CN107805789B - Preparation method of ruthenium sputtering target material - Google Patents
Preparation method of ruthenium sputtering target material Download PDFInfo
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- CN107805789B CN107805789B CN201711238266.XA CN201711238266A CN107805789B CN 107805789 B CN107805789 B CN 107805789B CN 201711238266 A CN201711238266 A CN 201711238266A CN 107805789 B CN107805789 B CN 107805789B
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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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Abstract
The invention provides a preparation method of a ruthenium sputtering target, which comprises the following steps: carrying out cold pressing molding on the ruthenium powder with the granularity of less than or equal to 325 meshes, wherein the cold pressing pressure is 250-350 MPa, so as to obtain a ruthenium blank; vacuumizing the ruthenium blank to 0.008-0.12 Pa, heating to 790-820 ℃ at a speed of 10-20 ℃/min, preserving heat for 30-50 min, heating to a first temperature at a speed of 5-10 ℃/min, and pressurizing at a pressure of 50-70 MPa; continuously heating to a second temperature, and keeping the temperature for 120-180 min; the first temperature is 1000-1200 ℃, and the second temperature is 1200-1350 ℃; and finally, cooling to 1000-1100 ℃ at a speed of 5-8 ℃/min, preserving the temperature for 55-65 min, and removing the pressure to obtain the ruthenium sputtering target. The ruthenium sputtering target prepared by the process has higher density. The relative density is more than 99.5%.
Description
Technical field
The present invention relates to ruthenium target technology field more particularly to a kind of preparation methods of ruthenium sputtering target material.
Background technique
Sputtering is to prepare one of major technique of thin-film material, and the ion that it utilizes ion source to generate passes through in a vacuum
Accelerate aggregation, and form the ion beam current of energy at high speed, bombard the surface of solids, ion and surface of solids atom occur kinetic energy and hand over
It changes, the atom of the surface of solids is made to leave solid and is deposited on substrate surface, the solid bombarded is to prepare sputtering method deposition film
Raw material, referred to as sputtering target material.Ruthenium sputtering target material is material important in perpendicular magnetic recording multi-layer film structure, pressure sintering preparation
Ruthenium target has many advantages, such as that easily molded, the period is short and equipment is simple, therefore is usually used in preparing ruthenium sputtering target material.
Patent " a kind of preparation method of ruthenium metal sputtering target ", application number: 201010581909.2, using pressure sintering,
Directly go out the ruthenium target that relative density is greater than 98% with ruthenium powder hot pressing.Target density is bigger, is more conducive to sputter coating, therefore
The sputtered film of high quality is obtained, the density of sputtering target material is generally the bigger the better.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of preparation method of ruthenium sputtering target material, the ruthenium of this method preparation
The density of sputtering target material is higher.
The present invention provides a kind of preparation methods of sputtering target material, comprising the following steps:
By the ruthenium powder cold moudling of granularity≤325 mesh, cold pressing pressure is 250~350MPa, obtains ruthenium base；
The ruthenium base be evacuated to after 0.008~0.12Pa and is warming up to 790~820 DEG C with 10~20 DEG C/min,
After keeping the temperature 30~50min, then the first temperature is warming up to 5~10 DEG C/min and is pressurizeed, moulding pressure is 50~70MPa；After of continuing rising
Temperature keeps the temperature 120~180min to second temperature；First temperature is 1000~1200 DEG C, and second temperature is 1200~1350 DEG C；
1000~1100 DEG C finally are cooled to 5~8 DEG C/min, 55~65min is kept the temperature, obtains ruthenium sputtering target material.
Preferably, the pressing time of the cold moudling is 15~20min.
Preferably, the ruthenium base is placed in vacuum hotpressing mold, is placed into vacuum hotpressing stove and is vacuumized.
Preferably, described to be evacuated to 0.01Pa.
Preferably, 800 DEG C are warming up to 10~20 DEG C/min.
Preferably, after keeping the temperature 55~65min, pressure is laid down, is cooled down with vacuum hotpressing stove, after being cooled to 10~40 DEG C, taken off
Mould obtains ruthenium sputtering target material.
The present invention provides a kind of preparation methods of ruthenium sputtering target material, comprising the following steps: by granularity≤325 mesh ruthenium powder
Cold moudling, cold pressing pressure are 250~350MPa, obtain ruthenium base；The ruthenium base is carried out after being evacuated to 0.008~0.12Pa
790~820 DEG C are warming up to 10~20 DEG C/min, after keeping the temperature 30~50min, then the first temperature are warming up to 5~10 DEG C/min
Pressurization, moulding pressure are 50~70MPa；It is continuously heating to second temperature, keeps the temperature 120~180min；First temperature be 1000~
1200 DEG C, second temperature is 1200~1350 DEG C；Finally 1000~1100 DEG C are cooled to 5~8 DEG C/min, heat preservation 55~
65min obtains ruthenium sputtering target material.Invention ruthenium sputtering target material density with higher obtained under above-mentioned technique.Experiment knot
Fruit shows: ruthenium sputtering target material relative density is greater than 99.5%.
