CN106567047A - Method of preparing high-purity microstructure-controllable Mo-Nb alloy target material through hot-pressing process - Google Patents
Method of preparing high-purity microstructure-controllable Mo-Nb alloy target material through hot-pressing process Download PDFInfo
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- CN106567047A CN106567047A CN201610970257.9A CN201610970257A CN106567047A CN 106567047 A CN106567047 A CN 106567047A CN 201610970257 A CN201610970257 A CN 201610970257A CN 106567047 A CN106567047 A CN 106567047A
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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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention provides a method of preparing a high-purity microstructure-controllable Mo-Nb alloy target material through a hot-pressing process. Through the hot-pressing process, a high-compact Mo-Nb alloy sputtering target material is produced, wherein compactness is more than 99%. Through a boron nitride and graphite combined mould, carbon seepage phenomenon is effectively prevented, thereby producing high-compact high-purity microstructure-controllable Mo-Nb alloy target material, wherein sintering temperature is reduced and cost is reduced. Meanwhile, problems of low compactness, coarse structure of smelting casting, non-uniform ingredient and excessive high cost of hot isostatic pressing in a powder metallurgy process are solved.
Description
Technical field
The invention belongs to high temperature refractory target preparation field, and in particular to a kind of pressure sintering prepares high-purity microstructure
Controllable molybdenum niobium alloy target method.
Background technology
With the development of computer, DTV and various digital products, the consumption of liquid crystal display is significantly greatly increased.Wherein
Quality important of the vitals thin film transistor (TFT) to liquid crystal display, and as the molybdenum target of production thin film transistor (TFT)
Material directly determines the quality of thin film transistor (TFT).Molybdenum has excellent electrical conductance and heat stability, is widely used in electrode, cloth
Wire material and barrier material.Molybdenum-niobium alloy material is answered due to its excellent conductive capability, antioxygenic property and relatively low plated film
Power, is widely used as important target in the thin film transistor (TFT) of liquid crystal display.Generally, molybdenum niobium alloy sputtering target material
The preparation technology for being adopted includes：
Melting and casting method：Melting and casting method refers to the alloy raw material melting of certain ingredients proportioning, then alloy solution is poured into a mould
In mould, ingot casting is formed, it is finally machined to make target.Impurity content to ensure ingot casting is as low as possible, and one
As carry out melting and casting in a vacuum.But in casting process, inside material structure, there are certain hole, these holes unavoidably
The microgranule in sputter procedure can be caused to splash, so as to affect the quality of thin film.
Powder metallurgic method：For the preparation of molybdenum niobium alloy target, conventional powder metallurgical technique is included a certain amount of molybdenum
After powder and the mixing of niobium powder, Jing isostatic cool pressings, vacuum-sintering obtain molybdenum niobium alloy target.As too growing up for crystal grain easily causes gas
Hole defect, the target relative density that this kind of technique is obtained only more than 80%, the porosity is big, produces microgranule and fly in sputter procedure
Splash, and then significantly reduce the quality of sputter coating.Heat and other static pressuring processes are to mix a certain proportion of molybdenum powder and niobium powder, Jing heat etc.
Static pressure obtains molybdenum niobium alloy target.The target relative density that this kind of technique is obtained can reach more than 98%, but be set due to used
Standby complicated, high cost.It is obtained after sintered blank using isostatic cool pressing, vacuum-sintering, then forged or rolling processing, obtain relative
The target of density more than 98%.But due to the low problem of sintered blank density, machining yield is low, and long flow path, complex operation,
High cost.The target of high densification, but the bad solution of carburizing problem of graphite can be obtained by the method for hot pressing, but by nitridation
The assembling die of boron and graphite can be prevented effectively from this problem, prepare high fine and close high-purity molybdenum niobium alloy target.
