WO2019111945A1 - 金スパッタリングターゲットの製造方法及び金膜の製造方法 - Google Patents
金スパッタリングターゲットの製造方法及び金膜の製造方法 Download PDFInfo
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- WO2019111945A1 WO2019111945A1 PCT/JP2018/044717 JP2018044717W WO2019111945A1 WO 2019111945 A1 WO2019111945 A1 WO 2019111945A1 JP 2018044717 W JP2018044717 W JP 2018044717W WO 2019111945 A1 WO2019111945 A1 WO 2019111945A1
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- gold
- sputtering target
- film
- sputtering
- target
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/02—Alloys based on gold
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
- H01J37/3411—Constructional aspects of the reactor
- H01J37/3414—Targets
- H01J37/3423—Shape
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
- H01J37/3411—Constructional aspects of the reactor
- H01J37/3414—Targets
- H01J37/3426—Material
Definitions
- the present invention relates to a method of manufacturing a gold sputtering target and a method of manufacturing a gold film.
- Au films deposited using a gold (Au) sputtering target are used in various fields because of the excellent chemical stability and electrical properties of Au itself.
- a gold (Au) sputtering target is used as an excitation electrode or the like formed on both sides of a quartz chip.
- an Au sputtering target capable of forming an Au film with a uniform film thickness distribution at the time of sputtering is required because the vibration frequency is adjusted by the film thickness of the Au film.
- a plate-like sputtering target such as a disk or a rectangular plate used for planar magnetron sputtering is generally known.
- cylindrical sputtering targets are also known.
- the cylindrical sputtering target improves the usage rate of the target material during sputtering compared to a plate-like sputtering target, so expansion starts with ceramic material targets and so on, and expansion to metal / alloy based targets is also possible.
- Application is also underway, and application to noble metal targets such as silver (Ag) is also being studied (see Patent Documents 1 and 2).
- the use of a cylindrical target is considered as well as a plate-like target.
- Crystal oscillator devices are used in portable devices, etc., and quartz oscillator devices themselves are also downsized in response to demands for smaller size, lighter weight, thinner, etc. Weight reduction, thickness reduction, etc. are required.
- the package size of the crystal unit is 5.0 ⁇ 3.2 mm (5032 size) to 3.2 ⁇ 2.5 mm (3225 size), 2.5 ⁇ 2.0 mm (2520 size), Miniaturization is progressing to 0 ⁇ 1.6 mm (2016 size) and 1.6 ⁇ 1.2 mm (1612 size), and along with this, the crystal oscillator (quartz chip) itself is also miniaturized .
- the quartz oscillator device is configured by forming an Au film as an electrode on both sides of a quartz chip (blank) as described above.
- the outer shape is trimmed by etching to round the corners, or the corners are mechanically rounded when pulled out with a press, and the center of gravity is at the center to stabilize the frequency.
- High smoothness is desirable because the rough surface of the crystal chip adversely affects the frequency characteristics.
- the electrode formed on the crystal chip it is desirable that the smoothness be high, that is, the variation in film thickness be small. Since the electrode has a three-dimensional structure having a thickness, when the crystal chip is miniaturized, the influence of the variation in film thickness on the three-dimensional shape becomes larger. Therefore, with the miniaturization of the crystal oscillator device and the like, it is required to further reduce the thickness variation of the Au film applied to the electrode.
- the variation of the mass of the Au film has a great influence on the frequency characteristics.
- a shape called a fork type or a tuning fork type is applied to a quartz oscillator having a frequency of 32 kHz.
- the tuning fork type quartz crystal vibrator is suitable for miniaturization, since the mass variation of the Au film affects the frequency characteristics, it is strongly demanded to reduce the mass variation based on the film thickness variation of the Au film. Since tuning fork type quartz oscillator is difficult to adjust the frequency, various devices have been made. For example, with respect to the formation of an Au film, the deposition method is shifted to the sputtering method.
- the present invention provides a method of manufacturing a gold sputtering target which makes it possible to improve the uniformity of film thickness distribution of a gold film, and a method of manufacturing a gold film which makes it possible to enhance the uniformity of film thickness distribution. With the goal.
- the method for producing a gold sputtering target of the present invention comprises gold and unavoidable impurities, has an average value of Vickers hardness of 40 to 60, an average crystal grain size of 15 ⁇ m to 200 ⁇ m, and gold on the surface to be sputtered. Manufacturing a gold sputtering target in which the ⁇ 110 ⁇ plane of the ⁇ 110 ⁇ plane is preferentially oriented.
- the method for producing a gold film of the present invention comprises gold and unavoidable impurities, has an average value of Vickers hardness of 40 to 60, an average crystal grain size of 15 ⁇ m to 200 ⁇ m, and has a gold sputtered surface.
- the method includes the steps of preparing a gold sputtering target whose ⁇ 110 ⁇ plane is preferentially oriented, and forming a gold film on a film-forming substrate by sputtering the gold sputtering target.
- a gold sputtering target of the present invention capable of obtaining a gold film excellent in uniformity of film thickness distribution can be produced with good reproducibility. Therefore, it becomes possible to improve the uniformity of the film thickness distribution of the gold film with good reproducibility. Furthermore, according to the method for producing a gold film of the present invention, it is possible to reproducibly provide a gold film excellent in uniformity of film thickness distribution.
- the sputtering target manufactured by applying the manufacturing method of embodiment consists of gold (Au) and an unavoidable impurity.
- the unavoidable impurities other than Au contained in the Au sputtering target are not particularly limited.
- the purity of Au in the sputtering target is set according to the usage of the target and the usage of the film formed using the target, and for example, the Au purity is set to 99.99% or more. By using a sputtering target having an Au purity of 99.99% or more, a high purity Au film can be obtained.
- the upper limit value of the Au purity of the sputtering target is not particularly limited, it is generally less than 99.999% in consideration of the production process and production cost of the Au sputtering target, the hardness of the Au sputtering target, and the like. Practically, 99.990% or more and 99.998% or less are preferable.
- the shape of the Au sputtering target of the embodiment is not particularly limited, and may be any of a plate and a cylinder.
- a typical shape of a plate-like sputtering target for example, a polygonal plate such as a disk or a rectangular plate may be mentioned.
- a hollow plate is formed by hollowing out a part of a disk or polygon plate, or a part of the surface of a disk or polygon plate is provided with an inclined part, a convex part, a recess or the like.
- the shape is not particularly limited.
- the shape of the cylindrical sputtering target is not particularly limited, and a shape or the like corresponding to the sputtering apparatus is applied.
