CN110421158A - A kind of production method of hypoxemia molybdenum niobium alloy target - Google Patents
A kind of production method of hypoxemia molybdenum niobium alloy target Download PDFInfo
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- CN110421158A CN110421158A CN201910668959.5A CN201910668959A CN110421158A CN 110421158 A CN110421158 A CN 110421158A CN 201910668959 A CN201910668959 A CN 201910668959A CN 110421158 A CN110421158 A CN 110421158A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- 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
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
- B22F3/101—Changing atmosphere
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B22F3/10—Sintering only
- B22F3/1039—Sintering only by reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B22F3/15—Hot isostatic pressing
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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
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- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
Abstract
The invention discloses a kind of methods for producing hypoxemia molybdenum niobium alloy target, comprising the following steps: 1, molybdenum powder is placed in vacuum sintering furnace is heat-treated;2, niobium metal powder and alkali halide MX are uniformly mixed to get mixed powder;3, molybdenum powder obtained in step 1 is put into V-type batch mixer with the mixed powder that step 2 obtains and is mixed, is put into after gum cover through isostatic cool pressing compression moulding;4, briquetting is placed in the dual-purpose sintering furnace of vacuum-hydrogen and is heat-treated.Compared with the existing technology, this method deoxygenation is at low cost by the present invention, and effect is good, and gained molybdenum niobium alloy target impurity, oxygen content are low, has excellent performance.
Description
Technical field
The invention belongs to metallurgical material technical fields, specifically design a kind of production method of hypoxemia molybdenum niobium alloy sputtering target material
Background technique
Due to its high-melting-point, high conductance and excellent corrosion resistance, molybdenum niobium alloy is widely used in thin film transistor (TFT)
Electrode deposition layer, touch screen contact layer.However, oxygen content excessively high in molybdenum niobium alloy then will lead to the generation of oxide.
On the one hand, this oxide, which can make target generate arcing effect in sputtering process, leads to local melting to influence sputtering vapor deposition
Effect.On the other hand, oxide is concentrated mainly on the interface of molybdenum niobium, to reduce the processability of molybdenum niobium target.Therefore,
The overall oxygen content of molybdenum niobium target is reduced, the especially oxygen content of interface is most important to the production of molybdenum niobium target.
At present there are mainly two types of the methods of production molybdenum niobium alloy target.
A kind of method is the method by pressureless sintering, i.e., first by molybdenum niobium mixed powder by after cold isostatic compaction, In
High temperature sintering is carried out under atmospheric pressure.This method can be divided into two methods of nitrogen atmosphere sintering and vacuum-sintering again.The former is by molybdenum
Niobium is placed in hydrogen and is sintered, although this method is conducive to exclude the impurity in alloy, but since metal niobium largely inhales hydrogen, burns
Tying base density can lower and easy cracking;The method that the latter thus uses heating in vacuum to be sintered, this method relative hydrogen sintering
Avoid the problem of niobium inhales hydrogen.But in order to reach enough density, when both sintering inevitable demand high temperature of method are long
Between keep the temperature: the mutual diffusion of molybdenum niobium is more serious during this, and the niobium in final product exists in the form of substitution solid solution
In molybdenum, processing performance is greatly reduced.
Another method is the method, such as patent " JP200232726A " etc. of hot isostatic pressing (HIP) sintering.This method
It is suppressed by mixing to be placed in jacket molybdenum powder and niobium powder, the closely knit of molybdenum niobium target is completed under conditions of relative low temperature.
However in the production process of this method, impurity is difficult to be completely exhausted out, and especially oxygen content is difficult to control.
To solve the above-mentioned problems, Japan Patent " JP2008280570A " proposes on the basis of HIP sintering
A method of reducing oxygen content.Its process, including crushed again after molybdenum powder is sintered first, it is then right in a reducing atmosphere
Molybdenum powder is restored, and wherein oxygen content will be reduced to 100ppm or less.Later, the molybdenum powder after reduction is mixed with niobium powder to progress again
Hot isostatic pressing is suppressed to obtain molybdenum niobium target.Oxygen content can be dropped to 500ppm hereinafter, but have a disadvantage in that needing by this method
Two-step sintering is wanted, and the hypoxemia molybdenum powder after first sintering is oxidized easily in mixed process later, to allow final oxygen
Content is difficult to control.
