CN108642464A - A kind of preparation method of high-purity ruthenium sputtering target material - Google Patents
A kind of preparation method of high-purity ruthenium sputtering target material Download PDFInfo
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- CN108642464A CN108642464A CN201810661515.4A CN201810661515A CN108642464A CN 108642464 A CN108642464 A CN 108642464A CN 201810661515 A CN201810661515 A CN 201810661515A CN 108642464 A CN108642464 A CN 108642464A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F2003/145—Both compacting and sintering simultaneously by warm compacting, below debindering temperature
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The present invention relates to powder metallurgical technologies, more particularly to a kind of preparation method of high-purity ruthenium sputtering target material, be mainly molded including broken, ball milling, die-filling, uniaxial hot pressing and etc., during die-filling, it is mutually filled using the powder of 3 kinds of different grain size ranks, last sinter molding.The present invention uses powder metallurgy process, target can be prepared at a temperature of less than material melting point, not only greatly reduce the operation difficulty of equipment, also the introducing of impurity in preparation process can effectively be controlled, also it can realize the controllable preparation of target tissue fineness by controlling granularity and the sintering process system of raw material high-purity ruthenium powder, to substantially reduce production cost while improving ruthenium target product quality stability, the high-performance and low-cost high-purity ruthenium target of microscopic structure uniform, controllable can be obtained.
Description
Technical field
The present invention relates to powder metallurgical technologies, and in particular to a kind of preparation method of high-purity ruthenium sputtering target material.
Background technology
As the key technology of integrated circuit and chip manufacturing, magnetron sputtering plating has equipment simple, easily controllable, thin
The many advantages such as film uniformity height.Wherein the quality of sputtering target material is to the coating effects of magnetron sputtering and the property of semiconductor devices
There can be decisive influence, therefore the sputtering target material of high quality becomes the indispensable critical material of electronic information technology industry.
Due to the membrane quality formed after target as sputter（Such as film thickness, uniformity）Integrated circuit and chip etc. can be significantly impacted
The performance of electronic product, and membrane quality, are heavily dependent on the tissue signature of sputtering target material, for example, grain size and its point
Cloth etc..Therefore, in order to improve the quality of ruthenium target, the crystallite dimension and crystal grain orientation for controlling target just seem very crucial.
High-purity target is mainly prepared using electron beam melting processes both at home and abroad at present, then by it is moulding processing and heat at
Science and engineering skill carries out tissue modulation to it, obtains ideal grain size, is then carrying out post-production, is completing finished product.
Complex process when electron-beam smelting, fusion process are high to appointed condition requirement, and power system load is very big, therefore
Manufacturing cost is very high.In addition, ruthenium belongs to high temperature refractory, fusing point is up to 2310 DEG C, prepares environment and belongs to hot environment, earthenware
Impurity in the environment such as crucible, heater, heat preservation component easily enters melt, impurity is mixed into causing high-purity target to prepare, to rear
Phase properties of product are very unfavorable.The following process of ingot casting needs to pass through plastic processing and heat treatment repeatedly, these processes are target again
Hidden danger has been buried in the reduction of material purity.
Invention content
The object of the present invention is to provide the preparation method of high-purity ruthenium sputtering target material, using powder metallurgy process, can less than
Target is prepared at a temperature of material melting point, not only greatly reduces the operation difficulty of equipment, also can effectively be controlled in preparation process
The introducing of impurity can also realize target tissue fineness by controlling granularity and the sintering process system of raw material high-purity ruthenium powder
Controllable preparation can obtain micro- to substantially reducing production cost while improving ruthenium target product quality stability
The controllable high-performance and low-cost high-purity ruthenium target of even tissue.
