TWI396759B - A method for producing a metal - based ceramic composite target containing noble metal - Google Patents

Description

Method for manufacturing metal-based ceramic composite target containing noble metal

The present invention relates to a method for producing a target, and more particularly to a method for producing a metal-based ceramic composite target containing a noble metal.

The hard disk is a modern main device for storing large amounts of data, and the data is mainly a magnetic film recording layer stored on a hard disk. The magnetic film recording layer is mainly composed of a cobalt (Pt) noble metal cobalt (Co) group. alloy. It is known that the magnetic film recording layer is coated on a hard disk by a sputtering process using a sputtering target.

In the prior art, a cobalt chromium-ruthenium dioxide (CoCrPt-SiO ₂ ) film is the main material of a magnetic recording film of a high-capacity hard disk. Among them, since the SiO ₂ ceramic is contained, the powder metallurgy process is required to prepare the CoCrPt-SiO ₂ target, that is, the Co powder, the Cr powder, the Pt powder and the SiO ₂ powder are mixed well, or the CoCrPt prealloy powder is selected. After the SiO ₂ powder is thoroughly mixed, the target is shaped and densified by a hot press process or a hot press process.

The conventional powder mixing method is divided into dry mixed powder and wet mixed powder. The main difference between the two is whether or not the powder is mixed in the solution, but the metal powder cannot be overcome regardless of the mixed powder method. The problem that the ceramic powders have a large difference in specific gravity and cannot be uniformly mixed.

In addition, in the wet mixing process, Co powder, Cr powder, Pt powder and SiO ₂ powder are mixed in a mixing sphere to form a mixed slurry. Therefore, after the wet mixing process is completed, when the mixed slurry is taken out from the mixing sphere, a part of the mixed slurry remains in the mixed sphere. Among them, since the content of Pt precious metal in the CoCrPt-SiO ₂ target is as high as 30% by weight (30 wt%) or more, the wet mixing process will cause a large amount of waste of Pt precious metal, thereby increasing the target. Manufacturing cost of materials.

Therefore, it is necessary to provide an innovative and progressive method for manufacturing a metal-based ceramic composite target containing precious metals to solve the above problems.

The present invention provides a method for producing a metal-based ceramic composite target containing a noble metal, the method comprising: (a) providing a magnetic metal powder and a ceramic powder, the purity of the powder being greater than 99.9%; (b) The ceramic powder and the magnetic metal powder are wet-mixed in a solvent to form a slurry, wherein the ceramic powder is coated on the surface of the magnetic metal powder; (c) drying the slurry to Forming a ceramic gold composite powder; (d) dry mixing the ceramic gold composite powder with the precious metal powder, the purity of the precious metal powder is greater than 99.9%; and (e) the ceramic after molding and densification mixing The gold composite powder and the noble metal powder form the metal-based ceramic composite target containing the noble metal.

In the manufacturing method of the present invention, the ceramic powder is uniformly coated on the surface of the magnetic metal powder by a wet mixing process, and after the drying process, the ceramic gold composite powder is obtained, and then the dry mixed powder is used. The process uniformly mixes the precious metal powder with the ceramic gold powder, and finally forms the ceramic gold composite powder into a dense target by a molding and densification process. The manufacturing method of the present invention can uniformly mix the magnetic metal powder, the ceramic powder and the precious metal powder, and can reduce waste of the precious metal powder in the target manufacturing process, thereby improving the quality of the target and reducing the target. Manufacturing cost of materials.

1 is a flow chart showing a method for producing a metal-based ceramic composite target containing noble metal according to the present invention; and FIG. 2 is a partially enlarged schematic view showing a metal-based ceramic composite target containing a noble metal according to the present invention. The method for manufacturing the metal-based ceramic composite target containing the noble metal can be applied to a film sputtering process in the magnetic recording industry, the photoelectric industry or the semiconductor industry. Referring to FIG. 1 and FIG. 2, first, referring to step S11, magnetic metal powder 11 and ceramic powder 12 are provided, and the purity of the powders 11, 12 is preferably greater than 99.9%. In the present embodiment, the purity of the magnetic metal powder 11 and the ceramic powder 12 is greater than 99.95%. The magnetic metal powder 11 may be cobalt or a cobalt chromium alloy.

In the present embodiment, the ceramic powder 12 is made of cerium oxide (SiO ₂ ) or titanium oxide (TiO ₂ ). The ceramic powder 12 preferably has a particle diameter of 0.07 to 1.0 μm.

Referring to step S12, the ceramic powder 12 and the magnetic metal powder 11 are wet-mixed in a solvent (for example, water or alcohol) to form a slurry, wherein the ceramic powder 12 is coated on the magnetic body. The surface of the metal powder 11. In step S12, the surface of the magnetic metal powder 11 and the surface of the ceramic powder 12 have different electrical charges, so that the ceramic powder 12 is coated on the surface of the magnetic metal powder 11 to enhance The uniformity of mixing. Preferably, the mixing time of the wet mixed powder is from 6 to 24 hours.

