TWI660060B - Airflow sputtering device and manufacturing method of sputtering target material - Google Patents

Abstract

The invention provides a gas flow sputtering device suitable for stably manufacturing a sputtering target material at a high sputtering rate for a long time. This airflow sputtering device includes: a pair of flat target materials arranged in a sputtering chamber so as to face each other with a sputtering surface spaced apart from each other; a pair of cooling devices for cooling each flat target material; and a fixed conductivity A component for fixing each flat target to a cooling device, the pair of flat targets having mounting portions extending from respective sides, and the mounting portions being held between the fixing member and the cooling device In a positional relationship, the pair of flat target materials are respectively fixed to a cooling device, the fixing member is covered by an insulating shielding member, and the insulating shielding member does not contact the pair of flat target materials.

Description

   Airflow sputtering device and manufacturing method of sputtering target material   

The invention relates to a gas flow sputtering device and a method for manufacturing a sputtering target material.

In the field of magnetic recording represented by a hard disk drive, as a material of a magnetic thin film responsible for recording, a material based on Co, Fe, or Ni of a ferromagnetic metal is used. For example, in a recording layer of a hard disk using an in-plane magnetic recording method, a Co-Cr-based or Co-Cr-Pt-based ferromagnetic alloy containing Co as a main component is used. In the recording layer of the hard disk using the perpendicular magnetic recording method which has been put into practical use in recent years, most of them are those in which non-magnetic particles such as oxides and carbon are dispersed in a Co-Cr-Pt-based ferromagnetic alloy mainly containing Co. Composite material.

From the viewpoint of high productivity, a sputtering target having a composition of the above materials is often sputtered to produce a magnetic thin film of a magnetic recording medium such as a hard disk. In the non-magnetic material particle-dispersed sputtering target, non-magnetic particles contained in the sputtering target cause an abnormal discharge, and the abnormal discharge becomes a cause of generation of particles. In recent years, as the storage capacity of hard disk drives has increased, the need to reduce particles from sputtering targets when manufacturing hard disk media has also increased.

A sputtering target is generally manufactured by a powder sintering method. It is known that miniaturization of non-magnetic particles in a sputtering target is very effective for reducing particles. For this reason, it is an effective method to mechanically pulverize and mix various raw material powders using a powerful ball mill or the like. However, in the current mechanical pulverization and mixing method, there is a physical limit to the miniaturization of the structure, and it is difficult to completely eliminate the generation of particles.

Therefore, in World Intellectual Property Organization Patent Publication No. 2013/136962, it is proposed to use physical vapor deposition (Physical Vapor Deposition (PVD) or Chemical Vapor Deposition (PVD) without using the existing mechanical crushing and mixing , CVD) method to refine the oxide. Specifically, a method of forming a magnetic material on a substrate by a PVD or CVD method, removing the formed magnetic material from the substrate, and pulverizing the magnetic material as a raw material is disclosed. This document discloses that according to this technique, it is possible to reduce the average particle diameter of the oxide in the sputtering target to 400 nm or less. In the example of this document, the content of forming a target material into a film using a direct current (DC) magnetron sputtering device is disclosed.

On the other hand, as a sputtering method, a gas flow sputtering method is also known (for example, Japanese Patent Laid-Open No. 2006-130378, Japanese Patent Laid-Open No. 2007-186771, and Japanese Patent Laid-Open No. 2008-1957). The air-flow sputtering method is a method in which sputtering is performed at a relatively high pressure, and sputtering particles are transported to a film-forming object substrate by a forced flow of gas to be deposited. This airflow sputtering method does not require high-vacuum exhaust. Therefore, it is not necessary to use a large-scale exhaust device such as the conventional sputtering method. Film formation can be performed by exhausting with a mechanical pump. . In addition, the airflow sputtering method can achieve a high-speed film formation at 10 to 1000 times that of a general sputtering method. Therefore, the air-flow sputtering method can reduce the equipment cost, shorten the film formation time, and reduce the film formation cost.

<Prior Art Literature>

<Patent Literature>

Patent Document 1: World Intellectual Property Organization Patent Publication No. 2013/136962

Patent Document 2: Japanese Patent Laid-Open No. 2006-130378

Patent Document 3: Japanese Patent Laid-Open No. 2007-186771

Patent Document 4: Japanese Patent Laid-Open No. 2008-1957

The invention disclosed in World Intellectual Property Organization Patent Publication No. 2013/136962 is a technology effective for miniaturizing the structure of a non-magnetic material particle-dispersed sputtering target, but it is necessary to implement the raw material for the sputtering target on the substrate Steps for forming a film by PVD or CVD. For this purpose, if a high-performance device such as a DC magnetron sputtering device is used for film formation, there is a problem that the manufacturing cost of the sputtering target is increased, and there is also a problem that the productivity is low. In this regard, the airflow sputtering method can quickly form a film and the equipment cost is low. Therefore, it can be considered that it is advantageous to use the airflow sputtering method to produce a sputtering target material.

However, attempts to produce raw materials for sputtering targets using a gas flow sputtering method have not been studied. The disclosures of Patent Documents 2 to 4 remain on a catalyst layer for manufacturing an electrode for a solid polymer fuel cell by a gas flow sputtering method, a semiconductor electrode layer for a dye-sensitized solar cell, a photocatalyst film, an antireflection film, and an electrochromic element , Transparent conductive film. Therefore, in the prior art, there has been no improvement in the device from the point of industrially manufacturing the raw materials of the sputtering target. In particular, in order to be used as a raw material for a sputtering target, a large amount of raw material is required, and therefore continuous sputtering is required to be performed stably for a long time. The device structure and manufacturing method for manufacturing the raw material for the sputtering target are still improved. Room.

The present invention has been made in view of the above circumstances, and a technical problem to be solved by the present invention is to provide a gas flow sputtering apparatus suitable for stably manufacturing a sputtering target material at a high sputtering rate for a long time. In addition, another technical problem to be solved by the present invention is to provide a target material for air flow sputtering. In addition, another technical problem to be solved by the present invention is to provide a method for manufacturing a sputtering target material by using the airflow sputtering device.

The present inventors have conducted intensive studies in order to solve the above-mentioned technical problems, and as a result, they have found that there is almost no problem in film thickness uniformity and surface properties of a sputtered film formed by a gas flow sputtering device for the purpose of manufacturing a raw material for a sputtering target. Therefore, in this object, it is more important to reduce the abnormal discharge at a high sputtering rate than to improve the quality of the sputtering film. Based on such a point of view, the inventors have found that an airflow sputtering apparatus using a flat-opposition target and having the following structure is effective.

In one aspect of the present invention, there is an airflow sputtering apparatus including: a sputtering chamber in which a vacuum can be formed inside; and a pair of flat targets arranged at a spaced-apart distance from each other by a spaced-apart sputtering surface. The sputtering chamber; a pair of cooling devices for cooling each flat target; a conductive fixing member for fixing each flat target to the cooling device; one or two or more gas exhaust ports for A sputter gas is supplied between the pair of flat target materials; and a component for depositing sputtered particles, which is arranged to face the gas discharge port through a space between the pair of flat target materials so as to be located at the gas discharge port; On the opposite side, wherein the pair of flat targets have mounting portions extending from respective sides, the pair of flat targets are in a positional relationship where the mounting portions are held by the fixing member and the cooling device. The materials are respectively fixed to the cooling device, and the fixing member is covered with an insulating shielding member that does not contact the pair of flat target materials.

In one embodiment of the airflow sputtering apparatus according to the present invention, the pair of flat target materials has conductivity.

In another embodiment of the airflow sputtering apparatus according to the present invention, the pair of flat target materials are directly or indirectly in contact with the cooling device by the fixing member in a state in which surfaces opposite to the sputtering surface are directly or indirectly in contact with the cooling device. fixed.

In still another embodiment of the airflow sputtering apparatus according to the present invention, a closest distance between each flat target and the insulating shielding member is adjusted to 0.1 to 5 mm.

In still another embodiment of the airflow sputtering apparatus according to the present invention, the insulating shielding member is selected from the group consisting of alumina, silica, zirconia, magnesium oxide, yttrium oxide, calcium oxide, titanium oxide, and boron nitride. A group consists of one or two or more materials.

In still another embodiment of the airflow sputtering apparatus according to the present invention, the insulating shielding member has a peripheral wall that is erected around the side surface of the flat target material at intervals along the side surface.

In still another embodiment of the airflow sputtering apparatus according to the present invention, the interval between the side surface of each flat target and the peripheral wall of the insulating shielding member is 0.1 to 2 mm.

In still another embodiment of the airflow sputtering apparatus according to the present invention, the insulating shielding member is arranged to cover an edge portion of a sputtering surface of each flat target.

In still another embodiment of the airflow sputtering apparatus according to the present invention, the pair of flat target materials are composed of a composite of a non-magnetic material and a magnetic material.

In another aspect of the present invention, a method for manufacturing a sputtering target material includes a step of performing sputtering using a gas flow sputtering apparatus according to the present invention.

In one embodiment of the method for producing a sputtering target material according to the present invention, sputtering is performed with a power density of 10 W / cm ² or more.

In another embodiment of the method for manufacturing a sputtering target material according to the present invention, the sputtering gas is represented by a flow rate on a total projected area of a sputtering surface of a pair of flat target materials opposed to each 1 cm ² And set the flow rate of the sputtering gas to 1 sccm / cm ² or more to perform sputtering.

