CN105986138A - Method for preparing ultra-pure nickel and platinum alloy target material - Google Patents
Method for preparing ultra-pure nickel and platinum alloy target material Download PDFInfo
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- CN105986138A CN105986138A CN201610471107.3A CN201610471107A CN105986138A CN 105986138 A CN105986138 A CN 105986138A CN 201610471107 A CN201610471107 A CN 201610471107A CN 105986138 A CN105986138 A CN 105986138A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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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
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
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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 discloses a method for preparing an ultra-pure nickel and platinum alloy target material. The preparing method includes the steps of high-purity prealloy powder preparation, alloy melting, purification of a melt through zone melting, mechanical rolling and control over grain size through heat treatment. According to ultra-pure nickel and platinum alloy, chloroplatinic acid ammonia with the purity larger than or equal to 99.995% and nickel chloride with the purity larger than or equal to 99.99% serve as raw materials, composite particles of the chloroplatinic acid ammonia and the nickel chloride are prepared with a gas atomization method, and then high-purity nickel and platinum pre-alloyed powder is obtained through a hydrogen leading-in reduction method; vacuum induction melting is carried out to obtain a nickel and platinum mother alloy; and finally, a zone melting method is adopted for purify the nickel and platinum mother alloy so as to obtain an ultra-pure nickel and platinum alloy. According to the ultra-pure nickel and platinum alloy target material prepared with the method, the contents of alkali metal ions (Na and K) and radioactive elements (U and Th) are low, other metal impurities are obviously reduced compared with a method in an existing literature, the oxygen content is obviously increased compared with the method in the existing literature, and the grain size is obviously improved compared with the method in the existing literature.
Description
Technical field
The present invention relates to a kind of superelevation pure nickel platinum alloy target and preparation method thereof, belong to field of manufacturing semiconductor devices.
Background technology
The nickel silicide prepared by nickel and nickel alloy (mainly NiPt) target is owing to having without live width benefit, showing without bridging
As advantages such as, sheet resistance are little, process annealing consumes less silicon atom and Ni silicide stress is little, it is widely used in Schottky
The fields such as discrete component and integrated circuit such as diode (SBD), complementary mos device (CMOS).On a large scale
And in ultra-large COMS integrated circuit, after entering 65nm and 45nm technology node, due to the restriction of live width effect, nickel and
Nickel silicide prepared by nickel alloy (mainly NiPt) target replaces Titanium silicide, cobalt silicide, becomes the most frequently used silicide,
To reduce resistance value and to reduce leakage current, it is thus achieved that higher device performance.
Semiconductor integrated circuit manufactures higher to the requirement of sputtering target material purity, mainly due to alkali metal ion (Na+、K+) form mobility ion the most in a insulating layer, reduce device performance.Radioelement (U, Th) can discharge alpha ray, causes
Components and parts produce soft breakdown.Heavy metal (Fe, Cr etc.) ion can produce interface electric leakage and oxygen element increase etc..Therefore must to
The content of upper several dvielements is controlled.Meanwhile, if the excessive number of field trash in target, in sputter procedure, easily at wafer
Upper formation microgranule (particle), causes interconnection line short circuit or open circuit, has a strong impact on the performance of thin film.In target, field trash is the biggest
Part is to be formed in melting and casting process, is mainly made up of oxide, and therefore in target, the control of oxygen content seems particularly
Important.On the other hand, the performance of wafer is had a great impact by the crystallite dimension of target, along with the increase of target crystalline grains size,
Film deposition rate tends to reducing.In suitable grain size range, plasma impedance when target uses is relatively low, thin film
Sedimentation rate is high and film gauge uniformity is good.