- the Au sputtering target has a surface to be sputtered (sputtered surface).
- the surface of the plate is a sputtered surface
- the surface of a cylinder is a sputtered surface.
- the Au sputtering target of the embodiment has a Vickers hardness of 40 or more and 60 or less.
- a Vickers hardness of 40 or more and 60 or less By performing sputtering film formation using an Au sputtering target having such Vickers hardness, an Au film excellent in uniformity of film thickness distribution can be formed. That is, that the Vickers hardness of Au sputtering target exceeds 60 HV means that the distortion which arose at the time of manufacture in the sputtering target remains. In such a case, the flying of particles from the target becomes uneven during sputtering, and the uniformity of the film thickness distribution is lost.
- the Vickers hardness of the Au sputtering target is preferably 55 HV or less.
- the Vickers hardness of the Au sputtering target is less than 40 HV, it is thought that the crystal orientation starts to break up due to the occurrence of crystal grain growth, thereby impairing the uniformity of the film thickness distribution.
- the Vickers hardness of the Au sputtering target is preferably 45 HV or more.
- the Vickers hardness of the Au sputtering target is measured as follows. In the case of a plate-like sputtering target, the measurement point is divided into three in 10 mm intervals on the arbitrary straight line of the sputtering surface (the surface to be sputtered) and in the thickness direction of the first cross section orthogonal to the sputtering surface.
- the average values (HV av1 , HV av2 , HV av3 ) of the sputtered surface, the first cross section, and the second cross section are averaged, and the average value is the average Vickers hardness of the plate-like Au sputtering target as a whole.
- the ratio (HV av 3 / HV tav ) to the Vickers hardness (HV tav ) is preferably in the range of 0.8 or more and 1.2 or less.
- the variation in Vickers hardness of the Au sputtering target within ⁇ 20%.
- the flying direction of particles at the time of sputtering can be made more uniform, and the uniformity of the film thickness distribution can be further improved.
- the measurement point is rotated by 90 ° from the first straight line by three points every 10 mm on an arbitrary first straight line parallel to the cylinder axis in the sputtering surface (cylindrical surface) 3 places on every 10 mm on the second straight line, and 1 place from the area divided into 3 in the thickness direction of the cross section orthogonal to the cylinder axis (5 mm in thickness in the example) (3 places in total) at intervals of 1.5 mm on a straight line in the thickness direction with respect to the sample of (a).
- the Vickers hardness of each of these measurement points is measured with a test force (press load) of 200 gf.
- the average value of Vickers hardness in the first straight line on the sputtering surface (HV av1), the average value of Vickers hardness in the second straight line (HV av2), and the average value of Vickers hardness in the cross section (HV av3 ) Is calculated respectively.
- the average values (HV av1 , HV av2 , HV av3 ) of the sputtered surface and the cross section are further averaged, and the value is taken as the average value (HV tav ) of the Vickers hardness of the cylindrical Au sputtering target as a whole.
- the variation in Vickers hardness of the Au sputtering target within ⁇ 20%.
- the flying direction of particles at the time of sputtering is further uniformed, and the uniformity of film thickness distribution is further improved.
- the cylindrical Au sputtering target the entire cylindrical surface is sputtered while rotating the cylindrical target. Therefore, the variation in the Vickers hardness at each part of the sputtering surface (cylindrical surface) is reduced, and the uniformity of the film thickness distribution is obtained. Can be improved.
- the average crystal grain size is preferably 15 ⁇ m or more and 200 ⁇ m or less.
- the uniformity of the film thickness distribution of the Au film can be further enhanced. That is, when the average crystal grain size of the Au sputtering target is less than 15 ⁇ m, the particles may not fly uniformly from the target at the time of sputtering, and the uniformity of the film thickness distribution may be impaired.
- the average crystal grain size of the Au sputtering target is preferably 30 ⁇ m or more.
- the average crystal grain size of the Au sputtering target exceeds 200 ⁇ m, the flightability of particles during sputtering may be reduced, and the uniformity of the film thickness distribution may be impaired.
- the average crystal grain size of the Au sputtering target is more preferably 150 ⁇ m or less.
- the average grain size of the Au sputtering target is measured as follows.
- the measurement point is a region divided into three in the thickness direction of the first cross section orthogonal to the sputtering surface, at three points of every 10 mm on an arbitrary straight line of the sputtering surface.
- the average value of the crystal grain size in the sputter surface (AD av1), the average value of the grain size in the first section (AD av2), and the average value of the grain size of the second section (AD av3 ) Is calculated respectively.
- the average values (AD av1 , AD av2 , AD av3 ) of the crystal grain sizes of the sputtered surface, the first cross section, and the second cross section are further averaged, and the value is obtained as a whole of the plate-like Au sputtering target.
- the ratio of the average crystal grain size of the target as a whole the average crystal grain size of the sputtering surface of the above-described (AD av1) (AD tav) (AD av1 / AD tav), the first section the average grain size (AD av2) ratio to the average crystal grain size of the target as a whole (AD tav) of (AD av2 / AD tav), and the average crystal grain size of the second section target as a whole of the (AD av3)
- the ratio (AD av 3 / AD tav ) to the average crystal grain size (AD tav ) is preferably in the range of 0.8 to 1.2, respectively.
- the variation of the average crystal grain size of the Au sputtering target within ⁇ 20%.
- the flying direction of the particles at the time of sputtering is made more uniform, and the uniformity of the film thickness distribution is further improved.
- the measurement point is rotated by 90 ° from the first straight line by three points every 10 mm on an arbitrary first straight line parallel to the cylinder axis in the sputtering surface (cylindrical surface) 3 places on every 10 mm on the second straight line, and 1 place from the area divided into 3 in the thickness direction of the cross section orthogonal to the cylinder axis (5 mm in thickness in the example) (3 places in total) at intervals of 1.5 mm on a straight line in the thickness direction with respect to the sample of (a).
- Average value of crystal grain size on first straight line of sputtered surface (AD av1 ), average value of crystal grain size on second straight line (AD av2 ), and average value of crystal grain size in cross section (AD av3 ) are calculated respectively.
- the average values (AD av 1 , AD av 2 , AD av 3 ) of these sputtered surfaces and cross sections are further averaged, and the value is taken as the average crystal grain size (AD tav ) as a whole of the cylindrical Au sputtering target.
