CN106513684B - A kind of production method of tungsten-molybdenum alloy rotary target material - Google Patents
A kind of production method of tungsten-molybdenum alloy rotary target material Download PDFInfo
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- CN106513684B CN106513684B CN201610989417.4A CN201610989417A CN106513684B CN 106513684 B CN106513684 B CN 106513684B CN 201610989417 A CN201610989417 A CN 201610989417A CN 106513684 B CN106513684 B CN 106513684B
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
A kind of production method of tungsten-molybdenum alloy rotary target material, the following steps are included: choosing tungsten powder and molybdenum powder first and carrying out mixing, mold is packed into after the completion of mixing to carry out being pressed into base, then it demoulds after sintering, form crude product, the crude product of preparation is machined, annealing, target is formed after Chemical Physics detection and ultrasonic cleaning, prepare tungsten dusty spray, tungsten dusty spray is sprayed to and forms product in the cavity of target, present invention process is simple, the production cost of rotary target material is not only reduced significantly, and the target of preparation has even tissue crystal grain tiny, the excellent performances such as high heat resistance impact, to be suitable for the production of large area TFT film.
Description
Technical field
The present invention relates to a kind of production method of rotary target material, a kind of tungsten-molybdenum alloy rotary target material is particularly related to
Production method.
Background technique
TFT film has the advantages that high-responsivity, high brightness, high contrast, is one of numerous industry basic materials, therefore
It is widely used in solar battery, liquid crystal display and plasma display field, in recent years, along with high-grade display
Fast development, tungsten-molybdenum alloy rotary target material are the important materials for preparing TFT film, currently, plate target is industrially widely used
Plated film is carried out, planar targets shape has cuboid, square, cylindrical body and irregular shape, cuboid, square and cylinder
Target be it is solid, in sputtering process, round ring magnet establishes toroidal magnetic field in target material surface, in the equidistant annular of distance between axles
Etched area is formed on surface, the disadvantage is that film deposition thickness uniformity is not easy to control, the utilization rate of plate target is low, only 20
~ 30%, the utilization rate of rotary target material can reach 80% or more, and the domestic TFT for also rarely having producer to be able to produce out qualification at present
Rotary target material, most of all in development phase, the core technology difficult point of TFT rotary target material is to control opening in forming process
Split the uniformity controlling shunk with TFT rotary target material in low-density problem and sintering process.
Summary of the invention
In order to solve the above-mentioned technical problem the present invention, provides a kind of production method of tungsten-molybdenum alloy rotary target material, technique
Simply, the production cost of rotary target material is not only reduced significantly, but also the target prepared has even tissue crystal grain tiny, high
The excellent performances such as heat shock resistance, to be suitable for the production of large area TFT film.
In order to solve the above-mentioned technical problem, used technical solution is the present invention: a kind of tungsten-molybdenum alloy rotary target material
Production method, comprising the following steps:
Step 1: it is close for 3 ~ 7 μm of tungsten powder and theory in 98% or more, Fei Shi average particle size to choose theoretical density respectively
Spend the molybdenum powder at 1 ~ 10 μm of 98% or more, Fei Shi average particle size, and according to (3 ~ 5): the mass ratio of (7 ~ 5) is put into double heap batch mixers
In, it is sufficiently mixed under conditions of revolving speed is 50r/min ~ 80 r/min, it is spare；
W content and molybdenum content are detected Step 2: arbitrarily choosing at 5 points in through the mixed material of step 1,
Until each test point tungsten content ratio error, between 0.01 ~ 0.05%, mixing is completed, spare；
Step 3: by 200 meshes are crossed through the mixed mixed material of step 2, it is spare；
Step 4: treated that mixed material is filled into the rubber sleeve equipped with tubular flexible mold for step 3 of learning from else's experience, and
Molybdenum disulphide powder is smeared in mold and mixed material contact surface, is vacuumized after then sealing rubber sleeve, and after vacuumizing