Patent 1,2 discloses the preparation method of a kind of high purity nickel platinum alloy target, and high-temperature heating is relatively in melting for the method
Ni, Pt of low-purity forms the NiPt alloy that impurity content is relatively low, carries out horizontal controlling hot rolling alloy grain size simultaneously.Patent
The preparation method of high purity nickel platinum alloy target disclosed in 3, uses vacuum melting and vacuum electron beam Melting control alloy purity, adopts
With forge hot, hot rolling, cold rolling and process of thermal treatment processing alloy control alloy grain size.The high purity nickel platinum that above patent system is standby
Alloy target material, purity >=99.995%, Si ＜ 1ppm, B ＜ 1ppm, Ca ＜ 0.05ppm, Al ＜ 0.05ppm, O ＜ 50ppm,；Brilliant
Particle size ＜ 100 μm.And it practice, alkali metal ion (Na+、K+) and the content of radioelement (U, Th) to semiconductor device
The impact of performance is the biggest, and the patent found at present does not has the research of this aspect, the most existing publication to prepare high purity nickel
The purity of platinum alloy target, oxygen content and crystallite dimension still have the space of improvement.
Based on present on problem, present inventors have proposed a kind of superelevation pure nickel platinum target and preparation method thereof, the party
Method includes prepared by high-purity prealloy, the melting of alloy, uses the zone refining purification to melt, and mechanical press and heat treatment are to crystalline substance
The control of particle size.Use the purity chloroplatinic acid ammonia more than or equal to 99.995% and the purity Nickel dichloride. more than or equal to 99.99%
Using the method for reaction-sintered to prepare high purity nickel platinum prealloy for raw material, then vacuum induction melting obtains nickel platinum mother conjunction
Gold, finally uses zone melting method to be purified by nickel platinum master alloy ingot and obtains superelevation pure nickel platinum alloy.The method not only ensures preparation
The alkali metal ion (Na, K) of the superelevation pure nickel platinum alloy obtained, radioelement (U, Th) content relatively low, and other is golden
Belong to impurity, oxygen content and the more existing open source literature of crystallite dimension to have clear improvement.
(patent 1Hui Jun, Li ShinHua, Long David, etal [P] .European patent:
EP2025768A1,2009-02-18；
Patent 2J. favour, Li Xinhua, D. bright grade [P]. Chinese patent, ZL101353732A, 2009-01-28.
Patent 3 Shao Ling, Wang Guangxin, Zhao Xueyi [P]. Chinese patent, ZL104018120A, 2014-09-03.)
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of superelevation pure nickel platinum target, the method includes high-purity prealloy
Prepared by powder, the melting of alloy, uses the zone refining purification to melt, mechanical press and the heat treatment control to crystallite dimension.
Using the purity chloroplatinic acid ammonia more than or equal to 99.995% and the purity Nickel dichloride. more than or equal to 99.99% is raw material, first passes through
Gas atomization prepares the composite particles of chloroplatinic acid ammonia and Nickel dichloride., the more logical hydrogen reduction method of employing obtains high purity nickel platinum and closes in advance
Bronze end, then vacuum induction melting obtains nickel platinum foundry alloy, finally uses zone melting method to be purified by nickel platinum master alloy ingot
To superelevation pure nickel platinum alloy.
The alkali metal ion (Na, K) of high purity nickel platinum alloy that the method not only ensures to prepare, radioelement (U,
Th) content is relatively low, and the more existing open source literature of other metal impurities, oxygen content and crystallite dimension has clear improvement.There is provided
A kind of CoCrPt-oxide alloy target and preparation method thereof, described sputtering target, objectionable impurities constituent content is low, crystallite dimension
Fine uniform, chemical analysis is uniformly and deviation nominal composition is less.
Another object of the present invention is to provide a kind of high purity nickel platinum target making and preparing in aforementioned manners, this nickel platinum
Alloy purity is more than or equal to 99.995%, Na content ＜ 0.1ppm, K content ＜ 0.2ppm, U content ＜ 0.5ppm, Th content ＜
0.5ppm, Si content ＜ 0.5ppm, B content ＜ 0.1ppm, Ca content ＜ 0.01ppm, Al content ＜ 0.1ppm, oxygen content is less than
50ppm, crystallite dimension is less than 80 microns.