In order to solve the above technical problems, the technical solution adopted in the present invention and its design are：A kind of high-purity ruthenium sputtering target
The preparation method of material, includes the following steps：
Step 1: broken：Crusher is used to be crushed purity for 99.95% or more high-purity ruthenium block stock, shaking-sieving obtains
It is 500 μm of powders below to granularity；It is 99.95% or more pure ruthenium coating that purity is lined in crusher；
Step 2: ball milling：The granularity obtained after will be broken is that 500 μm of powders below carry out ball milling, ball milling under nitrogen atmosphere
Ball is used in mixed way using the high-purity ruthenium ball of 3 kinds of different-diameters, and in the range of 5 ~ 15mm, ball milling ball purity is ball milling bulb diameter
99.95% or more, granularity is milled to as 200 μm hereinafter, carrying out multi-stage screening after ball milling（Using multilayer different pore size sieve by
Grade screening）, obtain a variety of granularity level（It is indicated with the aperture of adjacent two layers sieve）Powder；
Step 3: die-filling：Take the powder of wherein 3 kinds granularity level after screening, i.e. powder I, powder II and powder III, powder I
Granularity level is 10 μm or less（It is the aggregates for referring to the sieve that through hole diameter is 10 μm that granularity level, which is 10 μm or less,）,
II granularity level of powder is D1~D2μm（It refers to through aperture be D2Sieve and cannot by aperture be D1Sieve particle
Set）, 50 μm≤D1＜ D2≤ 120 μm, D2-D1=20 ~ 30 μm, the granularity level of powder III is D3~D4μm, 150 μm≤D3＜
D4≤ 200 μm, D4-D3=20 ~ 30 μm, the quality of powder I is the 1/3 ~ 1/2 of II mass of powder, and the quality of powder III is powder II
Three kinds of powders are uniformly mixed by the 1/5 ~ 1/3 of quality（If without screening, directly die-filling, then particle size distribution is wider,
Mutual filling effect is bad between each granularity, influences product consistency；If be used alone smaller particle size powder, cost compared with
Height, based on the moderate powder of granularity, by the gap of a small amount of big granularity being mixed between wherein having little influence on particle,
The powder of suitable small grain size is inserted in gap again, filling effect greatly improves, and is dropped under the premise of ensureing product consistency
Low production cost）, it is packed into graphite jig after drying, jolt ramming compresses, and the pressure-resistant limit of graphite jig is resistance to thermoae in 40MPa or more
Limit is at 2100 DEG C or more；
Step 4: uniaxial hot pressing is molded：The graphite jig for filling powder is put into progress uniaxial hot pressing burning in vacuum hotpressing stove
Knot, sintering process carry out under protective gas atmosphere, and sintering temperature is 1600 ~ 1800 DEG C, and sintering pressure is 5 ~ 20MP；In room temperature
To 1000 DEG C, heating rate is 5 ~ 10 DEG C/min；At 1000 DEG C to 1500 DEG C, heating rate is 5 ~ 8 DEG C/min；Extremely at 1500 DEG C
Sintering temperature, heating rate are that heating rate is 2 ~ 5 DEG C/min；30 ~ 120min is kept the temperature in sintering temperature, it is cold after the completion of sintering
But it, demoulds, obtains briquet；
Step 5: machining：Obtained briquet is subjected to surface sanding and polishing, dimensioned is carried out according to magnetron sputtering apparatus,
Obtain high-purity ruthenium sputtering target material.
In step 1, the thickness of the pure material coating is 50 ~ 80 μm.
In step 2,500 μm of powders below of granularity are subjected to ball milling in ball grinder, the volume point of nitrogen in ball grinder
Number is 99%.
It in step 2, is milled to that granularity is 200 μm or less, volume average particle size is 60 ~ 70 μm, then carries out multistage sieve
Point.
The size of graphite jig described in step 3 is：Outside dimension (120 ~ 180mm) * (100 ~ 130mm), inner cavity 20 ~
100mm。
Protective gas described in step 4 is argon gas, and the purity for the argon gas being filled with to vacuum hotpressing stove is 99.999% or more.
Compared with existing ruthenium target technology of preparing, it is an advantage of the invention that：
1. preparation process is relatively easy, technological parameter controllability is strong, and equipment and energy cost are relatively low, easily realizes extensive industry
Change；
2. manufacturing cost is relatively low, preparation process temperature substantially reduces, and can substantially reduce the possibility that impurity is mixed into preparation process
Property, purity is easier to ensure that；
3. target post-production and deformation technique are less, product microstructure is stablized, and the stabilization of its sputtering performance is conducive to；
4. the powder metallurgical technique used, can be by adjusting material powder granularity, control sintering process system, regulation and control processing technology
The methods of realize that the regulation and control of ruthenium target tissue fineness, the controllability of target performance are stronger.