Patent " AT15356U1 " is by increasing and sintered ingot existing after hot isostatic pressing molybdenum niobium mixed powder reaches closely knit
The step for being heat-treated under 1550 DEG C or so of nitrogen atmosphere, to reduce the whole oxygen content of molybdenum niobium alloy.However this method
The shortcomings that be, on the one hand the heat treatment in this way under high temperature can promote that counterdiffusion occurs between molybdenum niobium, to reduce its processability
Energy;On the other hand, there is stronger compatibility to oxygen due to niobium, the reduction oxygen content effect of this method is relatively limited.
For another example Patent No.: " CN201510938945.2 " provides a kind of preparation method of molybdenum niobium alloy sputtering target material,
Characterized by comprising the following steps: Step 1: molybdenum powder and niobium powder are placed in the mixing tank of batch mixer, by the mixing tank
It is vacuumized after sealing, then the molybdenum powder and niobium powder is uniformly mixed under the protection of argon gas, obtain mixed-powder;Institute
The mass ratio for stating molybdenum powder and niobium powder is (9~19): 1;Step 2: carrying out isostatic cool pressing to mixed-powder described in step 1, obtain
To slab, the slab is then subjected to pre-sintering processing under the conditions of vacuum or hydrogen atmosphere protection, obtains molybdenum niobium alloy
Preform;The pressure of the isostatic cool pressing is 100MPa~200MPa, and the dwell time is 5min~10min, the pre-sintering
The detailed process of processing are as follows: be warming up to 800 DEG C~1000 DEG C guarantors under conditions of heating rate is 2.5 DEG C/min~4 DEG C/min
Then warm 60min~120min is warming up to 1200 DEG C~1500 under conditions of heating rate is 1 DEG C/min~2.5 DEG C/min
DEG C heat preservation 120min~180min, then heating rate be 1 DEG C/min~2.5 DEG C/min under conditions of be warming up to 1600 DEG C~
1700 DEG C of heat preservation 120min~180min;Step 2: by the preform of molybdenum niobium alloy described in step 2 turn-milling cutting to its table
Surface roughness is 1.0 μm~3.0 μm, then carries out hot isostatic pressing to the molybdenum niobium alloy preform after turn-milling cutting, obtains molybdenum
Niobium alloy product;The pressure of the hot isostatic pressing is 100MPa~200MPa, and temperature is 1200 DEG C~1500 DEG C, when heat-insulation pressure keeping
Between be 1h~5h;Step 4: carrying out machining and surface grinding to the product of molybdenum niobium alloy described in step 3, molybdenum is obtained
Niobium alloy sputtering target material.It is the step for being heat-treated under a hydrogen atmosphere to reduce equally with patent " AT15356U1 "
The whole oxygen content of molybdenum niobium alloy.However the shortcomings that this method, is, on the one hand the heat treatment in this way under high temperature can promote molybdenum
Counterdiffusion occurs between niobium, to reduce its processing performance;On the other hand, there are stronger compatibility, this side to oxygen due to niobium
The reduction oxygen content effect of method is relatively limited.
Summary of the invention
To solve the above-mentioned problems, the purpose of the present invention is to provide a kind of methods for producing hypoxemia molybdenum niobium alloy target.
Relative to presently, there are method, this method deoxygenation is at low cost, and effect is good, and gained molybdenum niobium alloy target impurity, oxygen content are low, property
It can be excellent.