The preparation method of the superelevation pure nickel platinum alloy target that first mesh of the present invention is provided, comprises the steps:
A () high purity nickel platinum pre-alloyed powder preparation process is as follows, (1) chloroplatinic acid ammonia and the preparation of nickel chloride solution: with pure
Spending the chloroplatinic acid ammonia more than or equal to 99.995% and the purity Nickel dichloride. more than or equal to 99.99% is raw material, the atomic ratio of Ni:Pt
Example controls in the range of 99:1 to 60:40, is dissolved in deionized water, magnetic agitation 1-3h, makes both mix homogeneously systems
Obtain chloroplatinic acid ammonia and the solution of Nickel dichloride.；(2) gas atomization is dried: with the solution of chloroplatinic acid ammonia and Nickel dichloride. as raw material, uses
Spray drying method, control flow quantity be 6.0～11.0ml/min, atomization air pressure is 0.5～0.9MPa, inlet temperature be 200～
300 DEG C, hot air flow amount is 8.0～20.0L/min, prepare chloroplatinic acid ammonia and Nickel dichloride. Particles dispersed powder；(3) logical
Hydrogen reduction: by chloroplatinic acid ammonia and Nickel dichloride. Particles dispersed powder be placed in logical hydrogen reduction furnace, control H2Flow be 15.0～
24.0ml/min, temperature controls at 600～1000 DEG C, is incubated 3～6h, prepares high purity nickel platinum pre-alloyed powder.
B nickel platinum prealloy is placed in high purity aluminium oxide crucible by (), vacuum induction melting vacuum is better than 5x10-2Pa, casting
Temperature is in the range of 1500 DEG C～1750 DEG C.Mold is graphite jig high-purity, highdensity, graphite jig surface of internal cavity spraying nitrogen
Change boron coating and prevent the rising of carbon content in melt.
C () uses zone refining liquid metal cooling directional solidification (ZMLMC) purification to melt, detailed process is as follows,
After cleaning nickel platinum foundry alloy with acetone, it is put into high-purity Al2O3In skittele pot, put into homemade liquid metal cooled region
Melting apparatus for directional solidification.After being evacuated to 2～6Pa, reversely charging enters 0.04MPa argon shield, heats up and foundry alloy is carried out region
Melting directional solidification, during district is molten, cooling medium selects Ga-In-Sn liquid alloy, zone refining melting zone rate travel 60-
600 μm/s, melting zone width is 10～15mm, and zone refining number of times is 3-6 time, and melt temperature controls at 1500 DEG C～1700 DEG C of models
In enclosing.This process makes other metal impurities in foundry alloy assemble to foundry alloy one end, finally removes the part of accumulation of impurities,
To superelevation pure nickel platinum alloy.
D described superelevation pure nickel platinum alloy ingot is carried out mechanical press by (), mechanical press is cold rolling after first hot rolling, rolling direction
Alternately rolling to horizontal including level, hot rolling is rolled temperature and is controlled in the range of 900 DEG C～1200 DEG C.Hot rolling level is to rolling
Total deformation controls in the range of the 25%～35% of ingot blank thickness, and cross rolling total deformation controls at ingot blank thickness
In the range of 45%～55%.Cold rolling level controls in the range of the 5%～15% of ingot blank thickness to rolling total deformation, horizontal
Control in the range of the 25%～35% of ingot blank thickness to rolling total deformation.Rolling pass maximum deformation quantity controls at ingot blank
In the range of the 10%～20% of thickness；
E superelevation pure nickel platinum alloy after mechanical press is carried out annealing recrystallization process in the range of 650-800 DEG C by (), protect
After the temperature time is 2～4h, naturally cool to room temperature.Obtain the crystallite dimension superelevation pure nickel platinum alloy target blanks less than 80 μm；
F () carries out machining to described superelevation pure nickel platinum alloy target blanks, prepare described superelevation pure nickel platinum alloy
Target.
The present invention is by using high-purity prealloy to prepare, and vacuum melting and zone melting method combine and control alloy purity, adopt
With hot rolling, cold rolling direction and the adjustment of deflection, process of thermal treatment is coordinated to control alloy grain size.Prepare one
Superelevation pure nickel platinum alloy target, the alkali metal ion (Na, K) of this target, radioelement (U, Th) content relatively low, Er Qieqi
The more existing open source literature of its metal impurities, oxygen content and crystallite dimension has clear improvement.