Description of the drawings
Fig. 1 is the X-ray diffractogram of high-purity Ru powder before being sieved after ball milling in the embodiment of the present invention 1；
Fig. 2 is the microstructure photo of high-purity Ru powder before being sieved after ball milling in the embodiment of the present invention 1；
Fig. 3 is the gamma-spectrometric data of high-purity Ru powder before being sieved after ball milling in the embodiment of the present invention 1；
Fig. 4 is the X-ray diffractogram of high-purity Ru targets of through the embodiment of the present invention 1 method preparation；
Fig. 5 is the microstructure photo of high-purity Ru target material surfaces of through the embodiment of the present invention 1 method preparation；
Fig. 6 is the gamma-spectrometric data of high-purity Ru targets of through the embodiment of the present invention 1 method preparation.
Specific implementation mode
The present invention will be further described in detail with reference to the accompanying drawings and examples, and non-detailed portion is existing below
Technology uses the prior art that can realize.
A kind of preparation method of high-purity ruthenium sputtering target material, includes the following steps：
Step 1: broken：Crusher is used to be crushed purity for 99.95% or more high-purity ruthenium block stock, shaking-sieving obtains
It is 500 μm of powders below to granularity；It is 99.95% or more pure ruthenium coating that purity is lined in crusher；
Step 2: ball milling：The granularity obtained after will be broken is that 500 μm of powders below carry out ball milling, ball milling under nitrogen atmosphere
Ball is used in mixed way using the high-purity ruthenium ball of 3 kinds of different-diameters, and in the range of 5 ~ 15mm, ball milling ball purity is ball milling bulb diameter
99.95% or more, granularity is milled to as 200 μm hereinafter, carrying out multi-stage screening after ball milling（Using multilayer different pore size sieve by
Grade screening）, obtain a variety of granularity level（It is indicated with the aperture of adjacent two layers sieve）Powder；
Step 3: die-filling：Take the powder of wherein 3 kinds granularity level after screening, i.e. powder I, powder II and powder III, powder I
Granularity level is 10 μm or less（It is the aggregates for referring to the sieve that through hole diameter is 10 μm that granularity level, which is 10 μm or less,）,
II granularity level of powder is D1~D2μm（It refers to through aperture be D2Sieve and cannot by aperture be D1Sieve particle
Set）, 50 μm≤D1＜ D2≤ 120 μm, D2-D1=20 ~ 30 μm, the granularity level of powder III is D3~D4μm, 150 μm≤D3＜
D4≤ 200 μm, D4-D3=20 ~ 30 μm, the quality of powder I is the 1/3 ~ 1/2 of II mass of powder, and the quality of powder III is powder II
Three kinds of powders are uniformly mixed by the 1/5 ~ 1/3 of quality（If without screening, directly die-filling, then particle size distribution is wider,
Mutual filling effect is bad between each granularity, influences product consistency；If be used alone smaller particle size powder, cost compared with
Height, based on the moderate powder of granularity, by the gap of a small amount of big granularity being mixed between wherein having little influence on particle,
The powder of suitable small grain size is inserted in gap again, filling effect greatly improves, and is dropped under the premise of ensureing product consistency
Low production cost）, it is packed into graphite jig after drying, jolt ramming compresses, and the pressure-resistant limit of graphite jig is resistance to thermoae in 40MPa or more
Limit is at 2100 DEG C or more；
Step 4: uniaxial hot pressing is molded：The graphite jig for filling powder is put into progress uniaxial hot pressing burning in vacuum hotpressing stove
Knot, sintering process carry out under protective gas atmosphere, and sintering temperature is 1600 ~ 1800 DEG C, and sintering pressure is 5 ~ 20MP；In room temperature
To 1000 DEG C, heating rate is 5 ~ 10 DEG C/min；At 1000 DEG C to 1500 DEG C, heating rate is 5 ~ 8 DEG C/min；Extremely at 1500 DEG C
Sintering temperature, heating rate are that heating rate is 2 ~ 5 DEG C/min；30 ~ 120min is kept the temperature in sintering temperature, it is cold after the completion of sintering
But it, demoulds, obtains briquet；
Step 5: machining：Obtained briquet is subjected to surface sanding and polishing, dimensioned is carried out according to magnetron sputtering apparatus,
Obtain high-purity ruthenium sputtering target material.
