CN103071791A - Forming method of TiAl pipe target material in large length-diameter ratio - Google Patents
Forming method of TiAl pipe target material in large length-diameter ratio Download PDFInfo
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Abstract
The invention relates to a forming method of TiAl pipe target material in a large length-diameter ratio. The forming method comprises the following steps of (1) assembling of a sheath die; (2) packing and sealing welding of raw materials of Ti powder and Al powder; (3) vacuum heat degassing; (4) densification forming of hot isostatic pressure; (5) removing of the sheath die; and (6) product fine processing. According to the forming method disclosed by the invention, the structure of the sheath die is subjected to innovation design, excellent welding performance of the sheath die is ensured, the whole binding of the TiAl target material and a back pipe is realized, and segregation-free Ti and Al mixed powder which is uniform in composition is prepared through the optimization selection of raw material powder size and the vacuum material mixing; the powder packing density and the uniformity of the pipe target material are ensured by adopting a special powder packing technology; and the density and the straightness of the TiAl pipe target material after pressing forming can be ensured through optimized technological selection of the vacuum heat degassing and the densification forming.
Description
Technical field
The present invention relates to a kind of big L/D ratio TiAl pipe target 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, more and more with the demand of sputtering target material to plated film, wherein the TiAl target is one of material of tool coating and decoration film coating industry large usage quantity.The target product mainly is divided into flat target and pipe target at present, compares with planar targets, and the pipe target has the advantages such as utilization rate is high, the plated film continuity is good, film coating composition is even, is desirable sputtering target material, and market demand is huge.Terminal target plated film manufacturer just progressively carries out the update of magnetron sputtering apparatus at present, use the swivelling pipe target from using the conventional planar target to be transitioned into, therefore manage the standard selection that target is becoming magnetron sputtering apparatus, the market development of following pipe target has a high potential.
At present, domestic TiAl pipe target mainly adopts melting and hot-spraying technique technology to produce, and smelting technology can only prepare the TiAl pipe target of low-aluminum-content, if aluminium content is higher than 50%, the material segregation is serious, and (length 〉=1000mm) difficulty is large, yield rate is low to prepare big L/D ratio pipe target.Spraying technology shaping TiAl pipe target 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 the film quality requirement, far can't satisfy high-end coated product to the quality requirement of target.External high-quality TiAl pipe target adopts advanced magnetic levitation melting technology to produce, but expensive.Therefore, (length 〉=1000mm) development of forming technique is still to existing target product technology of preparing innovation, simultaneously to the significantly raising of plated film industry product quality for high-quality big L/D ratio TiAl integral tube target, promote the update of product, have important practical significance.
Summary of the invention
The object of the invention is to overcome the above-mentioned deficiency of prior art, a kind of big L/D ratio TiAl pipe target manufacturing process is provided, the TiAl pipe target product material of the method preparation organizes that crystal grain is tiny, oxygen content is low, density is high, steady quality is reliable, manages with the whole TiAl of big L/D ratio at high-end coated product to have clear superiority aspect the batch production of target.
Above-mentioned purpose of the present invention mainly is achieved by following technical solution:
A kind of big L/D ratio TiAl pipe target 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 loam cake, wireway and penstock; At first interior jacket is positioned over outer jacket inner, jacket bottom and interior jacket, outsourcing cover weld, and realize the location of interior jacket and outer jacket, then penstock are sleeved on the outer surface of interior jacket, and last outsourcing puts punching, the welding wireway;
Step (two), with the Ti powder with after the Al powder mixes, be packed in the thin wall wrap model that step () assembles, and carry out soldering and sealing after covering the jacket loam cake, realize the sealing of thin wall wrap model, wherein the Ti Powder Particle Size is the 100-200 order, the Al Powder Particle Size is below 325 orders;
Step (three), thin wall wrap model is positioned in the heat-treatment furnace heats, and vacuum degassing, the degasification temperature is 300 ℃-400 ℃, guarantees that vacuum in the thin wall wrap model after the degasification is greater than 10
-3Pa;
Step (four), thin wall wrap model is positioned over carries out densification in the high temperature insostatic pressing (HIP) stove;
Step (five), the thin wall wrap model after the densification removed in jacket and outer jacket, and carry out that machining obtains required size manage target with the integrally formed TiAl of penstock.