Its technical solution are as follows:
A kind of production method of hypoxemia molybdenum niobium target, comprising the following steps:
Step 1: molybdenum powder being placed in vacuum sintering furnace and is heat-treated, and treatment temperature is 1000-1300 DEG C, and the time is
0.5-6h;
Step 2: niobium metal powder and alkali halide MX are uniformly mixed to get mixed powder;
Step 2: molybdenum powder obtained in step 1 is put into V-type batch mixer with the mixed powder that step 2 obtains and is mixed, is put
Pass through isostatic cool pressing compression moulding after entering gum cover;
Step 4: briquetting is placed in the dual-purpose sintering furnace of vacuum-hydrogen and is heat-treated, is specifically included:
1. being heat-treated under 350~1200 DEG C of reproducibilities or inert atmosphere, heat treatment time 0.5-6h;
2. heat treatment is under 1200 DEG C~1500 DEG C vacuum to remove remaining alkali halide and hydrogen, according to vacuum pump
Pumping speed it is different, which is 1~6h;
Step 5: the briquetting after removal of impurities is suppressed by hot isostatic pressing, press temperature is 1300-1500 DEG C, and pressure is greater than
100MPa, 3~6h of pressing time;
Step 6: calendering and machining obtain the sputtering target material of required size, after obtaining molybdenum niobium sintered ingot, to it
Calendering processing is carried out, in the case where rolling, rolling temperature is 500-1500 DEG C, every task ratio 10-30%.
Further, in step 1, the oxygen content in molybdenum powder, then step 4 are reduced first to reduce in niobium powder after mixing
Oxygen content.
Further, step 1. in, the reproducibility is hydrogen, and it is broken to absorb hydrogen expander for niobium powder under a hydrogen atmosphere,
Surface area increases, and oxygen therein is more easy to remove.
Further, in step 4, after niobium metal powder is mixed with alkali halide MX, under hot conditions, part niobium
The niobium oxide of metal powder surface reacts with alkali halide MX, and reaction equation is as follows:
It is discharged system quickly in the gas among the above, reacting generation, chemical balance is mobile to reaction right, to promote
Reaction constantly carries out.
Further, the alkali halide MX is one or more of lithium, sodium, the halide of potassium.
Further, it in step 4, before hot isostatic pressing compacting, needs to be evacuated briquetting, be removed with reaching
Go the effect of adsorption impurity and gas.
Further, in step 1, the hypoxemia niobium metal Powder Particle Size is 5-300 μm;
Preferably, the granularity of niobium powder is 100-300 μm.
Further, in step 2, the molybdenum powder granularity is greater than 3 μm;
Preferably, molybdenum powder granularity is greater than 5 μm.
Further, when the hypoxemia niobium metal powder is mixed with alkali halide MX, liquid phase is including but not limited to used
Mixed method mixes niobium powder with MX aqueous solution, reach uniformly mixed by being stirred continuously in heating evaporation moisture process
The purpose of conjunction, wherein the amount of required alkali halide is the content for slightly more than needing for oxygen to be completely exhausted out.
Further, step 1. in, the inert gas be argon gas.
Further, step 2. in, the pressure of vacuum condition is about 0.001Pa.
The invention has the benefit that
Technology path of the invention includes that powder pre-treating, material mixing, molding, heat treatment, hot isostatic pressing, calendering and machinery add
Work step is rapid.Pretreatment includes that the molybdenum powder of weight will be needed first to heat under vacuum.Mixing step includes that will need the niobium powder of weight
Or hydrogenation niobium powder is mixed with alkali halide, then by mixed powder and the molybdenum powder of weight is needed to be mixed and made into alloyed powder.After molding,
The heat treatment step includes first heating the oxygen removed in mixed powder at low temperature, and temperature is then risen to higher temperature in vacuum
The remaining alkali halide of lower removing;If back is heat-treated in hydrogen, vacuum also can reach the purpose of dehydrogenation at this time.
Obtained alloy pig is suppressed at high temperature later and obtains the higher green compact of density, by further rolling and machining obtains
The sputtering target material of required size.
It is reacted present invention utilizes existing between alkali halide MX and niobium oxide:
Since the halide boiling point of niobium is lower, the gas for reacting generation is discharged system quickly, and chemical balance is right to reaction
Fang Yidong, to promote to react continuous progress.
