JP2670391B2 - Polycrystalline thin film manufacturing 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 apparatus for producing a polycrystalline thin film having a uniform crystal orientation.

[0002]

2. Description of the Related Art Oxide superconductors discovered in recent years are excellent superconductors having a critical temperature exceeding the temperature of liquid nitrogen. At present, this type of oxide superconductor is a practical superconductor. There are various problems to be solved in order to use this. One of the problems is that the critical current density of the oxide superconductor is low.

[0003] The problem that the critical current density of the oxide superconductor is low is largely due to the existence of electrical anisotropy in the crystal itself of the oxide superconductor. It is known that electricity easily flows in the a-axis direction and the b-axis direction of the crystal axis, but hardly flows in the c-axis direction. From such a viewpoint, in order to form an oxide superconductor on a base material and use it as a superconductor, an oxide superconductor having a good crystal orientation is formed on the base material, and It is necessary to orient the a-axis or b-axis of the crystal of the oxide superconductor in the direction in which electricity is to flow, and to orient the c-axis of the oxide superconductor in the other direction.

Therefore, various means have heretofore been attempted to form an oxide superconducting layer having good crystal orientation on a substrate such as a substrate or a metal tape. As one of the methods, a single crystal base material such as MgO or SrTiO ₃ having a crystal structure similar to that of an oxide superconductor is used, and an oxide superconducting layer is formed on these single crystal base materials by a film forming method such as sputtering. A method has been implemented.

If a film forming method such as sputtering is performed using the single crystal base material of MgO or SrTiO ₃ , the crystal of the oxide superconducting layer grows on the basis of the crystal of the single crystal base material. It is possible to improve the orientation, and the oxide superconducting layer formed on these single-crystal substrates exhibits a sufficiently high critical current density of about several hundred thousand to several million A / cm ^2. It is known to

[0006]

In order to use an oxide superconductor as a conductor, it is necessary to form an oxide superconducting layer having good crystal orientation on a long base material such as a tape. is there. However, if an oxide superconducting layer is formed directly on a base material such as a metal tape, the metal tape itself is polycrystalline and its crystal structure is significantly different from that of the oxide superconductor. Layers cannot be formed at all. In addition, there is a problem in that the heat treatment performed when forming the oxide superconducting layer causes a diffusion reaction between the metal tape and the oxide superconducting layer, which breaks down the crystal structure of the oxide superconducting layer and deteriorates the superconducting characteristics.

Therefore, conventionally, on a base material such as a metal tape,
2. Description of the Related Art An intermediate layer such as MgO or SrTiO ₃ is coated by using a sputtering apparatus, and an oxide superconducting layer is formed on the intermediate layer. However, the oxide superconducting layer formed on the intermediate layer of this kind by a sputtering apparatus has a critical current density much lower than that of the oxide superconducting layer formed on the single crystal substrate (for example, several thousand to 10,000 A / cm ^2). ) There was a problem that it showed only the degree. This is considered to be due to the following reason.

FIG. 16 shows a sectional structure of an oxide superconducting conductor in which an intermediate layer 2 is formed on a base material 1 such as a metal tape by a sputtering device, and an oxide superconducting layer 3 is formed on the intermediate layer 2 by a sputtering device. It shows. Here, FIG.
In the structure shown in (1), the oxide superconducting layer 3 is in a polycrystalline state, and a number of crystal grains 4 are randomly combined. Looking at each of these crystal grains 4 individually, the c-axis of the crystal of each crystal grain 4 is oriented perpendicular to the substrate surface, but the a-axis and b-axis are oriented in a random direction. It is thought that it is. Thus, for each crystal grain of the oxide superconducting layer, a
When the directions of the axis and the b-axis become disordered, it is considered that the quantum coupling of the superconducting state is lost at the crystal grain boundaries in which the crystal orientation is disordered, resulting in a decrease in the superconducting properties, particularly the critical current density. The oxide superconductor is in a polycrystalline state in which the a-axis and b-axis are not oriented because the intermediate layer 2 formed thereunder is in a polycrystalline state in which the a-axis and the b-axis are not oriented. This is probably because the oxide superconducting layer 3 grows so as to match the crystal of the intermediate layer 2 when the oxide superconducting layer 3 is formed.