It is to be noted that, according to different mixed materials and mixing conditions, in step S12, a pH adjustment step may be further included, and an acid or alkali solution is added to adjust the pH of the slurry to make the magnetic metal powder. The surface of 11 and the surface of the ceramic powder 12 have different electrical charges.

Referring to step S13, the slurry is dried to form a ceramic gold composite powder. in In this embodiment, the slurry is dried by a vacuum drying method, wherein the vacuum drying temperature is 80 ° C to 160 ° C, the vacuum drying time is 2 to 6 hours, and the vacuum drying vacuum is less than 760 torr (torr). .

Referring to step S14, the pottery gold composite powder and the precious metal powder 13 are dry-mixed, and the purity of the precious metal powder 13 is greater than 99.9%. In the present embodiment, the noble metal powder 13 is made of platinum (Pt), and its purity is more than 99.95%, and the mixing time of the dry mixed powder is preferably 4 to 8 hours.

Referring to step S15, the ceramic gold composite powder and the precious metal powder 13 after molding and densification are mixed to form the metal-based ceramic composite target 1 containing the noble metal of the present invention. In this embodiment, the forming and densification steps are performed by a hot pressing process or a hot isostatic pressing process, wherein the molding and densification temperature is 800 ° C to 1200 ° C, and molding is performed. And the densification time is 1 to 4 hours.

Preferably, the weight percentage of the ceramic powder 12 is 5% to 12%, and the weight percentage of the precious metal powder 13 is 20% to 50%, and the remaining weight percentage is the content of the magnetic metal powder 11. In this embodiment, the magnetic metal powder 11 is a cobalt chromium alloy, wherein the ceramic powder 12 is 5% to 12% by weight, and the precious metal powder 13 is 20% to 50% by weight. The weight percentage of chromium in the cobalt-chromium alloy is 4% to 16%, and the remaining weight percentage is the weight percentage of cobalt of the cobalt-chromium alloy.

The invention is illustrated by the following examples, which are not intended to be limited to the scope of the invention.

Example 1:

This example is exemplified by the production of a cobalt-chromium-platinum-niobium oxide (CoCrPt-SiO ₂ ) alloy sputtering target. First, a cobalt (Co) powder having a purity of up to 99.95% or more and a chromium (Cr) powder, a platinum (Pt) powder, and a cerium oxide (SiO ₂ ) powder having a purity of 99.95% or more are provided. 0.25 μm). Among them, the content of cobalt was 46% by weight (46 wt%), the content of chromium was 5 wt%, the content of platinum was 42 wt%, and the content of cerium oxide was 7 wt%. Next, the Co powder, the Cr powder, and the SiO ₂ powder were placed in a water having a pH of 7 and subjected to wet mixing for 18 hours. Next, the CoCr-SiO ₂ slurry is placed in a vacuum oven, and a vacuum drying step is performed in a vacuum degree of 76 torr, wherein the drying temperature is 120 ° C, and the drying time is 4 hours, and the SiO ₂ powder can be obtained. It is evenly coated on the surface of the Co powder and the Cr powder. Finally, the dried CoCr-SiO ₂ powder is mixed with the Pt powder in a dry mixed manner without solvent, and then the uniformly mixed powder is placed in a graphite mold by hot pressing. The CoCrPt-SiO ₂ target having high purity, fine structure and uniform composition was prepared by pressing the mixed powder into a target shape and densifying the target at 1100 ° C for 1.5 hours.

Example 2:

This example is exemplified by the production of a cobalt-chromium-platinum-titanium dioxide (CoCrPt-TiO ₂ ) alloy sputtering target. First, it provides magnetic cobalt (Co) powder with a purity of up to 99.95% or more, and chromium (Cr) powder, platinum (Pt) powder, and titanium dioxide (TiO ₂ ) powder with a purity of up to 99.95% or more (particle size 0.07 μm). ). Among them, the content of cobalt was 48 wt%, the content of chromium was 13 wt%, the content of platinum was 31 wt%, and the content of titanium dioxide was 8 wt%. Next, the Co powder, the Cr powder, and the TiO ₂ powder were placed in deionized water, and the pH of the solution was adjusted to 8 with aqueous ammonia, followed by wet mixing for 12 hours. Next, the CoCr-TiO ₂ slurry is placed in a vacuum oven, and a vacuum drying step is performed in a vacuum degree of 76 torr, wherein the drying temperature is 160 ° C and the drying time is 2 hours, and the TiO ₂ powder can be obtained. It is evenly coated on the surface of the Co powder and the Cr powder. Finally, the dried CoCr-TiO ₂ powder was taken and thoroughly mixed with the Pt powder in a dry mixed manner without solvent, and then the uniformly mixed powder was canned with stainless steel, followed by heat. Under the condition of 800 ° C and holding temperature for 4 hours, the powder is pressed into the shape of the target and the target is densified, then the CoCrPt-TiO ₂ target with high purity, fine structure and uniform composition can be obtained.

