A kind of big L/D ratio TiAl pipe target material manufacturing process
Technical field
The present invention relates to a kind of big L/D ratio TiAl pipe target material manufacturing process, belong to use in magnetron sputtering coating high-performance metal pipe preparation of target materials technical field.
Background technology
Along with the fast development of the industries such as decoration film coating, integrated circuit, flat-panel screens and tool surfaces coating, get more and more to the demand of plated film sputtering target material, wherein TiAl target is one of material of tool coating and decoration film coating industry large usage quantity.Current target product is mainly divided into flat target and pipe target, and compared with planar targets, pipe target has the advantages such as utilization rate is high, plated film continuity is good, film coating composition is even, and be desirable sputtering target material, market demand is huge.Current terminal target plated film manufacturer just progressively carries out the update of magnetron sputtering apparatus, be transitioned into from use conventional planar target and use swivelling pipe target, therefore pipe target is becoming the standard selection of magnetron sputtering apparatus, and following pipe target market development potential is huge.
At present, domestic TiAl pipe target material mainly adopts melting and hot-spraying technique technology to produce, smelting technology can only prepare the TiAl pipe target material of low-aluminum-content, if aluminium content is higher than 50%, material segregation is serious, and difficulty is large, yield rate is low to prepare big L/D ratio pipe target (length >=1000mm).Spraying technology shaping TiAl pipe target material also exists that density is low, stock utilization is low and the shortcoming such as oxygen content is high, can only be applied to the low and middle-end coated product lower to film quality requirement, far cannot meet the quality requirement of high-end coated product to target.External high-quality TiAl pipe target material adopts advanced magnetic levitation melting technology to produce, but expensive.Therefore, for the development of high-quality big L/D ratio TiAl integral tube target (length >=1000mm) forming technique, not still to existing target product technology of preparing innovation, simultaneously to the significantly raising of plated film industry product quality, promote the update of product, have important practical significance.
Summary of the invention
The object of the invention is to the above-mentioned deficiency overcoming prior art, a kind of big L/D ratio TiAl pipe target material manufacturing process is provided, TiAl pipe target material product material prepared by the method organizes that crystal grain is tiny, oxygen content is low, density is high, steady quality is reliable, in the batch production of the overall TiAl pipe target material of high-end coated product big L/D ratio, have clear superiority.
Above-mentioned purpose of the present invention is mainly achieved by following technical solution:
A kind of big L/D ratio TiAl pipe target material manufacturing process, comprises the steps:
Step (one), assembling thin wall wrap model: described thin wall wrap model comprises interior jacket, outer jacket, jacket bottom, jacket upper cover, wireway and penstock; First interior jacket is positioned over outer jacket inner, jacket bottom welds with interior jacket, outsourcing cover, the location of jacket and outer jacket in realizing, and then penstock is sleeved on the outer surface of interior jacket, last outsourcing puts punching, welding wireway;
Step (two), Ti powder is mixed with Al powder after, be packed in the thin wall wrap model that step () assembles, and carry out soldering and sealing after covering jacket upper cover, realize the sealing of thin wall wrap model, wherein Ti Powder Particle Size is 100-200 order, and Al Powder Particle Size is below 325 orders;
Step (three), thin wall wrap model is positioned in heat-treatment furnace and heats, and vacuum degassing, outgassing temperature is 300 DEG C-400 DEG C, ensures that the vacuum in the thin wall wrap model after degasification is greater than 10
-3pa;
Step (four), thin wall wrap model is positioned in high temperature insostatic pressing (HIP) stove and carries out densification;
Step (five), the thin wall wrap model after densification removed in jacket and outer jacket, and carry out the TiAl pipe target material integrally formed with penstock that machining obtains required size.
In above-mentioned big L/D ratio TiAl pipe target material manufacturing process, after being mixed with Al powder by Ti powder in step (two), the concrete steps be packed in the thin wall wrap model assembled are as follows:
(a), by thin wall wrap model horizontal positioned, then the Ti powder mixed and Al powder are adopted load shovel and deliver to bottom thin wall wrap model, then thin wall wrap model is erected vertical placement, filling shovel is extracted out, completes first time powder packing;
(b), afterwards by thin wall wrap model 90-degree rotation, make thin wall wrap model horizontal positioned, repeat step (a), complete second time powder packing, the like, complete four fillings altogether;
(c), thin wall wrap model is vertically put vertical, by the powder pressing in thin wall wrap model, complete first round powder packing;
D (), repetition step (a)-(c), complete second and take turns powder packing, the rest may be inferred, until the full thin wall wrap model of filling.