[0009] In addition to the application fields of the oxide superconductor, techniques for forming various alignment films on a polycrystalline base material by a sputtering apparatus are used. For example, in the field of optical thin films, the field of magneto-optical disks, the field of wiring boards, the fields of high-frequency waveguides, high-frequency filters, and cavity resonators. The problem is to form a good polycrystalline thin film. That is, if the crystal orientation of the polycrystalline thin film is good, the quality of the optical thin film, the magnetic thin film, and the wiring thin film formed thereon is improved.
It is more preferable if an optical thin film, a magnetic thin film, a thin film for wiring, and the like having good crystal orientation can be directly formed on a substrate.

As a core material of a magnetic head used in a high frequency band, a magnetic thin film such as permalloy or sendust which has high magnetic permeability and is thermally stable has been put to practical use. Conventionally, these magnetic thin films are formed on a predetermined substrate by vapor deposition or sputtering. However, if these magnetic thin films have low crystal orientation, it is difficult to control the magnetic anisotropy of the magnetic thin film. And the orientation of the crystal grains becomes disordered in the film plane, and there is a problem that the high frequency characteristics of the magnetic permeability are impaired. In addition, when the axial direction of the crystal axis in the film plane is disordered, local fluctuation called skew or ripple occurs in the in-plane magnetization, and the high-frequency characteristic of the magnetic permeability is impaired as described above. .

SUMMARY OF THE INVENTION The present invention has been made to solve the above-mentioned problem, and has a crystal axis c perpendicular to a film-forming surface of a substrate.
The axis can be oriented, and at the same time, the a-axis and b-axis of the crystal axis of the polycrystalline thin film can be aligned along a plane parallel to the film forming surface, thereby producing a polycrystalline thin film with excellent crystal orientation. The object is to provide a device that can

[0012]

According to the first aspect of the present invention, there is provided a substrate on which a polycrystalline thin film is formed.
Base material holder that supports the base material and the base material mounting surface of the base material holder
A zirconia-stabilized surface facing diagonally to the
And a sputter that sputters the constituent particles of the target.
The putter means and the base material mounting surface of the base material holder are inclined.
The ion source that irradiates rare gas ions from the
Stored in a container that can be evacuated,
Is the upper support plate joined to the bottom of the substrate holder and
Lower support plate pin-connected to the lower support plate and this lower support plate
It is equipped with a base to support the upper support plate and lower support
Angle that allows the relative angle of the plate to be adjusted through the pin joint
An adjusting mechanism is provided for the ionization of the rare gas from the ion source.
Beam to the substrate deposition surface at the desired inclination angle.
The ion beam is obliquely directed to the upper surface of the substrate.
C-axis of each crystal grain by sputtering while irradiating from the direction
Is perpendicular to the film-forming surface of the substrate, or the a-axis of each crystal grain or
Stabilized zirconia having a grain boundary tilt angle of 30 degrees or less formed by the b-axis
The feature is that the polycrystalline thin film can be formed freely.
In order to solve the above-mentioned problems, the invention according to claim 2
In the above configuration, the metal tape delivery device and the
A take-up device is provided, and gold is fed from the sending device to the substrate holder.
Metal tape can be sent out freely and metal on the base holder
The tape is configured to be freely wound by a winding device.

[0013]

When the constituent particles struck out of the target by sputtering are deposited on the film-forming surface of the base material, ions are simultaneously irradiated from an oblique direction, so that the constituent particles are efficiently activated. In addition to the c-axis orientation, the a-axis orientation and the b-axis orientation are also improved with respect to the film formation surface. As a result, even in the case of a polycrystalline thin film in which a large number of crystal grain boundaries are formed, all of the a-axis orientation, the b-axis orientation, and the c-axis orientation of each crystal grain are improved, and the film quality is improved. A crystalline thin film is obtained.
Further, in order to form a polycrystalline thin film having such good orientation, it is preferable that the ion irradiation angle be in the range of 40 to 60 degrees . Therefore, by operating the angle adjusting mechanism to adjust the ion irradiation angle to a suitable angle, a polycrystalline thin film with good orientation can be obtained. Also, the angle adjustment mechanism
The upper support plate connected to the bottom of the substrate holder and its
By adjusting the angle of the lower support plate that is pin-connected to
The on-illumination angle can be easily adjusted. Next, polycrystalline thin film
As specifically, stabilized zirconia can be used,
Irradiating rare gas ions from the diagonal direction onto the substrate film formation surface produces the same result.
Sometimes based on sputtered particles of stabilized zirconia from an oblique direction
The c-axis of each crystal grain is formed on the substrate
Formed by a-axis or b-axis of each crystal grain perpendicular to the film surface
Polycrystalline thin film of stabilized zirconia with grain boundary tilt angle of 30 or less
A film can be formed. Next, the metal tape delivery device is placed inside the container.
Setting up and winding device, from the delivery device to the substrate holder
Metal tape can be sent out freely and gold on the substrate holder
By configuring the generic tape to be freely wound by the winding device,
Continuous deposition of polycrystalline thin film on a long metal tape
it can.

