent Publication No. 1997-1997. This conventional example relates to a method of forming a TiN (titanium nitride) film, and was previously filed by the inventors of the present invention. The present invention is a different improvement of this conventional example.

A schematic diagram of this conventional device is shown in FIG. This device includes a vapor deposition tank 11, an electron beam evaporation source 15, a vapor deposited metal (metal titanium) 18, an ion gun 1B, and a vapor deposited metal (metal titanium).
The device includes a crystal oscillator 13 that detects the amount of evaporation for controlling the amount of evaporation of the crystal oscillator 18, a rate controller 14 that controls the crystal oscillator 13, and the like.

On the other hand, the hoop-shaped substrate 12 to which hydrogen is attached is an electron beam evaporation source (5
and located at a position facing the ion gun 16.

In such an apparatus, the deposited metal (metallic titanium) 18 on the electron beam evaporation source 5 is evaporated by heating with the electron beam. The vapor-deposited metal (metallic titanium) 18 is supplied by a certain amount of vapor-deposited film B (
This is done by supplying titanium metal (metal titanium) 18. On the other hand, the ion gun 16 irradiates nitrogen gas as an ion beam onto the substrate 12 to be vapor deposited to form a TiN film on the substrate 2 to be vapor deposited. At this time, a crystal oscillator 13 installed in a position where the nitrogen gas ion beam does not reach inside the deposition tank 1 and a rate controller 14 outside the deposition tank 1
Film formation is controlled. On the other hand, the amount of ion beam is detected and controlled by a Faraday cup (not shown).

The vapor deposited film formed in this way is not necessarily
It is formed not only on the vapor deposition tank 11 but also on the wall surface of the vapor deposition tank 11 or the mask plate 65 (shown in FIG. 6). Once a vapor deposited film is formed on the wall of the first vapor deposition tank, it is difficult to remove it later.
As shown in the figure, an anti-adhesion plate 62 made of polished stainless steel plate etc.
will be established. Therefore, vapor-deposited metal is deposited on the deposition prevention plate 62 and the mask plate 65.

After completing a series of operations, the vapor deposition tank 11 is opened to the atmosphere by introducing air, and the substrate 12 to be vapor deposited is taken out.

[Question to be solved by the invention 91 The inventors of the present invention have clarified the following problems as a result of various research experiments aimed at stabilizing the quality and reducing the cost of ion beam assisted vapor deposition films. .

The vapor-deposited metal (metallic titanium) 18 is supplied to the vapor-deposited 11 base material 12
A certain amount of vapor-deposited metal (metallic titanium) 1B each time the
However, it is impossible to maintain a constant liquid level of molten titanium during vapor deposition using this method.
Therefore, the flow of evaporated metal changes, which is one of the causes of quality variations in film quality, composition, etc.

A golden Ti of constant quality that is dense, corrosion resistant, and has excellent adhesion.
To obtain NffJ, clarify the titanium evaporation rate, nitrogen ion beam current density, and their correlation, and use 82
It must be managed so that the formation is 1I. Furthermore, it is necessary to set conditions that allow stable ion beam irradiation. The quality also depends on the geometrical positional relationship among the substrate 12 to be evaporated, the electron beam evaporation source I5, the ion gun 16 (nitrogen ion beam), and the like.

Among the various factors mentioned above, a metal Faraday cup is used to detect the ion beam current density, but the insulator that insulates the Faraday cup and the evaporation tank 11 (which is grounded) is easily contaminated with evaporation metal, etc., making it difficult to maintain its function. is difficult. Therefore, there is a problem that detection of the ion beam current density becomes unstable, and as a result, stable irradiation of the ion beam cannot be performed.

Next, as described above, a polished stainless steel plate is used as the deposition prevention plate 62 on the wall of the evaporation tank 11, but as the evaporation metal accumulates, it gradually becomes flaky as shown in FIG. 7(a). Eventually, it will peel off and fall off. When these flaky deposits fall onto the ion gun 16, a short circuit occurs, causing the ion gun 6 to stop or become unstable. In order to prevent this, there is a problem in terms of production efficiency that the adhesion prevention plate 62 must be frequently replaced and cleaned. The same thing can be said about the mass plate 65 as well.