Table 1 is the impurities analysis result of high purity nickel platinum alloy target.
Accompanying drawing explanation
Fig. 1 is the metallograph of the embodiment of the present invention 1 high purity nickel platinum alloy target；
Fig. 2 is the metallograph of the embodiment of the present invention 2 high purity nickel platinum alloy target；
Fig. 3 is the metallograph of comparative example high purity nickel platinum alloy target.
Detailed description of the invention
The present invention is further illustrated below in conjunction with the accompanying drawings, but is any limitation as the present invention never in any form, base
In present invention teach that any change or improvement made, belong to protection scope of the present invention.
The preparation method of the superelevation pure nickel platinum alloy target of the present invention, prepares including high-purity prealloy powder, the melting of alloy,
Use the zone refining purification to melt, mechanical press and the heat treatment control to crystallite dimension, it is characterised in that: described high-purity
The Nickel dichloride. that nickel platinum alloy powders uses the purity chloroplatinic acid ammonia more than or equal to 99.995% and purity to be more than or equal to 99.99% is
Raw material, first passes through gas atomization and prepares the composite particles of chloroplatinic acid ammonia and Nickel dichloride., then use logical hydrogen reduction method to obtain
High purity nickel platinum pre-alloyed powder, then vacuum induction melting obtains nickel platinum foundry alloy, finally uses zone melting method that nickel platinum is female
Alloy pig purifies and obtains superelevation pure nickel platinum alloy.
High purity nickel platinum pre-alloyed powder preparation process is as follows, (1) chloroplatinic acid ammonia and the preparation of nickel chloride solution: use purity
Chloroplatinic acid ammonia and the purity Nickel dichloride. more than or equal to 99.99% more than or equal to 99.995% are raw material, the atomic ratio of Ni:Pt
Control in the range of 99:1 to 60:40, be dissolved in deionized water, magnetic agitation 1-3h, make both mix homogeneously prepare
Chloroplatinic acid ammonia and the solution of Nickel dichloride.；(2) gas atomization is dried: with the solution of chloroplatinic acid ammonia and Nickel dichloride. as raw material, uses spray
Mist seasoning, controlling flow quantity is 6.0～11.0ml/min, and atomization air pressure is 0.5～0.9MPa, and inlet temperature is 200～300
DEG C, hot air flow amount is 8.0～20.0L/min, prepare chloroplatinic acid ammonia and Nickel dichloride. Particles dispersed powder；(3) logical hydrogen is also
Former: by chloroplatinic acid ammonia and Nickel dichloride. Particles dispersed powder be placed in logical hydrogen reduction furnace, control H2Flow is 15.0～24.0ml/
Min, temperature controls at 600～1000 DEG C, is incubated 3～6h, prepares high purity nickel platinum pre-alloyed powder.
The fusion process of alloy is as follows, and nickel platinum prealloy is placed in high purity aluminium oxide crucible, vacuum induction melting vacuum
It is better than 5x10-2Pa, cast temperature is in the range of 1500 DEG C～1750 DEG C.Mold is graphite jig high-purity, highdensity, graphite mo(u)ld
Tool surface of internal cavity spraying boron nitride coating prevents the rising of carbon content in melt.
Using zone refining liquid metal cooling directional solidification (ZMLMC) purification to melt, detailed process is as follows, with third
After ketone cleans nickel platinum foundry alloy, it is put into high-purity Al2O3In skittele pot, put into homemade liquid metal cooled region melting
Apparatus for directional solidification.After being evacuated to 2～6Pa, reversely charging enters 0.04MPa argon shield, heats up and foundry alloy is carried out zone refining
Directional solidification, makes other metal impurities in foundry alloy assemble to foundry alloy one end, finally removes the part of accumulation of impurities, obtain
Superelevation pure nickel platinum alloy.
During zone refining liquid metal cooling directional solidification, cooling medium selects Ga-In-Sn liquid alloy, region
Melting melting zone rate travel 60-600 μm/s, melting zone width is 10～15mm, and zone refining number of times is 3-6 time.Melt temperature control
System is in the range of 1500 DEG C～1700 DEG C.