In above-mentioned big L/D ratio TiAl pipe target manufacturing process, in the step (two) with the Ti powder with after the Al powder mixes, the concrete steps that are packed in the thin wall wrap model that assembles are as follows:
(1), with the thin wall wrap model horizontal positioned, adopt the filling shovel to deliver to the thin wall wrap model bottom in the Ti powder that mixes and Al powder again, then thin wall wrap model is erected vertical placement, will load shovel and extract out, finish the powder packing first time;
(2), afterwards with the thin wall wrap model 90-degree rotation, make the thin wall wrap model horizontal positioned, repeating step (1) is finished for the second time powder packing, the like, finish altogether four fillings;
(3), thin wall wrap model is vertically put vertical, with the powder pressing in the thin wall wrap model, finish first round powder packing;
(4), repeating step (1)-(3), finish 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 manufacturing process, when carrying out the welding of jacket loam cake in the step (two), every welding 20-30mm weld seam stops, the cooling thin wall wrap model, weld again afterwards, cause powder to react to prevent because of the heat that welding produces.
In above-mentioned big L/D ratio TiAl pipe target manufacturing process, the middle thin wall wrap model of step (four) carries out densification in the high temperature insostatic pressing (HIP) stove parameter is: 480 ℃～550 ℃ of temperature, pressure 100～110MPa, temperature retention time 2～5h.
In above-mentioned big L/D ratio TiAl pipe target manufacturing process, penstock is stainless steel tube, titanium pipe or carbon steel pipe.
In above-mentioned big L/D ratio TiAl pipe target 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 manufacturing process, the material of interior jacket, outer jacket, jacket bottom, jacket loam cake and wireway is aluminium.
In above-mentioned big L/D ratio TiAl pipe target manufacturing process, in the step (two) with the Ti powder with after the Al powder mixes through the mixed powder granulation of vacuum, so that powder has higher compacted density and uniform distribution in the filling process.
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 that adopts in the forming process, the thin wall wrap model that employing is comprised of interior jacket, outer jacket, penstock, jacket loam cake, lower cover and wireway, and the material of thin wall wrap model carried out preferably, guarantee that thin wall wrap model possesses good weldability, and the integral body that realizes TiAl target and penstock is bound, simultaneously so that powder is filled conveniently, and guaranteed the formed product quality;
(2) the present invention adopts special powder packing technique, in the powder packing process that each is taken turns, adopt four powder packings, and adopt and take turns types of feed more, until the full powder of filling in the thin wall wrap model, pipe target dress powder density and the uniformity have been guaranteed, avoid the inhomogeneous TiAl pipe target uneven thickness that causes of dress powder, thereby guaranteed the linearity of TiAl pipe target;
(3) the present invention chooses suitable Ti, Al Powder Particle Size proportioning, early stage powder-processed technology (vacuum is mixed the powder granulation) and powder packing technique, prepare homogeneous chemical composition, the Ti of segregation-free, Al mixed-powder efficiently solve Ti, Al powder because density differs the segregation lamination that causes greatly;
(4) the present invention is according to Ti, Al powder characteristics, adopt fine aluminium as sheath material and rational press temperature and temperature retention time, can guarantee that powder does not react with jacket, realizes densified moulding, can well be connected with the 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, guarantee density and linearity at compressing rear TiAl pipe target, and can obtain that material grains is tiny, homogeneous chemical composition, density is high, quality stability is good big L/D ratio TiAl pipe target (〉=φ 64 * φ 80 * 1200mm);
(6) TiAl that a large number of experiments show that process preparation of the present invention manages target density 〉=99%, oxygen content≤1000ppm, grain size≤50um.
Description of drawings
Fig. 1 is thin wall wrap model assembling schematic diagram in the TiAl pipe target manufacturing process of the present invention;
Fig. 2 is TiAl pipe target manufacturing process flow chart of the present invention.
The specific embodiment
The present invention is described in further detail below in conjunction with the drawings and specific embodiments:
To make a kind of φ of being of a size of 64 * φ 80 * 1200mm tubulose TiAl target as example, the specific embodiment of this method is described.
Step (one), thin wall wrap model design and processing, assembling
According to shaping TiAl pipe target shape of product, size, consider the weldability of amount of contraction, target and penstock monolithic molding and the jacket of powder, the design thin wall wrap model is selected the sheath material and the version that are fit to.Thin wall wrap model of the present invention comprises interior jacket 1, outer jacket 2, jacket bottom 3, jacket loam cake 4, wireway 5 and penstock 6, be illustrated in figure 1 as thin wall wrap model assembling schematic diagram in the TiAl pipe target manufacturing process of the present invention, at first the interior jacket 1 of drum is positioned over outer jacket 2 inside of drum, jacket bottom 3 welds with interior jacket 1, outer jacket 2, the location of jacket 1 and outer jacket 2 in realizing stays jacket loam cake 4 not fill (staying dress powder position).Then penstock 6 is sleeved on the outer surface of interior jacket 1, punches on the jacket 2 outside at last, welding wireway 5, whole jacket carries out airtight test.