Next, when releasing the inside of the deposition tank 11 to the atmosphere, there is a problem that the air contains a large amount of water and oxygen, so they are adsorbed and oxidized everywhere inside the deposition tank 11, and the ion gun 1
There was a problem that the rise time of 6 was long.

The purpose of the present invention is to solve the above-mentioned problems, set optimal conditions, and provide a method that can efficiently produce a uniform, high-quality deposited film at low cost while satisfying the optimal conditions. be.

[Means for solving T5B] The present invention has the following means to achieve the above object.

In order to form a uniform and high quality deposited film, the supply of deposited metal in the electron beam evaporation source 15 is made constant.

In other words, the evaporation speed of the deposited metal is stabilized by continuously supplying the metal. Furthermore, we will monitor the ion beam and control its stability by improving the Faraday cup. Also the metal evaporation speed, ion beam current density! & Clarify the setting of appropriate values and the correlation between those values. At the same time, the optimum geometric positional relationship between the substrate material to be deposited 2, the electron beam evaporation source 15, and the ion gun 16 is set.

In the deposition prevention plate 62 and the mask plate 65, the surfaces on which the vapor-deposited metal scatters and adheres are roughened to make it difficult to peel off. In addition, even if it peels off and falls, the effect on the ion gun 16 and the like can be ignored in terms of production.

When releasing into the atmosphere, first a low pressure inert gas is injected and the inside of the vapor deposition tank If is heated to prevent moisture absorption and oxidation, and then an ion generating gas is injected and supplied, and the tank is released into the atmosphere. A heating device is installed to heat one such vapor deposition tank.

[Function] An apparatus for continuously supplying a vapor-deposited metal wire to a crucible and melting and evaporating the vapor-deposited metal wire as described in claim 1(a), which is located in the vicinity of the crucible and is located near the crucible to supply the vapor-deposited metal wire to the crucible. By arranging the guide vibrator in the direction perpendicular to the liquid surface of the crucible and bending it in the opposite direction, the evaporated metal wire can be continuously supplied at a constant speed for a long period of time, and the evaporation flow can be reduced. can be kept constant.

As described in claim 1 (b), the ion beam detection device is stable for a long time because the insulator that insulates the Faraday cup for detecting the amount of the ion beam and the evaporation device has a stepped structure. It becomes possible to detect ion beams.

As recited in claim 1 (c), the apparatus includes an electron beam evaporation source and an ion gun, which are set so that the intersection angle between the evaporation flow and the ion beam is within 25 degrees; As described in claim 2 (f), in the formation of a titanium nitride film by the ion beam assisted vapor deposition method, the titanium evaporation rate (R) and the nitrogen ion beam current density (p) in the vicinity of the substrate to be vaporized are R=2~5Å/S, respectively.
p=30~200μA/c! r, and the R and the p
A method for forming a titanium nitride film in which the relationship between
As described above, by adopting a film forming method in which the substrate to be deposited is grounded, stable production of a TiN golden film can be achieved under optimal conditions.

As recited in claim 1 (d), the apparatus is provided with a substrate to be evaporated interposed between the electron beam evaporation source and an adhesion prevention plate with a roughened surface; As described in claim 2 (h), by using a film forming method in which a mask plate with a roughened surface is closely placed on a substrate to be deposited, peeling and falling of deposited metal can be prevented. The amount is significantly reduced, allowing long-term operation. In addition, the vapor deposition particles that had fallen in the form of flakes become fine powder, and the influence of falling becomes extremely small.

As described in claim 1 (e), a heating device for heating the inside of the vapor deposition tank is provided, and as described in claim 2 (su), the vapor deposition tank is heated. In the method of releasing to the atmosphere, inert gas is supplied to the vapor deposition tank in a low pressure state and heated, and then the gas of the ion generating means is supplied and released to the atmosphere, thereby eliminating the risk of moisture absorption and oxidation. disappears.

[Example] Next, as a specific example, the formation of T i NU as a surface treatment for an electric razor blade will be described.

FIG. 1 is a schematic diagram of ion beam assisted vapor deposition carbon according to the present invention. This device consists of a vapor deposition tank 11, an electron beam evaporation source 5, an ion reader 6, a crystal oscillator I3 for detecting and controlling the amount of evaporation of titanium metal, a rate controller 4, a substrate I2 to be vaporized, a vacuum pump 68, etc. ing.

