CN107805789A - Preparation method of ruthenium sputtering target material - Google Patents
Preparation method of ruthenium sputtering target material Download PDFInfo
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- CN107805789A CN107805789A CN201711238266.XA CN201711238266A CN107805789A CN 107805789 A CN107805789 A CN 107805789A CN 201711238266 A CN201711238266 A CN 201711238266A CN 107805789 A CN107805789 A CN 107805789A
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- ruthenium
- sputtering target
- temperature
- target material
- preparation
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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
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 method of ruthenium sputtering target material.
Background technology
Sputtering is to prepare one of major technique of thin-film material, and it utilizes ion caused by ion gun, 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 handed over
Change, the atom of the surface of solids is left solid and be 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, prepared by pressure sintering
Ruthenium target has the advantages that easy-formation, cycle are 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 ruthenium target of the relative density more than 98% with ruthenium powder hot pressing.Target density is bigger, is more advantageous to sputter coating, therefore
The sputtered film of high quality is obtained, the density of sputtering target material is typically the bigger the better.
The content of the invention
In view of this, it is an object of the invention to provide ruthenium prepared by a kind of preparation method of ruthenium sputtering target material, this method
The density of sputtering target material is higher.
The invention provides a kind of preparation method of sputtering target material, comprise the following steps：
By the ruthenium powder cold moudling of the mesh of granularity≤325, 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 being incubated 30~50min, then the first temperature is warming up to 5~10 DEG C/min and pressurizeed, moulding pressure is 50~70MPa；Continue to rise
Temperature is incubated 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 incubated, obtains ruthenium sputtering target material.
Preferably, the press time of the cold moudling is 15~20min.
Preferably, the ruthenium base is placed in vacuum hotpressing mould, is placed into vacuum hotpressing stove and is vacuumized.
Preferably, it is described to be evacuated to 0.01Pa.
Preferably, 800 DEG C are warming up to 10~20 DEG C/min.
Preferably, after being incubated 55~65min, pressure is laid down, is cooled with vacuum hotpressing stove, after being cooled to 10~40 DEG C, taken off
Mould, obtain ruthenium sputtering target material.
The invention provides a kind of preparation method of ruthenium sputtering target material, comprise the following steps：By the ruthenium powder of the mesh of granularity≤325
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 being incubated 30~50min, then the first temperature are warming up to 5~10 DEG C/min
Pressurization, moulding pressure is 50~70MPa；Second temperature is continuously heating to, is incubated 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, insulation 55~
65min, obtain ruthenium sputtering target material.The invention obtained ruthenium sputtering target material under above-mentioned technique has higher density.Experiment knot
Fruit shows：Ruthenium sputtering target material relative density is more than 99.5%.
Embodiment
The invention provides a kind of preparation method of ruthenium sputtering target material, comprise the following steps：
By the ruthenium powder cold moudling of the mesh of granularity≤325, 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 being incubated 30~50min, then the first temperature is warming up to 5~10 DEG C/min and pressurizeed, moulding pressure is 50~70MPa；Continue to rise
Temperature is incubated 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 incubated, obtains ruthenium sputtering target material.
The invention obtained ruthenium sputtering target material under above-mentioned technique has higher density.Test result indicates that：Ruthenium sputters
Target relative density is more than 99.5%.
For the present invention by the ruthenium powder cold moudling of the mesh of granularity≤325, cold pressing pressure is 250~350MPa, obtains ruthenium base.This hair
It is bright that ruthenium powder raw material was preferably crossed into 325 eye mesh screens, minus sieve is taken as hot pressing powder.The press time of the cold moudling is preferred
For 15~20min.
The ruthenium base is preferably placed in vacuum hotpressing mould 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 preferably to 800 DEG C with 10~20 DEG C/min.
The present invention lays down pressure, cooled with vacuum hotpressing stove, be cooled to 10~40 DEG C preferably after 55~65min is incubated
Afterwards, it is stripped, obtains ruthenium sputtering target material.
In order to further illustrate the present invention, 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 can not be interpreted as into limiting the scope of the present invention.
Embodiment 1
1. powder screens：The ruthenium powder that market is bought, 325 eye mesh screens are crossed, take minus sieve as hot pressing powder.
2. cold moudling：Hot pressing powder is fitted into alloy mold, pressure 350MPa compressing using hydraulic press,
Press time is 15min；Pressure release is stripped to obtain ruthenium base.
3. vacuum hotpressing：Ruthenium base is fitted into vacuum hotpressing mould, is put into vacuum hotpressing stove, is evacuated to 10-2Pa, opens
Heating is opened, with 15 DEG C/min, 800 DEG C is warming up to, is incubated 50min；Then with 8 DEG C/min, 1200 DEG C DEG C are warming up to, insulation
120min.Wherein when temperature is raised to 1100 DEG C, start to pressurize, moulding pressure 70MPa.
4. cooling：1000 DEG C are cooled to 8 DEG C/min, 60min is incubated, then lays down pressure, cool with stove.
5. after temperature drops to room temperature, blow-on door, after the demoulding, processing obtains ruthenium sputtering target material.