In above-mentioned big L/D ratio TiAl pipe target material manufacturing process, when carrying out the welding of jacket upper cover in step (two), often weld 20-30mm weld seam and stop, cooling thin wall wrap model, weld again afterwards, cause powder to react to prevent because of the heat of welding generation.
In above-mentioned big L/D ratio TiAl pipe target material manufacturing process, the parameter that the middle thin wall wrap model of step (four) carries out densification in high temperature insostatic pressing (HIP) stove is: temperature 480 DEG C ~ 550 DEG C, pressure 100 ~ 110MPa, temperature retention time 2 ~ 5h.
In above-mentioned big L/D ratio TiAl pipe target material manufacturing process, penstock is stainless steel tube, titanium pipe or carbon steel pipe.
In above-mentioned big L/D ratio TiAl pipe target material manufacturing process, the length of penstock is less than the length of interior jacket, outer jacket, and length difference is 60-80mm.
In above-mentioned big L/D ratio TiAl pipe target material manufacturing process, the material of interior jacket, outer jacket, jacket bottom, jacket upper cover and wireway is aluminium.
In above-mentioned big L/D ratio TiAl pipe target material manufacturing process, after being mixed with Al powder by Ti powder in step (two), mix powder granulation through vacuum, make powder in filling process, have higher compacted density and uniform distribution.
The present invention compared with prior art has following beneficial effect:
(1) the present invention has carried out innovative design to the structure of the thin wall wrap model adopted in forming process, adopt the thin wall wrap model be made up of interior jacket, outer jacket, penstock, jacket upper cover, lower cover and wireway, and carry out preferably to the material of thin wall wrap model, ensure that thin wall wrap model possesses good weldability, and the entirety realizing TiAl target and penstock is bound, make powder fill convenient simultaneously, and ensure that formed product quality;
(2) the present invention adopts special powder packing technique, four powder packings are adopted in the powder packing process that each is taken turns, and type of feed is taken turns in employing more, until the full powder of filling in thin wall wrap model, ensure that pipe target dress powder density and the uniformity, avoid the uneven TiAl pipe target material uneven thickness caused of dress powder, thus ensure that the linearity of TiAl pipe target material;
(3) the present invention chooses suitable Ti, Al Powder Particle Size proportioning, powder processing techniques in early stage (vacuum mixes powder granulation) and powder packing technique, prepare uniform composition, Ti, Al mixed-powder of segregation-free, efficiently solves the segregation lamination that Ti, Al powder causes because density difference is comparatively large;
(4) the present invention is according to Ti, Al powder characteristics, adopt fine aluminium as sheath material and reasonably press temperature and temperature retention time, can ensure that powder does not react with jacket, realize densified shaping, well can be connected with stainless steel penstock again, realize the binding of pipe overall target;
(5) the present invention is optimized Vacuum Heat degasification and the densified forming parameters of high temperature insostatic pressing (HIP) by lot of experiments, ensure at the density of compressing rear TiAl pipe target material and linearity, and the big L/D ratio TiAl pipe target material that material grains is tiny, uniform composition, density are high, quality stability is good can be obtained
(6) a large number of experiments show that TiAl pipe target material density >=99% prepared by present invention process method, oxygen content≤1000ppm, grain size≤50um.
Accompanying drawing explanation
Fig. 1 is thin wall wrap model assembling schematic diagram in TiAl pipe target material manufacturing process of the present invention;
Fig. 2 is TiAl pipe target material manufacturing process flow chart of the present invention.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail:
Be of a size of to manufacture one
tubulose TiAl target is example, and the detailed description of the invention of this method is described.
Step (one), thin wall wrap model design and process, assembling
According to shaping TiAl pipe target shape of product, size, consider the weldability of the amount of contraction of powder, target and penstock monolithic molding and jacket, design thin wall wrap model, selects applicable sheath material and version.Thin wall wrap model of the present invention comprises interior jacket 1, outer jacket 2, jacket bottom 3, jacket upper cover 4, wireway 5 and penstock 6, be illustrated in figure 1 thin wall wrap model assembling schematic diagram in TiAl pipe target material manufacturing process of the present invention, first the outer jacket 2 jacket in drum 1 being positioned over drum is inner, jacket bottom 3 welds with interior jacket 1, outer jacket 2, in realizing, jacket 1 and the location of outer jacket 2, stay jacket upper cover 4 not fill (staying dress powder position).Then penstock 6 is sleeved on the outer surface of interior jacket 1, finally punching on jacket 2 outside, welding wireway 5, whole jacket carries out airtight test.