The content of the invention
In order to solve the above problems, the present invention provides a kind of pressure sintering and prepares the controllable molybdenum niobium alloy target of high-purity microstructure
Material method, methods described prepare the controllable molybdenum niobium alloy target of microstructure by the assembling die hot pressing to boron nitride and graphite
Material；
Further, the method comprising the steps of：
(1) molybdenum powder 85%～95% is weighed by weight percentage, remaining is mixed for niobium powder；
(2) mixed-powder as obtained by step (1) is put into mould for hot pressed sintering, obtains sintered blank, and temperature-fall period is with stove
Cooling；
(3) sintered blank as obtained by step (2) is surface-treated and is machined, and is obtained the controllable molybdenum niobium of microstructure and is closed
Gold target material；
Further, in the step (2), sintering furnace is vacuum hotpressing stove；
Further, in the step (2), the holding temperature of vacuum hotpressing is 1600～1800 DEG C, and temperature retention time is 2～5
Hour, pressurization pressure is 30～100MPa；
Further, the hot pressing die in the step (2) is the assembling die of boron nitride and graphite, and outer layer is graphite
Sleeve pipe and pad of the internal layer for boron nitride；
Further, there are 30～90 minutes at 500～800 DEG C in the hot pressed sintering temperature-rise period in the step (2)
Holding stage；
Beneficial effects of the present invention are as follows：
1) the molybdenum niobium alloy sputtering target material of high densification can be prepared using the method for hot pressing of the present invention, consistency is reachable
To more than 99%；
2) carburization phenomena can effectively be prevented using the assembling die of boron nitride and graphite, obtains high fine and close high-purity microcosmic
The controllable molybdenum niobium alloy target of tissue, reduces sintering temperature, reduces cost；
3) overcome the low phenomenon of powder metallurgical technique consistency, the tissue of melting and casting is thick, uneven components, heat etc.
The shortcoming of static pressure high cost.
Description of the drawings
Fig. 1 is front view, top view and the explosive view of assembling die of the present invention.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, it is below in conjunction with drawings and Examples, right
The present invention is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, and
It is not used in the restriction present invention.Conversely, the present invention cover it is any be defined by the claims the present invention spirit and scope on do
Replacement, modification, equivalent method and scheme.Further, in order that the public has a better understanding to the present invention, below to this
It is in the detailed description of invention, detailed to describe some specific detail sections.Do not have these thin for a person skilled in the art
The description of section part can also understand the present invention completely.
The invention will be further described with specific embodiment below in conjunction with the accompanying drawings, but not as a limitation of the invention.
Most preferred embodiment is enumerated for of the invention below：
Embodiment 1
Molybdenum powder is from the product that the Luoyang Yong Zhuo tungsten and molybdenum materials company limited trade mark is FMo -1, the Fisher particle size difference of molybdenum powder
For 8.4 μm, niobium powder is from the product that Dongfang Tantalum Industry Co., Ltd., Ningxia Hui autonomy Region's trade mark is FNb -1, the Fisher particle size difference of niobium powder
For 12 μm,
The preparation technology of above-mentioned high-compactness molybdenum niobium alloy target, comprises the following steps：
(1) planetary ball mill, abrading-ball is added to select oxygen after the molybdenum powder of weighing 90%, 10% niobium powder by weight percentage
Change zirconium ball, ratio of grinding media to material is 2 to 1, and Ball-milling Time is 8 hours, obtains mixed-powder；
(2) add in the assembling die of boron nitride and graphite, using Shanghai Twilight by the mixed-powder of gained in step (1)
Vacuum hotpressing stove carries out hot pressed sintering, is incubated 30 minutes at 600 DEG C, is then warmed up to 1800 DEG C in sintering, is incubated 2 hours, protects
Pressurize during temperature pressure 30MPa, and furnace cooling obtains sintered blank to room temperature afterwards, and in whole process, vacuum is 1x10-3Pa；
(3) machine after being surface-treated by the sintered blank of gained in step (2).
Embodiment 2
Molybdenum powder is from the product that the Luoyang Yong Zhuo tungsten and molybdenum materials company limited trade mark is FMo -1, the Fisher particle size difference of molybdenum powder
For 8.4 μm, niobium powder is from the product that Dongfang Tantalum Industry Co., Ltd., Ningxia Hui autonomy Region's trade mark is FNb -1, the Fisher particle size difference of niobium powder
For 12 μm,
The preparation technology of above-mentioned high-compactness molybdenum niobium alloy target, comprises the following steps：
(1) planetary ball mill, abrading-ball is added to select oxygen after the molybdenum powder of weighing 95%, 5% niobium powder by weight percentage
Change zirconium ball, ratio of grinding media to material is 2 to 1, and Ball-milling Time is 8 hours, obtains mixed-powder；
(2) add in the assembling die of boron nitride and graphite, using Shanghai Twilight by the mixed-powder of gained in step (1)
Vacuum hotpressing stove carries out hot pressed sintering, is incubated 30 minutes at 600 DEG C, is then warmed up to 1800 DEG C in sintering, is incubated 2 hours, protects
Pressurize during temperature pressure 30MPa, and furnace cooling obtains sintered blank to room temperature afterwards, and in whole process, vacuum is 1x10-3Pa；
(3) machine after being surface-treated by the sintered blank of gained in step (2).