Specific embodiment
The present invention provides a kind of preparation methods of ruthenium sputtering target material, comprising the following steps:
By the ruthenium powder cold moudling of granularity≤325 mesh, cold pressing pressure is 250~350MPa, obtains ruthenium base；
The ruthenium base be evacuated to after 0.008~0.12Pa and is warming up to 790~820 DEG C with 10~20 DEG C/min,
After keeping the temperature 30~50min, then the first temperature is warming up to 5~10 DEG C/min and is pressurizeed, moulding pressure is 50~70MPa；After of continuing rising
Temperature keeps the temperature 120~180min to second temperature；First temperature is 1000~1200 DEG C, and second temperature is 1200~1350 DEG C；
1000~1100 DEG C finally are cooled to 5~8 DEG C/min, 55~65min is kept the temperature, obtains ruthenium sputtering target material.
Invention ruthenium sputtering target material density with higher obtained under above-mentioned technique.The results showed that ruthenium sputters
Target relative density is greater than 99.5%.
The ruthenium powder cold moudling of granularity≤325 mesh, cold pressing pressure are 250~350MPa by the present invention, obtain ruthenium base.This hair
It is bright that ruthenium powder raw material was preferably crossed into 325 mesh screens, take minus sieve as hot pressing powder.The pressing time of the cold moudling is preferred
For 15~20min.
The ruthenium base is preferably placed in vacuum hotpressing mold by the present invention, is placed into vacuum hotpressing stove and is vacuumized.
It is described to vacuumize preferably to 0.01Pa.
The present invention is heated up with 10~20 DEG C/min preferably to 800 DEG C.
The present invention preferably after keeping the temperature 55~65min, lays down pressure, cools down with vacuum hotpressing stove, is cooled to 10~40 DEG C
Afterwards, it demoulds, obtains ruthenium sputtering target material.
In order to further illustrate the present invention, below with reference to embodiment to a kind of preparation of ruthenium sputtering target material provided by the invention
Method is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
1. powder screens: the ruthenium powder that market is bought crosses 325 mesh screens, takes minus sieve as hot pressing powder.
2. cold moudling: hot pressing powder is fitted into alloy mold, using hydraulic press compression moulding, pressure 350MPa,
Pressing time is 15min；Pressure release demoulds to obtain ruthenium base.
3. vacuum hotpressing: ruthenium base is fitted into vacuum hotpressing mold, is put into vacuum hotpressing stove, and 10-2Pa is evacuated to, and is opened
Heating is opened, with 15 DEG C/min, 800 DEG C is warming up to, keeps the temperature 50min；Then with 8 DEG C/min, 1200 DEG C DEG C are warming up to, heat preservation
120min.Wherein when temperature is raised to 1100 DEG C, start to pressurize, moulding pressure 70MPa.
4. cooling: being cooled to 1000 DEG C with 8 DEG C/min, keep the temperature 60min, then lay down pressure, cool down with furnace.
5. blow-on door, after demoulding, processing obtains ruthenium sputtering target material after temperature drops to room temperature.
Using the density of ruthenium sputtering target material made from drainage testing example 1, test result are as follows: prepared by embodiment 1
The relative density of ruthenium sputtering target material is 99.51%.
Embodiment 2
1. powder screens: the ruthenium powder that market is bought crosses 325 mesh screens, takes minus sieve as hot pressing powder.
2. cold moudling: hot pressing powder is fitted into alloy mold, using hydraulic press compression moulding, pressure 250MPa,
Pressing time is 20min；Pressure release demoulds to obtain ruthenium base.
3. vacuum hotpressing: ruthenium base is fitted into vacuum hotpressing mold, is put into vacuum hotpressing stove, and 10-2Pa is evacuated to, and is opened
Heating is opened, with 20 DEG C/min, 800 DEG C is warming up to, keeps the temperature 30min；Then with 10 DEG C/min, 1350 DEG C are warming up to, heat preservation
180min.Wherein when temperature is raised to 1200 DEG C, start to pressurize, moulding pressure 50MPa.
4. cooling: being cooled to 1050 DEG C with 5 DEG C/min, keep the temperature 60min, then lay down pressure, cool down with furnace.
5. blow-on door, after demoulding, processing obtains ruthenium sputtering target material after temperature drops to room temperature.
Using the density of ruthenium sputtering target material made from drainage testing example 2, test result are as follows: prepared by embodiment 2
The relative density of ruthenium sputtering target material is 99.52%.
Embodiment 3
1. powder screens: the ruthenium powder that market is bought crosses 325 mesh screens, takes minus sieve as hot pressing powder.
2. cold moudling: hot pressing powder is fitted into alloy mold, using hydraulic press compression moulding, pressure 300MPa,
Pressing time is 18min；Pressure release demoulds to obtain ruthenium base.
3. vacuum hotpressing: ruthenium base is fitted into vacuum hotpressing mold, is put into vacuum hotpressing stove, and 10-2Pa is evacuated to, and is opened
Heating is opened, with 15 DEG C/min, 800 DEG C is warming up to, keeps the temperature 40min；Then with 5 DEG C/min, 1300 DEG C are warming up to, heat preservation
160min.Wherein when temperature is raised to 1150 DEG C, start to pressurize, moulding pressure 60MPa.