In another embodiment of the manufacturing method of the sputtering target raw material which concerns on this invention, sputtering is performed by setting the pressure of a sputtering gas to 10 Pa or more.

In still another embodiment of the method for manufacturing a sputtering target material according to the present invention, the component that accumulates sputtered particles is a used sputtering target, and includes depositing a sputter on an eroded portion of the sputtering target. Particle steps.

In still another embodiment of the method for producing a sputtering target material according to the present invention, the method further includes: making a total quality of the sputtered particles deposited on the insulating shielding member greater than that of the sputtered particles deposited. A step of the quality of the sputtered particles deposited on the part.

According to the present invention, since an abnormal discharge is unlikely to occur when a sputtering target material is produced using a gas flow sputtering apparatus, sputtering can be performed continuously and stably for a long time. As a result, it is possible to produce raw materials for sputtering targets with higher production efficiency and lower costs than in the prior art, especially for producing non-magnetic material particle-dispersed sputtering targets with finer structures.

10a, 10b‧‧‧ flat target

11‧‧‧Sputtering Room

12‧‧‧ Ministry of Space

13‧‧‧Sputtered particles

14‧‧‧Sputter gas outlet

15‧‧‧DC Power

16‧‧‧ Accumulated sputtered particles

17‧‧‧Sputtering gas

18‧‧‧ support (holding part)

19‧‧‧ interval adjustment mechanism

20‧‧‧ exhaust port

22‧‧‧Gas exhaust unit

24‧‧‧ entrance to the gas exhaust unit

26‧‧‧ Tubular parts

28‧‧‧Gas introduction pipe

29‧‧‧sealing material

45‧‧‧Conductive fixing parts

45a‧‧‧First fixing element

45b‧‧‧Second fixing element

46‧‧‧ diaphragm

47‧‧‧ back plate

48‧‧‧ cooling water

49‧‧‧Insulation shielding parts

50‧‧‧cooling device

51‧‧‧ Fasteners

52‧‧‧ Telescopic parts

101‧‧‧ side of target

102‧‧‧Mounting parts

103‧‧‧ Upper surface of plate target (sputtered surface)

104‧‧‧ the lower surface of the installation site

The lower surface of the 106‧‧‧ flat target

491‧‧‧Zhou Bi

492‧‧‧Side

493‧‧‧Top panel

501‧‧‧ Insulating shielding parts for cooling devices

502‧‧‧Fastener mounting base

503‧‧‧Fastener

D‧‧‧ The distance between the flat target and the substrate of the film-forming object

L1‧‧‧ Space between flat target and insulating shield

L3‧‧‧Distance between the lower surface of the upper panel of the insulating shielding member and the upper surface of the conductive fixing member

S ₁ Space between a pair of flat targets before sputtering

FIG. 1 is a schematic diagram showing an example of a basic structure inside an airflow sputtering apparatus according to the present invention.

FIG. 2-1 is a schematic diagram showing an example of a general equipment configuration of a gas flow sputtering apparatus according to the present invention.

FIG. 2-2 is a schematic diagram showing another example of the general equipment configuration of the airflow sputtering apparatus according to the present invention.

FIG. 2-3 is a schematic diagram showing still another example of the general equipment configuration of the airflow sputtering apparatus according to the present invention.

FIG. 3 is a schematic view showing a first example of a cross-sectional structure around a target and a fixed member for air-flow sputtering according to the present invention (without a back plate).

FIG. 4 is a schematic diagram illustrating a second example of a cross-sectional structure around a target and a fixed member for airflow sputtering according to the present invention (without a back plate).

FIG. 5 is a schematic diagram illustrating a third example of a cross-sectional structure around a target for airflow sputtering and a fixing member according to the present invention (without a back plate).

FIG. 6 is a schematic diagram illustrating a fourth example of a cross-sectional structure around a target and a fixed member for airflow sputtering according to the present invention (without a back plate).

FIG. 7 is a schematic diagram (using a back plate) showing a fifth example of a cross-sectional structure around a target for airflow sputtering and a fixing member according to the present invention.

FIG. 8 shows an example of the arrangement of the flat target material and the insulating shielding member in a plan view when the flat target material according to the present invention is fixed in the air flow sputtering apparatus.

FIG. 9 is a schematic diagram illustrating a configuration example of a sputtering gas discharge unit having a plurality of gas discharge ports.

Hereinafter, various embodiments of the airflow sputtering apparatus according to the present invention will be described in detail with reference to the drawings. FIG. 1 shows an example of the basic structure inside the airflow sputtering apparatus according to the present invention, and FIG. 2-1 to FIG. 2-3 show an outline of a device configuration example of the airflow sputtering apparatus according to the present invention. . In the sputtering chamber 11 capable of making the inside of a vacuum (= less than atmospheric pressure), the sputtering surfaces of a pair of flat targets 10a and 10b are arranged to face each other with a predetermined interval therebetween. From the standpoint that there is no unexpected condition and that the plasma density can be uniformly increased on the surface of the target and the corrosion rate can be effectively increased, it is preferable that a pair of flat targets 10a and 10b are arranged in a state before the start of sputtering. The sputtered surfaces are parallel to each other. However, it is also possible to perform sputtering by tilting the sputtering surfaces not parallel to each other. A negative voltage is applied to each of the targets 10a and 10b, and a plasma of a sputtering gas 17 such as Ar is generated in a space portion 12 between a pair of flat targets 10a and 10b. The plasma is caused to collide with each target. Sputtered particles 13.

Exemplary potentials of each device during sputtering are divided and shown in FIGS. 2-1 to 2-3. During sputtering, the pair of flat targets 10a and 10b need to be at the cathode potential. There is no particular limitation on the potentials of other parts as long as the sputtering device can be operated safely, but there is a better way from the viewpoint of stable operation. , Which is described below. In terms of safety, the outer wall of the sputtering chamber 11 is generally set to an anode potential. In general, it is effective to use an insulating member in a case where a portion other than a space between the anode potential portion and the cathode potential portion is required to be insulated.

Either a DC power source or an AC power source can be used as the power source of the airflow sputtering device. However, the DC power source 15 is preferable because the power source device is inexpensive and the sputtering rate per unit time is high. The generated sputtered particles 13 flow in from the sputter gas discharge port 14 and are driven by a forced air flow of the sputter gas 17 flowing into the space 12 between the pair of flat targets 10a and 10b in the direction of the arrow, and are deposited on the On the surface of a member 16 (typically, a film-forming object substrate) on which sputtered particles 13 are deposited, a space portion 12 (FIG. 2- 1 to 2-3, the outer side of the space enclosed by the dotted line) is provided so as to face the sputtering gas discharge port 14. In this specification, the space between a pair of flat targets means that the contour of the sputtering surface of one flat target extends along the normal direction of the sputtering surface toward the side close to the other flat target. The space surrounded by the formed pattern and the space surrounded by the formed pattern are formed by extending the outline of the sputtering surface of the other flat target along the normal direction of the sputtering surface toward the side close to the flat target. , The two spaces coincide. In addition, in the present specification, the meaning that the part on which the sputtered particles are deposited faces the sputter gas discharge port means a straight line extending from at least one sputter gas discharge port toward the gas discharge direction and the surface of the part on which the sputtered particles are deposited. There are intersections. The member 16 on which the sputtered particles 13 are deposited can be supported by a support 18. The holder 18 is provided on the opposite side of the sputtering gas discharge port 14 with a space portion 12 sandwiched between the pair of flat targets 10a and 10b. After that, the sputtering gas 17 is exhausted from the exhaust port 20. The exhaust port 20 can be provided behind the stand 18 (in other words, the inside). By providing the exhaust port 20 behind the support 18, the sputtered particles 13 accompanying the sputter gas 17 can be made to collide with the member 16 efficiently.

The airflow sputtering method can increase the power density and the airflow speed compared with a normal sputtering method, and thus can form a film at a high speed. However, if the power density is increased for high-speed film formation, abnormal discharge is liable to occur. This tendency is particularly remarkable when the target is made of a material containing an insulating material such as an oxide. If an abnormal discharge occurs during sputtering, the components near the place where the abnormal discharge occurs are damaged and the maintenance frequency is increased. The sputtering operation must be stopped. Therefore, in order to run the device stably for a long time, avoiding abnormal discharge is an important technical problem. In order to avoid abnormal discharge, it is effective to shorten the interval (S ₁ ) between the pair of flat targets 10a and 10b. Specifically, the interval between the pair of flat targets 10a and 10b before the start of sputtering is preferably 100 mm or less, more preferably 50 mm or less, even more preferably 45 mm or less, and even more preferably 40 mm or less. On the other hand, if the interval (S ₁ ) between the pair of flat targets 10a and 10b is excessively shortened, the amount of gas that transports the sputtered particles 13 becomes small, and the sputtered particles 13 adhere to the target surface again. The sputtered particles 13 are efficiently deposited on the component 16. When shortening the interval (S ₁ ) between a pair of flat targets 10a and 10b, it is also considered to increase the flow velocity of the sputtering gas between the two so that the sputtered particles 13 do not adhere to the pair. However, in this case, a large amount of sputtering gas and a vacuum pump with high exhaust capacity are required. From this viewpoint, the interval between the pair of flat plate targets 10a and 10b before the start of sputtering is preferably 10 mm or more, and more preferably 15 mm or more.