Rubber is placed on cold isostatic press, and first precompressed is carried out under conditions of pressure is 20 ~ 50MPa, forms crude green body, will be obtained
Crude green body carries out secondary compacting under conditions of 50-200MPa, until the density of green compact reaches the 60 ~ 62% of theoretical density, unloads and is depressed into
Normal pressure, it is spare；
Step 5: the tungsten-molybdenum alloy target green compact that step 4 is suppressed are placed in vacuum sintering funace, in hydrogen shield
Under atmosphere, pressure be 20 ~ 30MPa, temperature carries out hot pressed sintering under conditions of being 1000 ~ 1350 DEG C, adopted after 3 ~ 5h of heat-insulation pressure keeping
It is demoulded, is cooled to room temperature under conditions of 400 ~ 1000 DEG C with High temperature release technique, tungsten-molybdenum alloy target crude product is made, it is standby
With；
Step 6: being machined tungsten-molybdenum alloy target crude product obtained in step 5 to required size, it is subsequently placed in true
In empty annealing furnace, 1000 ~ 1600 DEG C of annealing 1 ~ 2h are warming up to, it is spare；
Step 7: the tungsten-molybdenum alloy target crude product handled through step 6 is carried out chemistry, physical detection, then through ultrasonic clear
It washes, target is made to reach qualified roughness, it is spare；
Step 8: step 3 of learning from else's experience treated mixed material, and mixed material is put into 2 ~ 3h of ball milling in ball mill, mistake
800 ~ 1000 meshes obtain tungsten dusty spray, spare；
Step 9: being sprayed using the method for plasma spraying to the outer surface of step 7 under inert gas shielding atmosphere
Tungsten dusty spray made from step 8, it is spare；
Step 10: target cavity obtained in step 9 is carried out vacuumize process, it is then passed through inert gas thereto,
Throughput is 500 ~ 1000SCCH, and the tungsten dusty spray cold spraying for obtaining step 8 under the ambient conditions of inert gas
Into the cavity of target, coating thickness is 0.1 ~ 0.2mm, and product is made.
Pressing time in the step 2 is 0.5 ~ 1h.
In the step 4 after isostatic cool pressing static pressure, unloads and use N grades of release pressure maintainings during being depressed into normal pressure, first
The cold pressure for waiting releases pressure maintaining of grade is 0.5 ~ 0.85 times of isostatic cool pressing pressure, and the pressure of rear stage release pressure maintaining is unloaded for previous stage
0.5 ~ 0.85 times for pressing dwell pressure, the dwell time at different levels is 1 ~ 10min, direct release after N grades of release pressure maintainings
To normal pressure, 3≤N≤5.
Tubular flexible mold is by the combination that forms with cylinder steel core, flexible jacket and flexible end cap in the step 4
Mold, flexible end cap are sleeved on the both ends of flexible steel core, and flexible jacket is sleeved on flexible ends and covers, flexible jacket and cylinder steel core
Between form the cavity for holding mixed material.
Hot pressed sintering includes following three phases in the step 5: 1) 1000 ~ 1200 DEG C, 5 ~ 10 DEG C of heating rate/
min；2) 1200 DEG C of 1 ~ 2h of heat preservation；3) 1200 ~ 1350 DEG C, 5 ~ 10 DEG C/min of heating rate；4) 1350 DEG C of heat preservation 3 ~ 5h, 5) 1350
DEG C ~ room temperature, 1 ~ 3 DEG C/min of rate of temperature fall.
Heating rate in the step 6 is 30 ~ 40 DEG C/min.
Machining is processed with electro-spark cutting machine and circle grinding machine in the step 7.
Inert gas in the step 9 is argon gas or nitrogen.
Target surrounds center axis rotation with the speed of 100 ~ 200r/min in the step 9, and the movement speed of spray gun is
500 ~ 1000mm/min, the temperature of working gas are 800 ~ 1300 DEG C, and spray distance is 40 ~ 60mm, and spray angle is 75 ~ 90 °,
Air pressure is 2 ~ 5MPa.
Beneficial effects of the present invention:
(1) rotary target material prepared by the present invention, can be during sputtering, and target can be around fixed bar magnet component
Rotation, thus 360 ° can uniformly be etched, while sputtered atom can fly to all directions, uniformity is good, and sputtering area is big, more
Easy to operate, high production efficiency is changed, target utilization is high, and has unique superiority to the deposition of part inner wall.
(2) in the present invention in isostatic cool pressing pressing process, using carrying out stage by stage, final pressure 200MPa, so that
When release, blank strength is enough to bear the tensile stress generated when elastic rubber mould is separated with green body, so that green body will not generate
Layering and crackle, effectively increase the consistency of green body.