[0014]

Embodiments of the present invention will be described below with reference to the drawings. FIG. 1 shows an embodiment of the apparatus of the present invention. The apparatus of this embodiment has a configuration in which an ion source for ion beam assist is provided in a sputtering apparatus.
The apparatus according to this embodiment includes a base material holder 11 for holding a base material A.
And a plate-like target 12 that is disposed diagonally above the substrate holder 11 at a predetermined interval, and opposed diagonally above the substrate holder 11 at a predetermined interval, and
An ion source 13 arranged apart from the target 12;
The apparatus mainly includes a sputter beam irradiation device 14 disposed below the target 12 toward the lower surface of the target 12. Reference numeral 15 in the drawing indicates a target holder holding the target 12.

The apparatus of this embodiment is housed in a vacuum container (not shown) so that the periphery of the substrate A can be maintained in a vacuum atmosphere. Further, an atmosphere gas supply source such as a gas cylinder is connected to the vacuum vessel, and the inside of the vacuum vessel is kept in a low pressure state such as a vacuum, and an inert gas atmosphere containing argon gas or another inert gas atmosphere or oxygen. The atmosphere can be set.

The substrate A has various shapes such as a plate, a wire, and a tape. The substrate A is made of a metal material or alloy such as silver, platinum, stainless steel, or copper, or various types of glass or metal. It is made of various ceramics. When a long metal tape (a tape made of Hastelloy or stainless steel) is used as the base material A, a feeding device and a winding device for the metal tape are provided inside the vacuum vessel, and the feeding device is continuously controlled from the feeding device. Base material A on material holder 11
It is preferable that the polycrystalline thin film can be continuously formed on the tape-shaped substrate by feeding the film and subsequently winding the film with a winding device.

The substrate holder 11 has a heater therein so that the substrate A positioned on the substrate holder 11 can be heated to a required temperature. An angle adjusting mechanism D is attached to the bottom of the substrate holder 11. The angle adjusting mechanism D includes an upper support plate 5 joined to the bottom of the substrate holder 11, a lower support plate 6 pin-connected to the upper support plate 5, and a base 7 for supporting the lower support plate 6. Is mainly composed. The upper support plate 5 and the lower support plate 6 are configured to be rotatable with respect to each other via a pin connection portion, so that the horizontal angle of the base material holder 11 can be adjusted .

The target 12 is for forming a target polycrystalline thin film, and has the same composition or a similar composition as the target polycrystalline thin film.
Specifically, as the target 12, MgO or Y ₂
Zirconia (YSZ), MgO, Sr stabilized with O ₃
TiO ₃ or the like is used, but is not limited to this, and a target suitable for the polycrystalline thin film to be formed may be used.

The ion source 13 has a structure in which an evaporation source is housed in a container and an extraction electrode is provided near the evaporation source. Then, a part of the atoms or molecules generated from the evaporation source is ionized, and the ionized particles are controlled by an electric field generated by an extraction electrode and irradiated as an ion beam. There are various methods for ionizing particles, such as a DC discharge method, a high-frequency excitation method, a filament method, and a cluster ion beam method. The filament type is a method in which a tungsten filament is energized and heated to generate thermoelectrons, which are collided with evaporated particles in a high vacuum to be ionized. In the cluster ion beam method, clusters of aggregated molecules coming out of vacuum from a nozzle provided at an opening of a crucible containing raw materials are bombarded with thermal electrons to be ionized and emitted. In this embodiment, the ion source 13 having the internal structure shown in FIG. 2 is used. The ion source 13 includes an extraction electrode 17, a filament 18, and an introduction tube 19 such as an Ar gas inside a cylindrical container 16, and can irradiate ions from a tip of the container 16 in a beam shape in parallel. Things.