As the sputtering time becomes longer, the thickness of the target material becomes thinner due to erosion. Therefore, if the interval between a pair of flat targets 10a and 10b is not supplemented, the interval gradually increases with the change in sputtering time, the voltage applied to the target gradually increases, and the risk of abnormal discharge increases. However, if the distance between the pair of flat target materials 10a, 10b is maintained within a certain range regardless of the thickness of the target material, for example, the interval between the pair of flat target materials 10a, 10b described above is appropriately maintained. Within this range, the risk of abnormal discharge will not increase. Therefore, in one embodiment of the airflow sputtering apparatus according to the present invention, the interval adjustment mechanism 19 is provided so that the pair of flat target materials can be etched when the pair of flat target materials 10a and 10b are eroded by sputtering. The interval is kept within a certain range, or can be set to the interval required at the start of sputtering. In FIG. 2, a pair of flat targets 10 a and 10 b are respectively fixed on the cooling device 50 to form an integrated structural element, and each integrated structural element can be moved by a corresponding interval adjustment mechanism 19.

The interval adjusting mechanism 19 is not particularly limited, and any known mechanism can be adopted, and examples thereof include linear motion mechanisms such as a cylinder linear motion mechanism and a ball screw linear motion mechanism. The driving method is not particularly limited, and examples thereof include motor driving, hydraulic driving, and pneumatic driving. From the viewpoint of being able to precisely adjust the position, a linear motion mechanism driven by a motor is preferred. The interval between a pair of flat targets 10a, 10b can be automatically changed to a desired setting value, or it can be changed manually. In addition, it is also possible to monitor the change in the interval between the pair of flat targets 10a, 10b during sputtering, and perform feedback control to maintain the initially set interval during sputtering. Feedback control can be manual or automatic. As a method of measuring a change in the interval between a pair of flat targets 10a and 10b, for example, a weight sensor may be provided to be able to measure the weight of each of the flat targets 10a and 10b, and the weight reduction amount of the target and the target may be used. And the projection area of the sputtering surface to calculate the average reduction in the thickness of the target (that is, the average increase in the interval between the targets). In order to automatically calculate the average reduction in target thickness, a computer can be installed in the device, or the calculation result can be displayed on a display attached to the device. In addition, it is also possible to consider a method in which the relationship between the discharge time and the cumulative power and the average reduction in the thickness of the target are obtained in advance for the flat targets 10a and 10b as sputtering targets. Based on this, at least according to the discharge time and the cumulative power The average reduction in target thickness was calculated.

Then, the interval adjustment mechanism 19 is manually or automatically operated so that the average interval between the two targets is reduced by an amount corresponding to the sum of the average reductions in the thickness of each target 10a, 10b, from the beginning to the end of the sputtering. So far, the interval between the pair of flat targets 10a and 10b can be maintained within a certain range. Since the voltage can change by more than 100V even if the interval between a pair of flat targets 10a and 10b changes by about 1 cm, from the viewpoint of continuous stable sputtering, a pair of flat plates from the start of sputtering to the end of sputtering The change in the average interval between the targets 10a and 10b is preferably 5 mm or less, more preferably 4 mm or less, still more preferably 3 mm or less, still more preferably 2 mm or less, even more preferably 1 mm or less.

As shown in FIG. 2-2, although the interval adjustment mechanism 19 can also be installed in the sputtering chamber 11, when the interval adjustment mechanism 19 is installed in the sputtering chamber 11, the interval adjustment mechanism 19 needs to be resistant to vacuum. When exposed to the plasma within 11, there is a possibility that particles may accumulate and cause an operation failure. Therefore, countermeasures to prevent this situation are needed for this. Furthermore, when oil such as lubricating oil is used in the interval adjustment mechanism 19, there is a possibility of evaporation in a vacuum atmosphere, and it is necessary to deal with this. Therefore, as shown in FIG. 2-3, at least a part of the preferred interval adjustment mechanism 19 is provided outside the sputtering chamber 11 (in FIG. 2-3, a linear motion such as a screw shaft in the case of a ball screw linear motion mechanism The components are provided in the chamber 11, but a power source such as a motor is provided outside the chamber 11.) As shown in FIG. 2-1, the interval adjustment mechanism 19 is more preferably provided outside the sputtering chamber 11 as a whole. When the interval adjustment mechanism 19 is provided outside the sputtering chamber 11, it is preferable to divide a part of the inside of the sputtering chamber 11 from the outside by a telescopic member 52. The telescopic member 52 is arranged to be able to follow the interval adjustment mechanism. 19's action expands and contracts and has atmospheric barrier properties. The telescopic member 52 expands and contracts in accordance with the movement of the interval adjustment mechanism 19, and even if the movable part of the interval adjustment mechanism 19 moves during sputtering, the inside of the sputtering chamber 11 can be isolated from the atmosphere and a vacuum (= less than atmospheric pressure) can be maintained. The telescopic member 52 is not particularly limited as long as it can perform the functions described above, and examples thereof include a bellows. As a material of the telescopic member, stainless steel, titanium, high nickel alloy (Hastelloy), aluminum, or the like is preferably used from the viewpoint of durability of repeated expansion and contraction in a state where an atmospheric pressure force is applied inside and outside.

In order to efficiently deposit the sputtered particles 13 on the member 16 on which the sputtered particles 13 are deposited, the direction of the forced airflow of the sputtering gas 17 is preferably perpendicular to the surface of the member 16 on which the sputtered particles 13 are deposited.

In order to prevent the growth of the sputtered particles adhering to the member 16 (typically, a film-forming object substrate) on which the sputtered particles 13 are deposited, the member 16 is preferably cooled. In the case of cooling, the material of the member 16 on which the sputtered particles 13 are deposited is not particularly limited, and plastic, glass, metal, ceramic, or the like can be used. Without cooling, the material of the member 16 on which the sputtered particles 13 are deposited is preferably a heat-resistant material such as glass, metal, or ceramic. This is because there is an effect that the gas flows toward the member 16 side during the gas flow sputtering, and the plasma may reach the vicinity of the member 16. Among them, in order to easily recover the attached sputtered particles, the component 16 is preferably selected from the group consisting of alumina, silicon oxide, zirconia, magnesium oxide, yttrium oxide, calcium oxide, titanium oxide, boron nitride, aluminum, iron, copper, and titanium. , Niobium, tantalum, tungsten, molybdenum, cobalt, chromium, nickel, and graphite; one or two or more materials; particularly, a material that does not react with sputtering particles and has poor wettability. In addition, it is preferable to select raw materials in consideration of contamination by end use. Furthermore, a method of directly depositing the same material as that of the sputtered particles 13 as the member 16 can also be adopted. In this case, a method may be considered in which sputtered particles are deposited on the eroded part of the used sputtering target to return to the original shape to regenerate the sputtering target. The sputter target thus regenerated can be pressurized and / or heated as needed.

The shape of the member 16 on which the sputtered particles 13 are deposited is not particularly limited, and generally a plate shape or a film shape can be adopted. In the airflow sputtering device, the member 16 on which the sputtered particles 13 are deposited can be supported on the support 18 by a method such as a clamp, a fastening screw, an adhesive, and an adhesive tape. In addition, in order to collect more sputtered particles, the component 16 can adopt a box-shaped container shape.

The sputtering gas 17 can be used alone or in combination of two or more of the following gases: rare gases such as He, Ar, Ne, Kr, and Xe; and atmospheric (air) gases such as N ₂ and O ₂ . Among them, Ar is preferred in terms of cost, and Kr and Xe are preferred from the viewpoint of efficiently moving the sputtered particles. In addition to the inert gas, N ₂ and / or O ₂ can be used as required. By using N ₂ and / or O ₂ , reactive sputtering of nitrides and oxides can be performed by using a metal as a target. Therefore, it is possible to obtain an advantage that cannot be obtained by the conventional manufacturing method: raw materials and composites in an unbalanced state can be made. High purity powdered material.

In the gas flow sputtering device, the flow rate of the sputtering gas can be made much larger than the flow rate of the DC magnetron sputtering device. By increasing the flow rate of the sputtering gas, deposition can be performed on a member on which sputtering particles are deposited at a high speed. In one embodiment of the airflow sputtering apparatus according to the present invention, the flow rate of the sputtering gas can be 1 sccm / cm ² or more. The flow rate of the sputtering gas is preferably 2 sccm / cm ² or more, and more preferably 5 sccm / cm ² or more. On the other hand, when the flow rate of the sputtering gas is too large, the pressure in the room will rise due to the limitation of the capacity of the exhaust pump. Therefore, it is preferably 200 sccm / cm ² or less, more preferably 100 sccm / cm ² or less, and even more preferably It is 50 sccm / cm ² or less. sccm refers to ccm (cm ³ / min) at 0 ° C and 1 atm. Here, the above-mentioned flow rate is a value obtained by dividing the flow rate of the sputtering gas by the total projected area of the opposing sputtering surfaces of the pair of flat targets 10a and 10b. For example, when the flow rate of the sputtering gas is 5000 sccm, and the two targets facing each other have a sputtering surface with a projection area of 10 cm × 10 cm = 100 cm ² , the flow rate is 5000 sccm / (100 × 2) cm ² = 25sccm / cm ² .