Specific embodiment
A kind of production method of tungsten-molybdenum alloy rotary target material, comprising the following steps:
Step 1: it is close for 3 ~ 7 μm of tungsten powder and theory in 98% or more, Fei Shi average particle size to choose theoretical density respectively
Spend the molybdenum powder at 1 ~ 10 μm of 98% or more, Fei Shi average particle size, and according to (3 ~ 5): the mass ratio of (7 ~ 5) is put into double heap batch mixers
In, it is sufficiently mixed under conditions of revolving speed is 50r/min ~ 80 r/min, it is spare；
W content and molybdenum content are detected Step 2: arbitrarily choosing at 5 points in through the mixed material of step 1,
Until each test point tungsten content ratio error, between 0.01 ~ 0.05%, mixing is completed, spare；
Step 3: by 200 meshes are crossed through the mixed mixed material of step 2, it is spare；
Step 4: treated that mixed material is filled into the rubber sleeve equipped with tubular flexible mold for step 3 of learning from else's experience, and
Molybdenum disulphide powder is smeared in mold and mixed material contact surface, is vacuumized after then sealing rubber sleeve, and after vacuumizing
Rubber is placed on cold isostatic press, and first precompressed is carried out under conditions of pressure is 20 ~ 50MPa, forms crude green body, will be obtained
Crude green body carries out secondary compacting under conditions of 50-200MPa, until the density of green compact reaches the 60 ~ 62% of theoretical density, unloads and is depressed into
Normal pressure, it is spare；
Step 5: the tungsten-molybdenum alloy target green compact that step 4 is suppressed are placed in vacuum sintering funace, in hydrogen shield
Under atmosphere, pressure be 20 ~ 30MPa, temperature carries out hot pressed sintering under conditions of being 1000 ~ 1350 DEG C, adopted after 3 ~ 5h of heat-insulation pressure keeping
It is demoulded, is cooled to room temperature under conditions of 400 ~ 1000 DEG C with High temperature release technique, tungsten-molybdenum alloy target crude product is made, it is standby
With；
Step 6: being machined tungsten-molybdenum alloy target crude product obtained in step 5 to required size, it is subsequently placed in true
In empty annealing furnace, 1000 ~ 1600 DEG C of annealing 1 ~ 2h are warming up to, it is spare；
Step 7: the tungsten-molybdenum alloy target crude product handled through step 6 is carried out chemistry, physical detection, then through ultrasonic clear
It washes, target is made to reach qualified roughness, it is spare；
Step 8: step 3 of learning from else's experience treated mixed material, and mixed material is put into 2 ~ 3h of ball milling in ball mill, mistake
800 ~ 1000 meshes obtain tungsten dusty spray, spare；
Step 9: being sprayed using the method for plasma spraying to the outer surface of step 7 under inert gas shielding atmosphere
Tungsten dusty spray made from step 8, it is spare；
Step 10: target cavity obtained in step 9 is carried out vacuumize process, it is then passed through inert gas thereto,
Throughput is 500 ~ 1000SCCH, and the tungsten dusty spray cold spraying for obtaining step 8 under the ambient conditions of inert gas
Into the cavity of target, coating thickness is 0.1 ~ 0.2mm, and product is made.
Pressing time in the step 2 is 0.5 ~ 1h.
In the step 4 after isostatic cool pressing static pressure, unloads and use N grades of release pressure maintainings during being depressed into normal pressure, first
The cold pressure for waiting releases pressure maintaining of grade is 0.5 ~ 0.85 times of isostatic cool pressing pressure, and the pressure of rear stage release pressure maintaining is unloaded for previous stage
0.5 ~ 0.85 times for pressing dwell pressure, the dwell time at different levels is 1 ~ 10min, direct release after N grades of release pressure maintainings
To normal pressure, 3≤N≤5.
Tubular flexible mold is by the combination that forms with cylinder steel core, flexible jacket and flexible end cap in the step 4
Mold, flexible end cap are sleeved on the both ends of flexible steel core, and flexible jacket is sleeved on flexible ends and covers, flexible jacket and cylinder steel core
Between form the cavity for holding mixed material.
Hot pressed sintering includes following three phases in the step 5: 1) 1000 ~ 1200 DEG C, 5 ~ 10 DEG C of heating rate/
min；2) 1200 DEG C of 1 ~ 2h of heat preservation；3) 1200 ~ 1350 DEG C, 5 ~ 10 DEG C/min of heating rate；4) 1350 DEG C of heat preservation 3 ~ 5h, 5) 1350
DEG C ~ room temperature, 1 ~ 3 DEG C/min of rate of temperature fall.
