CN102605332A - Ru sputtering target with high purity and preparation method thereof - Google Patents
Ru sputtering target with high purity and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an Ru sputtering target with a high purity and a preparation method of the target. The density of the Ru sputtering target is higher than 99%, and the average crystal grain size is 2-10 microns. The specific preparation method comprises the following steps: (1) pretreating powder; (2) filling the powder; and (3) sintering the powder: sending a mold filled with the high-purity Ru powder into a vacuum hot-pressing sintering furnace and performing bidirectional vacuum hot pressing and sintering, wherein the vacuum degree is 10<-2>Pa to 10<-4>Pa, the sintering temperature is 1100-1800 DEG C, and the sintering pressure is 30-60MPa. According to the invention, the Ru sputtering target is prepared by the bidirectional vacuum hot-pressing and sintering technology, the density is higher than 99%, the average crystal grain size is 2-10 microns, and the boundary and the core microstructure are uniform. The target used for magnetron sputtering can reduce paradoxical discharge in the sputtering process and can improve the sputtering speed rate and the uniformity of distribution of the film thickness. Meanwhile, by adopting the bidirectional pressing method, multiple pieces in one furnace can be synchronously pressed, and the related performance such as structural uniformity of the pressed target is equal to the performance of hot isostatic pressing, so that the production efficiency is improved, the production cost is saved and the power consumption is reduced.
Description
Technical field
The invention belongs to powder metallurgical technology, be specifically related to a kind of high-purity Ru sputtering target and preparation method thereof.
Background technology
Ru and Ru base alloy material have widely in the manufacturing of a lot of electronic products to be used; For example as the intermediate layer in the high-density perpendicular magnetic recording media, the coupling layer in high-performance, the high area recording density antiferromagnetic coupling magnetic recording media and as the bonding coat/Seed Layer in the copper base back-end metallation system of high density of integration semiconductor integrated circuit apparatus.These thin film layers are raw material with Ru or Ru base alloy target material generally, form through sputter-deposition technology such as magnetron sputtering.Generally speaking; All requires during these are used the sputtering target that adopts have less foreign matter content, morphological element even, have a high density; And tiny crystal grain, thereby phenomenons such as particle disengaging, membrane thickness unevenness and film composition be inhomogeneous can not appear in sputter procedure.
At present, the method for preparing high-purity Ru target mainly contains smelting process, powder metallurgic method etc.Smelting process can well be controlled the purity of target, but homogeneity of structure is relatively poor, and the target crystal grain that smelting method for preparing goes out is thick, and simultaneously, because the processibility of Ru target is relatively poor under the room temperature condition, the follow-up machining of the target that smelting method for preparing goes out difficulty is carried out; Powder metallurgic method is suitable for preparing homogeneous microstructure and the tiny target of crystal grain, therefore becomes the main preparation methods of present preparation high-purity Ru target, and sintering method commonly used has hot isostatic pressing, energising sintering process, vacuum hot-pressing.But powder metallurgic method is brought impurity element into easily (like O; N); And the large-size target of powder metallurgic method preparation, because dress powder lack of homogeneity, planeness and the parallelism of preparing target are relatively poor; Follow-up machining loss is bigger; The density of heart portion and edge differs bigger simultaneously, and edge's crystal grain is thicker, and therefore how controlling impurity content, reducing difference, the refining grain size of target heart portion and edge's density and keep the consistence of target heart portion and edge's weave construction is the key technical problem that powder metallurgic method prepares large-size target.