In the present embodiment, penstock 6 adopts stainless steel material manufacture, and in all the other, jacket 1, outer jacket 2, jacket bottom 3, jacket upper cover 4, wireway 5 are pure aluminum material manufacture.
In the present embodiment, the length of stainless steel penstock 6 is less than the length of interior jacket 1, outer jacket 2, and length difference is 60-80mm.Namely stainless steel penstock 6 two ends respectively reserve 30-40mm surplus, prevent in the densified process of the test of subsequent thermal isostatic pressed, and in causing because stainless steel penstock 6 is different from jacket aluminum amount of contraction, jacket 1 and outer jacket 2 break.
Step (two), raw material Ti powder, Al powder are selected and pretreatment
By selecting specific powder purity and grain size proportion, and mix powder granulation through vacuum, make powder in filling process, have higher compacted density and uniform distribution, and for post forming TiAl pipe target material, there is good structural state and density lays the first stone.Ensure that final material meets the requirement of target properties of product, select purity to be the Ti powder of 99.9%, the Al powder of 99.9% in the present embodiment, Ti Powder Particle Size is 100-200 order.Al Powder Particle Size is below 325 orders (-325 orders).
Step (three), powder packing and soldering and sealing
Detailed process is as follows:
A the Ti powder mixed and Al powder by thin wall wrap model horizontal positioned, then adopt and load shovel and deliver to bottom thin wall wrap model by (), then thin wall wrap model is slowly erected vertical placement, extracted out by filling shovel, complete first time powder packing;
By thin wall wrap model 90-degree rotation after (b), make thin wall wrap model horizontal positioned, repeat step (a), complete second time powder packing, the like, complete four fillings altogether;
C thin wall wrap model is vertically put vertical by (), by the powder pressing in thin wall wrap model, complete first round powder packing;
D () repeats step (a)-(c), complete second and take turns powder packing, the rest may be inferred, until the full thin wall wrap model of filling.
Whole powder packing process is not knocked, and produces layering to prevent powder because proportion is inconsistent.Repeat whole process and finally complete powder packing.
After filling, cover jacket upper cover 4 and weld, often welding the stopping of 20-30mm weld seam, cooling thin wall wrap model, proceeds welding afterwards again, causes powder to react to prevent because of the heat of welding generation.
Step (four), Vacuum Heat degasification
The hot degasification of TiAl pipe thin wall wrap model is carried out in heat-treatment furnace, adopts vacuum pump set to carry out degasification, protects simultaneously, be out of shape to prevent aluminium thin wall wrap model under outgassing temperature thin wall wrap model.While heating in degassing procedure, degasification, outgassing temperature is 300 DEG C-400 DEG C, and whole degassing procedure need carry out slow degasification with high vacuum manual gear plate valve, extracts out to prevent the powder in thin wall wrap model.Vacuum in final guarantee thin wall wrap model is greater than 10
-3pa.
Step (five), the densified shaping of high temperature insostatic pressing (HIP)
Thin wall wrap model after vacuum degassing is carried out high temperature insostatic pressing (HIP) densification, according to the heat and other static pressuring processes parameter that moulding material and thin wall wrap model Material selec-tion are optimized.Packaged thin wall wrap model is positioned in high temperature insostatic pressing (HIP) stove and carries out densification; High temperature insostatic pressing (HIP) parameter is adopted to be in the present embodiment: temperature 480 DEG C ~ 550 DEG C, pressure 100 ~ 110MPa, temperature retention time 2 ~ 5h.
Step (six), removal thin wall wrap model
After the densified shaping of high temperature insostatic pressing (HIP), aluminium jacket 1, outer aluminium jacket 2 material in removing by the method for Vehicle Processing, namely obtain high-compactness TiAl pipe and the integrally formed TiAl pipe target material of stainless steel penstock 6.
Step (seven), product fine finishining
Carry out a small amount of fine finishining by TiAl target product design dimensional requirement, namely produce required big L/D ratio TiAl pipe target product.Also comprise subsequent fine processing tube target cylindrical in the present embodiment, join the links such as cutting thread termination and test package.
Be illustrated in figure 2 TiAl pipe target material manufacturing process flow chart in the embodiment of the present invention.
TiAl pipe target material density >=99% prepared by present invention process method, oxygen content≤1000ppm, grain size≤50um.
By reference to the accompanying drawings embodiments of the invention are explained in detail above, but the present invention is not limited to above-described embodiment, in the ken that those of ordinary skill in the art possess, also can make various change under the prerequisite not departing from present inventive concept, as the shape and size etc. of shear web.
Be not described in detail content in description of the present invention and belong to professional and technical personnel in the field's known technology.