Preparation method according to claim 1, it is characterised in that: mechanical press is cold rolling after first hot rolling, rolling side
To including that level alternately rolls to horizontal, hot rolling is rolled temperature and is controlled in the range of 900 DEG C～1200 DEG C.
Hot rolling level controls in the range of the 25%～35% of ingot blank thickness to rolling total deformation, and cross rolling is total
Deformation amount controlling is in the range of the 45%～55% of ingot blank thickness.Cold rolling level controls at ingot blank thickness to rolling total deformation
5%～15% in the range of, cross rolling total deformation controls in the range of the 25%～35% of ingot blank thickness.Rolling road
Secondary maximum deformation quantity controls in the range of the 10%～20% of ingot blank thickness；
Superelevation pure nickel platinum alloy carries out annealing recrystallization process in the range of 650-800 DEG C, after temperature retention time is 2～4h,
Naturally cool to room temperature.
The nickel platinum alloy purity of the superelevation pure nickel platinum alloy target of the present invention is more than or equal to 99.995%, Na content ＜
0.1ppm, K content ＜ 0.2ppm, U content ＜ 0.5ppm, Th content ＜ 0.5ppm, Si content ＜ 0.5ppm, B content ＜
0.1ppm, Ca content ＜ 0.01ppm, Al content ＜ 0.1ppm, oxygen content is less than 50ppm, and crystallite dimension is less than 80 microns.
Heretofore described high purity nickel platinum alloy target and preparation method thereof is specifically described.
Embodiment 1
High purity nickel platinum alloy target of the present invention is made by the steps:
(a) with purity more than or equal to 99.995% chloroplatinic acid ammonia and purity more than or equal to 99.99% Nickel dichloride. be former
Material, the atomic ratio of Ni:Pt controls at 73:26, is dissolved in deionized water, magnetic agitation 3h, makes both mix homogeneously systems
Obtain chloroplatinic acid ammonia and the solution of Nickel dichloride.；Then with the solution of chloroplatinic acid ammonia and Nickel dichloride. as raw material, spray drying method, control are used
Flow quantity processed is 8.0ml/min, and atomization air pressure is 0.7MPa, and inlet temperature is 220 DEG C, and hot air flow amount is 10.0L/min,
Prepare chloroplatinic acid ammonia and Nickel dichloride. Particles dispersed powder；Finally by chloroplatinic acid ammonia and Nickel dichloride. Particles dispersed powder be placed in logical
In hydrogen reduction furnace, control H2Flow is 18.0ml/min, and temperature controls at 800 DEG C, is incubated 4h, prepares high purity nickel platinum prealloy powder
End.
B nickel platinum prealloy powder is placed in high purity aluminium oxide crucible by (), vacuum induction melting vacuum is better than 5x10-2Pa, waters
Casting temperature is in the range of 1500 DEG C ± 50 DEG C.Mold is graphite jig high-purity, highdensity, graphite jig surface of internal cavity spraying nitrogen
Change boron coating and prevent the rising of carbon content in melt.
C () uses zone refining liquid metal cooling directional solidification (ZMLMC) purification to melt, detailed process is as follows,
After cleaning nickel platinum foundry alloy with acetone, it is put into high-purity Al2O3In skittele pot, put into homemade liquid metal cooled region
Melting apparatus for directional solidification.After being evacuated to 2～6Pa, reversely charging enters 0.04MPa argon shield, heats up and foundry alloy is carried out region
Melting directional solidification, during district is molten, cooling medium selects Ga-In-Sn liquid alloy, zone refining melting zone rate travel 200 μ
M/s, melting zone width is 13mm, and zone refining number of times is 4 times, and melt temperature controls in the range of 1500 DEG C ± 50 DEG C.This process
Make other metal impurities in foundry alloy assemble to foundry alloy one end, finally remove the part of accumulation of impurities, obtain superelevation pure nickel
Platinum alloy.