Heating rate in the step 6 is 30 ~ 40 DEG C/min.
Machining is processed with electro-spark cutting machine and circle grinding machine in the step 7.
Inert gas in the step 9 is argon gas or nitrogen.
Target surrounds center axis rotation with the speed of 100 ~ 200r/min in the step 9, and the movement speed of spray gun is
500 ~ 1000mm/min, the temperature of working gas are 800 ~ 1300 DEG C, and spray distance is 40 ~ 60mm, and spray angle is 75 ~ 90 °,
Air pressure is 2 ~ 5MPa.
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1
A kind of production method of tungsten-molybdenum alloy rotary target material, comprising the following steps:
Step 1: choosing the tungsten powder and theoretical density that theoretical density is 3 μm in 98% or more, Fei Shi average particle size respectively
It is put into double heap batch mixers in 98% or more, Fei Shi average particle size, 1 μm of molybdenum powder, and according to the mass ratio of 3:7, is in revolving speed
It is sufficiently mixed under conditions of 50r/min, it is spare；
W content and molybdenum content are detected Step 2: arbitrarily choosing at 5 points in through the mixed material of step 1,
Until each test point tungsten content ratio error, between 0.01 ~ 0.05%, mixing is completed, spare；
Step 3: by 200 meshes are crossed through the mixed mixed material of step 2, it is spare；
Step 4: treated that mixed material is filled into the rubber sleeve equipped with tubular flexible mold for step 3 of learning from else's experience, and
Molybdenum disulphide powder is smeared in mold and mixed material contact surface, is vacuumized after then sealing rubber sleeve, and after vacuumizing
Rubber is placed on cold isostatic press, and first precompressed is carried out under conditions of pressure is 20 ~ 50MPa, forms crude green body, will be obtained
Crude green body carries out secondary compacting under conditions of 50-200MPa, until the density of green compact reaches the 60 ~ 62% of theoretical density, unloads and is depressed into
Normal pressure, it is spare；
Step 5: the tungsten-molybdenum alloy target green compact that step 4 is suppressed are placed in vacuum sintering funace, in hydrogen shield
Under atmosphere, pressure 20MPa, temperature carry out hot pressed sintering under conditions of being 1000 DEG C, High temperature release is used after heat-insulation pressure keeping 3h
Technique is demoulded under conditions of 400 DEG C, is cooled to room temperature, and tungsten-molybdenum alloy target crude product is made, spare；
Step 6: being machined tungsten-molybdenum alloy target crude product obtained in step 5 to required size, it is subsequently placed in true
In empty annealing furnace, 1000 DEG C of annealing 1h are warming up to, it is spare；
Step 7: the tungsten-molybdenum alloy target crude product handled through step 6 is carried out chemistry, physical detection, then through ultrasonic clear
It washes, target is made to reach qualified roughness, it is spare；
Step 8: step 3 of learning from else's experience treated mixed material, and mixed material is put into ball milling 2h in ball mill, mistake
800 meshes obtain tungsten dusty spray, spare；
Step 9: being sprayed using the method for plasma spraying to the outer surface of step 7 under inert gas shielding atmosphere
Tungsten dusty spray made from step 8, it is spare；
Step 10: target cavity obtained in step 9 is carried out vacuumize process, it is then passed through inert gas thereto,
Throughput is 500SCCH, and the tungsten dusty spray cold spraying for obtaining step 8 under the ambient conditions of inert gas is to target
In the cavity of material, product is made in coating thickness 0.1mm.
Pressing time in the step 2 is 0.5h.
Hot pressed sintering includes following three phases in the step 5: 1) 1000 ~ 1200 DEG C, 5 ~ 10 DEG C of heating rate/
min；2) 1200 DEG C of 1 ~ 2h of heat preservation；3) 1200 ~ 1350 DEG C, 5 ~ 10 DEG C/min of heating rate；4) 1350 DEG C of heat preservation 3 ~ 5h, 5) 1350
DEG C ~ room temperature, 1 ~ 3 DEG C/min of rate of temperature fall.
Heating rate in the step 6 is 30 DEG C/min.
Inert gas in the step 9 is argon gas.
Target surrounds center axis rotation with the speed of 100r/min in the step 9, and the movement speed of spray gun is 500mm/
Min, the temperature of working gas are 800 DEG C, spray distance 40mm, and spray angle is 75 °, air pressure 2MPa.
