CN106319457A - Manufacturing method of tungsten titanium tube target - Google Patents
Manufacturing method of tungsten titanium tube target Download PDFInfo
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- CN106319457A CN106319457A CN201510347491.1A CN201510347491A CN106319457A CN 106319457 A CN106319457 A CN 106319457A CN 201510347491 A CN201510347491 A CN 201510347491A CN 106319457 A CN106319457 A CN 106319457A
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Abstract
The invention provides a manufacturing method of a tungsten titanium tube target. The method comprises the steps of providing tungsten titanium mixed powder and a stainless steel hollow tube; carrying out isostatic cool pressing technology operation on the tungsten titanium mixed powder and the stainless steel hollow tube to form a tungsten titanium mixed powder and stainless steel initial blank; arranging the tungsten titanium mixed powder and stainless steel initial blank in a vacuum can to be subject to vacuum can vacuumizing, and carrying out hot isostatic pressing technology operation on the tungsten titanium mixed powder and stainless steel initial blank; removing the vacuum can, and obtaining the tungsten titanium tube target. Through the isostatic cool pressing technology, the tungsten titanium mixed powder and the stainless steel hollow tube are pre-molded, the half-density tungsten titanium mixed powder and stainless steel initial blank can be formed, and through the subsequent hot isostatic pressing technology, the better density operation can be achieved; through the hot isostatic pressing technology, comprehensive gas pressures equal in all directions can be applied to the vacuum can, and the tungsten titanium tube target for a semiconductor can be finally obtained, wherein the tungsten titanium tube target is high in density and more uniform in structure.
Description
Technical field
The present invention relates to semiconductor applications, particularly relate to the manufacture method of a kind of tungsten titanium pipe target, particular for
Penstock is the tungsten titanium pipe target of hollow pipe.
Background technology
In recent years, growing along with sputtering target material and sputtering technology, sputtering target material is in sputtering technology
Serving the most important effect, the quality of sputtering target material has directly influenced the quality of forming film after sputtering.
Sputtering target material is broadly divided into planar targets and pipe target, and described pipe target is generally made up of sputtering target material and penstock,
Compared with flat target, the utilization rate of pipe target is higher and after sputtering quality of forming film more preferable, have in target market
Huge development potentiality.
Tungsten titanium target material is a kind of more typical alloy target material of ratio, and tungsten-titanium alloy has low-resistance coefficient, well
Heat stability and non-oxidizability；Meanwhile, 304 rustless steels have high temperature resistant 800 DEG C, good processability,
The feature that toughness is high, therefore using tungsten, titanium mixed-powder as the raw material of sputtering target material, 304 rustless steels are hollow
Pipe is as penstock, and the tungsten titanium pipe target being made up of both raw materials has become the pipe of semiconductor applications large usage quantity
One of target.For now, for semiconductor manufacturing tungsten titanium pipe target not only to compactness, hardness and
Can there is the highest requirement by processing type, the interior tissue uniformity of material also be had the highest requirement simultaneously.
Tungsten titanium pipe target with hollow rustless steel hollow pipe as penstock, its manufacture method has a lot, main
Use casting metallurgy.Casting is metallurgical for be directly cast in solid rustless steel penstock by tungsten-titanium alloy, so
The described tungsten-titanium alloy of rear clamping, carries out the machinings such as turnery processing to described rustless steel penstock, makes described
Rustless steel penstock becomes hollow pipe, and makes the size and dimension of described rustless steel hollow pipe meet final finished
Demand.Described method is only used for the target material that fusing point is relatively low, and semiconductor sputtering target material manufacture
Tungsten and the target material fusing point such as tungsten alloy, Cr, Mo and ITO are higher, use the method cost that founding is metallurgical
To be greatly improved.Secondly, during general casting process, target material is in the temperature not phase of all directions
With, it being susceptible to segregation phenomena, the target material composition resulted in is uneven.In order to overcome this problem,
Occurring in that the manufacture using the method for powder metallurgy to realize tungsten titanium target material in industry, described powder metallurgy is logical
Cross and produce metal dust (adding or without non-metal powder), implement to shape and sintering, make material
Or the processing method of goods.Powder metallurgy has chemical composition and machinery, physical property, and the institute of uniqueness
Stating the pipe target forming temperature that technique compares casting metallurgical lower, temperature is generally the 60% of target material fusing point
To 70%, these performances can realize porous, the half fine and close or densification entirely that traditional casting process cannot be made
, microstructure can be used for the tungsten titanium pipe target that quasiconductor target makes uniformly.