Penstock 6 adopts the stainless steel material manufacturing in the present embodiment, and jacket 1, outer jacket 2, jacket bottom 3, jacket loam cake 4, wireway 5 are the pure aluminum material manufacturing in all the other.
The length of stainless steel penstock 6 is less than the length of interior jacket 1, outer jacket 2 in the present embodiment, and length difference is 60-80mm.Be that stainless steel penstock 6 two ends respectively reserve the 30-40mm surplus, prevent in the densified process of the test of follow-up high temperature insostatic pressing (HIP), because the stainless steel penstock 6 interior jackets that cause 1 different from jacket aluminum amount of contraction break with outer jacket 2.
Step (two), raw material Ti powder, Al powder are selected and preliminary treatment
By selecting specific powder purity and grain size proportion, and through the mixed powder granulation of vacuum, so that powder has higher compacted density and uniformly distribution in the filling process, and target has good structural state and density lays the first stone for post forming TiAl manages.Guarantee that final material satisfies the requirement of target properties of product, selecting purity in the present embodiment is 99.9% Ti powder, 99.9% Al powder, and the Ti Powder Particle Size is the 100-200 order.The Al Powder Particle Size is 325 orders following (325 orders).
Step (three), powder packing and soldering and sealing
Detailed process is as follows:
(1) with the thin wall wrap model horizontal positioned, adopt the filling shovel to deliver to the thin wall wrap model bottom in Ti powder and the Al powder that mixes again, then thin wall wrap model is slowly erected vertical placement, will load shovel and extract out, finish for the first time powder packing;
(2) afterwards with the thin wall wrap model 90-degree rotation, make the thin wall wrap model horizontal positioned, repeating step (1) is finished for the second time powder packing, the like, finish altogether four fillings;
(3) thin wall wrap model is vertically put vertical, with the powder pressing in the thin wall wrap model, finished first round powder packing;
(4) repeating step (1)-(3) are finished second and are taken turns powder packing, and the rest may be inferred, until the full thin wall wrap model of filling.
Whole powder packing process is not knocked, and produces layering because proportion is inconsistent to prevent powder.Whole process repeated is finally finished powder packing.
After filling, cover jacket loam cake 4 and welding, every welding 20-30mm weld seam stops, and the cooling thin wall wrap model is proceeded welding afterwards again, causes powder to react to prevent because of the heat that welding produces.
Step (four), Vacuum Heat degasification
The hot degasification of TiAl pipe thin wall wrap model is carried out in heat-treatment furnace, adopts the vacuum unit to carry out degasification, simultaneously thin wall wrap model is protected, and is out of shape under the degasification temperature to prevent the aluminium thin wall wrap model.Heating on one side in the degassing procedure, on one side degasification, the degasification temperature is 300 ℃-400 ℃, whole degassing procedure needs to carry out slow degasification with high vacuum manual gear plate valve, extracts out to prevent the powder in the thin wall wrap model.The final interior vacuum of thin wall wrap model that guarantees is greater than 10
-3Pa.
Step (five), the densified shaping of high temperature insostatic pressing (HIP)
Thin wall wrap model after the vacuum degassing is carried out the high temperature insostatic pressing (HIP) densification, according to the heat and other static pressuring processes parameter of moulding material and thin wall wrap model material selection optimization.Packaged thin wall wrap model is positioned over carries out densification in the high temperature insostatic pressing (HIP) stove; Adopt the high temperature insostatic pressing (HIP) parameter to be in the present embodiment: 480 ℃～550 ℃ of temperature, 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), remove interior aluminium jacket 1, outer aluminium jacket 2 materials with the method for Vehicle Processing, namely obtain high-compactness TiAl pipe and stainless steel penstock 6 integrally formed TiAl pipe targets.
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 as TiAl pipe target manufacturing process flow chart in the embodiment of the invention.
The TiAl pipe target density of process preparation of the present invention 〉=99%, oxygen content≤1000ppm, grain size≤50um.
The above has done detailed description to embodiments of the invention by reference to the accompanying drawings, but the present invention is not limited to above-described embodiment, in the ken that those of ordinary skills possess, also can under the prerequisite that does not break away from aim of the present invention, make various variations, such as shape and size of shear web etc.