The electron beam evaporation source 5 is a continuous supply bag @ 20. of metal titanium wire 2 as shown in FIG. It consists of an electron gun 25 and a crucible 28. FIG. 3 shows the relationship between the tip bending angle θ of the supply guide pipe 24 of two metal titanium wires and the continuous processing feed time, which was experimentally determined. Second
In the figure, a continuous supply device 112 for two metal titanium wires is shown.
0 is a supply roll 22, a bending straightening roll 23 for straightening the curl of the metal titanium wire 2, a guide pipe 24 for sending the metal titanium wire 2 to a predetermined position immediately above the crucible 28, and a vapor-deposited metal It is equipped with a water cooling block 26 for preventing deformation of the guide pipe 24 due to heat during melting and evaporation, a drive roll 27 for feeding the metal titanium wire 2I at a constant speed, and the like.

When operating the device, the bending angle of the tip of the guide vibrator 24 (
θ) is a major factor in determining the continuous supply time of the metal titanium wire 21. As shown in FIG. 3, when the tip bending angle (θ) is in the range of 0 to 5 degrees, the evaporated material in the crucible 28 is not uniformly melted immediately after the start of evaporation, and a hard zone exists locally, causing the metal titanium to melt. When the wire 2 contacts the 82-quality zone, the metal titanium wire 21 is deformed at the entrance of the guide pipe 24, making continuous supply impossible.

If the tip bending angle (θ) exceeds 8 degrees, it will deviate from the trajectory of the electron beam used to melt the deposited metal, making it impossible to supply the deposited metal to the crucible 28. Therefore, in order to perform stable continuous supply, it is necessary to set the tip bending angle (θ) to 5 to 8 degrees.

Vapor deposition conditions are set to uniformly and stably form golden T1Ni using the ion beam assisted vapor deposition method using a mesh blade plate for an electric razor made of stainless steel as the substrate 12 to be vapor deposited. The color tone of the TiN film is determined by its composition and structure. In order to keep the composition constant, it is necessary to control the titanium evaporation rate and nitrogen ion beam current density near the substrate as operating conditions. Experiments were conducted with a titanium evaporation rate (R) of 2 to 5 A/S and a nitrogen ion beam current density (ρ) of 30 to 200 μA/CIl+.
It has been found that a golden film can be obtained by performing vapor deposition under the conditions of 0.R-50. At this time, the value of the nitrogen ion beam current density ρ must be kept within ±8% accuracy. Further, in order to stabilize the ion beam irradiation, the substrate 12 to be deposited must be grounded.

The geometrical positional relationship between the evaporated @substrate work 2, the electron beam evaporation source work 5, and the ion gun 16 must also be considered. As shown in FIG. 1, the distance between the substrate 12 to be evaporated and the ion reader 6 is LIG, and the distance between the substrate 2 to be evaporated and the electron beam evaporator 15 is LllllB, and the distance between the substrate 12 to be evaporated and the electron beam evaporator 15 is LllllB, and the distance between the substrate 12 to be evaporated and the ion beam evaporator 6 is to be created by the ion reader 6. If the angle between the evaporation flow created by the ion beam and the electron beam evaporation source I5 is σ, LIG = 400~9
The experiment was conducted at 00aln and LBB=400 to 1000mm. As a result, it was found that the angle σ must be within 25 degrees.

In setting the above conditions, a Faraday cup 53 as shown in FIG. 4 was used to measure the ion beam. The amount of ion beam detected by the Faraday cup 53 is displayed by an ammeter 55 provided outside the vapor deposition tank 1. When using the Faraday cup 53 in a vapor deposition apparatus, the Faraday cup 53 and f! A@The insulator 54 that insulates the equipment is made of vapor-deposited metal (
In Fig. 4, it is easy to get dirty with titanium particles 51) (it is difficult for the conventional type to maintain its function). For this purpose, an evaporation flow guide 56 is provided which prevents the evaporation flow from going around and restricts the secondary electrons from entering the Faraday cup 53 by restricting the intake of the ion beam (nitrogen ions 52 in FIG. 4). The shape of the insulator 54 is stepped so that even if vapor-deposited metal adheres to the insulator 54, insulation can be maintained. As shown in FIG. 5, which is a time chart of the operation of the vapor deposition apparatus, the amount of ion beam can be detected with a Faraday cup 53 throughout the ion beam assisted vapor deposition and displayed outside the vapor deposition tank 1 for monitoring.