In addition, in the gas flow sputtering device, the pressure of the sputtering gas can be made much larger than the flow rate of the DC magnetron sputtering device. By increasing the air pressure, the advantage of reducing the discharge voltage can be obtained. In one embodiment of the airflow sputtering apparatus according to the present invention, the absolute pressure of the sputtering gas can be 10 Pa or more. The absolute pressure of the sputtering gas is preferably 20 Pa or more, more preferably 30 Pa or more, and even more preferably 40 Pa or more. On the other hand, when the absolute pressure of the sputtering gas is too high, abnormal discharge is likely to increase. Therefore, it is preferably 200 Pa or less, more preferably 150 Pa or less, and still more preferably 100 Pa or less. Here, the absolute pressure of the sputtering gas refers to the pressure in the space between the pair of opposing targets, and the pressure in the sputtering chamber 11 is usually highly uniform. Therefore, if it is the space in the sputtering chamber 11, Even when measured at other positions such as near the sputter gas discharge port 14 and near the exhaust port 20, substantially the same value can be obtained.

From the viewpoint of improving the productivity of producing a sputtered film by an airflow sputtering apparatus, it is preferable that the power density is high. However, when the power density is increased, there is a problem that abnormal discharge is liable to occur. In one embodiment of the airflow sputtering apparatus according to the present invention, the interval adjustment mechanism that maintains the interval between a pair of flat target materials within a certain range can reduce the occurrence of abnormal discharges. Therefore, it is possible to increase the power density. Allow the device to stably perform airflow sputtering for a long time. Exemplarily, the airflow sputtering device according to the present invention can operate at a power density of 10 W / cm ² or more, preferably can operate at a power density of 20 W / cm ² or more, and more preferably can operate at a power of 30 W / cm ² or more. Density operation. Although the upper limit of the power density is not set, the discharge voltage will increase when the power density is set too high. Therefore, the power density is generally adjusted so that the discharge voltage is below 1000V. It is better to reduce the occurrence of abnormal discharge. Possibly operate with a discharge voltage below 900V. Here, the power density refers to the total power ÷ the total area of the sputtering surfaces of the opposing targets (here, the total area of the projected areas of the opposing sputtering surfaces of a pair of flat targets). For example, when the sputtered surfaces are a pair of flat target materials with a length of 10 cm by 15 cm, the total projected area of the sputtered surfaces of the target material is 150 cm ² × 2 = 300 cm ² .

The material of the target is not particularly limited, and a conductive material such as a metal (including an alloy) can be appropriately used. In addition, an insulating material may be used, and a conductive material and an insulating material may be used together. As the material of the target, a ferromagnetic material containing one or more metal elements selected from the group consisting of Co, Fe, Ni, and Gd can be used. Non-magnetic materials (aluminum, copper, ruthenium, zinc, titanium, manganese, hafnium, zirconium, hafnium, chromium alloys, etc.), oxides, carbides, nitrides, carbonitrides, and carbon can also be used. Ability to use ferromagnetic and non-magnetic materials together. Examples of sputtering targets that can significantly reduce the effect of abnormal discharge by the airflow sputtering device according to the present invention include sputtering targets composed of a composite of a conductive material and an insulating material, and non-magnetic materials. A sputtering target made of a composite of a material and a magnetic material. Since such a composite body contains an insulating material or a non-magnetic material, abnormal discharge is particularly likely to occur during sputtering, so the advantages of using the airflow sputtering device according to the present invention are obvious. Examples of combinations of materials constituting a composite of a ferromagnetic material and a non-magnetic material include a Cr-Co alloy-based magnetic material containing a non-magnetic material, a Cr-Pt-Co alloy-based magnetic material containing a non-magnetic material, and Pt-Co alloy-based magnetic material of non-magnetic material, Pt-Fe alloy-based magnetic material containing non-magnetic material, Fe-Ni alloy-based magnetic material containing non-magnetic material, Fe-Co alloy-based magnetic material containing non-magnetic material Fe-Ni-Co alloy-based magnetic materials containing non-magnetic materials. In a typical embodiment, a non-magnetic material particle-dispersed sputtering target in which non-magnetic material particles are dispersed in a ferromagnetic material is provided as a sputtering target composed of a composite of a non-magnetic material and a magnetic material.

The purpose of the airflow sputtering device according to the present invention is not to form a high-quality sputtering film, but to manufacture a sputtering target material. In this case, it is preferable that the sputtering target used in the airflow sputtering apparatus according to the present invention can be produced at low cost. For example, in order to form a uniform sputtering film, a sputtering target having a high relative density is often used, but the sputtering target used in the airflow sputtering apparatus according to the present invention does not require such a high relative density. Therefore, in one embodiment, the relative density of the sputtering target for airflow sputtering according to the present invention can be 90% or less, 80% or less, and 70% or less. However, when the relative density is too low, it is difficult to ensure sufficient strength required for use as a sputtering target. In addition, the target itself has an increased resistance value, and electrical conductivity cannot be obtained in some cases. Therefore, the relative density of the sputtering target for airflow sputtering according to the present invention is preferably 40% or more, more preferably 50% or more, and still more preferably 60% or more. Only by low-temperature sintering or cold forming to aggregate the raw material powder into agglomerates, such low relative density target materials can be manufactured, and therefore can be manufactured at low cost. In addition, materials which have hitherto been difficult to form the shape of a target, such as difficult-to-sinter materials, low-melting materials, materials with large melting point differences, and materials requiring high purity, can also be used. It should be noted that the relative density is a value expressed as a percentage obtained by dividing a measured density by a theoretical density. The measured density was calculated from the weight and the volume obtained from the size and shape. The theoretical density is a value calculated theoretically based on the material composition constituting the sputtering target.

From the viewpoint of improving the productivity of producing a sputtered film by an air-flow sputtering device, the total projected area of the sputtered surfaces of a pair of flat targets opposing each other is preferably 300 cm ² or more, more preferably 500 cm ² or more, and even more preferably It is 1000 cm ² or more. There is no particular upper limit to the total projected area, but considering practicality, it is generally 10,000 cm ² or less, typically 8000 cm ² or less, and more typically 6000 cm ² or less. For example, when the sputtering surface of each flat target is a rectangular shape of 10 cm × 20 cm, the total projected area of the opposing sputtering surfaces of a pair of flat targets can be calculated as 10 cm × 20 cm × 2 = 400 cm ² .

The shape of the opposing sputtering surfaces of the flat target is not particularly limited, and examples thereof include a square, a rectangle, a polygon, an oval, and a circle. Among these, in order to efficiently collect the sputtered particles, a rectangular shape is preferable. In addition, the length of the opposing surface of the flat target in a direction perpendicular to the flow direction of the sputtering gas (Y in FIG. 1) is larger than the length in a direction parallel to the flow direction of the sputtering gas (X in FIG. 1). , Can increase the sputtering efficiency, so it is better. Specifically, Y / X ≧ 1, Y / X ≧ 1.2, and Y / X ≧ 1.5 are more preferable. However, it is difficult to handle the target material when Y / X is too large, so it is preferable that Y / X ≦ 20, more preferably Y / X ≦ 15, and even more preferably Y / X ≦ 10.

Although the respective thicknesses of the pair of flat targets are not particularly limited and may be appropriately set depending on the film-forming use time, etc., they are preferably thicker from the viewpoint of extending the time during which continuous sputtering can be performed. Therefore, the thickness of each flat target is preferably 3 mm or more, more preferably 5 mm or more, and even more preferably 10 mm or more. However, there is a technical limit to increasing the thickness, so it is generally 30 mm or less, typically 20 mm or less, and more typically 15 mm or less. In order to perform continuous sputtering for a long time, a plurality of flat target materials can be stacked and used. By adopting such a structure, it is not necessary to replace the sputtering target every time it is consumed.

After the flat targets 10a and 10b are fixed to the back plate 47 as needed, they can be mounted in the cooling device 50 in the air flow sputtering device. In the present invention, when the back plate 47 is used, the assembly of the flat plate target and the back plate is referred to as a "flat plate target", and the "flat plate target" as the assembly is fixed in the air flow sputtering apparatus. On the cooling device 50. Examples of the material of the back plate include copper, copper alloy, aluminum, aluminum alloy, titanium, titanium alloy, iron, iron alloy, molybdenum, molybdenum alloy, cobalt, and cobalt alloy.

When the back plate is not used, the flat plate targets 10 a and 10 b can be fixed to the cooling device 50 using the fixing member 45 described below. In addition, without using a back plate, the bottoms of the flat targets 10a and 10b can be formed into a back plate shape. In other words, it is possible to integrate the flat targets 10a and 10b with the back plate using the same material.

The method of fixing the flat targets 10 a and 10 b to the back plate 47 is not particularly limited, and examples thereof include a method of bonding with an adhesive and a method of diffusion bonding to the back plate 47. In the method of bonding by an adhesive, since the power density is set to be high as described above, the bonding portion also has a high temperature. Therefore, a heat-resistant conductive adhesive is preferably used. The conductive adhesive having heat resistance, specifically, preferably has a melting point of 200 ° C or higher.

The sputtering gas 17 flows into the sputtering chamber 11 from the sputtering gas discharge port 14 and flows through the space portion 12 between the pair of flat targets 10a and 10b in the direction of the arrow. There may be one sputter gas discharge port 14 or two or more. However, in order to cover the entire length of the side surface on the inflow side of the sputtering gas 17 of the pair of flat targets 10a and 10b (in other words, the length in the longitudinal direction of the slit that becomes the entrance of the space portion 12) (Y in FIG. 1) In order to reduce the deviation of the flow rate of the flowing sputtering gas 17, or in order to be able to adjust the flow rate of the sputtering gas 17, two or more sputtering gas discharge ports 14 are preferably provided along the length of the slit. When two or more sputtering gas discharge ports 14 are provided, in order to simplify the piping structure, a sputtering gas discharge unit 22 can be used. The sputtering gas discharge unit 22 can supply one or two or more gas supply pipes. The sputter gas is diverted and flows out of the discharge port with a larger number than the gas supply pipe. One or two or more sputtering gas discharge units 22 can be provided.

