CN104611673A - Manufacture method of molybdenum alloy target material - Google Patents
Manufacture method of molybdenum alloy target material Download PDFInfo
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Abstract
A manufacture method of a molybdenum alloy target material comprises the following steps: (1) molybdenum powder and at least one metallic element selected from titanium, chromium, niobium and tantalum groups are mixed with carbon powder to obtain uniform alloyed powder; (2) the alloyed powder is added into a pressurizing vessel, degassing process is carried out on the pressurizing vessel under vacuum, and a degassing hole is sealed; (3) pressurization and warming are carried out by a hot isostatic pressing technology, and oxygen is added into the pressurizing vessel such that the alloyed powder becomes an alloy blank; (4) the alloy blank undergoes annealing in a high temperature furnace; and (5) the alloy undergoes cutting, accurate grinding and machining to obtain a molybdenum alloy target material finished product. By the manufacture method, the know manufacture procedure of a molybdenum alloy target material can be simplified, production cycle of the molybdenum alloy target material can be shortened and plasticity of the molybdenum alloy material can be effectively raised.
Description
Technical field
The invention belongs to a kind of method for making of molybdenum alloy target, the processing procedure of known molybdenum alloy target can be simplified, reduce the production cycle of molybdenum alloy target, significantly reduce production cost.
Background technology
Molybdenum target material is widely used in the industries such as flat-panel monitor, microelectronics and optical glass coating.If plated film needs to add the characteristics such as heat-resisting and corrosion-resistant, the metal that molybdenum target material can add other sometimes becomes molybdenum alloy target.
And molybdenum is because its fusing point is high, so usually use the mode of powder metallurgy to manufacture this material.As patent number TW I310407 " sputter target material and method for making thereof ":
The molybdenum powder of preparation 6 microns of (μm) mean particle sizes, the niobium powder of 100 micron average particle size, the chromium powder end of 100 micron average particle size, the ti powder of 100 micron average particle size, the zirconium powder end of 100 micron average particle size, and the vanadium powder end of 100 micron average particle size.
Its manufacturing step is as follows:
(1) for manufacturing respectively this sample, by the molybdenum powder of specific atoms per-cent (%) and arbitrary Addition ofelements powder check weighing.
(2) V-type mixing tank is used the powder through check weighing to be mixed 10 minutes, to obtain raw material powder.
(3) all press (cold isostatic pressing, CIP) machine pressurized feedstock powder with cold, and form green compact.
(4) jaw crusher and disc refiner is used to pulverize green compact, to manufacture secondary powder.
(5) in V-type mixing tank, secondary powder is mixed 10 minutes, then insert in pressurizing vessel.After secondary powder is inserted pressurizing vessel, by tool except the upper cover of pore is welded in pressurizing vessel, with airtight hand-hole.
(6) under the vacuum of 450 degree Celsius, carry out degasification processing procedure by adding the pressurizing vessel having secondary powder, then sealing should except pore.
(7) hot isostatic pressing (hot isostatic pressing, HIP) machine is used to pressurize this pressurizing vessel sinter secondary powder.The operating condition of hot isostatic press is 1250 degree Celsius, 12,000 ten thousand handkerchief pressure and 5 hour activity duration.
(8) mechanical workout or plastic working (such as hot rolling) obtain last target size.
Sputtered target material sweep electron microscope (the Scanning Electron Microscope of patent number TW I310407 " sputter target material and method for making thereof ", SEM) microstructure as shown in Figure 4, sputtered target material has metallic element island and is scattered in microstructure in molybdenum base material, oxide fine particle be formed in the metallic element island in molybdenum base material with surrounding.
Right patent number TW I310407 " sputter target material and method for making thereof " is when preparing molybdenum alloy, raw material powder need be formed green compact with cold balancer pressurization, re-use jaw crusher and disc refiner pulverizes green compact, to manufacture secondary powder, and after sintering completes, target embryo just can be made into the molybdenum alloy sputtered target material of uniform composition after need carrying out the multi-program as previously discussed such as hot rolling again, not only expend time in and money, and the life cycle of the product time is longer.