It is using the reason of alkali halide, the vapour pressure of alkali metal oxide at high temperature is relatively high, true
It is easily drained, and these alkali metal oxides do not react with niobium, will not be dissolved in niobium under empty condition.
Since present invention aims at reduction oxygen contents, thus oxygen removal process must carry out under protective atmosphere;Relatively
In directly reacting under vacuum, in the case that hydrogen or inert gas there are, the holding time is more in atmosphere for alkali halide
It is long, it is more complete so as to allow reaction to carry out;Reaction more preferably carries out under a hydrogen atmosphere, this is because niobium powder absorbs hydrogen expander
Broken, surface area increases, and oxygen therein is more easy to remove.The first step of heat treatment is oxygen removal process, and temperature depends on used
The type of alkali metal, but 350 DEG C (boiling point of potassium oxide) can not be lower than.The preferred lithium of alkali halide, sodium, potassium halide,
Because the halide relative cost of rubidium and caesium is higher.This process duration is 0.5-6h, and length of time depends on this mistake
The carry out temperature of journey.After oxygen removal process, second step is to be evaporated under vacuum to remove alkali halide.This process
Temperature is 1200-1500 DEG C, time 1-6h.If being lower than 1200 DEG C, the evaporation rate of alkali halide is excessively slow;If being higher than
1500 DEG C, then the diffusion between molybdenum and niobium is accelerated, and can generate the displaced type solid solution of poor processability.If the time is less than 1h,
It is difficult to that alkali halide is all discharged;If overlong time, displaced type solid solution can be generated.
Specific embodiment
The concrete technology scheme that the present invention uses is as follows:
Molybdenum powder (oxygen content 500ppm or so) is put and carries out heat pre-treatment in a vacuum furnace by step 1.Treatment temperature
1000-1300 DEG C, time 0.5-6h, vacuum pressure is about 0.001Pa.Molybdenum powder granularity is greater than 3 μm, it is preferable that molybdenum powder granularity is big
In 5 μm.
Step 2 mixes niobium metal powder (oxygen content 2000ppm or so) with alkali halide MX.Due to alkali metal halogen
Solubility is higher in water by compound MX, uniformly mixed in order to achieve the effect that, the method for mixed method preferred liquid phase mixing.It is a kind of
Possible method is to mix niobium powder with MX aqueous solution, reaches uniform mixing by being stirred continuously in heating evaporation moisture process
Purpose.The amount of required alkali halide is the content for slightly more than needing for oxygen to be completely exhausted out.After mixing completely, by mixed powder
It is put into V-type batch mixer and mixes with molybdenum powder.In this step, niobium powder granularity is 5-300 μm;Preferably, the granularity of niobium powder is 100-
300μm。
Mixed powder is put into after gum cover through isostatic cool pressing compression moulding by step 3.Pressure is 100-200MPa, when pressure maintaining
Between 5-10min.
Briquetting is placed in the dual-purpose sintering furnace of vacuum-hydrogen and is heat-treated by step 4.Heat treatment includes two steps: first
Step be heat-treated under 350-1200 DEG C of reproducibility or inert atmosphere or vacuum, heat treatment time 0.5-6h, it is preferable to use
Reducing atmosphere or inert atmosphere;Second step is heat-treated under 1200 DEG C of -1500 DEG C of vacuum to remove remaining alkali halide
And hydrogen, different according to the pumping speed of vacuum pump, which is 1-6h.
Step 5 suppresses the briquetting after removal of impurities by hot isostatic pressing.Press temperature is 1300-1500 DEG C, and pressure is greater than
100MPa, pressing time 3-6h.If pressure is less than 100MPa or press temperature is too low or the pressing time is too short, green compact it is close
Degree is insufficient;If press temperature is excessively high or overlong time, with thousand, there are the risks that counterdiffusion causes processing performance to reduce.In addition,
It before hot isostatic pressing, needs to be evacuated briquetting, to have the function that remove adsorption impurity and gas.
Step 6 will also carry out calendering processing to it after obtaining molybdenum niobium sintered ingot.Because in sintered ingot there may be
Stomata, calendering can further increase the density of sintered ingot.In the case where rolling, rolling temperature is 500-1500 DEG C, every time
10-30% is compared in work.