As shown in FIG. 1, the ion source 13 has its central axis S inclined at an angle θ with respect to the upper surface (film forming surface) of the substrate A.
Therefore, they are inclined and face each other. Is preferably in the range of 40 to 60 degrees, and particularly preferably about 45 degrees. Therefore, the ion source 13 is arranged so as to be able to irradiate ions at an inclination angle θ with respect to the upper surface of the substrate A. The ions to be irradiated on the substrate A by the ion source 13 are mixed ions of argon and oxygen, or He ⁺ ,
Rare gas ions such as Ne ⁺ , Ar ⁺ , Xe ⁺ , and Kr ⁺ , or mixed ions of these and oxygen may be used.

The sputter beam irradiator 14 has the same configuration as the ion source 13 and can irradiate the target 12 with ions to strike out constituent particles of the target 12. In the apparatus of the present invention, it is important that the constituent particles of the target 13 can be beaten out. Therefore, a voltage is applied to the target 12 with a high-frequency coil or the like so that the constituent particles of the target 12 can be beaten out. The sputter beam irradiation device 14 may be omitted.

Next, by using the apparatus having the above-mentioned structure, Y is applied onto the base material A.
A case of forming a polycrystalline thin film of SZ will be described. In order to form a polycrystalline thin film on the substrate A, a target of YSZ is used, and ions irradiated from the ion source 13 are adjusted to an angle of about 45 degrees on the upper surface of the substrate holder 11 by adjusting the angle adjusting mechanism D. So that it can be irradiated with. Next, the base material A
The inside of the container containing the is evacuated to create a reduced pressure atmosphere. Then, the ion source 13 and the sputter beam irradiation device 14 are operated.

When the target 12 is irradiated with ions from the sputtering beam irradiation device 14, the constituent particles of the target 12 are beaten out and fly over the substrate A. And the base material A
At the same time, the constituent particles struck out of the target 12 are deposited, and at the same time, a mixed ion of Ar ions and oxygen ions is irradiated from the ion source 13. The irradiation angle θ at the time of this ion irradiation is most preferably 45 degrees, and is preferably in the range of 40 to 60 degrees. If θ is 90 degrees, the c-axis of the polycrystalline thin film is oriented at right angles to the deposition surface of the substrate A, but the (111) plane stands on the deposition surface of the substrate A, which is not preferable. . When θ is 30 degrees, the polycrystalline thin film does not even have c-axis orientation. If the ion irradiation is performed at an angle in the preferable range as described above, (10)
0) Face comes to stand.

By performing sputtering while performing ion irradiation at such an irradiation angle, the a-axis and the b-axis of the crystal axes of the YSZ polycrystalline thin film formed on the substrate A can be oriented. This seems to be due to the fact that the sputtered particles being deposited are efficiently activated by ion irradiation at an appropriate angle.

FIG. 3 shows a substrate A on which a polycrystalline thin film B of YSZ is deposited by the above method. Polycrystalline thin film B shown in FIG.
Has fine crystal grains 20 having a cubic crystal structure,
A large number of the crystal grains 20 are bonded and integrated via a crystal grain boundary, and the c-axis of the crystal axis of each crystal grain 20 is oriented at right angles to the upper surface (film formation surface) of the base material A, The axes a and b are oriented in the same direction and are in-plane oriented. The c-axis of each crystal grain 20 is oriented at right angles to the (upper surface) deposition surface of the substrate A. The a-axis (or b-axis) of each crystal grain 20 is joined and integrated at an angle between them (a grain boundary inclination angle K shown in FIG. 4) of 30 degrees or less.

After the YSZ polycrystalline thin film B is formed on the substrate A as described above, an oxide superconducting layer is formed on the polycrystalline thin film B. In order to form the oxide superconducting layer on the polycrystalline thin film B, sputtering is performed in an oxygen gas atmosphere or the like using a target having a composition similar to or the same as the target oxide superconductor to oxidize the polycrystalline thin film B. An object superconducting layer may be formed, or a laser vapor deposition method of irradiating the target with a laser beam to extract and vaporize constituent particles may be performed.

In the polycrystalline thin film B, the c-axis is oriented in a direction perpendicular to the film formation surface of the substrate A, and the a-axis and b-axis are aligned along a plane parallel to the film formation surface. Since it has good orientation, the oxide superconducting layer laminated on the polycrystalline thin film B by sputtering or laser vapor deposition is deposited and grown to match the orientation of the polycrystalline thin film B.