Using the density of ruthenium sputtering target material made from drainage testing example 1, test result is：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, 325 eye mesh screens are crossed, take minus sieve as hot pressing powder.
2. cold moudling：Hot pressing powder is fitted into alloy mold, pressure 250MPa compressing using hydraulic press,
Press time is 20min；Pressure release is stripped to obtain ruthenium base.
3. vacuum hotpressing：Ruthenium base is fitted into vacuum hotpressing mould, is put into vacuum hotpressing stove, is evacuated to 10-2Pa, opens
Heating is opened, with 20 DEG C/min, 800 DEG C is warming up to, is incubated 30min；Then with 10 DEG C/min, 1350 DEG C are warming up to, insulation
180min.Wherein when temperature is raised to 1200 DEG C, start to pressurize, moulding pressure 50MPa.
4. cooling：1050 DEG C are cooled to 5 DEG C/min, 60min is incubated, then lays down pressure, cool with stove.
5. after temperature drops to room temperature, blow-on door, after the demoulding, processing obtains ruthenium sputtering target material.
Using the density of ruthenium sputtering target material made from drainage testing example 2, test result is：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, 325 eye mesh screens are crossed, take minus sieve as hot pressing powder.
2. cold moudling：Hot pressing powder is fitted into alloy mold, pressure 300MPa compressing using hydraulic press,
Press time is 18min；Pressure release is stripped to obtain ruthenium base.
3. vacuum hotpressing：Ruthenium base is fitted into vacuum hotpressing mould, is put into vacuum hotpressing stove, is evacuated to 10-2Pa, opens
Heating is opened, with 15 DEG C/min, 800 DEG C is warming up to, is incubated 40min；Then with 5 DEG C/min, 1300 DEG C are warming up to, insulation
160min.Wherein when temperature is raised to 1150 DEG C, start to pressurize, moulding pressure 60MPa.
4. cooling：1000 DEG C are cooled to 6 DEG C/min, 60min is incubated, then lays down pressure, cool with stove.
5. after temperature drops to room temperature, blow-on door, after the demoulding, processing obtains ruthenium sputtering target material.
Using the density of ruthenium sputtering target material made from drainage testing example 3, test result is：Prepared by embodiment 3
The relative density of ruthenium sputtering target material is 99.51%.
As seen from the above embodiment, the invention provides a kind of preparation method of ruthenium sputtering target material, comprise the following steps：Will
The ruthenium powder cold moudling of the mesh of granularity≤325, cold pressing pressure is 250~350MPa, obtains 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 being incubated 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；Second temperature is continuously heating to, is incubated 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 incubated, obtains ruthenium sputtering target material.The invention under above-mentioned technique obtained ruthenium sputtering target material have compared with
High density.Test result indicates that：Ruthenium sputtering target material relative density is more than 99.5%.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (6)
1. a kind of preparation method of ruthenium sputtering target material, comprises the following steps：
By the ruthenium powder cold moudling of the mesh of granularity≤325, 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, insulation
After 30~50min, then the first temperature is warming up to 5~10 DEG C/min and pressurizeed, moulding pressure is 50~70MPa；It is continuously heating to
Second temperature, it is incubated 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, 55~65min is incubated, obtains ruthenium sputtering target material.
2. preparation method according to claim 1, it is characterised in that the press time of the cold moudling be 15~
20min。
3. preparation method according to claim 1, it is characterised in that the ruthenium base is placed in vacuum hotpressing mould, then is put
Enter in vacuum hotpressing stove and vacuumized.
4. preparation method according to claim 1, it is characterised in that described to be evacuated to 0.01Pa.
5. preparation method according to claim 1, it is characterised in that be warming up to 800 DEG C with 10~20 DEG C/min.
6. preparation method according to claim 3, it is characterised in that after 55~65min of insulation, pressure is laid down, with vacuum
Hot pressing furnace cools, and after being cooled to 10~40 DEG C, the demoulding, obtains ruthenium sputtering target material.
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| Application Number | Priority Date | Filing Date | Title |
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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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| CN107805789A true CN107805789A (en) | 2018-03-16 |
| CN107805789B CN107805789B (en) | 2019-09-03 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111270210A (en) * | 2020-03-17 | 2020-06-12 | 贵研铂业股份有限公司 | Ruthenium sputtering target with high oriented crystal grains and preparation method thereof |
Citations (5)
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|---|---|---|---|---|
| US20090114535A1 (en) * | 2005-06-16 | 2009-05-07 | Nippon Mining & Metals Co., Ltd. | Ruthenium-Alloy Sputtering Target |
| 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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2017
- 2017-11-30 CN CN201711238266.XA patent/CN107805789B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090114535A1 (en) * | 2005-06-16 | 2009-05-07 | Nippon Mining & Metals Co., Ltd. | Ruthenium-Alloy Sputtering Target |
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111270210A (en) * | 2020-03-17 | 2020-06-12 | 贵研铂业股份有限公司 | Ruthenium sputtering target with high oriented crystal grains and preparation method thereof |
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