A structure of such a gas exhaust unit 22 is shown in FIG. 9, for example. The gas exhaust unit 22 includes a gas introduction pipe 28 having an inlet 24 for introducing a sputtering gas 17 from a gas supply pipe (not shown), and a tubular member 26 connected to the gas introduction pipe 28, and a plurality of sputtering gases The discharge ports 14 are lined up on the side thereof. The sputtering gas 17 flowing in from the inlet 24 of the gas discharge unit 22 passes through the gas introduction pipe 28 and the inside of the tubular member 26 in this order, and then flows out from the plurality of sputtering gas discharge ports 14. The sputtering gas discharge ports 14 are preferably arranged along the longitudinal direction of the slit that becomes the entrance of the space portion 12.

At each discharge port, the sputter gas flowing from each sputter gas discharge port 14 can be controlled by a flow adjustment mechanism such as a mass flow controller, a flow control valve (butterfly valve, needle valve, gate valve, ball valve, ball valve) and the like. 17 can perform flow control, and such a flow adjustment mechanism can be provided according to the number of gas supply pipes connected to the gas discharge unit 22 to uniformly control the flow rate of the sputtering gas 17 flowing out from the plurality of discharge ports 14.

The relative positional relationship between the sputter gas discharge port 14 and the pair of flat targets 10a and 10b may be fixed, or a position adjustment mechanism capable of performing relative adjustment as required may be provided. Examples of the position adjustment mechanism include a structure in which a sealing material 29 such as a ferrule, an O-ring, a filler, and a gasket is used, a gas introduction pipe 28 is fixed to the wall of the sputtering chamber 11, and adjustment is performed by loosening the sealing material 29 The position where the gas introduction pipe 28 is spaced from the wall (see FIGS. 2-1 to 2-3). In this case, from the viewpoint of operability, it is preferable to provide the sealing material 29 outside the sputtering chamber 11.

The schematic diagram shown in FIG. 3 shows an example of a cross-sectional structure around the flat-plate sputtering targets 10 a and 10 b and the fixing member 45 according to the present invention without using the back plate 47. When the target has a mounting portion 102 extending from the side surface 101, the target is fixed to a position where the mounting portion 102 is sandwiched between the conductive fixing member 45 and the cooling device 50 via a diaphragm (indirect cooling plate) 46. Cooling device 50. The target material may be fixed to the cooling device 50 in a positional relationship where the mounting portion 102 is directly sandwiched between the conductive fixing member 45 and the cooling device 50 without the diaphragm 46 interposed therebetween. The cooling efficiency is higher when the diaphragm 46 is not present, but in this case, when the inside of the sputtering chamber 11 is evacuated, the cooling water 48 needs to be discarded in order to prevent the cooling water 48 from leaking from the cooling device 50. From a viewpoint, the diaphragm 46 is preferably provided.

The reason for using the conductive fixing member 45 is that it is difficult for the insulating material to obtain sufficient strength. The mounting portion 102 can be formed integrally with the flat target body portion. As long as the flat targets 10a and 10b can be fixed to the cooling device 50, the area where the mounting portion 102 is provided is not particularly limited, and the mounting portions 102 can be continuously provided around the side surfaces 101 of the flat targets 10a and 10b or can be intermittently mounted on A plurality of mounting sites 102 are provided at a plurality of positions necessary for fixing the flat targets 10 a and 10 b to the cooling device 50. From the viewpoint of the workability of the flat targets 10a and 10b and the strength of the mounting portion, it is preferable to continuously provide the mounting portions 102 around the side surfaces 101 of the flat targets 10a and 10b.

On the basis of stable discharge, it is preferable that the conductive fixing member 45 that holds the mounting portion 102 does not protrude upwards than the upper surfaces (sputtered surfaces) 103 of the flat targets 10a and 10b. Therefore, it is preferable that the upper surface of the mounting portion 102 extending from the side surface 101 is lower than the upper surface 103 of the flat targets 10a and 10b. In this case, if the cross section of the target is observed, a step is formed between the upper surface 103 of the flat target materials 10 a and 10 b and the upper surface of the mounting portion 102. On the other hand, from the viewpoint of ensuring the fixing strength between the flat targets 10a and 10b and the cooling device 50, the lower surface 104 of the mounting portion 102 extending from the side 101 is preferably the lower surface 106 of the flat targets 10a and 10b. Have the same height. That is, preferably, the lower surfaces 106 of the flat targets 10a and 10b and the lower surface 104 of the mounting portion 102 are located on the same plane.

The material of the conductive fixing member 45 is not particularly limited, but preferably has heat resistance. Examples of the heat-resistant conductive material include metals. Metals having a melting point higher than the melting point of aluminum (660.3 ° C) are particularly preferred. Metals having a melting point of 700 ° C or higher are more preferred, and metals having a melting point of 800 ° C or higher are more preferred. The metal is more preferably a metal having a melting point of 1,000 ° C or higher. Carbon such as graphite can also be used. For example, a material selected from the group consisting of iron, copper, titanium, niobium, tantalum, tungsten, molybdenum, cobalt, chromium, nickel, and graphite may be used alone, or two or more alloys (including stainless steel) or metals may be used in combination. -Graphite composite. Among them, stainless steel is preferred for reasons of high strength, easy purchase, and cheapness.

The shape and size of the conductive fixing member 45 are not particularly limited as long as the flat targets 10a and 10b can be fixed to the cooling device 50 under the positional relationship between the mounting portion 102 and the cooling fixing member 50 and the cooling device 50. However, for reasons of stable discharge, it is preferable that the upper surface of the conductive fixing member 45 does not protrude more upwardly than the upper surfaces of the flat targets 10a and 10b, and is more preferably located more than the upper surfaces of the flat targets 10a and 10b. Low position. In addition, the conductive fixing member 45 may be composed of an integrally molded product, or may be composed of a combination of two or more elements. For example, in the embodiment shown in FIG. 3, when a plurality of mounting portions 102 are continuously provided around the side surfaces 101 of the flat targets 10 a and 10 b, the conductive fixing member 45 can be a frame-shaped first fixing element. 45a and a frame-shaped second fixing element 45b placed on the first fixing element 45a, the first fixing element 45a has a lower surface on the same plane as the lower surface 104 of the mounting portion 102, The upper surface whose upper surface is on the same plane, and the inner surface which closely fits the side surface of the mounting portion 102; the second fixing element 45b has a lower surface on the same plane as the upper surface of the mounting portion 102, The upper surfaces of the lower surfaces 103 of the materials 10a and 10b are lower, and the inner surfaces of the flat targets 10a and 10b are in close contact with each other. In this case, for the reason that the sputtering device and the shielding shape can be simplified, it is preferable that the first fixing element 45a and the second fixing element 45b are stepless on the outer side surfaces of the first fixing element 45a and the second fixing element 45b. Contact in a continuous manner. In a typical embodiment, the first fixing element 45a and the second fixing element 45b can be provided in the form of rectangular frames, respectively.

The conductive fixing member 45 is preferably not sputtered. When the conductive fixing member 45 is sputtered, the required composition of the sputtered film cannot be obtained, and the frequency of maintenance of the conductive fixing member 45 is increased, which is inconvenient. In addition, although the entire amount of the sputtered particles is ideally deposited on the member 16, when the sputtering rate is increased in order to increase the production efficiency, many sputtered particles are scattered around the flat targets 10 a and 10 b. As a result, the sputtered ions also accumulate on the conductive fixing member 45 and easily spread further to the surroundings. When the deposition range of the sputtered particles becomes larger, when the sputtered particles are conductive, the position that should be the cathode potential may be short-circuited with the position of the anode (ground) potential. Therefore, it is preferable that the conductive fixing member 45 is covered with the insulating shielding member 49. From another perspective, it can be said that the insulating shielding member 49 can function as a member that deposits sputtered particles.

In the embodiment shown in FIG. 3, the insulating shielding member 49 includes a side plate 492 that covers the outer side surface of the conductive fixing member 45, and an upper panel 493 that covers the upper surface of the conductive fixing member 45. In order to improve the effect of preventing the conductive fixing member 45 from being sputtered, the distance L3 between the lower surface of the upper panel 493 of the insulating shielding member 49 and the upper surface of the conductive fixing member 45 is preferably 10 mm or less, more preferably 5 mm or less, more preferably 2 mm or less. Even if the lower surface of the upper panel 493 of the insulating shielding member 49 is in contact with the upper surface of the conductive fixing member 45, it does not cause abnormal discharge, so L3 may be zero.

The insulating shielding member 49 is preferably made of a heat-resistant material. The insulation resistance of the insulating shielding member 49 is such that the insulation breakdown voltage at the thickness of the provided member is preferably 1 kV or more, more preferably 2 kV or more, and even more preferably 10 kV or more. As a suitable example of the heat-resistant material constituting the insulating shielding member 49, one selected from the group consisting of aluminum oxide, silicon oxide, zirconia, magnesium oxide, yttrium oxide, calcium oxide, titanium oxide, and boron nitride can be mentioned. Or two or more. If these materials are used, the deposited sputtered particles can be easily recovered.