Patent document 1 (patent document 1:US 6284013B1) discloses the method that a kind of ordinary hot platen press prepares high-purity Ru sputtering target, and concrete is at 1700 ℃ of pressurization (pressure 200kg/cm with high-purity Ru powder
2) sintering obtains the target of Φ 110mm/t5mm.Having prepared specific density through this method is high-purity Ru sputtering target of 98%, but this patent do not announce the grain fineness number and the homogeneity of structure of concrete sintering process and high-purity Ru sputtering target.Patent document 2 (patent document 2: TOHKEMY 2007-113031A communique) disclose the method that a kind of powder metallurgic method prepares high-purity Ru sputtering target; Concrete technology is to handle commerce with Ru powder (purity is 3N) through thermal plasma, improves Ru powder purity and obtains the spheric fine particle simultaneously, has prepared through the method for hot isostatic pressing and has been of a size of Φ 400mm/t10mm; Purity is the Ru sputtering target of 4N or 5N; This method has been controlled impurity content, but does not announce the concrete grain-size size of the Ru sputtering target of preparing and the homogeneity of structure that this preparation method prepares target, simultaneously; The hot isostatic pressing method preparation cost is high; Efficient is low, and subsequent disposal (as removing jacket etc.) complex procedures, has increased production cost greatly.(patent document 3: the vacuum heating-press sintering method that TOHKEMY 2009-072652A communique) discloses a kind of unidirectional pressurization prepares the method for high-purity Ru sputtering target to patent document 3, through applying one deck and O at the graphite jig inwall
2Reacting activation can be higher than the tinsel of Ru, like Nb, Ti etc., through the reaction of coating and oxygen, has reduced the inner oxygen level of target, and has avoided graphite jig to contact with the direct of Ru target, has suppressed the diffusion of C to target.Though this method has been prepared C, high-purity Ru target that O content is low; But used coating has thicker diffusion layer with the ruthenium piece of being suppressed; Loss is bigger during following process, and mould all can not continue to use behind each hot pressed sintering, needs often to change; Improve production cost greatly, be unfavorable for suitability for industrialized production.Simultaneously, owing to adopt unidirectional pressing mode to suppress, after the pressing block number increased, lower floor's target density was lower, in addition, and the grain fineness number and the homogeneity of structure of this patent and unexposed Ru target.
Summary of the invention
The object of the present invention is to provide a kind of high-purity ruthenium sputtering target and method of manufacture thereof; Said sputtering target; When reducing objectionable impurities as far as possible, make the density of target high as far as possible, the crystal grain miniaturization; Thereby improved the film uniformity of spatter film forming, reduced the paradoxical discharge phenomenon of sputter procedure etc.; Another object of the present invention is to provide a kind of preparation method who obtains above-mentioned high purity ruthenium sputtering target material.
First purpose of the present invention is achieved in that the density of said ruthenium sputtering target more than 99%, and average grain size is 2～10 μ m.
C content is not more than 50ppm in the said ruthenium sputtering target, and O content is not more than 100ppm, and Zr content is not more than 50ppm.
The room temperature bending strength of said ruthenium sputtering target is not less than 700MPa.
In the X diffraction analysis, with the X-ray diffraction peak intensity ratio of (002) crystal face of formula (I) expression
Be 30%～50%.
Another object of the present invention is achieved in that said ruthenium sputtering target adopts the hot pressed method of bidirectional vacuum to make, and concrete preparation method comprises the steps:
(1) powder pre-treating: said high-purity ruthenium powder is through ball milling, stage treatment, and it is 1～10 μ m that the sintering target uses the particle diameter of ruthenium powder;
(2) powder packing: said ruthenium powder is loaded in the graphite jig through dress powder device;
(3) powder sintered: the mould that the high-purity ruthenium powder will be housed is sent into and is carried out the bidirectional vacuum hot pressed sintering in the vacuum heating-press sintering stove, and vacuum tightness is 10
-2～10
-4Pa, sintering temperature is 1100～1800 ℃, and sintering pressure is 30～60MPa, and soaking time is 1～5h.
The ball mill crushing technology of described high-purity ruthenium powder is for selecting planetary ball mill for use, and mill Jie stablizes ZrO for yttrium
2Ball, the preferred 2～5mm of the diameter of ball, drum's speed of rotation are 300～500rpm, and ball-to-powder weight ratio is 3: 1～10: 1, and the ball milling time is 5～60min.
Said high-purity ruthenium powder airflow milling technology is carried out stage treatment, and the particle diameter of the ruthenium powder of acquisition is 1～10 μ m, and pick-up rate is more than 50%.
The temperature rise rate of said vacuum heating-press sintering is 1～15 ℃/min, and the arbitrary temperature in 600～1100 ℃ is incubated processing, soaking time 30～60min.
Apply one deck inhibition C on two-half die inwall that contacts with the high-purity ruthenium powder in the said graphite jig and the Graphite pad uniformly and be diffused into aluminum oxide or zirconia coating in the Ru sputtering target.