Embodiment 3
Molybdenum powder is from the product that the Luoyang Yong Zhuo tungsten and molybdenum materials company limited trade mark is FMo -1, the Fisher particle size difference of molybdenum powder
For 8.4 μm, niobium powder is from the product that Dongfang Tantalum Industry Co., Ltd., Ningxia Hui autonomy Region's trade mark is FNb -1, the Fisher particle size difference of niobium powder
For 12 μm,
The preparation technology of above-mentioned high-compactness molybdenum niobium alloy target, comprises the following steps：
(1) planetary ball mill, abrading-ball is added to select oxygen after the molybdenum powder of weighing 90%, 10% niobium powder by weight percentage
Change zirconium ball, ratio of grinding media to material is 2 to 1, and Ball-milling Time is 8 hours, obtains mixed-powder；
(2) add in the assembling die of boron nitride and graphite, using Shanghai Twilight by the mixed-powder of gained in step (1)
Vacuum hotpressing stove carries out hot pressed sintering, is incubated 30 minutes at 600 DEG C, is then warmed up to 1850 DEG C in sintering, is incubated 3 hours, protects
Pressurize during temperature pressure 30MPa, and furnace cooling obtains sintered blank to room temperature afterwards, and in whole process, vacuum is 1x10-3Pa；
(3) machine after being surface-treated by the sintered blank of gained in step (2).
Embodiment 4
Molybdenum powder is from the product that the Luoyang Yong Zhuo tungsten and molybdenum materials company limited trade mark is FMo -1, the Fisher particle size difference of molybdenum powder
For 8.4 μm, niobium powder is from the product that Dongfang Tantalum Industry Co., Ltd., Ningxia Hui autonomy Region's trade mark is FNb -1, the Fisher particle size difference of niobium powder
For 12 μm,
The preparation technology of above-mentioned high-compactness molybdenum niobium alloy target, comprises the following steps：
(1) planetary ball mill, abrading-ball is added to select oxygen after the molybdenum powder of weighing 90%, 10% niobium powder by weight percentage
Change zirconium ball, ratio of grinding media to material is 2 to 1, and Ball-milling Time is 8 hours, obtains mixed-powder；
(2) add in the assembling die of boron nitride and graphite, using Shanghai Twilight by the mixed-powder of gained in step (1)
Vacuum hotpressing stove carries out hot pressed sintering, is incubated 30 minutes at 600 DEG C, is then warmed up to 1880 DEG C in sintering, is incubated 2 hours, protects
Pressurize during temperature pressure 30MPa, and furnace cooling obtains sintered blank to room temperature afterwards, and in whole process, vacuum is 1x10-3Pa；
(3) machine after being surface-treated by the sintered blank of gained in step (2).
Contrast case 1
As a comparison, molybdenum niobium alloy target is prepared using with identical molybdenum powder in above-mentioned case and niobium powder,
The preparation technology of above-mentioned high-compactness molybdenum niobium alloy target, comprises the following steps：
(1) planetary ball mill, abrading-ball is added to select oxygen after the molybdenum powder of weighing 90%, 10% niobium powder by weight percentage
Change zirconium ball, ratio of grinding media to material is 2 to 1, and Ball-milling Time is 8 hours, obtains mixed-powder；
(2) add in graphite jig by the mixed-powder of gained in step (1), carried out using Shanghai Twilight vacuum hotpressing stove
Hot pressed sintering, is incubated 30 minutes at 600 DEG C in sintering, is then warmed up to 1800 DEG C, is incubated 2 hours, pressurization pressure in insulating process
Strong 30MPa, afterwards furnace cooling obtain sintered blank to room temperature, in whole process, vacuum is 1x10-3Pa；
(3) machine after being surface-treated by the sintered blank of gained in step (2).