In addition to above-mentioned embodiment, the present invention can also be obtained by following embodiment:
Embodiment one
The molybdenum powder that granularity is 6.8 μm is put and is pre-processed in a vacuum furnace.Pretreatment temperature is 1200 DEG C, when pretreatment
Between 3 hours.Take 6-20 μm of granularity of hydrogenation niobium powder (oxygen content 2000ppm) to mix with potassium chloride, then with pretreated molybdenum
Powder mixing, wherein Mo: NbH: KCl weight ratio is 100: 10: 1, after the compacting 5-10min molding of 150-250MPa isostatic cool pressing
Obtain briquetting.Briquetting is heat-treated in hydrogen vacuum dual-purpose furnace: first in a hydrogen atmosphere 400-550 DEG C heat preservation 2-5 hours,
It is warming up to 650-800 DEG C of heat preservation 1-3 hours later, then pumps hydrogen, in 1200-1450 DEG C, vacuum pressure 0.001-
It is heat-treated 3-4 hours under 0.01Pa, obtains the molybdenum niobium alloy ingot of density 70-80%.Again by alloy pig in 100-200MPa,
HIP sintering, dwell time 4-6 hour are carried out at 1300-1450 DEG C.Thus obtained molybdenum niobium sintered blank, then rolled through subsequent
System, machining obtain 99% or more density, and oxygen content is less than the molybdenum niobium alloy target of 400ppm.
Embodiment two
It takes 50-300 μm of granularity of niobium powder (oxygen content 1500ppm) to mix with the sodium chloride of mass fraction 1.2-1.6%, passes through
Briquetting is obtained after 150-250MPa isostatic cool pressing compression moulding.Briquetting is sintered in vacuum hydrogen dual-purpose stove, first in nitrogen atmosphere
Lower 600-800 DEG C of heat preservation 3-5 hours, hydrogen is then pumped, is warming up to 1500-1700 DEG C of heat preservation 2-5 hours, finally by temperature liter
To 1900-2100 DEG C heat preservation 3-6 hours, vacuumize rear unvented air pressure and be maintained at 0.001-0.01Pa, obtain density 92-
96%, oxygen content is less than the sintering niobium ingot of 200ppm.
Claims (11)
1. a kind of production method of hypoxemia molybdenum niobium target, which comprises the following steps:
Step 1: molybdenum powder being placed in vacuum sintering furnace and is heat-treated, and treatment temperature is 1000-1300 DEG C, time 0.5-
6h;
Step 2: niobium metal powder and alkali halide MX are uniformly mixed to get mixed powder;
Step 3: the mixed powder for obtaining molybdenum powder in step 1 with step 2 obtains is put into V-type batch mixer and is mixed, gum cover is put into
Pass through isostatic cool pressing compression moulding afterwards;
Step 4: briquetting is placed in the dual-purpose sintering furnace of vacuum-hydrogen and is heat-treated, is specifically included:
1. being heat-treated under 350~1200 DEG C of reproducibilities or inert atmosphere, heat treatment time 0.5-6h;
2. heat treatment is under 1200 DEG C~1500 DEG C vacuum to remove remaining alkali halide and hydrogen, according to the pumping of vacuum pump
Fast different, which is 1~6h;
Step 5: the briquetting after removal of impurities is suppressed by hot isostatic pressing, press temperature is 1300-1500 DEG C, and pressure is greater than
100MPa, 3~6h of pressing time;
Step 6: calendering and machining obtain the sputtering target material of required size, after obtaining molybdenum niobium sintered ingot, carry out to it
Calendering processing, in the case where rolling, rolling temperature is 500-1500 DEG C, every task ratio 10-30%.
2. production method according to claim 1, which is characterized in that in step 1, the oxygen content in molybdenum powder is first reduced,
Step 4 is again to reduce the oxygen content in niobium powder after mixing.