In concrete powder metallurgical technique, typically use hot-pressing sintering technique.Described hot-pressing sintering technique
Be specially and ready powder filled in a particular mold, be subsequently placed in vacuum hotpressing stove, in vacuum or
Under person's inert gas conditions, using forcing press, act on mould by upper and lower two pressure heads, heats up in limit
Pressurizeing in limit, until pressure and temperature all reaches setting value, keeps one under the conditions of the pressure and temperature set
Furnace cooling after the section time, comes out of the stove.
But, during realizing hot pressed sintering, needs match according to the size design of tungsten titanium pipe target
Mould, tungsten titanium pipe target size receives the restriction of die size and intensity, and this mould is costly and relatively rapid wear
Consumption.Additionally, uniaxially pressurize time during hot pressed sintering, its action direction is only single direction, uses
The uniformity of the internal organizational structure of the tungsten titanium pipe target that described method is made is poor, consistency is relatively low, it is impossible to
The sputtering technology that satisfied requirement is the highest.
The most accordingly, it is necessary to propose the manufacture method of a kind of new tungsten titanium pipe target, to overcome
The defect of prior art.
Summary of the invention
The problem that the present invention solves is to provide the manufacture method of a kind of new tungsten titanium pipe target, thus improves and partly lead
The body consistency of tungsten titanium pipe target and uniform texture.
For solving the problems referred to above, the present invention provides the manufacture method of a kind of tungsten titanium pipe target.Comprise the steps:
Tungsten, titanium mixed-powder and rustless steel hollow pipe are provided；
Described tungsten, titanium mixed-powder and described rustless steel hollow pipe are carried out isostatic cool pressing technique, formed tungsten,
Titanium mixed-powder and rustless steel initial blank；
Described tungsten, titanium mixed-powder and rustless steel initial blank are loaded vacuum canning and to described vacuum packet
After set evacuation, described tungsten, titanium mixed-powder and rustless steel initial blank are carried out heat and other static pressuring processes,
Form tungsten-titanium alloy；
Remove described vacuum canning, it is thus achieved that with described tungsten-titanium alloy as target, with described rustless steel hollow pipe
Tungsten titanium pipe target for penstock.
Optionally, the technological temperature of described isostatic cool pressing technique is 25 DEG C to 200 DEG C, and environmental stress is
150MPa to 160MPa, the process time under described technological temperature and environmental stress be 10 minutes to 30
Minute.
Optionally, described heat and other static pressuring processes includes heating technique and HIP sintering technique.
Optionally, the technological temperature of described heating technique is 250 DEG C to 500 DEG C, is incubated 3 at said temperatures
Hour to 4 hours.
Optionally, the technological temperature of described HIP sintering technique is 1050 DEG C to 1200 DEG C, environment pressure
Strong is 150MPa to 180MPa, the process time under described technological temperature and environmental stress be 3 hours to 6
Hour.
Optionally, during described vacuum canning evacuation, the vacuum of described vacuum canning is at least
For 2E-3Pa, and described vacuum canning is made to keep shutting state during described heat and other static pressuring processes.
Optionally, the tungsten after described isostatic cool pressing, titanium mixed-powder and rustless steel initial blank are loaded very
After empty jacket, before described vacuum canning evacuation, described manufacture method also includes: use argon arc welding
The mode connect shuts described vacuum canning；A deaeration pipe is drawn at described vacuum canning；
Described vacuum step carries out evacuation by described deaeration pipe to vacuum canning.
Optionally, before removing described vacuum canning, also include: described vacuum canning is gone pressure cooling.
Optionally, it is provided that tungsten, the step of titanium mixed-powder include: tungsten powder and titanium valve are provided；Use mixed powder
Machine carries out mechanical mixture to tungsten, titanium powder.