Next, as for the deposition prevention plate 62 and the mask plate 65, in order to prevent the deposited metal from becoming flakes and peeling off and falling, as shown in FIG. At least the surface to which the vapor-deposited metal adheres of the mask plate 65, which is disposed closely to the deposition plate 62 and the substrate I2 to be vapor-deposited, is blast-polished.

The purpose of this blast polishing is to roughen the surfaces of the adhesion prevention plate 62 and the mask plate 65, and the method is not limited. In particular, the adhesion prevention plates 62 are installed closely near the electron beam evaporation source 15. Deposition prevention plate 62 and mask plate 65
Due to the roughening of the surface, peeling and falling of the attached vapor-deposited metal 66 is significantly reduced, allowing continuous operation for a long time. Also, the seventh
As shown in Fig. 7(a), the deposited metal 66, which had conventionally peeled off and fallen in the form of flakes, is now in the form of fine powder and falls under the ion gun, as shown in Fig. 7(b). The influence on devices such as 16 can be reduced.

The release of the vapor deposition tank 11 to the atmosphere after ion beam assisted vapor deposition will be explained with reference to FIG. First, an inert gas such as nitrogen gas is used as the gas, and the gas pressure is 2 k.
It is supplied from liquid nitrogen 84 as a low pressure gas of less than g/al. In addition, in order to prevent dew condensation within the vapor deposition tank 11, the inside of the vapor deposition tank 11 is heated to 40° C. or higher using a halogen lamp 85 before leakage occurs. Further, a small amount of the same gas (nitrogen gas) is leaked from the gas cylinder 88 through the gas flow rate regulator 87 to the gas introduction part F of the ion generating means when the gas is released to the atmosphere. Even after it is released into the atmosphere, the gas is kept flowing until it is evacuated again. By releasing the gas to the atmosphere in this manner, the evacuation time and the start-up time of the ion gun 16 can be shortened.

[Effects of the Invention] By using the method and the configuration of the apparatus as described above, the following effects can be obtained.

As described in claim 1 (a), there is provided an apparatus for continuously supplying a vapor-deposited metal wire to a crucible to melt and evaporate it, the device being located near the crucible and for supplying the vapor-deposited metal wire. By arranging the guide pipe in the direction perpendicular to the liquid level of the crucible and bending it in the opposite direction, the vapor-deposited metal wire can be supplied continuously for a long period of time at a constant speed. The effect is that the liquid level of molten titanium is kept constant, and therefore the flow of evaporated metal is constant, and a deposited film with constant quality such as film quality and composition can be efficiently produced.

As described in claim 1 (b), the ion beam detection device has a stepped structure insulator that insulates the Faraday cup for detecting the amount of ion beam and the evaporation device, thereby improving the insulation of the insulator. Deterioration is less likely to occur, and the ion beam current density can be stably detected, which in turn enables stable ion beam irradiation and enables efficient production.

As recited in claim 1 (c), the apparatus includes an electron beam evaporation source and an ion gun, which are set so that the intersection angle between the evaporation flow and the ion beam is within 25 degrees; As described in claim 2 (f), in the formation of a titanium nitride film, the titanium evaporation rate (R) and the nitrogen ion beam current density (p) in the vicinity of the substrate to be deposited are respectively:
R=2~5λ/S, p=30~200μA/-,
The method for forming a titanium nitride film in which the relationship between the R and the p is approximately p=40R-50, and as described in claim 2 (g), the substrate to be deposited is grounded. By employing a film forming method performed in this manner, it is possible to obtain a gold-colored TiNM that is dense, has excellent corrosion resistance, and has a constant quality of adhesion under optimal conditions.