In order to prevent abnormal discharge, the insulating shielding member 49 is preferably not in contact with the targets 10a and 10b. If the distance between the insulating shielding member 49 and the targets 10a and 10b is increased for this purpose, the conductive fixing member 45 is not insulated. The portion covered by the shielding member 49 becomes large, and the effect of preventing the conductive fixing member 45 from being sputtered becomes weak. Therefore, when each pair of flat targets 10a and 10b is viewed from the top, the closest distance (L1) between each target 10a and 10b and the insulating shielding member 49 is preferably adjusted to 0.1 mm or more, and more preferably 0.3 mm or more. , And more preferably adjusted to 0.5mm or more. In addition, the closest distance (L1) is preferably adjusted to 5 mm or less, more preferably 3 mm or less, and even more preferably 1 mm or less.

In the embodiment shown in FIG. 3, when each of the flat targets 10 a and 10 b is viewed from the top, the closest gap (L1) is generated between the targets 10 a and 10 b and the insulating shielding member 49. In this case, there is a possibility that the sputtering gas intrudes from the gap and the conductive fixing member 45 is sputtered. Therefore, in order to improve the effect of preventing the conductive fixing member 45 from being sputtered, as shown in FIG. 4, it is also possible to employ an insulating shielding member 49 to cover the upper surfaces (sputtered surfaces) 103 of each of the flat targets 10 a and 10 b. The edge of the way. Even in this case, it is preferable to adjust the closest distance (L1) between each target 10a, 10b and the insulating shielding member 49 to be within the above-mentioned range.

If necessary, in order to reduce the deposition of sputtered ions on the insulating shielding member 49, the insulating shielding member 49 may be covered with another shielding member. The shielding member in this case preferably has heat resistance, regardless of whether it has conductivity or insulation.

When it is necessary to pay attention, when the material of the shielding member 49 is changed from insulating to conductive, the discharge voltage is increased corresponding to the increase in the discharge power. Therefore, the shielding member 49 and the conductive fixing member 45 are generated. The risk of an arc discharge increases. Therefore, in order to perform long-term stable sputtering, the shielding member 49 needs to be insulating.

Since the cooling device 50 is in contact with each of the flat targets 10a and 10b, it can become a cathode potential. Therefore, in order to prevent the cooling device 50 from being sputtered, it is preferable to arrange an insulating shielding member 501 for the cooling device so as to cover the outer side surface of the cooling device 50. Although the insulating shielding member 501 can cover at least a part of the outer surface of the cooling device 50 to obtain a sputtering prevention effect, it is preferable to cover the entire outer surface. The insulating shielding member 501 can directly contact the outer surface of the cooling device 50. A suitable material for the insulating shielding member 501 for the cooling device is the material described for the insulating shielding member 49.

The schematic diagram shown in FIG. 7 shows a cross-sectional structure example of the flat-plate sputtering targets 10 a and 10 b according to the present invention when the back plate 47 is used. The function of each constituent element and its preferred mode indicated by the same element symbol are as described in FIG. 3, and redundant descriptions are omitted, and the description will focus on a structure different from the embodiment of FIG. 3. A portion of the back plate 47 of the target extends from the side surface 101 to form a mounting portion 102. The target is fixed to the cooling device 50 in a positional relationship in which the mounting portion 102 is directly sandwiched between the conductive fixing member 45 and the cooling device 50. In this embodiment, since the back plate 47 is present, when the sputtering chamber 11 is evacuated, there is no risk of cooling water leakage, and therefore, it is not necessary to insert the diaphragm 46.

In this embodiment, the target materials 10 a and 10 b can be fixed to the cooling device 50 in a positional relationship between the mounting portion 102 being sandwiched by the conductive fixing member 45 and the cooling device 50. The shape of the conductive fixing member 45, The size is not particularly limited. In the embodiment shown in FIG. 7, the conductive fixing member 45 is an integrally formed product and has a frame structure having a lower surface on the same plane as the upper surface of the mounting portion 102, and located on the flat target 10 a, The upper surface at a position where the upper surface 103 of 10b is low, and the inner surface that closely adheres to the side surfaces 101 of the flat targets 10a and 10b. In a typical embodiment, the conductive fixing member 45 can be provided as a rectangular frame.

In the embodiment of FIGS. 3 and 7, the insulating shielding member 49 has a side surface 101 along the flat targets 10 a and 10 b, and a peripheral wall 491 standing upright around the side surface 101 with an interval L1 therebetween. Since the peripheral wall 491 is present, the side surfaces of the flat targets 10a and 10b are hidden, so that it is easy to stabilize the discharge. In addition, an effect that the conductive fixing member 45 of the plasma is difficult to be sputtered can also be expected.

The peripheral wall 491 is not necessary. As shown in FIG. 5, a method in which the peripheral wall 491 is not provided can be adopted. In addition, as shown in FIG. 6, the upper panel 493 of the insulating shielding member 49 can be thickened to increase the strength of the insulating shielding member. According to this aspect, since the target side surface can also be hidden, the same effect as that of the peripheral wall 491 can be expected.

The configuration of the insulating shielding member 49 is not limited to the embodiment shown in FIGS. 3 to 7, and other embodiments can be adopted. For example, in the embodiment shown in FIG. 2-2, the side plate 492 does not exist in the insulating shielding member 49. In the embodiment shown in FIGS. 2-3, the fastener mounting base 502 is covered by the upper panel 493 and the side panel 492 of the insulating shielding member 49.

8 is a plan view showing an example of an arrangement relationship between the flat target materials 10a and 10b and the insulating shielding member 49 when the rectangular flat target materials 10a and 10b are used. In the embodiment shown in FIG. 8, rectangular flat targets 10 a and 10 b are arranged around a peripheral wall 491 of a rectangular frame-shaped insulating shielding member 49.

In order to maintain stable discharge, the interval L1 between the side surfaces 101 of the flat targets 10a and 10b and the peripheral wall 491 of the insulating shielding member 49 is preferably 0.1 mm or more, more preferably 0.2 mm or more, and even more preferably 0.3 mm or more. . In addition, for the reason that the fixing member 45 is prevented from being sputtered, the interval L1 is preferably 2 mm or less, more preferably 1.5 mm or less, and even more preferably 1 mm or less.

As a method of fixing the flat targets 10a and 10b to the cooling device 50, there may be mentioned a method in which one or two or more through holes are provided in the conductive fixing member 45, and if the diaphragm 46 is provided, one is also provided thereon. Or two or more through holes, and further, a mounting hole is provided in the cooling device 50, and fasteners 51 such as bolts and screws are sequentially inserted into the through holes and the mounting holes for fixing (see FIGS. 3 to 6). One or two or more through holes may be provided in the mounting portion 102 to insert the fastener 51 (see FIG. 7). In addition, as a method of fixing the insulating shielding member 49, a method is provided in which a through hole is provided in the insulating shielding member 49, and further, a mounting hole is also provided in the insulating shielding member 501 for a cooling device, and bolts, Fasteners 503 such as screws are sequentially inserted into the through hole and the mounting hole for fixing. In this case, when the fastener 503 is made of metal, in order to prevent the fastener 503 from being sputtered, it is preferable to ground the fastener 503 to an anode potential.

From the viewpoint of durability, the mounting hole for the fastener 503 is more preferably a metal material than an insulating material such as ceramic. Therefore, a fastener mounting base 502 made of metal may be provided on the outer surface of the insulating shielding member 501 for the cooling device, and a mounting hole may be provided in the fastener mounting base 502. The fastener mounting base 502 can be directly arranged on the outer surface of the insulating shielding member 501 so as to surround the outer surface of the insulating shielding member 501. In the case where the fastener 503 is made of metal, in order to prevent the fastener 503 from being sputtered, it is preferable to ground the fastener 503 to an anode potential. Further, in order to prevent the fastener mounting base 502 from being sputtered, it is preferable to ground the fastener mounting base 502 to make it an anode potential.

According to an embodiment of the airflow sputtering apparatus according to the present invention, the sputtering rate is set to 0.005 g / h / cm ² or more, preferably 0.01 g / h / cm ² or more, and more preferably 0.02 g / h / cm ² The above is, for example, 0.005 to 0.1 g / h / cm ² , and continuous sputtering can be performed for 5 hours or more without abnormal discharge. However, the reference area of the sputtering rate refers to the total area of the sputtering surfaces of the opposing targets (here, the total projected area of the opposing sputtering surfaces of a pair of flat targets). In addition, the sputtered film obtained by sputtering using the airflow sputtering apparatus according to the present invention can be peeled off from a member on which sputtered particles are accumulated and recovered, and then pulverized and used as a sputtering target raw material. By sintering this raw material, a sputtering target can be manufactured. In particular, the present invention is useful as a method for efficiently producing a non-magnetic material particle-dispersed sputtering target having a fine structure.

According to one embodiment of the method for manufacturing a sputtering target material using the airflow sputtering apparatus according to the present invention, the total quality of the sputtered particles deposited on the insulating shielding member 49 can be made larger than the sputtered particles deposited on the above-mentioned layer. The quality of the sputtered particles deposited on the part 16. For example, the ratio of the total quality of the sputtered particles deposited on the insulating shielding member 49 to the quality of the sputtered particles deposited on the member 16 can be 2 or more, 3 or more, and 4 or more. Therefore, in terms of improving productivity, it is also important to recover the sputtered particles deposited on the insulating shielding member 49 as a sputtering target material.

[Example]

Although the embodiments of the present invention are shown below, providing these embodiments is considered to better understand the present invention and its advantages, and is not intended to limit the invention.