The present invention is through the technology of bidirectional vacuum hot pressed sintering; Prepared density more than 99%; Average crystal grain is the ruthenium sputtering target of 2～10 μ m, and the room temperature bending strength of this ruthenium sputtering target is not less than 700MPa, uses this target to carry out magnetron sputtering; Reduce the paradoxical discharge phenomenon of sputter procedure, improved the homogeneity of sputter rate and film thickness distribution; Simultaneously, use the method for two-way compacting can realize that a stove polylith suppresses simultaneously, and it is suitable to suppress the performance of correlated performance such as homogeneity of structure and hot isostatic pressing of target, has improved production efficiency, has practiced thrift production cost, cuts down the consumption of energy.
Description of drawings
Fig. 1 loads the vertical section synoptic diagram of mould behind the powder for the present invention;
Fig. 2 is the XRD analysis collection of illustrative plates of ruthenium sputtering target material of the present invention;
Fig. 3 is the SEM figure of ruthenium sputtering target material fracture of the present invention.
Among the figure: 1-outer die casing, 2-two-half die, 3-cushion block, 4-coating, 5-pad, 6-Ru powder.
Embodiment
Below in conjunction with accompanying drawing the present invention is further described, but never in any form the present invention is limited, any change or improvement based on training centre of the present invention is done all belong to protection scope of the present invention.
Highly purified ruthenium sputtering target material of the present invention, its density are more than 99%, and average grain size is 2～10 μ m.
C content is not more than 50ppm in the said ruthenium sputtering target, and O content is not more than 100ppm, and Zr content is not more than 50ppm.
The room temperature bending strength of said ruthenium sputtering target is not less than 700MPa.
In the X diffraction analysis, with the X-ray diffraction peak intensity ratio of (002) crystal face of formula (I) expression
Be 30%～50%.
The present invention has prepared above-mentioned highly purified ruthenium sputtering target material through following method, and said ruthenium sputtering target adopts the hot pressed method of bidirectional vacuum to make, and concrete preparation method comprises the steps:
(1) powder pre-treating: said high-purity ruthenium powder is through ball milling, stage treatment, and it is 1～10 μ m that the sintering target uses the particle diameter of ruthenium powder;
(2) powder packing: said ruthenium powder is loaded in the graphite jig through dress powder device;
(3) powder sintered: the mould that the high-purity ruthenium powder will be housed is sent into and is carried out the bidirectional vacuum hot pressed sintering in the vacuum heating-press sintering stove, and vacuum tightness is 10
-2～10
-4Pa, sintering temperature is 1100～1800 ℃, and sintering pressure is 30～60MPa, and soaking time is 1～5h.
The ball mill crushing technology of described high-purity ruthenium powder is for selecting planetary ball mill for use, and mill Jie stablizes ZrO for yttrium
2Ball, the preferred 2～5mm of the diameter of ball, drum's speed of rotation are 300～500rpm, and ball-to-powder weight ratio is 3: 1～10: 1, and the ball milling time is 5～60min.
Said high-purity ruthenium powder carries out stage treatment through airflow milling technology, and the median size of the ruthenium powder of acquisition is 1～10 μ m, and pick-up rate is more than 50%.
The temperature rise rate of said vacuum heating-press sintering is 1～15 ℃/min, and the arbitrary temperature in 600～1100 ℃ is incubated processing, soaking time 30～60min.
Apply one deck inhibition C on two-half die inwall that contacts with the high-purity ruthenium powder in the said graphite jig and the Graphite pad uniformly and be diffused into aluminum oxide or zirconia coating in the Ru sputtering target.
Preparing method to Ru sputtering target material among the present invention specifies below in conjunction with specific embodiment.
High-purity ruthenium sputtering target according to the invention makes through following steps:
(1) powder pre-treating: selecting purity for use is high-purity Ru powder of 3N5, and this high-purity Ru powder is carried out the planetary type ball-milling break process, and mill is situated between and is the yttrium stable zirconium oxide ball; Diameter is 2mm; Ball-to-powder weight ratio is 3: 1 (mass ratio), and the ball mill revolution speed is 500rpm, and the ball milling time is 5min; Ball milling is after the airflow milling stage treatment, and the ruthenium powder that obtains particle diameter and be 1～10 μ m uses as raw material powder.