Optionally, the mass ratio of described tungsten powder and titanium valve is 8.95:1 to 9.05:1.
Optionally, it is provided that tungsten, the step of titanium mixed-powder also include: carrying out mechanical mixture with mixed powder machine
Before, it is filled with in mixed powder machine in noble gas makes mixed powder machine and reaches malleation.
Optionally, during tungsten powder and titanium valve are carried out mechanical mixture with mixed powder machine, add in mixed powder machine
Entering medium ball, described medium ball is titanium ball or tungsten ball.
Optionally, the mass ratio of described medium ball and described tungsten, titanium mixed-powder is 2.5:1 to 3.5:1.
Compared with prior art, technical scheme has the advantage that first employing isostatic cool pressing work
Skill carries out densification first and preforming to tungsten, titanium mixed-powder and rustless steel hollow pipe, forms half fine and close
Tungsten, titanium mixed-powder and rustless steel initial blank, make follow-up heat and other static pressuring processes to tungsten, titanium mixing
Powder and rustless steel initial blank can carry out more preferable densification；Then to tungsten, titanium mixed-powder and stainless
Steel initial blank carries out heat and other static pressuring processes, and described heat and other static pressuring processes includes: first described tungsten, titanium are mixed
Close powder and rustless steel initial blank loads in vacuum canning and by described vacuum canning evacuation, then pass through
To described vacuum canning apply each to impartial and omnibearing gas pressure with to described tungsten, titanium mixed-powder
HIP sintering technique is carried out with rustless steel initial blank.By described heat and other static pressuring processes, finally obtain
Obtain pipe target fine and close, consistent internal structure, close to required form.
Further, during using said method to form tungsten titanium pipe target, use vacuum canning rather than mould,
And described jacket unbounded size system, it is to avoid the problem that pipe target size is limited by die size and intensity.
Further, use mixed powder machine that tungsten, titanium powder are carried out mechanical mixture before isostatic cool pressing technique,
Make described tungsten, titanium powder more uniformly mix, prepare composition uniformly, the tungsten of segregation-free, titanium
Mixed-powder, efficiently solves tungsten, titanium mixed-powder causes because the density difference of tungsten powder and titanium valve is relatively big
Segregation lamination, improve processing performance and the mechanical performance of target material.
Further, the penstock of described tungsten titanium pipe target is rustless steel hollow pipe, and its shape meets with size
The finally finished requirement to hollow shape penstock, after described heat and other static pressuring processes, described tungsten titanium pipe target can be direct
One-shot forming, eliminates in prior art and solid rustless steel penstock is carried out the machinings such as turning to obtain
The processing step of hollow pipe, improves the make efficiency of tungsten titanium pipe target.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the manufacture method of the tungsten titanium pipe target of the embodiment of the present invention；
Fig. 2 be the tungsten titanium pipe target of the embodiment of the present invention manufacture method in the technological principle of isostatic cool pressing technique
Figure；
Fig. 3 be the tungsten titanium pipe target of the embodiment of the present invention manufacture method in vacuum canning mould assembling signal
Figure；
Fig. 4 be the tungsten titanium pipe target of the embodiment of the present invention manufacture method in the technological principle of heat and other static pressuring processes
Figure.
Detailed description of the invention
In tungsten titanium pipe target manufacturing process, the method using hot pressed sintering, need the chi according to tungsten titanium pipe target
The mould that very little design matches, therefore tungsten titanium pipe target size receives the restriction of die size and intensity, this mould
Tool costly and is easier to loss.Additionally, uniaxially pressurize time during hot pressed sintering, its action direction
It is only single direction, the uniformity using the internal organizational structure of the tungsten titanium pipe target that described method makes is poor,
Consistency is relatively low, it is impossible to the sputtering technology that satisfied requirement is the highest.