In step 1, the thickness of the pure material coating is 50 ~ 80 μm.
In step 2,500 μm of powders below of granularity are subjected to ball milling in ball grinder, the volume point of nitrogen in ball grinder
Number is 99%.
It in step 2, is milled to that granularity is 200 μm or less, volume average particle size is 60 ~ 70 μm, then carries out multistage sieve
Point.
The size of graphite jig described in step 3 is：Outside dimension (120 ~ 180mm) * (100 ~ 130mm), inner cavity 20 ~
100mm。
Protective gas described in step 4 is argon gas, and the purity for the argon gas being filled with to vacuum hotpressing stove is 99.999% or more.
Embodiment 1
The high-purity ruthenium block that purity by industry purification is 99.95% or more is using crusher in crushing at 500 μm small below
Grain, and ball milling is carried out under nitrogen protection atmosphere, ball milling bulb diameter is respectively：The number ratio of 5mm, 10mm, 15mm, three bulbs is
9:4:1, gross mass and the quality of material ratio of ball are 3:1, it is 60 μm to be milled to granularity in 200 μm or less, volume average particle size；Ball
The X-ray diffractogram of high-purity Ru powder before being sieved after mill is as shown in Figure 1, diffraction maximum shows there was only pure ruthenium phase, inside powder not
Containing other phases, therefore cleanliness factor is very high；By the basic principle of material phase analysis it is found that the crystalline substance of the intensity display material of XRD diffraction maximums
Change degree, diffraction peak intensity is higher, illustrates that its crystallization is more perfect；It can be seen that high-purity Ru powder has higher crystallinity；It is sieved after ball milling
The microstructure of high-purity Ru powder before point is as shown in Figure 2, it is seen then that ruthenium powder is by the very tiny ultra-fine ruthenium powder of grain size
（Minimum is less than 5um）Reunite and becomes tens microns to up to a hundred microns；This is the feature of ball milling powder；Illustrate ball of the present invention
The powder granularity of mill reaches ultra-fine rank, and this hyperfine structure helps to improve the performance of later stage target；Before being sieved after ball milling
The gamma-spectrometric data of high-purity Ru powder is as shown in figure 3, display powder only has the peak value of Ru elements, and the peak without other elements substantially
Value can be explained powder in conjunction with Fig. 1 and be free of other impurities, and purity is reliable；Ball milling, screening（Multi-stage screening）Afterwards, take 10 μm of granularity with
Under, 80 ~ 100 μm, the powders of 180 ~ 200 μm of three kinds of granularity level, be 1 according to mass ratio:3:1 ratio is uniformly mixed, and is done
It is fitted into high-strength graphite mold after dry, needs to be separated with gasket between ruthenium powder and stamping, prevent from bonding, then place into upper and lower mould
Punching；Then powder jolt ramming is compressed to the push-down head for being put into high temperature hot pressing furnace, and adjust position and ensure that mold is located at push-down head
Center, material is pressurized uniform when ensuring pressurization；Start cooling water recirculation system, vacuum hotpressing stove is vacuumized, is evacuated to
When vacuum degree≤20Pa, it is filled with the Ar of purity >=99.999%；When hot pressing furnace inside and outside air pressure balance, pressurization is started to warm up, temperature is worked as
When degree is to 1000 DEG C, heating rate is 10 DEG C/min；For temperature at 1000 to 1500 DEG C, heating rate is 8 DEG C/min, temperature
At 1500 to 1600 DEG C, heating rate is 5 DEG C/min；Start to pressurize while heating, application pressure is 5MPa；In most final temperature
1600 DEG C of heat preservation 30min of degree and then closing heating system carry out natural cooling so that hot pressing in-furnace temperature is down to room temperature；It removes
Except ram pressures, vacuum breaker（Gas inside and outside furnace body is set to be connected）, graphite jig is taken out from vacuum hotpressing stove, demoulding is taken out
Sample briquet, density 10.1g/cm3；High-purity ruthenium briquet is subjected to surface sanding and polishing, ruler is carried out according to magnetron sputtering apparatus
Very little processing obtains high-purity ruthenium target；The X-ray diffractogram of high-purity Ru targets is as shown in figure 4, still there was only pure ruthenium phase, diffraction maximum
Intensity is equally higher, it is seen that its crystallinity is good；The microstructures of high-purity Ru target material surfaces as shown in figure 5, due to use heat
Pressure pressure is smaller, therefore consistency is not high, and hole occurs in material surface；The gamma-spectrometric data of high-purity Ru targets is as shown in fig. 6, can
See, the target of preparation still only has the peak of ruthenium element, illustrates that preparing environment maintains good cleanliness factor, there is no material after molding
It is mixed into other impurities.