(2) powder packing: through the powder packing device 5 blocks of target desired raw material powder are packed into (as shown in Figure 1) in the graphite jig, middlely separate, carry out the compression mouldings simultaneously of 5 targets through Graphite pad.
(3) powder sintering process: the graphite jig that will fill the Ru powder is inserted in the two-way hot pressed body of heater of vacuum and is carried out Thermocompressed sintering and forming, and sintering temperature is 1100 ℃, and sintering pressure is 60MPa, and sintering vacuum tightness is 10
-2～10
-3Pa is raised to 600 ℃ from room temperature, and temperature rise rate is 15 ℃/min, 600 ℃ of insulation 1h, and with the continued elevated temperature, temperature rise rate is 5 ℃/min, when temperature is raised to 1100 ℃, begins insulation, insulation 5h.
Be that with embodiment 1 difference said ball mill crushing technology is: the diameter of yttrium stable zirconium oxide ball is 6mm, and ball-to-powder weight ratio is 6: 1, and drum's speed of rotation is 400rpm, and the ball mill crushing time is 30min.Said sintering process is: sintering temperature is 1800 ℃, and sintering pressure is 30MPa, and sintering vacuum tightness is 10
-2～10
-3Pa is raised to 600 ℃ from room temperature, and temperature rise rate is 15 ℃/min; 600 ℃ of insulation 30min, with the continued elevated temperature, temperature rise rate is 10 ℃/min; When temperature is raised to 1300 ℃, be incubated 1h again, with the continued elevated temperature, temperature rise rate is 5 ℃/min; When temperature is elevated to 1800 ℃, under this temperature, be incubated 1h.
Be that with embodiment 1 difference said ball mill crushing technology is: the diameter of yttrium stable zirconium oxide ball is 10mm, and ball-to-powder weight ratio is 10: 1, and drum's speed of rotation is 300rpm, and the ball mill crushing time is 60min.Said sintering process is: sintering temperature is 1500 ℃, and sintering pressure is 50MPa, and sintering vacuum tightness is 10
-2～10
-3Pa is raised to 600 ℃ from room temperature, and temperature rise rate is 15 ℃/min; 600 ℃ of insulation 30min, with the continued elevated temperature, temperature rise rate is 5 ℃/min; When temperature is raised to 1100 ℃, continue elevated temperature subsequently again, temperature rise rate becomes 1 ℃/min; When temperature is raised to 1500 ℃, under this temperature, be incubated 3h.
Be that with embodiment 1 difference said ball mill crushing technology is: the diameter of yttrium stable zirconium oxide ball is 2mm, and ball-to-powder weight ratio is 6: 1, and drum's speed of rotation is 400rpm, and the ball mill crushing time is 30min.Said sintering process is: sintering temperature is 1500 ℃, and sintering pressure is 50MPa, and sintering vacuum tightness is 10
-3～10
-4Pa is raised to 800 ℃ from room temperature, and temperature rise rate is 15 ℃/min, 800 ℃ of insulation 30min; With the continued elevated temperature, temperature rise rate is 5 ℃/min, when temperature is raised to 1100 ℃, and insulation 40min; Temperature rise rate changes 1 ℃/min into, when temperature is raised to 1500 ℃, under this temperature, is incubated 3h.
Comparative example 1
Be that with embodiment 3 differences said ruthenium powder is through ball mill crushing and stage treatment, the mean diameter of said original ruthenium powder is 20～50 μ m, and the size-grade distribution of starting powder is extremely inhomogeneous.
Comparative example 2
Be that with embodiment 3 differences said sintering process adopts the mode sinter molding of hot isostatic pressing, its sintering process is an Ar-sintering, and sintering temperature is 1300 ℃, and sintering pressure is 130MPa, and soaking time is 2h.
Through particle-size analyzer, XRD, SEM, GDMS (glow discharge mass spectrometry appearance), C, N, O analyser, characterization methods such as tensile testing machine carry out performance evaluation to the Ru sputtering target target that uses method for preparing; Simultaneously, use method sputter Ru film on Si (100) sheet of magnetron sputtering, and the film uniformity of film is estimated through methods such as step appearance, SEM.