Thus, the oxide superconducting layer formed on the polycrystalline thin film B becomes an oxide superconducting layer in a polycrystalline state. In each of the crystal grains of the oxide superconducting layer, a base material is used. The c-axis through which electricity does not easily flow is oriented in the thickness direction of A, and the a-axes or b-axes are oriented in the longitudinal direction of the base material A. Therefore, the obtained oxide superconducting layer has excellent quantum coupling properties at the crystal grain boundaries and has little deterioration in superconducting properties at the crystal grain boundaries, so that it is easy to conduct electricity in the longitudinal direction of the substrate A, and the critical current density is excellent. Things are obtained.

(Production Example) An apparatus having the structure shown in FIG. 1 was used, and the inside of the container accommodating this apparatus was evacuated to 3.0 × 10 ^-4 torr by a vacuum pump. Base material is width 1
Hastelloy C, 0mm, 0.5mm thick, 10cm long
276 tape was used. A target made of YSZ (stabilized zirconia) was used, and a sputtering voltage of 1000 was used.
V, sputtering current 100 mA, irradiation angle of the ion source beam is set to 45 degrees or 90 degrees, and the assist voltage of the ion source is set to 300 V, 500 V, and 700 V, respectively, and the current of the ion source is set to 15 to 50 mA, respectively. After setting, ion irradiation was performed simultaneously with sputtering on the substrate to form a film-like YSZ layer having a thickness of 0.3 μm.

For each YSZ polycrystalline thin film obtained, C
An X-ray diffraction test was conducted by the θ-2θ method using uKα rays. FIGS. 5 to 7 are diagrams showing the diffraction intensity of the sample measured by appropriately changing the ion beam voltage and the ion beam current at an incident angle of 45 degrees of the ion source. From the results shown in FIGS. 5 to 7, peaks of the (200) plane or the (400) plane of YSZ are recognized, and the (100) plane of the YSZ polycrystalline thin film is oriented along a plane parallel to the substrate surface. It was found that the YSZ polycrystalline thin film was formed with its C-axis oriented vertically to the upper surface of the substrate.
From the comparison of the magnitudes of the peaks shown in FIGS. 5 to 7, the larger the beam current and the smaller the beam voltage, that is, the larger the amount of ion irradiation at a lower speed, the better the c of the polycrystalline thin film. It was found that the axial orientation could be improved.

8 to 10 show the incident angle 90 of the ion source.
FIG. 6 is a diagram showing the diffraction intensity of a sample measured by appropriately changing the ion beam voltage and the ion beam current in degrees. 8 to 1
From the result shown in FIG. 0, it was confirmed that the c-axis orientation was sufficient even when the incident angle of the ion source was 90 degrees.

Next, it was measured whether the a-axis or the b-axis of the YSZ polycrystalline thin film was oriented in the c-axis oriented sample as described above. For the measurement, see FIG.
As shown in FIG. 5, X-rays are irradiated at an angle θ to the YSZ polycrystalline thin film formed on the base material A, and 2θ (58.7 degrees) with respect to the incident X-rays in a vertical plane including the incident X-rays. )
The X-ray counter 25 is installed at the position of the angle of, and the value of the horizontal angle φ with respect to the vertical plane including the incident X-ray is appropriately changed,
That is, the orientation of the a-axis or the b-axis of the polycrystalline thin film B was measured by measuring the diffraction intensity obtained by rotating the substrate A by the rotation angle φ as indicated by the arrow in FIG. . The results are shown in FIGS.

As shown in FIG. 12, in the case of a sample manufactured by setting the incident angle of the ion beam to 45 degrees, when φ is set to 90 degrees and 0 degrees, ie, every 90 degrees with respect to the rotation angle φ. The peak of the (311) plane of YSZ appears. This corresponds to the (011) peak of YSZ in the substrate plane, and it became clear that the a-axes or b-axes of the YSZ polycrystalline thin film are oriented. On the other hand, as shown in FIG.
In the case of the sample manufactured by setting the degree, no special peak was observed, and it was found that the directions of the a-axis and the b-axis were disordered.

From the above results, it has been clarified that the polycrystalline thin film of the sample manufactured by the apparatus of the present invention has not only c-axis orientation but also a-axis orientation and b-axis orientation. Therefore, it was clarified that a polycrystalline thin film such as YSZ having excellent orientation can be produced by implementing the apparatus of the present invention.