3. production method according to claim 1, which is characterized in that step 1. in, the reproducibility be hydrogen, in hydrogen
Niobium powder absorbs hydrogen expander and is crushed under atmosphere, and surface area increases, and oxygen therein is more easy to remove.
4. production method according to claim 1, which is characterized in that in step 4, niobium metal powder and alkali metal halogenation
After object MX mixing, at high temperature, niobium oxide and the alkali halide MX on niobium metal powder surface react, and reaction equation is as follows:
It is discharged system quickly in the gas among the above, reacting generation, chemical balance is mobile to reaction right, to promote to react
Constantly carry out.
5. production method according to claim 1 or 3, which is characterized in that the alkali halide MX is lithium, sodium, potassium
One or more of halide.
6. production method according to claim 1, which is characterized in that in step 4, before hot isostatic pressing compacting, need
Briquetting is evacuated, to have the function that remove adsorption impurity and gas.
7. production method according to claim 1, which is characterized in that in step 1, the niobium metal Powder Particle Size is 5-
300μm;
Preferably, the granularity of niobium powder is 100-300 μm.
8. production method according to claim 1, which is characterized in that in step 2, the molybdenum powder granularity is greater than 3 μm;
Preferably, molybdenum powder granularity is greater than 5 μm.
9. production method according to claim 1 or 3, which is characterized in that the hypoxemia niobium metal powder and alkali metal halogenation
When object MX is mixed, including but not limited to using the method for liquid phase mixing, i.e., niobium powder is mixed with MX aqueous solution, by being steamed in heating
It is stirred continuously during shampoo point and reaches mixed uniformly purpose, wherein the amount of required alkali halide is slightly more than to need
The content that oxygen is completely exhausted out.
10. production method according to claim 1, which is characterized in that step 1. in, the inert gas be argon gas.
11. production method according to claim 1, which is characterized in that step 2. in, the pressure of vacuum condition is about
0.001Pa。
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Cited By (5)
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CN111254306A (en) * | 2020-01-20 | 2020-06-09 | 郑州大学 | Preparation method of molybdenum-niobium alloy with low oxygen content |
CN114029484A (en) * | 2021-11-08 | 2022-02-11 | 宁波江丰电子材料股份有限公司 | Preparation method of tantalum-titanium alloy target material |
CN114799163A (en) * | 2022-04-02 | 2022-07-29 | 山东格美钨钼材料股份有限公司 | Low-oxygen molybdenum-niobium alloy target production line and technological process thereof |
CN115502403A (en) * | 2022-09-29 | 2022-12-23 | 宁波江丰电子材料股份有限公司 | Preparation method of large-size and high-density molybdenum target |
CN116813346A (en) * | 2023-08-17 | 2023-09-29 | 宁波江丰电子材料股份有限公司 | Preparation method and application of niobium oxide target |
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2019
- 2019-07-22 CN CN201910668959.5A patent/CN110421158A/en not_active Withdrawn
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111254306A (en) * | 2020-01-20 | 2020-06-09 | 郑州大学 | Preparation method of molybdenum-niobium alloy with low oxygen content |
CN111254306B (en) * | 2020-01-20 | 2021-04-16 | 郑州大学 | Preparation method of molybdenum-niobium alloy with low oxygen content |
CN114029484A (en) * | 2021-11-08 | 2022-02-11 | 宁波江丰电子材料股份有限公司 | Preparation method of tantalum-titanium alloy target material |
CN114029484B (en) * | 2021-11-08 | 2023-09-12 | 宁波江丰电子材料股份有限公司 | Preparation method of tantalum-titanium alloy target |
CN114799163A (en) * | 2022-04-02 | 2022-07-29 | 山东格美钨钼材料股份有限公司 | Low-oxygen molybdenum-niobium alloy target production line and technological process thereof |
CN115502403A (en) * | 2022-09-29 | 2022-12-23 | 宁波江丰电子材料股份有限公司 | Preparation method of large-size and high-density molybdenum target |
CN116813346A (en) * | 2023-08-17 | 2023-09-29 | 宁波江丰电子材料股份有限公司 | Preparation method and application of niobium oxide target |
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