- the ratio of the average crystal grain size of the target as a whole of the first average grain size of the sputtering face described above (AD av1) (AD tav) (AD av1 / AD tav)
- the sputtering surface the average ratio of grain diameter (AD tav) of the target as a whole of the second average grain diameter (AD av2) (AD av2 / AD tav)
- the ratio (AD av 3 / AD tav ) to the average crystal grain size (AD tav ) of each is preferably in the range of 0.8 or more and 1.2 or less.
- the variation of the average crystal grain size of the Au sputtering target within ⁇ 20%.
- the flying direction of particles at the time of sputtering is further uniformed, and the uniformity of the film thickness distribution is further improved.
- the cylindrical Au sputtering target the entire cylindrical surface is sputtered while rotating the cylindrical target, so that the variation in average crystal grain size in each part of the sputtered surface (cylindrical surface) is reduced to make the film thickness distribution uniform.
- the sex can be further improved.
- the ⁇ 110 ⁇ plane of Au is preferentially oriented on the sputtering surface.
- Au has a face-centered cubic lattice structure, and among the crystal planes constituting it, the ⁇ 110 ⁇ plane is more easily sputtered than other crystal planes.
- X-ray diffraction of the sputtered surface of the Au sputtering target is carried out that the sputtered surface is preferentially oriented to the ⁇ 110 ⁇ plane, and the following formula (1) of Wilson is obtained from the diffraction intensity ratio of each crystal surface of Au.
- the orientation index N of each crystal plane is determined from the above, and the case where the orientation index N of the ⁇ 110 ⁇ plane is larger than 1 and the largest among the orientation indices N of all crystal planes is shown.
- the orientation index N of Au ⁇ 110 ⁇ plane is more preferably 1.3 or more.
- I / I (hkl) is the diffraction intensity ratio of (hkl) plane in X-ray diffraction
- JCPDS ⁇ I / I (hkl) is (hkl) plane in JCPDS (Joint Committee for Powder Diffraction Standards) card diffraction intensities of all crystal planes in the diffraction intensity ratio
- ⁇ (I / I (hkl )) is the sum of the diffraction intensity ratio of the total crystal surface in the X-ray diffraction
- ⁇ (JCPDS ⁇ I / I (hkl)) is JCPDS card It is the sum of ratios.
- the Au sputtering target of the embodiment is a sputtered Au film based on the combination of the above-mentioned Vickers hardness of 40 or more and 60 or less, the average crystal grain size of 15 ⁇ m or more and 200 ⁇ m or less and the ⁇ 110 ⁇ plane of Au preferentially oriented. This makes it possible to significantly improve the uniformity of the film thickness distribution. That is, by the synergistic action of the Vickers hardness, the average grain size, and the individual effects of the preferred orientation plane of Au mentioned above, the flightability and uniformity of the particles at the time of sputtering, and further the stability of the flight direction of the particles. Improve.
- the manufacturing method of the Au sputtering target of the embodiment described above is made of gold and unavoidable impurities, the average value of Vickers hardness is 40 to 60, the average crystal grain size is 15 ⁇ m to 200 ⁇ m, and the surface to be sputtered Manufacturing a gold sputtering target in which the ⁇ 110 ⁇ plane of gold is preferentially oriented.
- the method of manufacturing an Au sputtering target includes, for example, a step of preparing a gold ingot having a gold purity of 99.99% or more, and a first step of processing the gold ingot to form a desired plate-like or cylindrical gold billet. It comprises a processing step, a second processing step of processing a gold billet while reducing its thickness under pressure to form a desired plate-like or cylindrical target material, and a heat treatment step of heat-treating the target material. Is preferred.
- the manufacturing method of Au sputtering target of embodiment is explained in full detail.
- a plate-like Au sputtering target it can be manufactured by a manufacturing method combining casting, cutting, forging, and heat treatment of an Au raw material.
- rolling may be applied instead of forging of the Au raw material.
- a cylindrical Au sputtering target it can be manufactured by a manufacturing method combining casting, cutting, pipe processing, and heat treatment of an Au raw material.
- pipe processing include extrusion processing such as the Raflo method, drawing processing, forging processing and the like.
- the Au raw material In the casting process of the Au raw material, it is melted in a graphite crucible or a ceramic crucible in a vacuum atmosphere or an inert atmosphere, or while blowing an inert gas onto the surface of the molten metal using an air melting furnace, or a carbon-based solid sealing material It is preferable to carry out melting in a graphite crucible or a ceramic crucible while covering the surface of the molten metal and casting in a graphite or cast iron mold. Next, the surface defects on the outer peripheral surface of the cast Au ingot are removed by grinding.
- the Au purity of the Au ingot is preferably 99.99% or more (4N or more).
- the upper limit of the Au purity of the Au ingot is not particularly limited, and is set according to the purity required for the Au sputter film, but the production process, hardness, etc. of the Au sputtering target are taken into consideration. Preferably, it is less than 99.999%.
- the cast Au ingot is processed into a desired plate or cylindrical gold billet (first processing step).
- a plate-like Au sputtering target for example, a plate-like gold billet is produced by grinding and removing surface defects on the outer peripheral surface of the Au ingot formed into a plate-like shape.
- a cylindrical gold billet is produced by grinding and removing surface defects on the outer peripheral surface of a cylindrically shaped Au ingot, and hollowing out the inside.
- the gold billet is processed into a desired plate-like or cylindrical target material (second processing step).
- the plate-like Au ingot is forged into a desired plate shape.
- the forging process of the Au ingot is preferably performed hot at 200 ° C. or more and 800 ° C. or less, and is further performed so that the working ratio (cross-section reduction rate or thickness reduction rate) becomes 50% or more and 90% or less Is preferred.
- the forging process may be performed a plurality of times, and heat treatment may be performed on the way. When the forging process is performed a plurality of times, the processing rate is adjusted so that the processing rate as a whole is 50% or more and 90% or less.
- the processing rate of forging may be subjected to cold rolling, if necessary.
- the processing rate of the rolling process depends on the processing rate at the time of forging, but is preferably 50% to 90%.
- a rolling process may be applied to the process of processing the Au ingot.
- the rolling process of the Au ingot is preferably performed in the range of 200 ° C. or more and 800 ° C. or less hot as in the forging step, and the working ratio (cross sectional reduction rate or thickness reduction rate) is 50% or more and 90% It is preferable to carry out so that it may become the following ranges.
- a cylindrical Au billet is processed into a pipe shape by extrusion, drawing, forging, or the like such as the Raflo method.