The machining is processed with electro-spark cutting machine and circle grinding machine.
In the step 4 after isostatic cool pressing static pressure, unloads and use 3 grades of release pressure maintainings during being depressed into normal pressure, first
The cold pressure for waiting releases pressure maintaining of grade is 0.5 times of isostatic cool pressing pressure, and the pressure of rear stage release pressure maintaining is previous stage release guarantor
0.5 times of pressure pressure, dwell time at different levels are 1min, directly unload after N grades of release pressure maintainings and are depressed into normal pressure.
The tubular flexible mold is soft by the composable mold that forms with cylinder steel core, flexible jacket and flexible end cap
Property end cap is sleeved on the both ends of flexible steel core, and flexible jacket is sleeved on flexible ends and covers, shape between flexible jacket and cylinder steel core
At the cavity for holding mixed material.
Embodiment 2
A kind of production method of tungsten-molybdenum alloy rotary target material, comprising the following steps:
Step 1: choosing the tungsten powder and theoretical density that theoretical density is 7 μm in 98% or more, Fei Shi average particle size respectively
It is put into double heap batch mixers in 98% or more, Fei Shi average particle size, 0 μm of molybdenum powder, and according to the mass ratio of 5:5, is 80 in revolving speed
It is sufficiently mixed under conditions of r/min, it is spare；
W content and molybdenum content are detected Step 2: arbitrarily choosing at 5 points in through the mixed material of step 1,
Until each test point tungsten content ratio error, between 0.01 ~ 0.05%, mixing is completed, spare；
Step 3: by 200 meshes are crossed through the mixed mixed material of step 2, it is spare；
Step 4: treated that mixed material is filled into the rubber sleeve equipped with tubular flexible mold for step 3 of learning from else's experience, and
Molybdenum disulphide powder is smeared in mold and mixed material contact surface, is vacuumized after then sealing rubber sleeve, and after vacuumizing
Rubber is placed on cold isostatic press, and first precompressed is carried out under conditions of pressure is 20 ~ 50MPa, forms crude green body, will be obtained
Crude green body carries out secondary compacting under conditions of 50-200MPa, until the density of green compact reaches the 62% of theoretical density, unloads and is depressed into often
Pressure, it is spare；
Step 5: the tungsten-molybdenum alloy target green compact that step 4 is suppressed are placed in vacuum sintering funace, in hydrogen shield
Under atmosphere, pressure 30MPa, temperature carry out hot pressed sintering under conditions of being 1350 DEG C, High temperature release is used after heat-insulation pressure keeping 5h
Technique is demoulded under conditions of 1000 DEG C, is cooled to room temperature, and tungsten-molybdenum alloy target crude product is made, spare；
Step 6: being machined tungsten-molybdenum alloy target crude product obtained in step 5 to required size, it is subsequently placed in true
In empty annealing furnace, 1600 DEG C of annealing 2h are warming up to, it is spare；
Step 7: the tungsten-molybdenum alloy target crude product handled through step 6 is carried out chemistry, physical detection, then through ultrasonic clear
It washes, target is made to reach qualified roughness, it is spare；
Step 8: step 3 of learning from else's experience treated mixed material, and mixed material is put into ball milling 3h in ball mill, mistake
1000 meshes obtain tungsten dusty spray, spare；
Step 9: being sprayed using the method for plasma spraying to the outer surface of step 7 under inert gas shielding atmosphere
Tungsten dusty spray made from step 8, it is spare；
Step 10: target cavity obtained in step 9 is carried out vacuumize process, it is then passed through inert gas thereto,
Throughput is 1000SCCH, and the tungsten dusty spray cold spraying for obtaining step 8 under the ambient conditions of inert gas is to target
In the cavity of material, product is made in coating thickness 0.2mm.
Pressing time in the step 2 is 1h.
Hot pressed sintering includes following three phases in the step 5: 1) 1000 ~ 1200 DEG C, 5 ~ 10 DEG C of heating rate/
min；2) 1200 DEG C of 1 ~ 2h of heat preservation；3) 1200 ~ 1350 DEG C, 5 ~ 10 DEG C/min of heating rate；4) 1350 DEG C of heat preservation 3 ~ 5h, 5) 1350
DEG C ~ room temperature, 1 ~ 3 DEG C/min of rate of temperature fall.