Particularly, the median size of testing original ruthenium powder through particle-size analyzer, the bending strength of on tensile testing machine, testing target through the three point bending test method is through the occupation rate of XRD analysis target (002) crystal face; Through sem analysis different zones grain-size; Film uniformity of the film that obtains by magnetron sputtering through the analysis of step appearance etc., through C, N, O analyser C to the target prepared, N, O content is analyzed.
Can know by table 1 and Fig. 3; Used ruthenium powder is through broken stage treatment; The median size of powder is 20～50 μ m, directly uses the compacting target, can form the crystal grain (shown in the comparative example 1 of Fig. 2) of growing up unusually in the target that obtains; In sputter procedure, the paradoxical discharge phenomenon be may occur or crystal grain integral body comes off, film forming film uniformity and film quality had a strong impact on.
Can know by Fig. 3; The target grain-size of preparing through the foregoing description is all in 2～10 mu m ranges; The grain fineness number that this shows the target edge that goes out through method for preparing and central zone is suitable; The homogeneity of structure of overall target is better, and the grain fineness number of some embodiment also is superior to the result of hot isostatic pressing.
Can know that by Fig. 2 and table 2 ratio (calculation formula of ratio is suc as formula shown in (I)) of target (002) crystal face through the preparation of this method has brought up to 30～50% by 16.7% of pulverulence, and is approaching with the result of hot isostatic pressing.According to patent documentation said (reference JP2007-113032A), can improve the sputter rate of target greatly through the ratio that improves (002) crystal face.And can know that by table 2 the target center zone differs less with the ratio of fringe region (002) crystal face, has proved that further edge and central zone structure property differ less.
Can be known that by table 2 use the specific density of the Ru sputtering target of this method preparation to be not less than 99%, C content is not more than 50ppm, O content is not more than 100ppm, and N content is not more than 10ppm.Use the Ru sputtering target of this method preparation to carry out sputter, the homogeneity of the Ru film that obtains is better, and film thickness distribution is that the difference of thickness and thinnest part is 2～6%.
The different crushing process powder of table 1 median size
| | Embodiment | 1 | |
|
|
Comparative example 1 | Comparative example 2 |
| Starting powder particle diameter d
50/ |
20～50 | 20～50 | 20～50 | 20～50 | ?20～50 | 20～50 | |
| Broken back powder diameter d
50/ |
5～10 | 3～10 | 5～10 | 6～10 | ?20～50 | 4～10 | |
| Zr content/ppm in the |
10 | 20 | 45 | 35 | ?0.35 | 30 | |
| 1～10 μ m powder pick-up rate after the classification | 55％ | 65％ | 50％ | 75％ | ?- | 55％ |
The performance evaluation of different embodiment of table 2 and comparative example
In sum, the performance of the Ru sputtering target through method for preparing near or be superior to the result of hot isostatic pressing, and can realize that through this method a stove polylith suppresses simultaneously, compare with the hot isostatic pressing method, both improved production efficiency, reduced production cost again.
Claims (9)
1. high-purity ruthenium sputtering target, it is characterized in that: the density of said ruthenium sputtering target is more than 99%, and average grain size is 2～10 μ m.
2. high-purity ruthenium sputtering target according to claim 1 is characterized in that: C content is not more than 50ppm in the said ruthenium sputtering target, and O content is not more than 100ppm, and Zr content is not more than 50ppm.
3. high-purity ruthenium sputtering target according to claim 1 is characterized in that: the room temperature bending strength of said ruthenium sputtering target is not less than 700MPa.