Contrast case 2
As a comparison, molybdenum niobium alloy target is prepared using with identical molybdenum powder in demonstration case and niobium powder,
The preparation technology of above-mentioned high-compactness molybdenum niobium alloy target, comprises the following steps：
(1) planetary ball mill, abrading-ball is added to select oxygen after the molybdenum powder of weighing 90%, 10% niobium powder by weight percentage
Change zirconium ball, ratio of grinding media to material is 2 to 1, and Ball-milling Time is 8 hours, obtains mixed-powder；
(2) mixed-powder obtained by step (1) is adopted into cold isostatic compaction, obtains suppressing base, wherein pressing pressure is
200MPa；
(3) the compacting base obtained by step (2) is sintered in vacuum sintering furnace, in control temperature-rise period, vacuum is not more than
5x10-3Pa, wherein being incubated 30 minutes in 600 DEG C and 1500 DEG C, is heated to be incubated 3 hours when 2000 DEG C, afterwards furnace cooling,
Vacuum is kept in cooling procedure in 1x10-3Pa, finally obtains sintered blank；
(4) machine after be surface-treated the sintered blank obtained in step (3).
The density of above-mentioned molybdenum niobium alloy target is determined respectively using drainage, molybdenum niobium alloy target is tested and be calculated
Density and relative density, as shown in table 1.
The performance indications of 1 Different Preparation target of table
As can be seen from Table I, by the method for hot pressing, high cause can be prepared using the assembling die of boron nitride and graphite
Close high-purity molybdenum niobium alloy target, reduces the porosity while reduces cost, obtains the tiny tissue of crystal grain, is conducive to obtaining
The sputtered film of even tissue.
Embodiment described above, simply one kind of the present invention more preferably specific embodiment, those skilled in the art
The usual variations and alternatives that member is carried out in the range of technical solution of the present invention all should be comprising within the scope of the present invention.
Claims (6)
1. a kind of pressure sintering prepares the controllable molybdenum niobium alloy target method of high-purity microstructure, it is characterised in that methods described is led to
The assembling die hot pressing to boron nitride and graphite is crossed, the controllable molybdenum niobium alloy target of microstructure is prepared.
2. method according to claim 1, it is characterised in that the method comprising the steps of：
(1) molybdenum powder 85%～95% is weighed by weight percentage, remaining is mixed for niobium powder；
(2) mixed-powder as obtained by step (1) is put into mould for hot pressed sintering, obtains sintered blank, temperature-fall period furnace cooling；
(3) sintered blank as obtained by step (2) is surface-treated and is machined, and obtains the controllable molybdenum niobium alloy target of microstructure
Material.
3. method according to claim 2, it is characterised in that sintering furnace is vacuum hotpressing stove in the step (2).
4. method according to claim 2, it is characterised in that the holding temperature of vacuum hotpressing is in the step (2)
1600～1800 DEG C, temperature retention time is 2～5 hours, and pressurization pressure is 30～100MPa.
5. method according to claim 2, it is characterised in that the hot pressing die in the step (2) is boron nitride and stone
The assembling die of ink, outer layer are the sleeve pipe and pad of the internal layer for boron nitride of graphite.
6. method according to claim 2, it is characterised in that in the hot pressed sintering temperature-rise period in the step (2)
There is the holding stage of 30～90 minutes when 500～800 DEG C.
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Cited By (3)
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|---|---|---|---|---|
| CN108273994A (en) * | 2018-03-30 | 2018-07-13 | 东莞市晟日电子科技有限公司 | The preparation facilities and method of high-density molybdenum niobium alloy target |
| CN109280892A (en) * | 2018-11-13 | 2019-01-29 | 江苏迪丞光电材料有限公司 | The preparation method and target of flat-panel monitor molybdenum alloy sputtering target |
| CN111842900A (en) * | 2020-07-31 | 2020-10-30 | 河南科技大学 | Hot-pressing sintering method of high-purity cobalt target |
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| CN108273994A (en) * | 2018-03-30 | 2018-07-13 | 东莞市晟日电子科技有限公司 | The preparation facilities and method of high-density molybdenum niobium alloy target |
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| CN109280892A (en) * | 2018-11-13 | 2019-01-29 | 江苏迪丞光电材料有限公司 | The preparation method and target of flat-panel monitor molybdenum alloy sputtering target |
| CN111842900A (en) * | 2020-07-31 | 2020-10-30 | 河南科技大学 | Hot-pressing sintering method of high-purity cobalt target |
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Application publication date: 20170419 |