On the other hand, FIG. 14 shows the results of using the sample of the YSZ polycrystalline thin film used in FIG. 12 and testing the crystal orientation of each crystal grain of the polycrystalline layer of this sample. In this test, when performing X-ray diffraction by the method described above with reference to FIG. 11, the diffraction peak was measured when the angle of φ was set to a value of −10 degrees to 45 degrees in increments of 5 degrees. is there. FIG.
It is clear from the results shown in that the diffraction peak of the obtained YSZ polycrystalline thin film appears within a grain boundary inclination angle of 30 ° but disappears at 45 °. Therefore, it was found that the grain boundary inclination angle of the crystal grain of the obtained polycrystalline thin film was within 30 degrees, and it was revealed that the thin film had good orientation.

FIG. 15 shows another embodiment of the apparatus of the present invention. In the apparatus of this example, the same components as those of the apparatus shown in FIG. 1 are denoted by the same reference numerals, and the description thereof will be omitted. The apparatus of this example is different from the apparatus shown in FIG. 1 in that three targets 12 are provided, three sputter beam irradiation devices 14 are provided, and a high frequency power supply 30 is connected to the substrate A and the target 12. is there.

In the apparatus of this example, three targets 1
2, 12, and 12, different types of particles can be beaten out and deposited on the base material A to form a composite film, so that a polycrystalline film having a more complicated composition can be manufactured. Further, the high frequency power supply 30 is operated to set the target 12
Can also be sputtered. When the above method is carried out using the apparatus of this example, a polycrystalline thin film having excellent orientation can be obtained as in the case of the apparatus shown in FIG.

By the way, if the above method is carried out using the apparatus having the structure shown in FIG. 1 or FIG. 13, an optical thin film having good orientation, a magnetic thin film of a magneto-optical disk having good orientation, and a thin film having good orientation can be obtained. Any of a thin film for fine wiring for an integrated circuit, a dielectric thin film used for a high-frequency waveguide, a high-frequency filter, a cavity resonator, or the like can be formed. That is, if these thin films are formed on the polycrystalline thin film B having a good crystal orientation by a film forming method such as sputtering, laser vapor deposition, vacuum vapor deposition, or CVD (chemical vapor deposition), the polycrystalline thin film B is excellent. As these thin films are deposited or grown with consistency,
The orientation becomes good.

By manufacturing these thin films with the apparatus of the present invention, a high-quality thin film having good orientation can be obtained. Therefore, optical thin films have excellent optical characteristics, magnetic thin films have excellent magnetic characteristics, and Migration does not occur in a thin film, and a thin film having good dielectric properties can be obtained in a dielectric thin film.

[0040]

As described above, according to the present invention, the ion beam can be irradiated at a predetermined angle from an oblique direction when the constituent particles hit from the target by sputtering are deposited on the film-forming surface of the substrate. In addition, as a result of efficiently activating the constituent particles, it is possible to improve the a-axis orientation and the b-axis orientation in addition to the c-axis orientation with respect to the film forming surface of the substrate. Therefore, by using the apparatus of the present invention, even in a polycrystalline thin film in which many crystal grain boundaries are formed, all of the a-axis orientation, the b-axis orientation, and the c-axis orientation of each crystal grain are improved. Can be formed into a polycrystalline thin film. In addition, in order to form a polycrystalline thin film having such good orientation, it is preferable to set the ion irradiation angle to a desired range . Therefore, by operating the angle adjusting mechanism to adjust the ion irradiation angle to a suitable angle, a polycrystalline thin film with good orientation can be obtained. In addition, in the angle adjustment mechanism,
The upper support plate connected to the bottom and the lower support pined to it
The ion irradiation angle can be adjusted by adjusting the angle of the support plate.
It can be easily adjusted. Furthermore, the polycrystal obtained by the device of the present invention
Of stabilized zirconia formed on a metallic substrate composed of
In the crystal thin film, the grain boundary tilt angle of crystal grains is within 30 degrees.
Therefore, the crystal orientation is excellent and the quality is high. Especially many
Stabilized Zirconia Formed on Metallic Substrates
Is a polycrystalline thin film, and the grain boundary tilt angle of crystal grains is within 30 degrees.
Have not been obtained in the past and were manufactured using the device of the present invention.
Polycrystalline thin film has excellent crystal orientation that has never existed before
It is a polycrystalline thin film.