D described superelevation pure nickel platinum alloy ingot is carried out mechanical press by (), mechanical press is cold rolling after first hot rolling, rolling direction
Alternately rolling to horizontal including level, hot rolling is rolled temperature and is controlled in the range of 1100 DEG C.Hot rolling level is to rolling total deformation
Amount control in the range of the 30% ± 5 of ingot blank thickness, cross rolling total deformation control ingot blank thickness 45% ± 5 model
In enclosing.Cold rolling level controls in the range of the 9% ± 5 of ingot blank thickness to rolling total deformation, cross rolling total deformation control
System is in the range of the 25% ± 5 of ingot blank thickness.Rolling pass maximum deformation quantity controls 10% ± 5 scope at ingot blank thickness
In；
E superelevation pure nickel platinum alloy after mechanical press is carried out annealing recrystallization process in the range of 700 ± 50 DEG C by (), protect
After the temperature time is 3h, naturally cool to room temperature.Obtain the crystallite dimension superelevation pure nickel platinum alloy target blanks less than 80 μm；
F () carries out machining to described superelevation pure nickel platinum alloy target blanks, prepare described superelevation pure nickel platinum alloy
Target.
Embodiment 2
Difference from Example 1 is that the atomic ratio of described high purity nickel platinum alloy target Ni:Pt is 25:75.Described
The zone-melting melt temperature of foundry alloy controls in the range of 1600 ± 50 DEG C.
Comparative example 1
Difference from Example 1 be provided without purity more than or equal to 99.995% chloroplatinic acid ammonia and purity be more than or equal to
The Nickel dichloride. of 99.99% is raw material, prepares high purity nickel platinum prealloy powder by the method for gas atomization, is provided without district simultaneously
Described nickel platinum master alloy ingot zone-refine is become superelevation pure nickel platinum to close by territory melting liquid metal cooling directional solidification (ZMLMC) method
Ingot.The purity nickel more than or equal to 99.99% and the purity platinum more than or equal to 99.995% is simply used to carry out very as raw material
Empty induction melting, the step (a) not i.e. being prepared in method and (c).During mechanical press, hot rolling and cold rolling all use water
Square to rolling.
The impurities analysis result of table 1 high purity nickel platinum alloy target
Claims (10)
1. a superelevation pure nickel platinum alloy target, it is characterised in that: described nickel platinum alloy purity is more than or equal to 99.995%, Na
Content ＜ 0.1ppm, K content ＜ 0.2ppm, U content ＜ 0.5ppm, Th content ＜ 0.5ppm, Si content ＜ 0.5ppm, B content
＜ 0.1ppm, Ca content ＜ 0.01ppm, Al content ＜ 0.1ppm, oxygen content is less than 50ppm, and crystallite dimension is less than 80 microns.
2. a preparation method for superelevation pure nickel platinum alloy target, prepares including superelevation pure nickel platinum prealloy powder, the melting of alloy,
Use the zone refining purification to melt, mechanical press and the heat treatment control to crystallite dimension, it is characterised in that: described high-purity
The Nickel dichloride. that nickel platinum alloy powders uses the purity chloroplatinic acid ammonia more than or equal to 99.995% and purity to be more than or equal to 99.99% is
Raw material, first passes through gas atomization and prepares the composite particles of chloroplatinic acid ammonia and Nickel dichloride., then use logical hydrogen reduction method to obtain
High purity nickel platinum pre-alloyed powder, then vacuum induction melting obtains nickel platinum foundry alloy, finally uses zone melting method that nickel platinum is female
Alloy pig purifies and obtains superelevation pure nickel platinum alloy.