<1. Verification of effect of interval adjustment of flat target>

(Test example 1)

Using the flat target sputtering device with the structure shown in Figure 1 and Figure 2-1 (however, the installation structure of the sputtering target uses the structure shown in Figure 3), follow the steps shown in Figure 3 and Figure 8. The structural mounting sputtering target forms a sputtering film under the following conditions. As the interval adjustment mechanism of a pair of flat targets, a ball screw linear motion mechanism is used. The ingot produced by the sintering method is machined into a predetermined shape to prepare a sputtering target.

In addition, as shown in FIG. 9, the sputtering gas discharge unit has a plurality of gas discharge ports arranged in a row along the entire length of the slit that becomes the entrance of the space portion 12. The number of discharge ports provided in the sputtering gas discharge unit is twenty.

In addition, the shape of the first fixing element is a rectangular frame, and the material of the first fixing element is stainless steel. The shape of the second fixing element is a rectangular frame, and the material of the second fixing element is stainless steel.

<Airflow sputtering conditions>

‧Power supply: DC power supply

‧Power density: 44W / cm ²

‧Sputtering gas pressure: 85Pa

‧Sputtering gas flow rate (sum of flow rate of each discharge port): Ar: 21.8sccm / cm ²

‧Total sputtering time: 250hr

‧Target shape: rectangular flat

‧Target size: 85mm (X direction) × 135mm (Y direction) × 20mmt

‧Total projected area of target: about 230cm ²

‧Target material: Cu

‧Target relative density: 99%

‧The interval S ₁ between a pair of flat targets before the start of sputtering: 30mm

‧Distance between flat target and substrate of film-forming object D: 80mm

‧Material of film-forming object substrate: stainless steel

‧Dimensions of the substrate of the film formation object: 200mm × 200mm × 3mmt

‧Temperature of film-forming object substrate: 40 ℃

‧Material of insulating shield: alumina (insulation breakdown voltage: 50kV)

‧Distance L1 between flat target and insulating shielding member: 0.5mm

‧Distance L3 between the lower surface of the upper panel of the insulating shielding member and the upper surface of the conductive fixing member: 0.1 mm or less

‧Target cooling: use cooling water

‧ Fixing method of fixing element and insulating shielding member to cooling device: bolt connection

‧Insulating shield for cooling device: alumina (insulation breakdown voltage: 50kV).

In Test Example 1, the interval adjustment mechanism was not used, and sputtering was continuously performed during the above sputtering time. As a result, although it was possible to perform continuous sputtering for more than 5 hours per batch without abnormal discharge in the initial stage of sputtering, the average interval S ₁ between a pair of flat targets exceeded 37 mm (total sputtering time). (Approximately 100 hours), abnormal discharge increased and it was difficult to maintain stable sputtering. In addition, based on the results of this test, the relationship between the discharge time and the cumulative power and the average reduction in target thickness was determined. The sputtering rate in this test was 0.062 g / h / cm ² . After the sputtering test, the ratio of the increased weight of the film-forming object substrate to the reduced weight of the target was 22%. After the sputtering test, the ratio of the increased weight of the insulating shielding member to the reduced weight of the target was 51%. It should be noted that the average interval S ₁ between a pair of flat targets in the test was measured with a vernier caliper.

(Test Example 2)

Based on the relationship between the discharge time obtained in Test Example 1, the cumulative power, and the average reduction in the thickness of the target, during the sputtering, the interval was adjusted manually by the interval adjustment mechanism to make the average interval of a pair of flat targets. A sputtered film was formed under the same conditions as in Test Example 1 except that the variation range was 5 mm or less. As a result, in the test, abnormal discharge could not occur after the total sputtering time of 250 hours. The sputtering rate in this test was 0.069 g / h / cm ² . After the sputtering test, the ratio of the increased weight of the film-forming object substrate to the reduced weight of the target was 26%. After the sputtering test, the ratio of the increased weight of the insulating shielding member to the reduced weight of the target was 46%.

(Test Example 3)

During sputtering, the sputtering chamber is opened periodically (every 10 hours) to measure the weight of a pair of flat targets, and the average interval variation is calculated. The interval adjustment mechanism is used to manually adjust the interval so that the variation is 5 mm or less. Except that, a sputtered film was formed under the same conditions as in Test Example 1. As a result, in the test, abnormal discharge could not occur after the total sputtering time of 250 hours. The sputtering rate in this test was 0.067 g / h / cm ² . After the sputtering test, the ratio of the increased weight of the film-forming object substrate to the reduced weight of the target was 25%. After the sputtering test, the ratio of the increased weight of the insulating shielding member to the reduced weight of the target was 48%.

<2. Verification of effect of insulating shielding member>

(Test Example 4)

A sputtering film was formed under the same sputtering conditions as in Test Example 1 except that the insulating shielding member was removed for a sputtering test. In this case, abnormal discharge occurs between the target fixing element and other anode potential components, and film formation cannot be performed stably, and film formation is stopped at the beginning. It was found in the sputtering chamber that abnormal discharge traces remained on the surfaces of the target and the fixing member.

(Test Example 5)

A sputtering film was formed under the same sputtering conditions as in Test Example 1 except that the distance L1 between the flat target and the insulating shielding member was set to 0 to make the two contact. In this case, abnormal discharge occurs frequently between the target and the insulating shield, and film formation is stopped at 30 minutes. The sputtering rate in this test was 0.064 g / h / cm ² . After the sputtering test, the ratio of the increased weight of the film-forming object substrate to the reduced weight of the target was 31%. After the sputtering test, the ratio of the increased weight of the insulating shielding member to the reduced weight of the target was 44%.

(Test Example 6)

A sputtering film was formed under the same sputtering conditions as in Test Example 1 except that the distance L1 between the flat target and the insulating shielding member was set to 2.2 mm. In this case, although the film was initially formed with few abnormal discharges and stable film formation was possible, the abnormal discharge occurred frequently after 3 hours and the discharge was stopped. It was found in the sputtering chamber that the fixed parts were also sputtered. The sputtering rate in this test was 0.062 g / h / cm ² . After the sputtering test, the ratio of the increased weight of the film-forming object substrate to the reduced weight of the target was 25%. After the sputtering test, the ratio of the increased weight of the insulating shielding member to the reduced weight of the target was 44%.

(Test Example 7)

A sputtering film was formed under the same sputtering conditions as in Test Example 1 except that the distance L1 between the flat target and the insulating shielding member was set to 0.1 mm. In this case, although the film was initially formed with a small number of abnormal discharges and stable film formation was possible, the abnormal discharge occurred frequently after 2 hours and the discharge was stopped. It was found in the sputtering chamber that abnormal discharge traces remained between the target and the insulating shield. The sputtering rate in this test was 0.067 g / h / cm ² . After the sputtering test, the ratio of the increased weight of the film-forming object substrate to the reduced weight of the target was 30%. After the sputtering test, the ratio of the increased weight of the insulating shielding member to the reduced weight of the target was 51%.

(Test Example 8)

A sputtering film was formed under the same sputtering conditions as in Test Example 1 except that the distance L1 between the flat target and the insulating shielding member was set to 1.5 mm. In this case, there are few abnormal discharges and stable film formation, and the film formation is finished as planned after 5 hours have passed. However, when the sputtering chamber was checked, it was found that the fixing member was also sputtered. The sputtering rate in this test was 0.069 g / h / cm ² . After the sputtering test, the ratio of the increased weight of the film-forming object substrate to the reduced weight of the target was 26%. After the sputtering test, the ratio of the increased weight of the insulating shielding member to the reduced weight of the target was 46%.

(Test Example 9)

A sputtering film was formed using the same sputtering conditions as in Test Example 1 except that the airflow sputtering conditions were changed to the following conditions.

‧Power density: 22W / cm ²

‧Sputtering gas pressure: 70Pa

‧Sputtering gas flow rate (total flow rate of each discharge port): Ar: 32.7 sccm / cm ²

‧Target material: Cu-TiO ₂ -SiO ₂

‧Relative density of target: 95%

‧The distance L1 between the flat target and the insulating shield: 0.4mm

• The interval S ₁ between a pair of flat targets before the start of sputtering: 20 mm.

In this case, there are few abnormal discharges and stable film formation, and the film formation is finished as planned after 5 hours have passed. The sputtering chamber was checked, and no abnormality was found. The sputtering rate in this test was 0.013 g / h / cm ² . After the sputtering test, the ratio of the increased weight of the film-forming object substrate to the reduced weight of the target was 28%. After the sputtering test, the ratio of the increased weight of the insulating shielding member to the reduced weight of the target was 48%.

The sputtered film of Test Example 9 was peeled from the substrate and recovered. This film was then pulverized to obtain a fine powder. This was filled into a mold made of carbon and hot-pressed under a vacuum atmosphere, a temperature of 1000 ° C., a holding time of 2 hours, and a pressure of 30 MPa to obtain a sintered body. Next, a thermal isotropic pressing process (HIP) is performed. The conditions for thermal isotropic pressure processing are: a heating rate of 300 ° C / hour, a holding temperature of 1000 ° C, and a holding time of 2 hours. The pressure of the Ar gas is gradually increased from the beginning of the heating, and the pressure is maintained at 150 MPa in the 1000 ° C heat preservation. . After the heat preservation, the natural cooling is performed directly in the furnace. The average diameter of the oxide particles in the sintered body was observed with a microscope and measured, and it was found to be 0.4 μm.

(Test Example 10)

A sputtering film was formed using the same sputtering conditions as in Test Example 1 except that the airflow sputtering conditions were changed to the following conditions.