Heating rate in the step 6 is 40 DEG C/min.
Inert gas in the step 9 is argon gas or nitrogen.
Target surrounds center axis rotation with the speed of 200r/min in the step 9, and the movement speed of spray gun is
1000mm/min, the temperature of working gas are 1300 DEG C, spray distance 60mm, and spray angle is 90 °, and air pressure is
5MPa。
The machining is processed with electro-spark cutting machine and circle grinding machine.
In the step 4 after isostatic cool pressing static pressure, unloads and use 4 grades of release pressure maintainings during being depressed into normal pressure, first
The cold pressure for waiting releases pressure maintaining of grade is 0.85 times of isostatic cool pressing pressure, and the pressure of rear stage release pressure maintaining is previous stage release guarantor
0.85 times of pressure pressure, the dwell time at different levels is 10min, directly unloads after the 4th grade of release pressure maintaining and is depressed into normal pressure.
The tubular flexible mold is soft by the composable mold that forms with cylinder steel core, flexible jacket and flexible end cap
Property end cap is sleeved on the both ends of flexible steel core, and flexible jacket is sleeved on flexible ends and covers, shape between flexible jacket and cylinder steel core
At the cavity for holding mixed material.
Embodiment 3
A kind of production method of tungsten-molybdenum alloy rotary target material, comprising the following steps:
Step 1: choosing the tungsten powder and theoretical density that theoretical density is 5 μm in 98% or more, Fei Shi average particle size respectively
It is put into double heap batch mixers in 98% or more, Fei Shi average particle size, 6 μm of molybdenum powder, and according to the mass ratio of 4:6, is in revolving speed
It is sufficiently mixed under conditions of 65r/min, it is spare；
W content and molybdenum content are detected Step 2: arbitrarily choosing at 5 points in through the mixed material of step 1,
Until each test point tungsten content ratio error, between 0.01 ~ 0.05%, mixing is completed, spare；
Step 3: by 200 meshes are crossed through the mixed mixed material of step 2, it is spare；
Step 4: treated that mixed material is filled into the rubber sleeve equipped with tubular flexible mold for step 3 of learning from else's experience, and
Molybdenum disulphide powder is smeared in mold and mixed material contact surface, is vacuumized after then sealing rubber sleeve, and after vacuumizing
Rubber is placed on cold isostatic press, and first precompressed is carried out under conditions of pressure is 20 ~ 50MPa, forms crude green body, will be obtained
Crude green body carries out secondary compacting under conditions of 50-200MPa, until the density of green compact reaches the 60 ~ 62% of theoretical density, unloads and is depressed into
Normal pressure, it is spare；
Step 5: the tungsten-molybdenum alloy target green compact that step 4 is suppressed are placed in vacuum sintering funace, in hydrogen shield
Under atmosphere, pressure 25MPa, temperature carry out hot pressed sintering under conditions of being 1100 DEG C, High temperature release is used after heat-insulation pressure keeping 4h
Technique is demoulded under conditions of 700 DEG C, is cooled to room temperature, and tungsten-molybdenum alloy target crude product is made, spare；
Step 6: being machined tungsten-molybdenum alloy target crude product obtained in step 5 to required size, it is subsequently placed in true
In empty annealing furnace, 1300 DEG C of annealing 1.5h are warming up to, it is spare；
Step 7: the tungsten-molybdenum alloy target crude product handled through step 6 is carried out chemistry, physical detection, then through ultrasonic clear
It washes, target is made to reach qualified roughness, it is spare；
Step 8: step 3 of learning from else's experience treated mixed material, and mixed material is put into 2 ~ 3h of ball milling in ball mill, mistake
900 meshes obtain tungsten dusty spray, spare；
Step 9: being sprayed using the method for plasma spraying to the outer surface of step 7 under inert gas shielding atmosphere
Tungsten dusty spray made from step 8, it is spare；
Step 10: target cavity obtained in step 9 is carried out vacuumize process, it is then passed through inert gas thereto,
Throughput is 700SCCH, and the tungsten dusty spray cold spraying for obtaining step 8 under the ambient conditions of inert gas is to target
In the cavity of material, product is made in coating thickness 0.15mm.
Pressing time in the step 2 is 0.75h.