- the extrusion processing is preferably performed cold, and the outer diameter and thickness of the pipe are determined by the shape of the die (inner diameter etc.) and the shape of the mandrel (outside diameter etc.) Control.
- the extrusion ratio it is preferable to adjust the extrusion ratio (outside diameter of billet / outside diameter of pipe) to be 1.5 or more and 3.0 or less.
- the extrusion ratio By setting the extrusion ratio to 1.5 or more, it is possible to break the cast structure to easily obtain a uniform recrystallized structure and to improve the controllability and uniformity of hardness in the subsequent heat treatment step. However, when the extrusion ratio exceeds 3.0, the internal strain becomes too large, and cracks and wrinkles easily occur.
- the outer diameter and thickness of the pipe are controlled by the shape (outside diameter etc.).
- it is preferable to adjust the processing rate per time to 2% or more and 5% or less.
- the drawing process is preferably performed repeatedly several times, and in such a case, it is preferable to adjust the total processing rate to 50% or more and 90% or less.
- the total processing ratio By setting the total processing ratio to 50% or more, it is possible to break the cast structure to easily obtain a uniform recrystallized structure and to improve the controllability and uniformity of hardness in the subsequent heat treatment step. However, if the total processing ratio exceeds 90%, the internal strain becomes too large, and cracks, wrinkles and the like easily occur.
- the forging step is preferably performed with the processing rate adjusted to 30% or more and 80% or less.
- the processing rate is adjusted to 30% or more, it is possible to break the cast structure to easily obtain a uniform recrystallized structure and to improve the controllability and uniformity of hardness in the subsequent heat treatment step.
- the processing rate exceeds 80%, the internal strain becomes too large, and cracks and wrinkles are easily generated.
- the plate-like target material produced in the forging process or the rolling process, and the pipe-like target material produced in the pipe processing are heated, for example, at a temperature of 200 ° C. or more and 500 ° C. or less in the atmosphere or in an inert gas atmosphere.
- the heat treatment recrystallizes the metal structure of the target material.
- an Au sputtering target having a Vickers hardness of 40 or more and 60 or less can be obtained.
- the heat treatment step may be performed multiple times. After the heat treatment step, a step of adjusting the shape of the sputtering target by cutting or the like may be performed as necessary.
- the heat treatment temperature is less than 200 ° C.
- the internal strain generated at the time of processing can not be sufficiently removed, and the Vickers hardness may exceed 60.
- the metal structure of the target material can not be sufficiently recrystallized, there is a possibility that the sputtered surface can not be preferentially oriented to the ⁇ 110 ⁇ plane.
- the heat treatment temperature exceeds 500 ° C.
- the Vickers hardness may be less than 40.
- the recrystallized structure may grow too much, and the average crystal grain size may exceed 200 ⁇ m, or the sputtered plane may be preferentially oriented to crystal planes other than the ⁇ 110 ⁇ plane.
- the holding time (heat treatment time) according to the heat treatment temperature is preferably, for example, 10 minutes or more and 120 minutes or less. If the heat treatment time is too short, there is a possibility that the removal of the strain is insufficient or the metal structure can not be sufficiently recrystallized. On the other hand, if the heat treatment time is too long, the Vickers hardness may be too low, or the average grain size may be too large.
- the Vickers hardness is 40 or more and 60 or less, and the variation in Vickers hardness is controlled by controlling the working ratio in the step of processing the Au ingot into a plate or cylindrical shape and the temperature of the recrystallization heat treatment step.
- the Au sputtering target of the embodiment can be used not only for forming an electrode film (Au film) of a quartz oscillator device, but also for forming an Au film applied to various electronic components.
- the method for producing a gold (Au) film of the embodiment is composed of gold and unavoidable impurities, has an average value of Vickers hardness of 40 to 60, an average crystal grain size of 15 ⁇ m to 200 ⁇ m, and a sputtered surface Forming a gold (Au) film on a film-forming substrate by preparing a gold (Au) sputtering target in which the ⁇ 110 ⁇ plane of gold is preferentially oriented and sputtering the gold sputtering target Have a process.
- the process of preparing the Au sputtering target includes each process for manufacturing the Au sputtering target by the manufacturing method of the embodiment described above, and specific conditions and the like are as described above.
- the film formation step of the Au film is a step of forming the Au film on the film formation substrate by sputtering the Au sputtering target of the embodiment.
- the Au sputtering target may be either a plate-like target or a cylindrical target, as shown in the above-mentioned method of producing an Au sputtering target.
- DC sputtering two-pole, three-pole or four-pole
- RF sputtering magnetron sputtering
- ion beam sputtering ion beam sputtering
- ECR electrotron cyclotron resonance
- an Au film for example, a quartz substrate (quartz crystal oscillator) on which the Au sputtering target of the embodiment and the Au film are deposited, a semiconductor substrate, a glass substrate, a substrate such as a metal substrate, a resin film
- a film-forming substrate such as a metal film or a film such as a composite film of resin and metal is disposed in a vacuum chamber of a sputtering apparatus, and the inside of the vacuum chamber is evacuated to a predetermined degree of vacuum.
- a sputtering gas such as Ar gas or nitrogen gas is introduced into the chamber.
- the sputtering method to be applied for example, DC sputtering method, RF sputtering method, magnetron sputtering method, etc., between the Au sputtering target and the film formation substrate while generating plasma in the vacuum chamber.
- a DC voltage or an RF voltage is applied, and in the ion beam sputtering method, an Au sputtering target is irradiated with an ion beam.
- An Au film is formed by depositing sputtered particles (Au particles) emitted from an Au sputtering target by irradiation of ionized sputter gas molecules or ion beams on a film formation substrate.
- the sputtering conditions in the film formation process of the Au film are not particularly limited. It is appropriately set according to the sputtering method to be applied, the sputtering apparatus, the shape of the Au sputtering target, the thickness and the area of the Au film to be formed, and the like.
- the sputtering apparatus used for forming the Au film is not particularly limited, and various sputtering apparatuses such as sheet type, batch type, multi-chamber type, load lock type, and in-line type can be applied. Since the Au sputtering target may be either a plate-like target or a cylindrical target as described above, a sputtering apparatus according to the shape of these Au sputtering targets is applied.
- the film formation process of the Au film is not limited to the process of film formation by the sputtering method and conditions described in the examples described later, and for example, the Au film is formed by applying the conditions as shown below It is also good.
- an Au sputtering target and a film formation substrate are set in a DC sputtering apparatus.
- the inside of the sputtering apparatus is evacuated to a final vacuum of 8 ⁇ 10 ⁇ 4 Pa or less.