In order to the consistency making described tungsten titanium pipe target is higher, organizational structure evenly, and avoids tungsten titanium pipe target
The problem that size is limited by die size and intensity, the present inventor is first to tungsten, titanium mixed-powder
Carry out isostatic cool pressing technique with rustless steel hollow pipe, form half compactness and the tungsten of preforming, titanium mixed powder
Behind end and rustless steel initial blank, more described tungsten, titanium mixed-powder and rustless steel initial blank are carried out heat
Isostatic pressing process, it is thus achieved that densification, the tungsten titanium pipe target of consistent internal structure.Secondly, described high temperature insostatic pressing (HIP)
Technique uses vacuum canning rather than mould, it is to avoid tungsten titanium pipe target size is by die size and intensity
The problem limited.Again, described rustless steel hollow pipe can be designed to final finished shape according to product specification
State (for hollow shape), eliminates in prior art and is used to make rustless steel hollow pipe become hollow shape
The mechanical processing steps such as turning, improve the make efficiency of tungsten titanium pipe target.
Understandable, below in conjunction with the accompanying drawings for enabling the above-mentioned purpose of the present invention, feature and advantage to become apparent from
The specific embodiment of the present invention is described in detail.
Refer to the flow process of manufacture method one embodiment that Fig. 1, Fig. 1 are the tungsten titanium pipe targets of the embodiment of the present invention
Schematic diagram, the manufacture method of the present embodiment tungsten titanium pipe target includes following basic step:
Step S1: tungsten powder, titanium valve and rustless steel hollow pipe are provided；
Step S2: mixed with titanium valve by tungsten powder, forms tungsten, titanium mixed-powder；
Step S3: tungsten, titanium mixed-powder and rustless steel hollow pipe are carried out isostatic cool pressing technique, formed tungsten,
Titanium mixed-powder and rustless steel initial blank；
Step S4: the tungsten after isostatic cool pressing, titanium mixed-powder and rustless steel initial blank are loaded vacuum packet
In set, then described vacuum canning is carried out evacuation；
Step S5: heat the vacuum canning after evacuation and be incubated, completes densification again；
Step S6: carry out heat to completing the tungsten of densification again, titanium mixed-powder and rustless steel initial blank
Isostatic sintering technique；
Step S7: vacuum canning is gone pressure cooling；
Step S8: remove vacuum canning, it is thus achieved that tungsten titanium target pipe.
In order to the manufacture method of the tungsten titanium pipe target of the embodiment of the present invention is better described, below in conjunction with reference
Fig. 2 to Fig. 4, is further described the specific embodiment of the present invention.
First step S1, it is provided that tungsten powder, titanium valve and rustless steel hollow pipe.
In the present embodiment, described tungsten powder and titanium valve are the high-purity powder of purity more than 99.9%, and described tungsten
The mass ratio of powder and titanium valve is 8.95:1 to 9.05:1.The granularity of described tungsten powder is 4 μm to 5 μm, described titanium valve
Granularity be that 40 μm are to 45 μm.
It should be noted that the size of mesh of the screen cloth owing to using when preparing tungsten powder and titanium valve is 45 μm,
Therefore it is respectively less than 45 μm by its granularity of powder of described sieve mesh.
In the present embodiment, the material of the rustless steel hollow pipe used is 304 rustless steels, and described rustless steel is resistance to
High temperature more than 800 DEG C, has good processability, a feature that toughness is high.
Then perform step S2, tungsten powder is mixed with titanium valve, form tungsten, titanium mixed-powder.
In the present embodiment, formed described tungsten, titanium mixed-powder concrete technology for by tungsten powder and titanium valve according to
Mass ratio is that the ratio of 8.95:1 to 9.05:1 carries out mechanical mixture with mixed powder machine, and concrete mass ratio is according to pipe target
Size depending on.
The incorporation time of described mechanical mixture is 23 hours to 25 hours.When the mixing of described mechanical mixture
Between little less than 23 constantly, owing to the mixing of described tungsten powder and titanium valve is uniform not enough, easily cause described tungsten,
The segregation lamination that titanium mixed-powder causes because the density difference of tungsten powder and titanium valve is relatively big, and then reduce
The processing performance of target material and mechanical performance；When the incorporation time of described mechanical mixture is little more than 25 constantly,
Owing to described tungsten powder and titanium valve the most fully and uniformly mix, will not generation effect again, waste the process time,
Increase process costs.