Be not described in detail content in the specification of the present invention and belong to this area professional and technical personnel's known technology.
Claims (8)
1. a big L/D ratio TiAl pipe target manufacturing process is characterized in that: comprise the steps:
Step (one), assembling thin wall wrap model: described thin wall wrap model comprises interior jacket (1), outer jacket (2), jacket bottom (3), jacket loam cake (4), wireway (5) and penstock (6); At first interior jacket (1) is positioned over outer jacket (2) inside, jacket bottom (3) welds with interior jacket (1), outer jacket (2), the location of jacket (1) and outer jacket (2) in realizing, then penstock (6) is sleeved on the outer surface of interior jacket (1), the upper punching of last outer jacket (2), welding wireway (5);
Step (two), with the Ti powder with after the Al powder mixes, be packed in the thin wall wrap model that step () assembles, and carry out soldering and sealing after covering jacket loam cake (4), realize the sealing of thin wall wrap model, wherein the Ti Powder Particle Size is the 100-200 order, and the Al Powder Particle Size is below 325 orders;
Step (three), thin wall wrap model is positioned in the heat-treatment furnace heats, and vacuum degassing, the degasification temperature is 300 ℃-400 ℃, guarantees that vacuum in the thin wall wrap model after the degasification is greater than 10
-3Pa;
Step (four), thin wall wrap model is positioned over carries out densification in the high temperature insostatic pressing (HIP) stove;
Step (five), the thin wall wrap model after the densification removed in jacket (1) and outer jacket (2), and carry out that machining obtains required size with the integrally formed TiAl pipe of penstock (6) target.
2. a kind of big L/D ratio TiAl pipe target manufacturing process according to claim 1 is characterized in that: in the described step (two) with the Ti powder with after the Al powder mixes, the concrete steps that are packed in the thin wall wrap model that assembles are as follows:
(1), with the thin wall wrap model horizontal positioned, adopt the filling shovel to deliver to the thin wall wrap model bottom in the Ti powder that mixes and Al powder again, then thin wall wrap model is erected vertical placement, will load shovel and extract out, finish the powder packing first time;
(2), afterwards with the thin wall wrap model 90-degree rotation, make the thin wall wrap model horizontal positioned, repeating step (1) is finished for the second time powder packing, the like, finish altogether four fillings;
(3), thin wall wrap model is vertically put vertical, with the powder pressing in the thin wall wrap model, finish first round powder packing;
(4), repeating step (1)-(3), finish second and take turns powder packing, the rest may be inferred, until the full thin wall wrap model of filling.
3. a kind of big L/D ratio TiAl according to claim 1 manages the target manufacturing process, it is characterized in that: when carrying out jacket loam cake (4) welding in the described step (two), every welding 20-30mm weld seam stops, the cooling thin wall wrap model, weld again afterwards, cause powder to react to prevent because of the heat that welding produces.
4. a kind of big L/D ratio TiAl according to claim 1 manages the target manufacturing process, it is characterized in that: the middle thin wall wrap model of described step (four) carries out densification in the high temperature insostatic pressing (HIP) stove parameter is: 480 ℃～550 ℃ of temperature, pressure 100～110MPa, temperature retention time 2～5h.
5. a kind of big L/D ratio TiAl according to claim 1 manages the target manufacturing process, it is characterized in that: described penstock (6) is stainless steel tube, titanium pipe or carbon steel pipe.
6. a kind of big L/D ratio TiAl according to claim 1 manages the target manufacturing process, and it is characterized in that: the length of described penstock (6) is less than the length of interior jacket (1), outer jacket (2), and length difference is 60-80mm.
7. a kind of big L/D ratio TiAl according to claim 1 manages the target manufacturing process, and it is characterized in that: the material of described interior jacket (1), outer jacket (2), jacket bottom (3), jacket loam cake (4) and wireway (5) is aluminium.
8. a kind of big L/D ratio TiAl according to claim 1 manages the target manufacturing process, it is characterized in that: in the described step (two) with the Ti powder with after the Al powder mixes through the mixed powder granulation of vacuum, so that powder has higher compacted density and distributes uniformly in the filling process.