Preparation method the most according to claim 2, it is characterised in that: described superelevation pure nickel platinum pre-alloyed powder preparation process
As follows:
(1) chloroplatinic acid ammonia and the preparation of nickel chloride solution: with purity more than or equal to 99.995% chloroplatinic acid ammonia and purity be more than
Nickel dichloride. equal to 99.99% is raw material, and the atomic ratio of Ni:Pt controls, in the range of 99:1 to 60:40, to be dissolved in
In ionized water, magnetic agitation 1-3h, make both mix homogeneously prepare the solution of chloroplatinic acid ammonia and Nickel dichloride.；
(2) gas atomization is dried: with the solution of chloroplatinic acid ammonia and Nickel dichloride. as raw material, uses spray drying method, controls flow quantity
Being 6.0～11.0ml/min, atomization air pressure is 0.5～0.9MPa, and inlet temperature is 200～300 DEG C, and hot air flow amount is
8.0～20.0L/min, prepare chloroplatinic acid ammonia and Nickel dichloride. Particles dispersed powder；
(3) logical hydrogen reduction: by chloroplatinic acid ammonia and Nickel dichloride. Particles dispersed powder be placed in logical hydrogen reduction furnace, control H2Flow is
15.0～24.0ml/min, temperature controls at 600～1000 DEG C, is incubated 3～6h, prepares superelevation pure nickel platinum pre-alloyed powder.
Preparation method the most according to claim 2, it is characterised in that: the fusion process of described alloy is as follows, by pre-for nickel platinum
Alloyed powder is placed in high purity aluminium oxide crucible, and vacuum induction melting vacuum is better than 5x10-2Pa, cast temperature is at 1500 DEG C～1750
In the range of DEG C, mold is graphite jig high-purity, highdensity, and graphite jig surface of internal cavity spraying boron nitride coating prevents in melt
The rising of carbon content.
5. according to the preparation method described in claim 2, it is characterised in that: described employing zone refining liquid metal cooling orientation is solidifying
Admittedly the i.e. ZMLMC purification to melt, detailed process is as follows, after cleaning nickel platinum foundry alloy with acetone, is put into high-purity Al2O3Post
In shape crucible, put into homemade liquid metal cooled region melting apparatus for directional solidification.After being evacuated to 2～6Pa, reversely charging enters
0.04MPa argon shield, heats up and foundry alloy is carried out zone refining directional solidification, make other metal impurities in foundry alloy assemble
To foundry alloy one end, finally remove the part of accumulation of impurities, obtain superelevation pure nickel platinum alloy.
Preparation method the most according to claim 2, it is characterised in that: zone refining liquid metal cooling directional solidification process
In, cooling medium select Ga-In-Sn liquid alloy, zone refining melting zone rate travel 60-600 μm/s, melting zone width be 10～
15mm, zone refining number of times is 3-6 time, and melt temperature controls in the range of 1500 DEG C～1700 DEG C.
Preparation method the most according to claim 2, it is characterised in that: mechanical press is cold rolling after first hot rolling, rolling direction
Alternately rolling to horizontal including level, hot rolling is rolled temperature and is controlled in the range of 900 DEG C～1200 DEG C.
Preparation method the most according to claim 7, it is characterised in that: hot rolling level controls at ingot blank to rolling total deformation
In the range of the 25%～35% of thickness, cross rolling total deformation controls in the range of the 45%～55% of ingot blank thickness,
Cold rolling level controls in the range of the 5%～15% of ingot blank thickness to rolling total deformation, and cross rolling total deformation controls
In the range of the 25%～35% of ingot blank thickness, rolling pass maximum deformation quantity controls 10%～20% model at ingot blank thickness
In enclosing.
Preparation method the most according to claim 2, it is characterised in that: superelevation pure nickel platinum alloy is in the range of 650-800 DEG C
Carry out annealing recrystallization process, after temperature retention time is 2～4h, naturally cool to room temperature.
Preparation method the most according to claim 2, it is characterised in that: it is characterized in that: described nickel platinum alloy purity is big
In equal to 99.995%, Na content ＜ 0.1ppm, K content ＜ 0.2ppm, U content ＜ 0.5ppm, Th content ＜ 0.5ppm, Si contain
Amount ＜ 0.5ppm, B content ＜ 0.1ppm, Ca content ＜ 0.01ppm, Al content ＜ 0.1ppm, oxygen content is less than 50ppm, crystal grain
It is smaller in size than 80 microns.
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| CN113278935A (en) * | 2021-05-07 | 2021-08-20 | 昆明贵研新材料科技有限公司 | Platinum oxide electrode and preparation method and application thereof |
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