In the present embodiment, described blending processes of powders uses dry pigmentation.In the mixing carrying out described tungsten powder and titanium valve
Before, the present embodiment is also filled with in mixed powder machine in noble gas makes mixed powder machine and reaches malleation, to get rid of mixed powder
Air in machine cavity body, is so possible to prevent described tungsten powder and titanium valve during mixed powder to aoxidize.This reality
Executing the noble gas used in example is argon, ensures that argon is full of mixed powder machine cavity body in mixed process, and
The pressure of described argon is more than atmospheric pressure, in order to avoid air penetrates in mixed powder machine cavity body.
In order to preferably by tungsten powder and titanium valve mix homogeneously, in the mixed process carrying out described tungsten powder and titanium valve
In, add medium ball, after mixed powder is uniform, described medium ball is taken out.In the present embodiment, in order to prevent
Introducing other impurity, the material of described medium ball is identical with tungsten powder or titanium valve material, and the most described medium ball is
Titanium ball or tungsten ball.When described medium ball is titanium ball, described titanium ball and described tungsten, the matter of titanium mixed-powder
Amount ratio is 2.5:1 to 3.5:1；When described medium ball is tungsten ball, described tungsten ball and described tungsten, titanium mixing
The mass ratio of powder is 2.5:1 to 3.5:1.
In conjunction with reference to Fig. 2, perform step S3, tungsten, titanium mixed-powder 201 are loaded in hollow mould, mould
Tool center place rustless steel hollow pipe 202, insert in cold isostatic press, by described mould apply from
The pressure of all directions, carries out cold etc. quiet to described tungsten, titanium mixed-powder 201 and rustless steel hollow pipe 202
Pressure technique, completes densification first, forms tungsten, titanium mixed-powder and rustless steel initial blank 203.Wherein,
It is hollow shape that described rustless steel hollow pipe 202 meets the design specification requirement to penstock shape, i.e. penstock.
In the present embodiment, the technological temperature of described isostatic cool pressing technique is room temperature 25 DEG C to 200 DEG C, described cold
The pressure during isostatic pressing process applied described mould is 150MPa to 160MPa, at described process warm
Process time under degree and pressure is 10 minutes to 30 minutes, due to described isostatic cool pressing technique all directions
Temperature, pressure are the most identical, by the molding in advance of described technique, obtain half cause that consistency is about about 60%
Close tungsten, titanium mixed-powder and rustless steel initial blank 203, makes the subsequent forming technique can be more preferable simultaneously
Fine and close.
When environmental stress is less than 10 minutes less than 150MPa or process time, owing to pressure not or applies
The time of pressure falls short of, it is impossible to reach the tungsten of half densification, titanium mixed-powder and rustless steel initial blank 203.
Owing to the technological temperature of isostatic cool pressing technique is room temperature, isostatic cool pressing product reaches certain at said temperatures
Increasing pressure after consistency or the process time is difficult to further densification, therefore pressure is higher than 160MPa or technique
Time, more than within 30 minutes, the most not producing effect, makes cost waste the process time while becoming greatly.
In conjunction with reference to Fig. 3, perform step S4, at the beginning of tungsten good for isostatic cool pressing, titanium mixed-powder and rustless steel
Beginning blank 203 loads in jacket 301, shuts described jacket 301, and described jacket 301 draws a deaeration pipe
305 and by described deaeration pipe 305 evacuation, form vacuum canning 301'.
In the present embodiment, described jacket 301 includes jacket thin-walled 302, jacket lower cover 303 and jacket upper cover
Plate 304；Described jacket 301 uses the stainless steel welded molding that thickness is 2mm to 3mm.Described not
The jacket intensity of rust steel matter is relatively big, is possible to prevent described jacket under the heating condition of subsequent technique to occur
Deformation or cracking.
In the present embodiment, first by described jacket thin-walled 302 and jacket lower cover by the way of argon arc welding
303 weld, and then tungsten good for isostatic cool pressing, titanium mixed-powder and rustless steel initial blank 203 are filled
Enter in the jacket of unwelded described jacket upper cover plate 304, after covering jacket upper cover plate 304, pass through argon arc welding again
Jacket 301 is soldered to the upper surface of described jacket thin-walled 302 by the mode connect, and makes described jacket 301 be sealed
Extremely.