- Ar gas is introduced into the sputtering apparatus, the vacuum degree is adjusted to, for example, about 0.4 Pa to 0.53 Pa, and the film-forming substrate is etched, for example, for 5 minutes.
- pre-sputtering is performed, for example, under the conditions of input power: DC 500 W and sputtering time: 5 minutes.
- an Au film is formed by performing sputtering under the conditions of, for example, input power: DC 500 W and sputtering time: 5 minutes. After film formation, the film is cooled in a sputtering apparatus and taken out after 1 hour.
- the Vickers hardness of the Au sputtering target used in the film forming process the average crystal grain size, the preferred orientation plane ( ⁇ 110 ⁇ plane) of the Au crystal plane in the sputtering plane, etc. Based on this, it is possible to obtain an Au film which is excellent in the uniformity of the film thickness distribution. Therefore, the film thickness distribution is uniform in various devices such as quartz oscillator devices, semiconductor devices, LED devices, LCD devices, OLED devices, magnetic devices, battery devices, optical devices, and various materials such as electronic materials and functional materials. It is possible to provide an Au film which is excellent in the properties and uniformity of resistance value based thereon. By these, it becomes possible to achieve improvement in the manufacturing yield of various devices and various materials, miniaturization, high functionality, and the like.
- the film forming method of the embodiment since the variation in film thickness can be reduced, the choice of film forming conditions can be expanded, the conditions for forming the film can be simplified, and the Au film can be formed efficiently. can do. Furthermore, since the variation of the film thickness of the Au film is small, for example, in the quartz vibrator, the mass variation of the Au film can be reduced, and therefore the yield of the product can be improved.
- Example 1 First, an Au block was inserted into a graphite crucible and melted. Au molten metal was cast into a graphite mold to prepare an Au ingot. By grinding and removing the surface of the Au ingot, an Au billet (purity 99.99%, analysis by solid-state emission analysis and ICP) having a width of 190 mm, a length of 270 mm and a thickness of 50 mm was produced. Then, the Au billet was hot forged at a temperature of 800 ° C. to form an Au target material having a width of 70 mm, a length of 200 mm, and a thickness of 45 mm. The processing rate during forging was 80% in all three axial directions.
- the forged Au target material was heat treated at a temperature of 500 ° C. for 30 minutes.
- the heat-treated Au target material was ground to prepare a disk-shaped Au sputtering target having a diameter of 152.4 mm and a thickness of 5 mm.
- Two Au sputtering targets were prepared for measuring the characteristics of each part and measuring the film thickness characteristics. The same applies to the following examples and comparative examples.
- the Vickers hardness of the obtained Au sputtering target was measured according to the measurement method of the plate-like sputtering target described above (apparatus name: mitsutoyo HM-123).
- the average value (HV av1 ) of the Vickers hardness of a sputtering surface is 50.5
- the Vickers hardness of the 1st section the average value (HV av2) is 52.1
- the mean value of Vickers hardness of the second section HV av3
- the average value of these values Vickers hardness of the target as a whole (HV tav) ) was 51.4.
- HV tav The ratio of each part of the Vickers hardness for the Vickers hardness of the target as a whole (HV tav) (HV av1, HV av2, HV av3) is, HV av1 / HV tav is 0.98, HV av2 / HV tav 1.01 , HV av3 / HV tav was 1.00.
- the average crystal grain size of the Au sputtering target was measured according to the measurement method of the plate-like sputtering target described above (apparatus name: OLYMPUS DSX500). As a result, the average grain size (AD tav ) of the entire target was 34.2 ⁇ m.
- the sputtered surface of the Au sputtering target was subjected to X-ray diffraction, and the crystal plane preferentially oriented was evaluated according to the method described above. As a result, it was confirmed that the ⁇ 110 ⁇ plane of Au is preferentially oriented on the sputtered surface.
- the orientation index N of the ⁇ 110 ⁇ plane was determined according to the method described above, the orientation index N of the ⁇ 110 ⁇ plane was 1.32. The characteristics were evaluated by using such an Au sputtering target in a film forming process described later.
- Examples 2 to 7, Comparative Examples 1 to 2 An Au billet manufactured in the same manner as in Example 1 was forged by applying the processing ratio shown in Table 1 in the same manner as in Example 1. Next, heat treatment was performed on the forged Au target material under the conditions shown in Table 1. After that, the Au target material after the heat treatment was ground to produce an Au sputtering target having the same shape as that of Example 1. The Vickers hardness, average grain size, preferred orientation plane of sputtered surface, and orientation index N of ⁇ 110 ⁇ plane of these Au sputtering targets were measured and evaluated in the same manner as in Example 1. The measurement results are shown in Table 2. The characteristics were evaluated by using such an Au sputtering target in a film forming process described later. In the Au sputtering target of Comparative Example 1, the crystal grain boundaries could not be clearly identified, and therefore, the average crystal grain size could not be measured (indicated as “-” in Table 1).
- Each Au sputtering target according to the above-described Examples 1 to 7 and Comparative Examples 1 to 2 is attached to a sheet sputtering apparatus (apparatus name: ANELVA SPF 530H), and the inside of the apparatus is evacuated to 1 ⁇ 10 -3 Pa or less. Sputtering was performed under the conditions of gas pressure: 0.4 Pa, input power: DC 100 W, target-substrate distance: 40 mm, and sputtering time: 5 minutes to form an Au film on a 6-inch Si substrate (wafer). The film thickness distribution of the obtained Au film was evaluated as follows.
- a substrate on which an Au film is formed is attached to a fluorescent X-ray film thickness meter, measurement time: 60 seconds, repeated measurement: 10 times, measurement start point: substrate edge, measurement point interval: 5 mm, The film thickness was measured.
- the film thickness measurement axes were four axes, that is, two vertical and horizontal axes passing through the center of the substrate, and two vertical and horizontal axes passing through the center of the substrate in a state rotated 45 degrees therefrom.
- the 10-point average film thickness of each measurement point was calculated, the standard deviation of the measurement values at the same measurement position of 4 axes was calculated, and the average value of the standard deviation of all measurement positions was calculated. This value is shown in Table 3 as the standard deviation ⁇ of the film thickness.
- the resistance value of the Au film was measured by the four probe method, and the standard deviation ⁇ of the resistance value was determined in the same manner as the film thickness. The results are shown in Table 3 as the standard deviation ⁇ of the resistance value of the Au film.