<Airflow sputtering conditions>

‧Power density: 28W / cm ²

‧Sputtering gas pressure: 25Pa

‧Sputtering gas flow rate (total flow rate of each discharge port): Ar: 14.2 sccm / cm ²

‧Target material: Cu-TiO ₂

‧Target relative density: 97%

‧Target size: 143mm (X direction) x 493mm (Y direction) x 30mmt

‧Total projected area of target: about 1410cm ²

‧The distance L1 between the flat target and the insulating shielding member is 0.8mm.

In this case, there are few abnormal discharges and stable film formation, and the film formation is finished as planned after 5 hours have passed. In addition, in the sputtering chamber, no abnormality was found. The sputtering rate in this test was 0.011 g / h / cm ² . After the sputtering test, the ratio of the increased weight of the film-forming object substrate to the reduced weight of the target was 40%. After the sputtering test, the ratio of the increased weight of the insulating shielding member to the reduced weight of the target was 42%.

(Test Example 11)

Using a flat target opposing airflow sputtering device having a structure as shown in FIG. 1 and FIG. 2-1 (however, the installation structure of the sputtering target adopts the structure shown in FIG. 4), the sputtering is installed according to the structure shown in FIG. 4. The sputtering target is formed on the plating target under the following conditions. A sputtering film was formed using the same device structure and sputtering conditions as in Test Example 1 except that the airflow sputtering conditions were changed to the following conditions.

<Airflow sputtering conditions>

‧The distance L1 between the flat target and the insulating shielding member is 4.5mm; • The distance L3 between the lower surface of the upper panel of the insulating shielding member and the upper surface of the conductive fixing member: 4.6 mm.

In this case, there are few abnormal discharges and stable film formation, and the film formation is finished as planned after 5 hours have passed. However, when the sputtering chamber was checked, it was found that the fixing member was also sputtered. The sputtering rate in this test was 0.028 g / h / cm ² . After the sputtering test, the ratio of the increased weight of the film-forming object substrate to the reduced weight of the target was 48%. After the sputtering test, the ratio of the increased weight of the insulating shielding member to the reduced weight of the target was 37%.

(Test Example 12)

Use a flat target opposing airflow sputtering device with a structure as shown in Figures 1 and 2-1 (however, the installation structure of the sputtering target uses the structure shown in Figure 5). The sputtering target is formed on the plating target under the following conditions. A sputtering film was formed using the same device structure and sputtering conditions as in Test Example 1 except that the airflow sputtering conditions were changed to the following conditions.

<Airflow sputtering conditions>

‧ The distance L1 between the flat target and the insulating shielding member: 0.6mm; ‧ The distance L3 between the lower surface of the upper panel of the insulating shielding member and the upper surface of the conductive fixing member: 0.1mm.

In this case, there are few abnormal discharges and stable film formation, and the film formation is finished as planned after 5 hours have passed. However, when the sputtering chamber was checked, it was found that the fixing member was also sputtered. The sputtering rate in this test was 0.034 g / h / cm ² . After the sputtering test, the ratio of the increased weight of the film-forming object substrate to the reduced weight of the target was 44%. After the sputtering test, the ratio of the increased weight of the insulating shielding member to the reduced weight of the target after the sputtering test was 40%.

(Test Example 13)

Using a flat target opposing airflow sputtering device having a structure as shown in FIG. 1 and FIG. 2-1 (however, the installation structure of the sputtering target adopts the structure shown in FIG. 6), the sputtering is installed according to the structure shown in FIG. 6. The sputtering target is formed on the plating target under the following conditions. A sputtering film was formed using the same device structure and sputtering conditions as in Test Example 1 except that the airflow sputtering conditions were changed to the following conditions.

<Airflow sputtering conditions>

‧ The distance L1 between the flat target and the insulating shielding member: 0.6mm; ‧ The distance L3 between the lower surface of the upper panel of the insulating shielding member and the upper surface of the conductive fixing member: 0.5mm.

In this case, there are few abnormal discharges and stable film formation, and the film formation is finished as planned after 5 hours have passed. In addition, in the sputtering chamber, no abnormality was found. The sputtering rate in this test was 0.007 g / h / cm ² . After the sputtering test, the ratio of the increased weight of the film-forming object substrate to the reduced weight of the target was 27%. After the sputtering test, the ratio of the increased weight of the insulating shielding member to the reduced weight of the target was 48%.

(Test Example 14)

Using a flat target opposing airflow sputtering device having a structure as shown in FIG. 1 and FIG. 2-1 (however, the installation structure of the sputtering target adopts the structure shown in FIG. 7), the sputtering is installed according to the structure shown in FIG. 7. The sputtering target is formed on the plating target under the following conditions. A sputtering film was formed using the same device structure and sputtering conditions as in Test Example 1 except that the airflow sputtering conditions were changed to the following conditions.

<Airflow sputtering conditions>

‧Power density: 33W / cm ²

‧Sputtering gas pressure: 130Pa

‧Sputtering gas flow rate (sum of the flow rate of each discharge port): Ar: 33.3sccm / cm ²

‧Target size: 100mm (X direction) × 150mm (Y direction) × 10mmt

‧Total projection area of target: 300cm ²

‧The interval S ₁ between a pair of flat targets before the start of sputtering: 20mm

‧The distance L1 between the flat target and the insulating shield: 0.2mm

‧Distance L3 between the lower surface of the upper panel of the insulating shielding member and the upper surface of the conductive fixing member: 0.2mm

‧Material of back plate: Cu (structure integrated with target).

In this case, there are few abnormal discharges and stable film formation, and the film formation is finished as planned after 5 hours have passed. In addition, in the sputtering chamber, no abnormality was found. The sputtering rate in this test was 0.033 g / h / cm ² . After the sputtering test, the ratio of the increased weight of the film-forming object substrate to the reduced weight of the target was 24%. After the sputtering test, the ratio of the increased weight of the insulating shielding member to the reduced weight of the target was 48%.

Claims (16)

An airflow sputtering device includes: a sputtering chamber capable of becoming a vacuum inside; a pair of flat target materials arranged in the sputtering chamber so as to face each other with a spaced space therebetween; a pair of cooling devices For cooling each plate target; a conductive fixing member for fixing each plate target to the cooling device; one or two or more gas exhaust ports for connecting the pair of plate targets A sputter gas is supplied between the two; and a member accumulating sputtered particles is arranged to face the gas discharge port through a space portion between the pair of flat target materials so as to be located at a portion of the gas discharge port; On the opposite side, wherein the pair of flat targets have a mounting portion extending from a respective side, and the position of the mounting portion is held by the fixing member and the cooling device, the pair of flat targets Targets are respectively fixed to the cooling device, and wherein the fixing member is covered by an insulating shielding member, and the insulating shielding member does not contact the pair of flat target materials. The airflow sputtering device according to item 1 of the scope of patent application, wherein the pair of flat target materials has conductivity. The airflow sputtering device according to item 1 or item 2 of the scope of patent application, wherein the pair of flat targets are in a state where the surfaces opposite to the sputtering surface directly or indirectly contact the cooling device, It is fixed by the fixing member. According to the air flow sputtering device described in the first or second scope of the patent application, the closest distance between each flat target and the insulating shielding member is adjusted to 0.1 to 5 mm. The airflow sputtering device according to item 1 or item 2 of the scope of the patent application, wherein the insulating shielding member is selected from the group consisting of alumina, silica, zirconia, magnesium oxide, yttrium oxide, calcium oxide, and titanium oxide. And one or two or more materials of a group consisting of boron nitride. The airflow sputtering device according to item 1 or item 2 of the patent application scope, wherein the insulating shielding member has a peripheral wall, and the peripheral wall surrounds the spaced-apart space along the side of each flat target. The side is set upright. The airflow sputtering device according to item 6 of the scope of patent application, wherein an interval between the side surface of each flat target and the peripheral wall of the insulating shielding member is 0.1 to 2 mm. The airflow sputtering device according to the first or second aspect of the patent application, wherein the insulating shielding member is arranged to cover one edge portion of the sputtering surface of each flat target. The airflow sputtering device according to item 1 or item 2 of the scope of the patent application, wherein the pair of flat target materials is composed of a composite of a non-magnetic material and a magnetic material. According to the airflow sputtering device described in the first or second scope of the patent application, the fixing member does not protrude toward the upper side than the upper surfaces of the pair of flat target materials. A method for manufacturing a sputtering target material includes the step of performing sputtering by using a gas flow sputtering device according to any one of claims 1 to 10 of the scope of patent application. The manufacturing method according to item 11 of the scope of patent application, wherein sputtering is performed with a power density of 10 W / cm ² or more. The manufacturing method according to claim 11 or claim 12, wherein the flow rate on the total projected area of the sputtered surfaces opposite to the pair of flat target materials per 1 cm ² is used to represent the sputtering. The flow rate of the plating gas is set to 1 sccm / cm ² or more to perform sputtering. The manufacturing method according to claim 11 or claim 12, wherein the sputtering is performed by setting the pressure of the sputtering gas to 10 Pa or more. The manufacturing method according to claim 11 or claim 12, wherein the component that accumulates sputtered particles is a used sputtering target and includes depositing at an eroded portion of the sputtering target Steps of sputtering particles. The manufacturing method according to claim 11 or claim 12, further comprising: making a total quality of the sputtered particles deposited on the insulating shielding member greater than that on the member on which the sputtered particles are deposited. Steps of quality of stacked sputter particles.