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| CN104226870A (en) * | 2014-07-21 | 2014-12-24 | 北京有色金属研究总院 | Covering method for hot isostatic pressing of aluminum-stainless steel composite pipe |
| CN104831245A (en) * | 2015-05-29 | 2015-08-12 | 西北有色金属研究院 | Hot isostatic pressing production method of tubular molybdenum alloy sputtering target |
| CN104889398A (en) * | 2015-05-15 | 2015-09-09 | 安泰科技股份有限公司 | Anti-abrasion anti-etching alloy rod production method through powder metallurgy process |
| CN105817627A (en) * | 2016-03-28 | 2016-08-03 | 航天材料及工艺研究所 | Preparation method for integrally-formed tungsten tube target material with large length-to-diameter ratio |
| CN106521430A (en) * | 2015-09-09 | 2017-03-22 | 宁波江丰电子材料股份有限公司 | Production technology of tantalum aluminum target |
| CN106676484A (en) * | 2015-11-10 | 2017-05-17 | 航天长征睿特科技有限公司 | Binding method of chrome pipe target material |
| CN107385399A (en) * | 2017-07-25 | 2017-11-24 | 北京兴荣源科技有限公司 | A kind of pressing method of vanadium pipe target |
| CN108817379A (en) * | 2018-05-23 | 2018-11-16 | 航天材料及工艺研究所 | A kind of powder metallurgy superalloy properties of product stability of improving fills out powder device |
| CN108930020A (en) * | 2018-08-24 | 2018-12-04 | 爱发科电子材料（苏州）有限公司 | Molybdenum niobium target manufacture craft |
| CN111299613A (en) * | 2020-03-27 | 2020-06-19 | 宁波江丰电子材料股份有限公司 | Machining method of titanium-aluminum alloy target material, product and application thereof |
| CN111438356A (en) * | 2020-04-13 | 2020-07-24 | 河北晟华新材料科技有限公司 | Titanium-aluminum target material for physical vapor deposition and preparation method thereof |
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| CN104226870A (en) * | 2014-07-21 | 2014-12-24 | 北京有色金属研究总院 | Covering method for hot isostatic pressing of aluminum-stainless steel composite pipe |
| CN104889398A (en) * | 2015-05-15 | 2015-09-09 | 安泰科技股份有限公司 | Anti-abrasion anti-etching alloy rod production method through powder metallurgy process |
| CN104831245A (en) * | 2015-05-29 | 2015-08-12 | 西北有色金属研究院 | Hot isostatic pressing production method of tubular molybdenum alloy sputtering target |
| CN106521430A (en) * | 2015-09-09 | 2017-03-22 | 宁波江丰电子材料股份有限公司 | Production technology of tantalum aluminum target |
| CN106676484A (en) * | 2015-11-10 | 2017-05-17 | 航天长征睿特科技有限公司 | Binding method of chrome pipe target material |
| CN105817627A (en) * | 2016-03-28 | 2016-08-03 | 航天材料及工艺研究所 | Preparation method for integrally-formed tungsten tube target material with large length-to-diameter ratio |
| CN107385399A (en) * | 2017-07-25 | 2017-11-24 | 北京兴荣源科技有限公司 | A kind of pressing method of vanadium pipe target |
| CN108817379A (en) * | 2018-05-23 | 2018-11-16 | 航天材料及工艺研究所 | A kind of powder metallurgy superalloy properties of product stability of improving fills out powder device |
| CN108930020A (en) * | 2018-08-24 | 2018-12-04 | 爱发科电子材料（苏州）有限公司 | Molybdenum niobium target manufacture craft |
| CN108930020B (en) * | 2018-08-24 | 2020-06-19 | 爱发科电子材料（苏州）有限公司 | Molybdenum niobium target material manufacturing process |
| CN111299613A (en) * | 2020-03-27 | 2020-06-19 | 宁波江丰电子材料股份有限公司 | Machining method of titanium-aluminum alloy target material, product and application thereof |
| CN111438356A (en) * | 2020-04-13 | 2020-07-24 | 河北晟华新材料科技有限公司 | Titanium-aluminum target material for physical vapor deposition and preparation method thereof |
| CN112981342A (en) * | 2021-02-04 | 2021-06-18 | 山东昊轩电子陶瓷材料有限公司 | Production process of integrally-formed tube target |
| CN112981342B (en) * | 2021-02-04 | 2022-02-18 | 山东昊轩电子陶瓷材料有限公司 | Production process of integrally-formed tube target |
| CN116145090A (en) * | 2022-12-30 | 2023-05-23 | 苏州六九新材料科技有限公司 | Titanium-based tubular alloy target and preparation method thereof |
| CN116145090B (en) * | 2022-12-30 | 2024-04-12 | 苏州六九新材料科技有限公司 | Titanium-based tubular alloy target and preparation method thereof |
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