- the Vickers hardness is in the range of 40 to 60, and the variation in Vickers hardness of each portion is also small.
- the average crystal grain size is in the range of 15 ⁇ m to 200 ⁇ m
- the ⁇ 110 ⁇ plane is preferentially oriented on the sputtered surface
- the orientation index N of the ⁇ 110 ⁇ plane is larger than 1.
- Example 8 to 12 An Au billet manufactured in the same manner as in Example 1 was forged by applying the working ratio shown in Table 4 in the same manner as in Example 1. Next, the forged Au target material was heat-treated under the conditions shown in Table 4. After that, the Au target material after the heat treatment was ground to produce an Au sputtering target having the same shape as that of Example 1.
- the Vickers hardness of the obtained Au sputtering target was measured in the same manner as in Example 1. Furthermore, the average crystal grain size of the Au sputtering target was measured according to the measurement method of the plate-like sputtering target described above. As a measurement result, the average grain size (AD av 1 , AD av 2 , AD av 3 ) of each of the sputtered surface, the first cross section, and the second cross section, the average value of these respective values (the average crystal grain size as the whole target) The ratio of the average grain size (AD av1 , AD av2 , AD av3 ) of each portion to (AD tav )) and the average grain size (AD tav ) of the whole target is shown in Table 5.
- the sputtered surface of the Au sputtering target was subjected to X-ray diffraction, and the preferentially oriented crystal plane was evaluated according to the method described above.
- the orientation index N of the ⁇ 110 ⁇ plane was determined according to the method described above.
- Table 5 The results are shown in Table 5.
- the film forming process was performed in the same manner as in Example 1, and the standard deviation ⁇ of the film thickness of the Au film and the standard deviation ⁇ of the resistance value were obtained. The results are shown in Table 6.
- Examples 13 to 21, Comparative examples 3 to 4 First, an Au block was inserted into a graphite crucible and melted. Au molten metal was cast into a graphite mold to prepare an Au ingot. By grinding and removing the surface of the Au ingot, an Au billet (purity 99.99%) having a width of 200 mm, a length of 300 mm, and a thickness of 45 mm was produced. Subsequently, the Au billet was hot-rolled at a temperature of 800 ° C. to obtain an Au target material having a width of 70 mm, a length of 200 mm, and a thickness of 45 mm. The processing rate at the time of rolling was 80% as the reduction rate of thickness. The rolled Au target material was heat treated under the conditions shown in Table 7. The heat-treated Au target material was ground to prepare a disk-shaped Au sputtering target having a diameter of 152.4 mm and a thickness of 5 mm.
- the obtained Au sputtering target it carried out similarly to Example 1 and measured the average value ( HVtav ) of the Vickers hardness as the whole target, and the average grain size ( ADtav ) as the whole target. Furthermore, the crystal plane preferentially oriented on the sputtered surface of the Au sputtering target was evaluated in the same manner as in Example 1, and the orientation index N of the ⁇ 110 ⁇ plane was determined in the same manner as in Example 1. The results are shown in Table 8. Using such an Au sputtering target, the film forming process was performed in the same manner as in Example 1, and the standard deviation ⁇ of the film thickness of the Au film and the standard deviation ⁇ of the resistance value were obtained. The results are shown in Table 9.
- Example 22 First, an Au block was inserted into a graphite crucible and melted. Au molten metal was cast into a graphite mold to prepare an Au ingot. The surface of the Au ingot was ground and removed, and hollowed with an inner diameter of 50 mm to produce a cylindrical Au billet (purity 99.99%) having an outer diameter of 100 mm, an inner diameter of 50 mm, and a length of 200 mm. Next, with the core inserted in the hollow portion of the cylindrical Au billet, the core is heated to a temperature of 800 ° C. and hot forged, and a pipe-shaped Au target having an outer diameter of 80 mm, an inner diameter of 50 mm and a length of 400 mm or more It was a material.
- the processing rate at the time of forging was 35% as the reduction rate of thickness.
- the forged pipe-like Au target material was heat-treated at a temperature of 500 ° C. for 30 minutes. By grinding the Au target material after the heat treatment, a cylindrical Au sputtering target having an outer diameter of 70 mm, an inner diameter of 65 mm, and a length of 350 mm was produced.
- the Vickers hardness of the obtained Au sputtering target was measured according to the measuring method of the cylindrical sputtering target mentioned above.
- the average Vickers hardness (HV av1 ) on the first straight line of the sputter surface as a result of measuring the Vickers hardness of each measurement point with a test force (press load) of 200 gf is 50.6, the second of the sputter surface
- the average value (HV av2 ) of the Vickers hardness on the straight line of 2 is 50.4, the average value (HV av3 ) of the Vickers hardness at the cross section is 52.0, and the average value of these respective values (Vickers hardness as the whole target (HV tav )) was 51.0.
- the ratio of the Vickers hardness (HV av1 , HV av2 , HV av3 ) of each part to the Vickers hardness (HV tav ) as the entire target is HV av1 / HV tav 0.99, HV av2 / HV tav 0. 99, HVav3 / HVtav was 1.02.
- the average crystal grain size of the Au sputtering target was measured according to the measurement method of the cylindrical sputtering target described above. As a result, the average grain size (AD tav ) of the entire target was 38.1 ⁇ m.
- the sputtered surface of the Au sputtering target was subjected to X-ray diffraction, and the crystal plane preferentially oriented was evaluated according to the method described above. As a result, it was confirmed that the ⁇ 110 ⁇ plane of Au is preferentially oriented on the sputtered surface.
- the orientation index N of the ⁇ 110 ⁇ plane was determined according to the method described above, the orientation index N of the ⁇ 110 ⁇ plane was 1.31. The characteristics were evaluated by using such a cylindrical Au sputtering target in a film forming process described later.
- Examples 23 to 28, Comparative Examples 5 to 6 An Au billet manufactured in the same manner as in Example 22 was subjected to forging processing to which a processing ratio shown in Table 10 was applied in the same manner as in Example 22 to prepare an Au target material. Next, heat treatment was performed on the forged Au target material under the conditions shown in Table 10. Thereafter, the Au target material after the heat treatment was ground to produce an Au sputtering target having the same shape as that of Example 22. The Vickers hardness and the average grain size (AD tav ) of these Au sputtering targets were measured in the same manner as in Example 22.
- Example 22 Furthermore, the crystal plane preferentially oriented to the sputtered surface of the Au sputtering target was evaluated in the same manner as in Example 22, and the orientation index N of the ⁇ 110 ⁇ plane was obtained in the same manner as in Example 22. The results are shown in Table 11. The characteristics were evaluated by using such a cylindrical Au sputtering target in a film forming process described later.