Embodiment 2
Difference from example 1 is that：In ball milling step, ball milling bulb diameter is respectively：5mm, 8mm, 13mm, three bulbs
Number ratio is 9:3:2, gross mass and the quality of material ratio of ball are 2:1, granularity is milled in 200 μm or less, volume average particle size
It is 63 μm；In die-filling step, 10 μm of granularity or less, 60 ~ 80 μm, the powders of 140 ~ 160 μm of three kinds of granularity level are taken, according to matter
Amount is than being 2:4:1 ratio is uniformly mixed；In uniaxial hot pressing forming step, when temperature be room temperature to 1000 DEG C when, heating rate
For 10 DEG C/min；For temperature at 1000 to 1500 DEG C, heating rate is 7 DEG C/min, and temperature is at 1500 to 1600 DEG C, heating speed
Degree is 4 DEG C/min；Start to pressurize while heating, application pressure is 10MPa；In 1600 DEG C of heat preservation 60min of final temperature；Demoulding
The density for taking out sample green body is 10.3g/cm3。
Embodiment 3
Difference from example 1 is that：In ball milling step, ball milling bulb diameter is respectively：5mm, 7mm, 14mm, three bulbs
Number ratio is 8:3:1, gross mass and the quality of material ratio of ball are 2:1, granularity is milled in 200 μm or less, volume average particle size
It is 65 μm；In die-filling step, 10 μm of granularity or less, 50 ~ 70 μm, 150 ~ 170 μm of three kinds of powders are taken, are 2 according to mass ratio:5:
1 ratio is uniformly mixed；In uniaxial hot pressing forming step, when temperature be room temperature to 1000 DEG C when, heating rate be 10 DEG C/min；
Temperature at 1000 to 1500 DEG C, heating rate be 6 DEG C/min, temperature at 1500 to 1700 DEG C, heating rate be 3 DEG C/
min；Start to pressurize while heating, application pressure is 15MPa；In 1700 DEG C of heat preservation 60min of final temperature；Sample is taken out in demoulding
The density of green body is 10.5g/cm3。
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, though
So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any technology people for being familiar with this profession
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, as long as be without departing from technical solution of the present invention content, it is right according to the technical essence of the invention
Any simple modification, equivalent change and modification made by above example, in the range of still falling within technical solution of the present invention.
Claims (6)
1. a kind of preparation method of high-purity ruthenium sputtering target material, which is characterized in that include the following steps：
Step 1: broken：Crusher is used to be crushed purity for 99.95% or more high-purity ruthenium block stock, shaking-sieving obtains
It is 500 μm of powders below to granularity；It is 99.95% or more pure ruthenium coating that purity is lined in crusher；
Step 2: ball milling：The granularity obtained after will be broken is that 500 μm of powders below carry out ball milling, ball milling under nitrogen atmosphere
Ball is used in mixed way using the high-purity ruthenium ball of 3 kinds of different-diameters, and in the range of 5 ~ 15mm, ball milling ball purity is ball milling bulb diameter
99.95% or more, granularity is milled to as 200 μm hereinafter, carrying out multi-stage screening after ball milling, obtains the powder of a variety of granularity level；
Step 3: die-filling：Take the powder of wherein 3 kinds granularity level after screening, i.e. powder I, powder II and powder III, powder I
Granularity level is 10 μm hereinafter, II granularity level of powder is D1~D2μm, 50 μm≤D1＜ D2≤ 120 μm, D2-D1=20 ~ 30 μm, powder
The granularity level of material III is D3~D4μm, 150 μm≤D3＜ D4≤ 200 μm, D4-D3=20 ~ 30 μm, the quality of powder I is powder II
The 1/3 ~ 1/2 of quality, the quality of powder III are the 1/5 ~ 1/3 of II mass of powder, and three kinds of powders are uniformly mixed, are packed into after dry
Graphite jig, jolt ramming compress, and the pressure-resistant limit of graphite jig is in 40MPa or more, and heat-resistant limit is at 2100 DEG C or more；
Step 4: uniaxial hot pressing is molded：The graphite jig for filling powder is put into progress uniaxial hot pressing burning in vacuum hotpressing stove
Knot, sintering process carry out under protective gas atmosphere, and sintering temperature is 1600 ~ 1800 DEG C, and sintering pressure is 5 ~ 20MP；In room temperature
To 1000 DEG C, heating rate is 5 ~ 10 DEG C/min；At 1000 DEG C to 1500 DEG C, heating rate is 5 ~ 8 DEG C/min；Extremely at 1500 DEG C
Sintering temperature, heating rate are that heating rate is 2 ~ 5 DEG C/min；30 ~ 120min is kept the temperature in sintering temperature, it is cold after the completion of sintering
But it, demoulds, obtains briquet；
Step 5: machining：Obtained briquet is subjected to surface sanding and polishing, dimensioned is carried out according to magnetron sputtering apparatus,
Obtain high-purity ruthenium sputtering target material.