Hot pressed sintering includes following three phases in the step 5: 1) 1000 ~ 1200 DEG C, 5 ~ 10 DEG C of heating rate/
min；2) 1200 DEG C of 1 ~ 2h of heat preservation；3) 1200 ~ 1350 DEG C, 5 ~ 10 DEG C/min of heating rate；4) 1350 DEG C of heat preservation 3 ~ 5h, 5) 1350
DEG C ~ room temperature, 1 ~ 3 DEG C/min of rate of temperature fall.
Heating rate in the step 6 is 35 DEG C/min.
Inert gas in the step 9 is argon gas or nitrogen.
Target surrounds center axis rotation with the speed of 150r/min in the step 9, and the movement speed of spray gun is 750mm/
Min, the temperature of working gas are 1050 DEG C, spray distance 50mm, and spray angle is 80 °, air pressure 3.5MPa.
The machining is processed with electro-spark cutting machine and circle grinding machine.
In the step 4 after isostatic cool pressing static pressure, unloads and use N grades of release pressure maintainings during being depressed into normal pressure, first
The cold pressure for waiting releases pressure maintaining of grade is 0.5 ~ 0.85 times of isostatic cool pressing pressure, and the pressure of rear stage release pressure maintaining is unloaded for previous stage
0.5 ~ 0.85 times for pressing dwell pressure, the dwell time at different levels is 1 ~ 10min, direct release after N grades of release pressure maintainings
To normal pressure, 3≤N≤5.
The tubular flexible mold is soft by the composable mold that forms with cylinder steel core, flexible jacket and flexible end cap
Property end cap is sleeved on the both ends of flexible steel core, and flexible jacket is sleeved on flexible ends and covers, shape between flexible jacket and cylinder steel core
At the cavity for holding mixed material.
Claims (9)
1. a kind of production method of tungsten-molybdenum alloy rotary target material, it is characterised in that: the following steps are included:
Step 1: choosing the tungsten powder and theoretical density that theoretical density is 3~7 μm in 98% or more, Fei Shi average particle size respectively
The molybdenum powder for being 1~10 μm in 98% or more, Fei Shi average particle size, and by above-mentioned raw materials according to (3~5): the mass ratio of (7~5)
It is put into double heap batch mixers, is sufficiently mixed under conditions of revolving speed is 50r/min~80r/min, it is spare；
W content and molybdenum content are detected Step 2: arbitrarily choosing at 5 points in through the mixed material of step 1, until
Each test point tungsten content ratio error between 0.01~0.05%, complete, spare by mixing；
Step 3: by 200 meshes are crossed through the mixed mixed material of step 2, it is spare；
Step 4: treated that mixed material is filled into the rubber sleeve equipped with tubular flexible mold, and in mould for step 3 of learning from else's experience
Tool smears molybdenum disulphide powder with the contact surface of mixed material, vacuumizes after then sealing rubber sleeve, and by the rubber after vacuumizing
Gum cover is placed on cold isostatic press, and first precompressed is carried out under conditions of pressure is 20~50MPa, forms crude green body, will be obtained
Crude green body carries out secondary compacting under conditions of 50-200MPa, until the density of green compact reaches the 60~62% of theoretical density, release
It is spare to normal pressure；
Step 5: by step 4 suppress tungsten-molybdenum alloy target green compact be placed in vacuum sintering funace, hydrogen shield atmosphere,
Pressure is 20~30MPa, temperature carries out hot pressed sintering under conditions of being 1000~1350 DEG C, using height after 3~5h of heat-insulation pressure keeping
Warm releasing process is demoulded under conditions of 400~1000 DEG C, is cooled to room temperature, and tungsten-molybdenum alloy target crude product is made, spare；
Step 6: being machined tungsten-molybdenum alloy target crude product obtained in step 5 to required size, it is subsequently placed in vacuum and moves back
In stove, 1000~1600 DEG C of annealing 1~2h are warming up to, it is spare；
Step 7: the tungsten-molybdenum alloy target crude product handled through step 6 is carried out chemistry, physical detection, be then cleaned by ultrasonic,
Machining makes target reach qualified roughness, spare；
Step 8: step 3 of learning from else's experience treated mixed material, and mixed material is put into 2~3h of ball milling in ball mill, cross 800
~1000 meshes obtain tungsten dusty spray, spare；
Step 9: being sprayed using the method for plasma spraying to the outer surface of step 7 under inert gas or nitrogen protection atmosphere
Tungsten dusty spray made from step 8 is applied, it is spare；
Step 10: target cavity obtained in step 9 is carried out vacuumize process, it is then passed through inert gas, air-flow thereto
Amount is 500~1000SCCH, and arrives the tungsten dusty spray cold spraying that step 8 obtains under the ambient conditions of inert gas
In the cavity of target, coating thickness is 0.1~0.2mm, and product is made.