- the Au sputtering targets according to Examples 22 to 28 and Comparative Examples 5 to 6 described above are attached to a cylindrical sputtering apparatus, and the inside of the apparatus is evacuated to 1 ⁇ 10 ⁇ 3 Pa or less, and then Ar gas pressure: 0.4 Pa, Sputtering was performed under the conditions of input power: DC 100 W, target-substrate distance: 40 mm, and sputtering time: 5 minutes to form an Au film on a 6-inch Si substrate (wafer).
- the film thickness distribution of the obtained Au film was measured according to the method described above, and the standard deviation ⁇ of the film thickness of the Au film was determined. Further, the standard deviation ⁇ of the resistance value of the Au film was determined according to the method described above. The results are shown in Table 12.
- the Vickers hardness is in the range of 40 or more and 60 or less, and it can be seen that the variation in Vickers hardness of each part is also small.
- the average crystal grain size is in the range of 15 ⁇ m to 200 ⁇ m
- the ⁇ 110 ⁇ plane is preferentially oriented on the sputtered surface
- the orientation index N of the ⁇ 110 ⁇ plane is larger than 1.
- Example 29 to 33 An Au billet manufactured in the same manner as in Example 22 was subjected to a forging process to which the processing ratio shown in Table 13 was applied as in Example 22. Next, the forged Au target material was heat-treated under the conditions shown in Table 13. Thereafter, the Au target material after the heat treatment was ground to produce an Au sputtering target having the same shape as that of Example 22.
- the Vickers hardness of the obtained Au sputtering target was measured in the same manner as in Example 22. Furthermore, the average crystal grain size of the Au sputtering target was measured according to the measurement method of the cylindrical sputtering target described above. As a measurement result, the average value (AD av 1 , AD av 2 , AD av 3 ) of the crystal grain size of each of the first sputtered surface, the second sputtered surface, and the cross section, and the average value of these respective values (average as a whole target) the ratio of the crystal grain size (AD tav)), and the average crystal grain size of each section to the average crystal grain size of the target as a whole (AD tav) (AD av1, AD av2, AD av3), shown in Table 14.
- the sputtered surface of the Au sputtering target was subjected to X-ray diffraction, and the crystal plane preferentially oriented was evaluated according to the method described above, and the orientation index N of the ⁇ 110 ⁇ plane was determined.
- the results are shown in Table 14.
- the film forming process was carried out in the same manner as in Example 22, and the standard deviation ⁇ of the film thickness of the Au film and the standard deviation ⁇ of the resistance value were measured. The results are shown in Table 15.
- the method for producing an Au sputtering target of the present invention is useful for producing an Au sputtering target used for film formation of an Au film used for various applications. Further, according to the method for producing an Au film using the Au sputtering target produced by the production method of the present invention, it is possible to obtain an Au film excellent in uniformity of film thickness distribution and resistance value. Therefore, the characteristics of the Au film used for various applications can be enhanced.
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Abstract
Description
まず、Au塊を黒鉛るつぼに挿入して溶解した。Au溶湯を黒鉛鋳型に鋳造してAuインゴットを作製した。Auインゴットの表面を研削除去することによって、幅が190mm、長さが270mm、厚さが50mmのAuビレット(純度99.99%、固体発光分析およびICPにて分析)を作製した。次いで、Auビレットを800℃の温度で熱間鍛造し、幅が70mm、長さが200mm、厚さが45mmのAuターゲット素材とした。鍛造時の加工率は三軸方向共に80%とした。鍛造後のAuターゲット素材を500℃の温度で30分間熱処理した。熱処理後のAuターゲット素材を研削加工して、直径が152.4mm、厚さが5mmの円板状のAuスパッタリングターゲットを作製した。Auスパッタリングターゲットは、各部の特性測定と膜厚特性の測定のために2個作製した。以下の実施例および比較例も同様である。