2. a kind of preparation method of high-purity ruthenium sputtering target material as described in claim 1, it is characterised in that：It is described in step 1
The thickness of pure material coating is 50 ~ 80 μm.
3. a kind of preparation method of high-purity ruthenium sputtering target material as described in claim 1, it is characterised in that：In step 2, by grain
500 μm of powders below of degree carry out ball milling in ball grinder, and the volume fraction of nitrogen is 99% in ball grinder.
4. a kind of preparation method of high-purity ruthenium sputtering target material as described in claim 1, it is characterised in that：In step 2, ball milling
To granularity be 200 μm or less, volume average particle size is 60 ~ 70 μm, then carry out multi-stage screening.
5. a kind of preparation method of high-purity ruthenium sputtering target material as described in claim 1, it is characterised in that：Graphite described in step 3
The size of mold is：Outside dimension (120 ~ 180mm) * (100 ~ 130mm), 20 ~ 100mm of inner cavity.
6. a kind of preparation method of high-purity ruthenium sputtering target material as described in claim 1, it is characterised in that：It is protected described in step 4
Shield gas is argon gas, and the purity for the argon gas being filled with to vacuum hotpressing stove is 99.999% or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810661515.4A CN108642464B (en) | 2018-06-25 | 2018-06-25 | Preparation method of high-purity ruthenium sputtering target material |
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| CN109158163A (en) * | 2018-10-23 | 2019-01-08 | 广东迪奥应用材料科技有限公司 | The crusher and its manufacturing method of high-purity material is deposited |
| CN110893467A (en) * | 2019-12-24 | 2020-03-20 | 湖南欧泰稀有金属有限公司 | Grinding tank and preparation method of high-purity superfine ruthenium powder |
| CN110983265A (en) * | 2019-12-24 | 2020-04-10 | 湖南欧泰稀有金属有限公司 | Preparation method of special-shaped ruthenium product |
| 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 |
| CN114378294A (en) * | 2021-12-29 | 2022-04-22 | 盐城金美新材料有限公司 | High-purity tantalum plate and preparation method thereof |
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| 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 |
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| JP2005153127A (en) * | 2003-11-28 | 2005-06-16 | Olympus Corp | Optical element molding die and its manufacturing method |
| 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 |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109158163A (en) * | 2018-10-23 | 2019-01-08 | 广东迪奥应用材料科技有限公司 | The crusher and its manufacturing method of high-purity material is deposited |
| CN110893467A (en) * | 2019-12-24 | 2020-03-20 | 湖南欧泰稀有金属有限公司 | Grinding tank and preparation method of high-purity superfine ruthenium powder |
| CN110983265A (en) * | 2019-12-24 | 2020-04-10 | 湖南欧泰稀有金属有限公司 | Preparation method of special-shaped ruthenium product |
| CN110983265B (en) * | 2019-12-24 | 2022-03-11 | 湖南欧泰稀有金属有限公司 | Preparation method of special-shaped ruthenium product |
| 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 |
| CN114378294A (en) * | 2021-12-29 | 2022-04-22 | 盐城金美新材料有限公司 | High-purity tantalum plate and preparation method thereof |
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