Described jacket 301 draws a deaeration pipe 305, is connected with vacuum equipment by deaeration pipe 305, will be equipped with
The jacket 301 of tungsten, titanium mixed-powder and rustless steel initial blank 203 is placed in heating furnace, opens vacuum
Equipment forms vacuum canning 301' to described jacket 301 evacuation, makes the vacuum in described vacuum canning 301'
Reach 2E-3Pa.
In conjunction with reference to Fig. 3, perform step S5, the vacuum canning 301' after described evacuation is heated also
Insulation, completes densification again.
In the present embodiment, when the vacuum in described vacuum canning 301' reaches 2E-3Pa, start heating furnace
Described vacuum canning 301' is heated；Described vacuum canning 301' is heated to 250 DEG C extremely by room temperature
After 500 DEG C, insulation 3 hours to 4 hours at said temperatures, complete densification again, form consistency more preferable
Tungsten, titanium mixed-powder and rustless steel initial blank 203.
In heating furnace intensification and insulating process, vacuum equipment is constantly in opening, so that described
Vacuum in vacuum canning 301' is all the time maintained at least at 2E-3Pa；After insulation terminates, take from heating furnace
Go out described vacuum canning 301', close described deaeration pipe 305 when continuing to keep its inner vacuum,
Described vacuum canning 301' is made to be internally formed an airtight vacuum environment.
In conjunction with reference to Fig. 4, perform step S6, tungsten, titanium mixed-powder and rustless steel initial blank 203 are entered
Row HIP sintering technique.
In the present embodiment, will be equipped with tungsten, titanium mixed-powder and rustless steel initial blank 203 and hold one's breath true
Empty jacket 301' is placed in high temperature insostatic pressing (HIP) stove, first carries out increasing temperature and pressure, makes technological temperature reach 1050 DEG C extremely
1200 DEG C, environmental stress reach 150MPa to 180MPa, make described vacuum canning 301' by from each to
The gas pressure of impartial and omnibearing 150MPa to 180MPa；After increasing temperature and pressure step, described
It is incubated 3 hours to 6 hours under technological temperature and environmental stress.
In the present embodiment, technological temperature, environmental stress and temperature retention time are done optimized collocation.
When described technological temperature is less than 1050 DEG C, owing to temperature is inadequate, cause described tungsten, titanium mixed powder
Cannot be diffused up hill and dale, after affecting sinter molding between end and each material of rustless steel initial blank 203
Tungsten titanium pipe target mass；When described technological temperature higher than 1200 DEG C time, too high technological temperature make described very
Empty jacket 301' is in rugged environment, easily causes deformation or the cracking of vacuum canning 301', what is more
Described vacuum canning 301' fusing may be made or make described vacuum canning 301' and described tungsten, titanium mixed powder
End reacts, and causes scrapping of tungsten titanium pipe target.
When described environmental stress less than 150MPa time, due on described vacuum canning 301' apply power not
Enough big, cause described tungsten, titanium mixed-powder and rustless steel initial blank 203 cannot sinter molding up hill and dale,
And the consistency of the tungsten titanium pipe target finally obtained is poor；When described environmental stress is more than 180MPa, for
It is complete the described tungsten of best sinter molding, titanium mixed-powder and rustless steel initial blank 203, it is difficult to
Further fine and close, then improve environmental stress to obtaining that consistency is high, the tungsten titanium pipe target of consistent internal structure
Through nonsensical, wasting the energy on the contrary, the most too high environmental stress may make described vacuum canning 301'
Deform upon or ftracture.
When described temperature retention time is little less than 3 constantly, owing to executing the stressed time under proper temperature and pressure
Fall short of, cause described tungsten, titanium mixed-powder and rustless steel initial blank 203 cannot fully sintered molding,
The consistency of the tungsten titanium pipe target obtained is poor；When temperature retention time is little more than 6 constantly, best for being complete
The described tungsten of sinter molding, titanium mixed-powder and rustless steel initial blank 203, it is difficult to fine and close further,
It is further added by temperature retention time to waste the energy on the contrary, reduce the manufacture efficiency of tungsten titanium pipe target.