実施例1と同様にして作製したAuビレットに対して、実施例1と同様に表1に示す加工率を適用した鍛造加工を施してAuターゲット素材を作製した。次いで、鍛造後のAuターゲット素材に表1に示す条件で熱処理を施した。この後、熱処理後のAuターゲット素材を研削加工することによって、実施例1と同一形状のAuスパッタリングターゲットを作製した。これらAuスパッタリングターゲットのビッカース硬さ、平均結晶粒径、スパッタ面の優先配向面、および{110}面の配向指数Nを、実施例1と同様にして測定および評価した。それらの測定結果を表2に示す。このようなAuスパッタリングターゲットを後述する成膜工程に供して特性を評価した。なお、比較例1のAuスパッタリングターゲットでは、結晶粒界を明瞭に識別することができなかったため、平均結晶粒径を測定することはできなかった(表1中には「-」と表記)。
実施例1と同様にして作製したAuビレットに対して、実施例1と同様に表4に示す加工率を適用した鍛造加工を施してAuターゲット素材を作製した。次いで、鍛造後のAuターゲット素材に表4に示す条件で熱処理を施した。この後、熱処理後のAuターゲット素材を研削加工することによって、実施例1と同一形状のAuスパッタリングターゲットを作製した。
まず、Au塊を黒鉛るつぼに挿入して溶解した。Au溶湯を黒鉛鋳型に鋳造してAuインゴットを作製した。Auインゴットの表面を研削除去することによって、幅が200mm、長さが300mm、厚さが45mmのAuビレット(純度99.99%)を作製した。次いで、Auビレットを800℃の温度で熱間圧延し、幅が70mm、長さが200mm、厚さが45mmのAuターゲット素材とした。圧延時の加工率は厚さの減少率として80%とした。圧延後のAuターゲット素材を表7に示す条件で熱処理した。熱処理後のAuターゲット素材を研削加工して、直径が152.4mm、厚さが5mmの円板状のAuスパッタリングターゲットを作製した。
まず、Au塊を黒鉛るつぼに挿入して溶解した。Au溶湯を黒鉛鋳型に鋳造してAuインゴットを作製した。Auインゴットの表面を研削除去すると共に、内径50mmでくり抜き加工することによって、外径が100mm、内径が50mm、長さが200mmの円筒状Auビレット(純度99.99%)を作製した。次いで、円筒状Auビレットの中空部に芯材を挿入した状態で、800℃の温度に加熱して熱間鍛造し、外径が80mm、内径が50mm、長さが400mm以上のパイプ状Auターゲット素材とした。鍛造時の加工率は厚さの減少率として35%とした。鍛造後のパイプ状Auターゲット素材を500℃の温度で30分間熱処理した。熱処理後のAuターゲット素材を研削加工することによって、外径が70mm、内径が65mm、長さが350mmの円筒状のAuスパッタリングターゲットを作製した。
実施例22と同様にして作製したAuビレットに対して、実施例22と同様に表10に示す加工率を適用した鍛造加工を施してAuターゲット素材を作製した。次いで、鍛造後のAuターゲット素材に表10に示す条件で熱処理を施した。この後、熱処理後のAuターゲット素材を研削加工することによって、実施例22と同一形状のAuスパッタリングターゲットを作製した。これらAuスパッタリングターゲットのビッカース硬さ、および平均結晶粒径(ADtav)を、実施例22と同様にして測定した。さらに、Auスパッタリングターゲットのスパッタ面に優先配向している結晶面を実施例22と同様して評価すると共に、{110}面の配向指数Nを実施例22と同様して求めた。それらの結果を表11に示す。このような円筒状のAuスパッタリングターゲットを後述する成膜工程に供して特性を評価した。
実施例22と同様にして作製したAuビレットに対して、実施例22と同様に表13に示す加工率を適用した鍛造加工を施してAuターゲット素材を作製した。次いで、鍛造後のAuターゲット素材に表13に示す条件で熱処理を施した。この後、熱処理後のAuターゲット素材を研削加工することによって、実施例22と同一形状のAuスパッタリングターゲットを作製した。
Claims (15)
- 金および不可避不純物からなり、ビッカース硬さの平均値が40以上60以下であり、平均結晶粒径が15μm以上200μm以下であり、スパッタされる表面に金の{110}面が優先配向している金スパッタリングターゲットを製造する工程を具備する金スパッタリングターゲットの製造方法。
- 前記ビッカース硬さの平均値が45以上55以下であり、前記平均結晶粒径が30μm以上150μm以下である、請求項1に記載の金スパッタリングターゲットの製造方法。
- 前記金の{110}面の配向指数Nが1.3以上である、請求項3に記載の金スパッタリングターゲットの製造方法。
- 前記スパッタリングターゲット全体としての前記ビッカース硬さのばらつきが±20%以内である、請求項1ないし請求項4のいずれか1項に記載の金スパッタリングターゲットの製造方法。
- 前記スパッタリングターゲット全体としての前記平均結晶粒径のばらつきが±20%以内である、請求項1ないし請求項5のいずれか1項に記載の金スパッタリングターゲットの製造方法。
- 前記スパッタリングターゲットの金純度が99.99%以上99.999%未満である、請求項1ないし請求項6のいずれか1項に記載の金スパッタリングターゲットの製造方法。
- 前記金スパッタリングターゲットの製造工程は、
99.99%以上の金純度を有する金インゴットを用意する工程と、
前記金インゴットを加工して所望の板状または円筒状の金ビレットを形成する第1の加工工程と、
前記金ビレットを加圧下で板厚を減少させつつ加工して、所望のプレート状または円筒状のターゲット素材を形成する第2の加工工程と、
前記ターゲット素材を熱処理する熱処理工程と
を具備する、請求項1ないし請求項7のいずれか1項に記載の金スパッタリングターゲットの製造方法。 - 前記金スパッタリングターゲットの製造工程は、
99.99%以上の金純度を有する金インゴットを用意する工程と、
前記金インゴットを板状の金ビレットに加工する第1の加工工程と、
前記金ビレットに、加工率が50%以上90%以下となるように、200℃以上800℃以下の温度で熱間鍛造または熱間圧延、または冷間圧延を施して、プレート状のターゲット素材を得る第2の加工工程と、
前記ターゲット素材を200℃以上500℃以下の温度で10分以上120分以下保持することにより熱処理する熱処理工程と
を具備する、請求項1ないし請求項7のいずれか1項に記載の金スパッタリングターゲットの製造方法。 - 前記金スパッタリングターゲットの製造工程は、
99.99%以上の金純度を有する金インゴットを用意する工程と、
前記金インゴットを円筒状の金ビレットに加工する第1の加工工程と、
前記金ビレットに、冷間で押出比が1.5以上3.0以下の押出加工を施す、冷間で1回当たりの加工率が2%以上5%以下の引き抜き加工を複数回施す、または200℃以上800℃以下の温度で加工率が30%以上80%以下の熱間鍛造を施して、円筒状のターゲット素材を得る第2の加工工程と、
前記ターゲット素材を200℃以上500℃以下の温度で10分以上120分以下保持することにより熱処理する熱処理工程と
を具備する、請求項1ないし請求項7のいずれか1項に記載の金スパッタリングターゲットの製造方法。 - 金および不可避不純物からなり、ビッカース硬さの平均値が40以上60以下であり、平均結晶粒径が15μm以上200μm以下であり、スパッタされる表面に金の{110}面が優先配向している金スパッタリングターゲットを用意する工程と、
前記金スパッタリングターゲットをスパッタリングすることにより、被成膜基材上に金膜を成膜する工程と
を具備する金膜の製造方法。 - 前記金スパッタリングターゲットの前記ビッカース硬さの平均値が45以上55以下であり、前記平均結晶粒径が30μm以上150μm以下であり、前記金の{110}面の配向指数Nが1.3以上である、請求項12に記載の金膜の製造方法。
- 前記金スパッタリングターゲット全体としての前記ビッカース硬さのばらつきが±20%以内である、請求項11ないし請求項13のいずれか1項に記載の金膜の製造方法。
- 前記金スパッタリングターゲット全体としての前記平均結晶粒径のばらつきが±20%以内である、請求項11ないし請求項14のいずれか1項に記載の金膜の製造方法。
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JP2019558247A JP7214650B2 (ja) | 2017-12-06 | 2018-12-05 | 金スパッタリングターゲットの製造方法及び金膜の製造方法 |
RU2020122019A RU2784174C2 (ru) | 2017-12-06 | 2018-12-05 | Способ получения золотой пленки с использованием золотой распыляемой мишени |
EP18885294.1A EP3722454A4 (en) | 2017-12-06 | 2018-12-05 | GOLD SPRAY TARGET PRODUCTION PROCESS AND GOLD FILM PRODUCTION PROCESS |
CN201880078451.3A CN111433387A (zh) | 2017-12-06 | 2018-12-05 | 金溅射靶的制造方法和金膜的制造方法 |
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