4. high-purity ruthenium sputtering target according to claim 1 is characterized in that: in the X diffraction analysis, be 30%～50% with the X-ray diffraction peak intensity ratio of (002) crystal face of formula (I) expression,
5. the preparation method of the said high-purity ruthenium sputtering target of claim 1 is characterized in that: said ruthenium sputtering target adopts the hot pressed method of bidirectional vacuum to make, and concrete preparation method comprises the steps:
(1) powder pre-treating: said high-purity ruthenium powder is through ball milling, stage treatment, and it is 1～10 μ m that the sintering target uses the particle diameter of ruthenium powder;
(2) powder packing: said ruthenium powder is loaded in the graphite jig through dress powder device;
(3) powder sintered: the mould that the high-purity ruthenium powder will be housed is sent into and is carried out the bidirectional vacuum hot pressed sintering in the vacuum heating-press sintering stove, and vacuum tightness is 10
-2～10
-4Pa, sintering temperature is 1100～1800 ℃, and sintering pressure is 30～60MPa, and soaking time is 1～5h.
6. the preparation method of high-purity ruthenium sputtering target according to claim 5 is characterized in that: described high-purity ruthenium powder selects for use the mode of planetary type ball-milling to carry out ball mill crushing, and mill Jie stablizes ZrO for yttrium
2Ball, the preferred 2～10mm of the diameter of ball, drum's speed of rotation are 300～500rpm, and ball-to-powder weight ratio is 3: 1～10: 1, and the ball milling time is 5～60min.
7. the preparation method of high-purity ruthenium sputtering target according to claim 5 is characterized in that: said high-purity ruthenium powder carries out stage treatment through airflow milling technology, and the particle diameter of the ruthenium powder of acquisition is 1～10 μ m, and pick-up rate is more than 50%.
8. the preparation method of high-purity ruthenium sputtering target according to claim 5 is characterized in that: the temperature rise rate of said vacuum heating-press sintering is 1～15 ℃/min, and the arbitrary temperature in 600～1100 ℃ is incubated processing, soaking time 30～60min.
9. the preparation method of high-purity ruthenium sputtering target according to claim 5 is characterized in that: apply one deck inhibition C on two-half die inwall that contacts with the high-purity ruthenium powder in the said graphite jig and the Graphite pad uniformly and be diffused into aluminum oxide or zirconia coating in the Ru sputtering target.
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| 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 |
| CN104458370A (en) * | 2014-11-23 | 2015-03-25 | 昆明贵金属研究所 | Method for preparing glow discharge mass spectrometer analysis test sample |
| CN104465979A (en) * | 2013-09-25 | 2015-03-25 | 中国科学院上海硅酸盐研究所 | Method for directly preparing hollow thermoelectricity sample |
| CN107805789A (en) * | 2017-11-30 | 2018-03-16 | 清远先导材料有限公司 | Preparation method of ruthenium sputtering target material |
| CN108642464A (en) * | 2018-06-25 | 2018-10-12 | 河南科技大学 | A kind of preparation method of high-purity ruthenium sputtering target material |
| CN109355632A (en) * | 2018-12-18 | 2019-02-19 | 郑州大学 | A method of improving molybdenum and its alloy sputtering target grain uniformity |
| CN116043175A (en) * | 2022-11-24 | 2023-05-02 | 先导薄膜材料（广东）有限公司 | Thick plane target material and preparation method thereof |
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| 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 |
| CN104458370A (en) * | 2014-11-23 | 2015-03-25 | 昆明贵金属研究所 | Method for preparing glow discharge mass spectrometer analysis test sample |
| CN107805789A (en) * | 2017-11-30 | 2018-03-16 | 清远先导材料有限公司 | Preparation method of ruthenium sputtering target material |
| CN107805789B (en) * | 2017-11-30 | 2019-09-03 | 清远先导材料有限公司 | Preparation method of ruthenium sputtering target material |
| CN108642464A (en) * | 2018-06-25 | 2018-10-12 | 河南科技大学 | A kind of preparation method of high-purity ruthenium sputtering target material |
| CN108642464B (en) * | 2018-06-25 | 2020-08-28 | 河南科技大学 | Preparation method of high-purity ruthenium sputtering target material |
| CN109355632A (en) * | 2018-12-18 | 2019-02-19 | 郑州大学 | A method of improving molybdenum and its alloy sputtering target grain uniformity |
| CN116043175A (en) * | 2022-11-24 | 2023-05-02 | 先导薄膜材料（广东）有限公司 | Thick plane target material and preparation method thereof |
| CN116043175B (en) * | 2022-11-24 | 2024-09-17 | 先导薄膜材料(江苏)有限公司 | Thick plane target material and preparation method thereof |
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