It should be noted that during increasing temperature and pressure, heating rate can be 250 DEG C/H to 350 DEG C/H,
Rate of pressure rise can be 20MPa/H to 30MPa/H.
When heating rate is higher than 350 DEG C/H, the furnace temperature in high temperature insostatic pressing (HIP) stove is not easy diffusion, causes heat etc.
Non-uniform temperature in static pressure stove, produces furnace temperature deviation, affects described tungsten, titanium mixed-powder and rustless steel
The sinter molding of initial blank 203；When heating rate is less than 250 DEG C, the heating-up time is long, causes work
The skill time lengthens, and production efficiency reduces, and production cost uprises, and the most described heating rate is preferably 250 DEG C/H
To 350 DEG C/H.In order to coordinate described heating rate, described rate of pressure rise is preferably 20MPa/H extremely
30MPa/H, makes described technological temperature and environmental stress almost reach setting value within the same time.
Perform step S7, to described vacuum canning 301'(as shown in Figure 3) go pressure cooling.
In the present embodiment, described tungsten, titanium mixed-powder complete high temperature insostatic pressing (HIP) with rustless steel initial blank 203 and become
After type, close high temperature insostatic pressing (HIP) stove, make described vacuum canning 301'(as shown in Figure 3) naturally cool to stove
Room temperature 25 DEG C to 200 DEG C, The method avoids the rapid drawdown of temperature so that the tungsten-titanium alloy target after molding
More solid.
Perform step S8, remove described vacuum canning 301'(as shown in Figure 3), it is thus achieved that closed by described tungsten titanium
The tungsten titanium pipe target that gold target material and rustless steel penstock are constituted.
By described vacuum canning 301'(as shown in Figure 3) after furnace cooling, added by machineries such as turnery processing
The sheath material on described tungsten titanium target material surface is removed by work technique, it is thus achieved that with described tungsten-titanium alloy as target,
Tungsten titanium pipe target with described 304 rustless steel hollow pipes as penstock.
Disclose as above with preferred embodiment although the present invention is own, but the present invention is not limited to this.Any
Skilled person, without departing from the spirit and scope of the present invention, all can make various changes or modifications,
Therefore protection scope of the present invention should be as the criterion with claim limited range.
Claims (13)
1. the manufacture method of a tungsten titanium pipe target, it is characterised in that including:
Tungsten, titanium mixed-powder and rustless steel hollow pipe are provided；
Described tungsten, titanium mixed-powder and described rustless steel hollow pipe are carried out isostatic cool pressing technique, formed tungsten,
Titanium mixed-powder and rustless steel initial blank；
Described tungsten, titanium mixed-powder and rustless steel initial blank are loaded vacuum canning and to described vacuum packet
After set evacuation, described tungsten, titanium mixed-powder and rustless steel initial blank are carried out heat and other static pressuring processes,
Form tungsten-titanium alloy；
Remove described vacuum canning, it is thus achieved that with described tungsten-titanium alloy as target, with described rustless steel hollow pipe
Tungsten titanium pipe target for penstock.
2. the manufacture method of tungsten titanium pipe target as claimed in claim 1, it is characterised in that described isostatic cool pressing work
The technological temperature of skill is 25 DEG C to 200 DEG C, and environmental stress is 150MPa to 160MPa, in described technique
Process time at temperature and environmental stress is 10 minutes to 30 minutes.
3. the manufacture method of tungsten titanium pipe target as claimed in claim 1, it is characterised in that described high temperature insostatic pressing (HIP) work
Skill includes heating technique and HIP sintering technique.
4. the manufacture method of tungsten titanium pipe target as claimed in claim 3, it is characterised in that described heating technique
Technological temperature is 250 DEG C to 500 DEG C, at said temperatures insulation 3 hours to 4 hours.