Next, as a polycrystalline thin film, a concrete
Luconia can be used, and rare gas ions can be slanted
Irradiates the film forming surface of the substrate from the same time and stabilizes it from an oblique direction
To deposit the sputtered particles of zirconia on the substrate film formation surface.
And connect the c-axis of each crystal grain perpendicularly to the film formation surface of the substrate.
The grain boundary tilt angle formed by the a-axis or the b-axis of the crystal grain is set to 30 or less.
It is possible to form a polycrystalline thin film of stabilized zirconia. next,
Provide a metal tape feeding device and winding device inside the container,
The metal tape is fed from the feeding device to the material holder.
At the same time, wind the metal tape on the substrate holder with the winding device.
By being configured so that it can be scraped off
A crystal thin film can be continuously formed.

[Brief description of the drawings]

FIG. 1 is a block diagram showing an embodiment of a device of the present invention.

FIG. 2 is a sectional view showing an example of an ion source of the apparatus of the present invention.

FIG. 3 is a configuration diagram showing a polycrystalline thin film manufactured by the apparatus of the present invention.

FIG. 4 is an enlarged plan view of the polycrystalline thin film shown in FIG.

FIG. 5 is a graph showing an X-ray diffraction result of a sample of the present invention manufactured at a beam voltage of 300V.

FIG. 6 is a graph showing an X-ray diffraction result of a sample of the present invention manufactured at a beam voltage of 500V.

FIG. 7 is a graph showing an X-ray diffraction result of a sample of the present invention manufactured at a beam voltage of 700V.

FIG. 8 is a graph showing an X-ray diffraction result of a comparative sample manufactured at a beam voltage of 300V.

FIG. 9 is a graph showing an X-ray diffraction result of a comparative sample manufactured at a beam voltage of 500V.

FIG. 10 is a graph showing an X-ray diffraction result of a comparative sample manufactured at a beam voltage of 700V.

FIG. 11 is a configuration diagram for explaining a test apparatus used for examining a-axis orientation.

FIG. 12 is a graph showing a diffraction peak on the (311) plane of a polycrystalline thin film manufactured by the apparatus of the present invention.

FIG. 13 is a diagram (31) of a polycrystalline thin film in a comparative example.
It is a graph which shows the diffraction peak of 1) plane.

FIG. 14 is a graph showing diffraction peaks of the polycrystalline thin film manufactured by the apparatus of the present invention at every rotation angle of 5 degrees.

FIG. 15 is a configuration diagram showing another embodiment of the device of the present invention.

FIG. 16 is a configuration diagram showing a polycrystalline thin film manufactured by a conventional apparatus.

[Explanation of symbols]

A: substrate, B: polycrystalline thin film, D: angle adjustment mechanism, θ: inclination angle, w: rotation angle, 11:
Substrate holder, 12 target, 13 ion source, 14 sputter beam irradiation device, 15 target holder,

Claims (2)

(57) [Claims] 1. A substrate for supporting a polycrystalline thin film is supported.
The substrate holder and the substrate mounting surface of the substrate holder
And a stabilized zirconia target placed opposite to each other,
Sputtering means for sputtering the constituent particles of the target
And from the diagonal direction with respect to the substrate mounting surface of the substrate holder
Can be evacuated to an ion source that irradiates rare gas ions
It is housed in a container, and is attached to the base holder at the bottom of the base holder.
Support plate and a lower support plate pin-connected to the upper support plate
And a base for supporting this lower support plate,
The relative angle between the support plate and the lower support plate
An angle adjustment mechanism that can adjust the degree is provided.
The rare gas ion beam of
It is configured to be able to irradiate at an oblique angle, and irradiates the ion beam from the oblique direction to the upper surface of the substrate.
By putting it, the c-axis of each crystal grain can be
The grain boundary tilt angle between the a-axis or the b-axis of each crystal grain
Form a stabilized zirconia polycrystalline thin film with a temperature below 30 degrees
An apparatus for producing polycrystalline thin films characterized by being made free. 2. A device for feeding and winding a metal tape inside a container.
A device is provided to feed the metal from the delivery device to the substrate holder.
The tape can be sent out freely and the metal tape on the substrate holder is
The winding device can be used to wind the rope freely.
The polycrystalline thin film manufacturing apparatus according to claim 1.