As described in claim 1 (d), an apparatus having a substrate to be evaporated interposed between a single beam evaporation source and an adhesion prevention plate having a roughened surface; What I did,
And, as described in claim 2 (h), by using a film forming method in which a mask plate with a roughened surface is closely placed on the substrate to be vapor deposited, the adhering vapor deposited metal peels off and falls off. In addition, the amount of peeling and falling of the vapor-deposited metal changes from flakes to fine powder, and the number of stops of the ion gun is greatly reduced, making it possible to operate for a long time. Furthermore, this eliminates the need for frequent replacement and cleaning of the adhesion prevention plate, resulting in the effect of increasing production efficiency. The same thing can be said about mask plates.

As described in claim 1 (e), a heating device for heating the inside of the steam Wfi is provided;
As described in claim 2, in a method of opening a vapor deposition tank to the atmosphere, an inert gas is supplied into the vapor deposition tank in a low pressure state and heated, and the gas of the ion generating means is By supplying water and releasing it to the atmosphere, there is no need to worry about moisture absorption or oxidation. This has the effect of solving the conventional problem of adsorption and oxidation everywhere in the deposition tank, which prolongs the evacuation time or the start-up time of the ion gun.

[Brief explanation of drawings]

FIG. 1 is a schematic diagram of an apparatus for explaining an embodiment of an ion beam assisted vapor deposition apparatus of the present invention, FIG. 2 is a schematic diagram of an apparatus for explaining an embodiment of an electron beam evaporation source of the present invention, and FIG. 4 is a correlation diagram showing the experimental results of the electron beam evaporation source of the present invention, FIG. 4 is a structural diagram showing an embodiment of the ion beam detection device of the present invention, and FIG. 5 is for explaining the operation of the evaporation device of the present invention. 6 is a schematic diagram of an apparatus for explaining the deposition prevention plate and the mask plate. FIG. 7(a) is an operation explanatory diagram for explaining the conventional deposition prevention plate. (b) is an operation explanatory diagram for explaining the present invention in detail, FIG. 8 is a schematic diagram of the apparatus for explaining the method of releasing the vapor deposition apparatus of the present invention to the atmosphere, and FIG. 9 is a conventional vapor deposition apparatus. It is a schematic diagram. II...41 tank E2...Substrate to be evaporated 13...Crystal oscillator E4...Late controller E5...
Electron beam evaporation source Engineering 8... Ion gun 18... Evaporated metal (metal titanium) 25... Electron gun 53...
・Faraday cup... Anti-adhesive plate 5... Mask plate Patent applicant Matsushita Electric Works Co., Ltd. Representative patent attorney Taketoshimaru (2 idiots) 4th WJ 15 Figure & Tsuji

Claims (2)

[Claims] (1) An ion beam assisted vapor deposition apparatus comprising at least one of the following apparatuses. (a) An apparatus for continuously supplying a vapor-deposited metal wire to a crucible to melt and evaporate it, the apparatus being located near the crucible and having a guide pipe for supplying the vapor-deposited metal wire in a direction perpendicular to the liquid level of the crucible. A vapor-deposited metal wire feeding device that is placed in the opposite direction and bent in the opposite direction. (b) An ion beam detection device that has a stepped structure with an insulator that insulates a Faraday cup that detects the amount of ion beam and a vapor deposition device. (c) An apparatus comprising an electron beam evaporation source and an ion gun, which are set so that the intersection angle between the evaporation flow and the ion beam is within 25 degrees. (d) An apparatus having a substrate to be evaporated interposed between the electron beam evaporation source and an adhesion prevention plate with a roughened surface. (e) A heating device for heating the inside of the vapor deposition tank. (2) An ion beam assisted vapor deposition method comprising at least one of the following methods. (f) Titanium evaporation rate (R) and nitrogen ion beam current density (p) near the substrate to be deposited in the formation of a titanium nitride film
) are respectively R=2-5 Å/S, p=30-200 μÅ/c
m^3, and the relationship between the R and the p is approximately p=4
A method for forming a titanium nitride film that is 0R-50. (g) A film forming method performed by grounding the substrate to be deposited. (H) A film forming method in which a mask plate with a roughened surface is closely placed on a substrate to be deposited. (i) A method of opening a vapor deposition tank to the atmosphere, in which an inert gas is brought into a low pressure state and is supplied into the vapor deposition tank and heated, and then gas from an ion generating means is supplied and released to the atmosphere.