5. the manufacture method of tungsten titanium pipe target as claimed in claim 3, it is characterised in that described high temperature insostatic pressing (HIP) burns
The technological temperature of knot technique is 1050 DEG C to 1200 DEG C, and environmental stress is 150MPa to 180MPa,
Process time under described technological temperature and environmental stress is 3 hours to 6 hours.
6. the manufacture method of tungsten titanium pipe target as claimed in claim 3, it is characterised in that to described vacuum canning
During evacuation, the vacuum of described vacuum canning is at least 2E-3Pa, and at described high temperature insostatic pressing (HIP)
Technical process make described vacuum canning keep shutting state.
7. the manufacture method of tungsten titanium pipe target as claimed in claim 1, it is characterised in that also include: by described
After tungsten after isostatic cool pressing, titanium mixed-powder and rustless steel initial blank load vacuum canning, to described very
Before empty jacket evacuation, the mode of argon arc welding is used to shut described vacuum canning；In described vacuum packet
A deaeration pipe drawn by set；
Described vacuum step carries out evacuation by described deaeration pipe to vacuum canning.
8. the manufacture method of tungsten titanium pipe target as claimed in claim 1, it is characterised in that also include: remove institute
Before stating vacuum canning, described vacuum canning is gone pressure cooling.
9. the manufacture method of tungsten titanium pipe target as claimed in claim 1, it is characterised in that described offer tungsten, titanium
The step of mixed-powder includes: provide tungsten powder and titanium valve；Use mixed powder machine that tungsten, titanium powder are carried out machinery
Mixing.
10. the manufacture method of tungsten titanium pipe target as claimed in claim 9, it is characterised in that described tungsten powder and titanium valve
Mass ratio be 8.95:1 to 9.05:1.
The manufacture method of 11. tungsten titanium pipe targets as claimed in claim 9, it is characterised in that described offer tungsten, titanium
The step of mixed-powder also includes: before carrying out mechanical mixture with mixed powder machine, is filled with inertia in mixed powder machine
Gas reaches malleation in making mixed powder machine.
The manufacture method of 12. tungsten titanium pipe targets as claimed in claim 9, it is characterised in that tungsten powder and titanium valve are used
During mixed powder machine carries out mechanical mixture, adding medium ball in mixed powder machine, described medium ball is titanium ball
Or tungsten ball.
The manufacture method of 13. tungsten titanium pipe targets as claimed in claim 12, it is characterised in that described medium ball and
Described tungsten, the mass ratio of titanium mixed-powder are 2.5:1 to 3.5:1.
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| CN201510347491.1A CN106319457A (en) | 2015-06-19 | 2015-06-19 | Manufacturing method of tungsten titanium tube target |
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| CN106312071A (en) * | 2015-06-19 | 2017-01-11 | 宁波江丰电子材料股份有限公司 | A tungsten-titanium tube target manufacture method |
| CN108580905A (en) * | 2018-01-22 | 2018-09-28 | 宁波江丰电子材料股份有限公司 | Preparation method, chromium tantalum-titanium alloy sputtering target material and the application of chromium tantalum-titanium alloy sputtering target material |
| CN109097747A (en) * | 2018-09-12 | 2018-12-28 | 芜湖映日科技有限公司 | A kind of production method of cast target |
| CN111155061A (en) * | 2018-11-07 | 2020-05-15 | 宁波江丰电子材料股份有限公司 | Preparation method of WTi alloy target |
| CN111299572A (en) * | 2019-11-28 | 2020-06-19 | 天钛隆（天津）金属材料有限公司 | Production method of titanium and titanium alloy seamless tube |
| CN111375881A (en) * | 2018-12-28 | 2020-07-07 | 宁波江丰电子材料股份有限公司 | Method for manufacturing target material |
| CN111604503A (en) * | 2020-06-12 | 2020-09-01 | 钢铁研究总院 | FeCrAl stainless steel composite pipe blank and preparation method thereof |
| CN114086130A (en) * | 2021-11-16 | 2022-02-25 | 宁波江丰电子材料股份有限公司 | Preparation method of tungsten-titanium alloy tube target |
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| CN111604503A (en) * | 2020-06-12 | 2020-09-01 | 钢铁研究总院 | FeCrAl stainless steel composite pipe blank and preparation method thereof |
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