In the manufacturing method of the present invention, the ceramic powder is uniformly coated on the surface of the magnetic metal powder by a wet mixing process, and after the drying process, the ceramic gold composite powder is obtained, and then the dry mixed powder is used. The process uniformly mixes the precious metal powder with the ceramic gold powder, and finally forms the ceramic gold composite powder into a dense target by a molding and densification process. The manufacturing method of the present invention can uniformly mix the magnetic metal powder, the ceramic powder and the precious metal powder, and can reduce waste of the precious metal powder in the target manufacturing process, thereby improving the quality of the target and reducing the target. Manufacturing cost of materials.

The above embodiments are merely illustrative of the principles and effects of the invention and are not intended to limit the invention. Therefore, those skilled in the art can make modifications and changes to the above embodiments without departing from the spirit of the invention. The scope of the invention should be as set forth in the appended claims.

1‧‧‧Metal-based ceramic composite target containing noble metal of the present invention

11‧‧‧Magnetic metal powder

12‧‧‧Ceramic powder

13‧‧‧ precious metal powder

1 is a flow chart showing a method of manufacturing a metal-based ceramic composite target containing noble metal according to the present invention; and FIG. 2 is a view showing a part of a metal-based ceramic composite target containing noble metal of the present invention. Zoom in on the schematic.

Claims (20)

A method for manufacturing a metal-based ceramic composite target containing a noble metal-containing noble metal, comprising the steps of: (a) providing a magnetic metal powder and a ceramic powder, the purity of the powder being greater than 99.9%; (b) the ceramic The powder and the magnetic metal powder are wet-mixed in a solvent to form a slurry, wherein the ceramic powder is coated on the surface of the magnetic metal powder; (c) drying the slurry to form a ceramic a gold composite powder; (d) dry mixing the ceramic gold powder with the precious metal powder, the purity of the noble metal powder being greater than 99.9%; and (e) the ceramic gold composite after molding and densification mixing The powder and the precious metal powder form the metal-based ceramic composite target containing the noble metal. The manufacturing method of claim 1, wherein in the steps (a) and (d), the magnetic metal powder, the ceramic powder and the precious metal powder have a purity of more than 99.95%. The manufacturing method of claim 1, wherein in the step (a), the weight percentage of the ceramic powder is 5% to 12%, and the weight percentage of the precious metal powder is 20% to 50%, and the remaining weight percentage is It is the content of the magnetic metal powder. The manufacturing method of claim 3, wherein in the step (a), the magnetic metal powder system is cobalt or a cobalt alloy. The manufacturing method of claim 4, wherein in the step (a), the cobalt alloy is a cobalt chromium alloy. The manufacturing method of claim 5, wherein in the step (a), the chromium chromium alloy has a chromium percentage of 4% to 16%. The manufacturing method of claim 1, wherein in the step (a), the ceramic powder system is cerium oxide (SiO ₂ ) or titanium oxide (TiO ₂ ). The manufacturing method of claim 1, wherein in the step (a), the ceramic powder has a particle diameter of 0.07 to 1.0 μm. The manufacturing method of claim 1, wherein in the step (a), the precious metal powder system is platinum (Pt). The production method of claim 1, wherein water or alcohol is used as the solvent in the step (b). The manufacturing method of claim 1, wherein in the step (b), the surface of the magnetic metal powder and the surface of the ceramic powder have different electrical charges, so that the ceramic powder is coated on the magnetic metal powder. The surface of the body. The manufacturing method of claim 1, wherein in step (b), a pH adjusting step is further included, and an acid or alkali solution is added to adjust the pH of the slurry. The manufacturing method of claim 1, wherein in the step (b), the mixing time of the wet mixed powder is 6 to 24 hours. The manufacturing method of claim 1, wherein the slurry is dried in a vacuum drying method in the step (c). The manufacturing method of claim 14, wherein in the step (c), the vacuum drying temperature is from 80 ° C to 160 ° C, and the vacuum drying time is from 2 to 6 hours. The manufacturing method of claim 15, wherein in the step (c), the degree of vacuum of the vacuum drying is less than 760 torr. The manufacturing method of claim 1, wherein in the step (d), the dry mixing powder The mixing time is 4 to 8 hours. The manufacturing method of claim 1, wherein the forming and densifying steps are carried out in the step (e) by a hot press or a hot press. The method of claim 18, wherein in the step (e), the molding and densification temperature is from 800 ° C to 1200 ° C, and the molding and densification time is from 1 to 4 hours. The manufacturing method of claim 1, wherein the method for producing the metal-based ceramic composite target containing the noble metal is applied to a film sputtering process in the magnetic recording industry, the photovoltaic industry, or the semiconductor industry.