4. cooling: being cooled to 1000 DEG C with 6 DEG C/min, keep the temperature 60min, then lay down pressure, cool down with furnace.
5. blow-on door, after demoulding, processing obtains ruthenium sputtering target material after temperature drops to room temperature.
Using the density of ruthenium sputtering target material made from drainage testing example 3, test result are as follows: prepared by embodiment 3
The relative density of ruthenium sputtering target material is 99.51%.
As seen from the above embodiment, the present invention provides a kind of preparation methods of ruthenium sputtering target material, comprising the following steps: will
The ruthenium powder cold moudling of granularity≤325 mesh, cold pressing pressure are 250~350MPa, obtain ruthenium base；The ruthenium base is vacuumized
Be warming up to 790~820 DEG C after to 0.008~0.12Pa with 10~20 DEG C/min, after keeping the temperature 30~50min, then with 5~10 DEG C/
Min is warming up to the pressurization of the first temperature, and moulding pressure is 50~70MPa；It is continuously heating to second temperature, keeps the temperature 120~180min；
First temperature is 1000~1200 DEG C, and second temperature is 1200~1350 DEG C；Finally 1000 are cooled to 5~8 DEG C/min~
1100 DEG C, 55~65min is kept the temperature, ruthenium sputtering target material is obtained.Invention ruthenium sputtering target material obtained under above-mentioned technique have compared with
High density.The results showed that ruthenium sputtering target material relative density is greater than 99.5%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (4)
1. a kind of preparation method of ruthenium sputtering target material, comprising the following steps:
By the ruthenium powder cold moudling of granularity≤325 mesh, cold pressing pressure is 250~350MPa, obtains ruthenium base；The cold moudling
Pressing time is 15~20min；
The ruthenium base be evacuated to after 0.008~0.12Pa and is warming up to 790~820 DEG C with 10~20 DEG C/min, heat preservation
After 30~50min, then the first temperature is warming up to 5~10 DEG C/min and is pressurizeed, moulding pressure is 50~70MPa；It is continuously heating to
Second temperature keeps the temperature 120~180min；First temperature is 1000~1200 DEG C, and second temperature is 1200~1350 DEG C；
1000~1100 DEG C finally are cooled to 5~8 DEG C/min, after keeping the temperature 55~65min, pressure is laid down, with vacuum hotpressing stove
Cooling, after being cooled to 10~40 DEG C, demoulding obtains ruthenium sputtering target material.
2. preparation method according to claim 1, which is characterized in that the ruthenium base is placed in vacuum hotpressing mold, then is put
Enter in vacuum hotpressing stove and is vacuumized.
3. preparation method according to claim 1, which is characterized in that described to be evacuated to 0.01Pa.
4. preparation method according to claim 1, which is characterized in that be warming up to 800 DEG C with 10~20 DEG C/min.
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| CN201711238266.XA CN107805789B (en) | 2017-11-30 | 2017-11-30 | Preparation method of ruthenium sputtering target material |
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| CN201711238266.XA CN107805789B (en) | 2017-11-30 | 2017-11-30 | Preparation method of ruthenium sputtering target material |
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| CN107805789B true CN107805789B (en) | 2019-09-03 |
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| CN111270210B (en) * | 2020-03-17 | 2021-11-12 | 贵研铂业股份有限公司 | Ruthenium sputtering target with high oriented crystal grains and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102485378A (en) * | 2010-12-06 | 2012-06-06 | 北京有色金属研究总院 | Preparation method of ruthenium metal sputtering target material |
| CN102605332A (en) * | 2012-03-25 | 2012-07-25 | 昆明贵金属研究所 | Ru sputtering target with high purity and preparation method thereof |
| CN104032270A (en) * | 2014-06-12 | 2014-09-10 | 贵研铂业股份有限公司 | Large-sized ruthenium-based alloy sputtering target and preparation method thereof |
| CN105441881A (en) * | 2014-08-29 | 2016-03-30 | 宁波江丰电子材料股份有限公司 | Making method of chromium target and making method of combination of chromium target |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006134743A1 (en) * | 2005-06-16 | 2006-12-21 | Nippon Mining & Metals Co., Ltd. | Ruthenium-alloy sputtering target |
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- 2017-11-30 CN CN201711238266.XA patent/CN107805789B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102485378A (en) * | 2010-12-06 | 2012-06-06 | 北京有色金属研究总院 | Preparation method of ruthenium metal sputtering target material |
| CN102605332A (en) * | 2012-03-25 | 2012-07-25 | 昆明贵金属研究所 | Ru sputtering target with high purity and preparation method thereof |
| CN104032270A (en) * | 2014-06-12 | 2014-09-10 | 贵研铂业股份有限公司 | Large-sized ruthenium-based alloy sputtering target and preparation method thereof |
| CN105441881A (en) * | 2014-08-29 | 2016-03-30 | 宁波江丰电子材料股份有限公司 | Making method of chromium target and making method of combination of chromium target |
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