2. a kind of production method of tungsten-molybdenum alloy rotary target material as described in claim 1, it is characterised in that: in the step 4
Secondary compacting time be 0.5~1h.
3. a kind of production method of tungsten-molybdenum alloy rotary target material as described in claim 1, it is characterised in that: in the step 4
After isostatic cool pressing static pressure, unloads and use N grades of release pressure maintainings during being depressed into normal pressure, the pressure of the cold equal releases pressure maintaining of the first order
Be 0.5~0.85 times of isostatic cool pressing pressure, the pressure of rear stage release pressure maintaining be previous stage release dwell pressure 0.5~
0.85 times, the dwell time at different levels is 1~10min, directly unloads after N grades of release pressure maintainings and is depressed into normal pressure, 3≤N≤5.
4. a kind of production method of tungsten-molybdenum alloy rotary target material as described in claim 1, it is characterised in that: in the step 4
Tubular flexible mold is sleeved on by the composable mold that forms with cylinder steel core, flexible jacket and flexible end cap, flexible end cap
The both ends of flexible steel core, flexible jacket are sleeved on flexible ends and cover, and are formed between flexible jacket and cylinder steel core mixed for holding
Close the cavity of material.
5. a kind of production method of tungsten-molybdenum alloy rotary target material as described in claim 1, it is characterised in that: in the step 5
Hot pressed sintering includes following three phases: 1) 1000~1200 DEG C, 5~10 DEG C/min of heating rate；2) 1200 DEG C heat preservation 1~
2h；3) 1200~1350 DEG C, 5~10 DEG C/min of heating rate；4) 1350 DEG C of heat preservation 3h, 5) 1350 DEG C~room temperature, rate of temperature fall 1
~3 DEG C/min.
6. a kind of production method of tungsten-molybdenum alloy rotary target material as described in claim 1, it is characterised in that: in the step 6
Heating rate be 30~40 DEG C/min.
7. a kind of production method of tungsten-molybdenum alloy rotary target material as described in claim 1, it is characterised in that: in the step 7
Machining is processed with electro-spark cutting machine and circle grinding machine.
8. a kind of production method of tungsten-molybdenum alloy rotary target material as described in claim 1, it is characterised in that: in the step 9
Inert gas be argon gas.
9. a kind of production method of tungsten-molybdenum alloy rotary target material as described in claim 1, it is characterised in that: in the step 9
Target surrounds center axis rotation with the speed of 100~200r/min, and the movement speed of spray gun is 500~1000mm/min, work
The temperature of gas is 800~1300 DEG C, and spray distance is 40~60mm, and spray angle is 75~90 °, air pressure 2
~5MPa.
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| CN107746080B (en) * | 2017-11-16 | 2019-06-04 | 金堆城钼业股份有限公司 | A kind of preparation method of molybdenum disulfide target |
| CN108004514B (en) * | 2017-12-28 | 2019-10-15 | 福州大学 | A kind of preparation method of the rotary target material with automatic adaptation cushion layer |
| CN108907630B (en) * | 2018-08-14 | 2020-08-07 | 合肥工业大学 | Manufacturing method of W/Mo/graphite composite anode target material for X-ray tube of CT machine |
| CN110184502A (en) * | 2019-03-18 | 2019-08-30 | 苏州康科斯柔性电子有限公司 | A kind of aluminium tantalum rotary target material and preparation method thereof |
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| CN110357626B (en) * | 2019-07-26 | 2022-02-18 | 中国建筑材料科学研究总院有限公司 | Doped tungsten oxide target material and preparation method thereof |
| CN114436640A (en) * | 2020-11-06 | 2022-05-06 | 湖南七点钟文化科技有限公司 | Preparation method of zinc oxide aluminum alloy target |
| CN114436642A (en) * | 2020-11-06 | 2022-05-06 | 湖南七点钟文化科技有限公司 | Preparation method of indium tin oxide alloy target material |
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| CN104439247B (en) * | 2014-12-30 | 2017-08-29 | 山东昊轩电子陶瓷材料有限公司 | The preparation method of molybdenum alloy target |
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