And research display: molybdenum crystal belongs to body-centered cubic crystal structure (Body-Centered Cubic CrystalStructure, BCC), independent slip-system is less, when there is stress deformation, its intercrystalline compatible deformation ability, grain boundaries easily produces stress concentration and causes crackle, causes intercrystalline cracking.Meanwhile, the molybdenum alloy that the various technology of industrial employing is produced is all containing impurity such as a small amount of oxygen, carbon, nitrogen, and the existence of these residual impurity has had a strong impact on mechanical property and the weave construction of molybdenum alloy component.The solubleness of impurity element in molybdenum such as oxygen, carbon, nitrogen are very low.These elements exist with forms such as oxide compound, carbide, nitride, and Shen Dian in crystal boundary, subgrain boundary and comprise dislocation defect around, not only weaken grain-boundary strength, and hinder dislocation motion, facilitate crack to generate, make molybdenum alloy demonstrate typical brittleness at room temperature.
Edge this, in order to solve the aforesaid drawbacks, the present inventor is the method that positive searching solves, and after repeatedly testing and improveing, finally creates a kind of method for making of molybdenum alloy target.
Summary of the invention
The object of the present invention is to provide a kind of method for making of molybdenum alloy target, not only can simplify processing procedure, reduce the production cycle of molybdenum alloy target, significantly reduce production cost, also reduce the impact of impurity element oxygen on molybdenum plasticity, better properties is provided.
To achieve the above object, the invention provides a kind of method for making of molybdenum alloy target, the steps include:
Step (1) by quantitative molybdenum powder be selected from titanium, chromium, niobium and tantalum group at least one elemental metalpowder be respectively divided at least three parts, then every part of molybdenum powder and every part are selected from titanium, chromium, the powder of at least one metallic element of niobium and tantalum group and the powder of carbon and are mixed into aliquot powder mix respectively again, after at least dividing three groups every aliquot powder mix, mix respectively again and be finally combined, then more all powder mixs are mixed into uniform alloy powder;
This alloy powder inserts in pressurizing vessel by step (2), under vacuo pressurizing vessel is carried out degasification processing procedure, and sealing is except pore;
Step (3) utilizes heat and other static pressuring processes to pressurize, heat, and is added into oxygen in this pressurizing vessel, makes this alloy powder become alloy embryo;
This alloy embryo is annealed in 1500 degree Celsius to 1600 degree of High Temperature Furnaces Heating Apparatuss Celsius by step (4);
This alloy embryo of step (5) becomes molybdenum alloy target finished product through cutting, fine grinding, mechanical workout.
Wherein, be selected from this titanium, chromium, niobium and tantalum group the atomic percent of at least one elemental metalpowder be that one of percentage is to 50 percent.
Wherein, this alloy preform utilizes High Temperature Furnaces Heating Apparatus to anneal, and the temperature of this High Temperature Furnaces Heating Apparatus is 1500 degree to 1600 degree Celsius Celsius.
Wherein, the shape of this molybdenum alloy target finished product is dull and stereotyped.
Wherein, the shape of this molybdenum alloy target finished product is pipe.
Wherein, the crystal boundary of this molybdenum alloy target finished product is oval.
The present invention contrasts effect of prior art:
One, method for making system of the present invention by molybdenum powder be selected from titanium, chromium, niobium and tantalum group at least one metallic element mix with the powder of carbon after, directly utilize hot isostatic pressing that alloy powder is added gentleness and pressurize into alloy preform, pulverize again to manufacture secondary powder after not needing the method for making as known techniques alloy powder first need be utilized cold balancer pressurized feedstock powder to form raw embryo, and after sintering completes, target embryo does not need to carry out the multi-programs such as hot rolling again, not only few compared with the step of known molybdenum alloy target, and the production cycle of molybdenum alloy target can be reduced, significantly can lower production cost.
In the manufacturing processed of two, molybdenum alloy target of the present invention, adjust appropriate carbon and be present in molybdenum alloy, effectively can improve the plasticity of molybdenum alloy material, reduce and mould crisp transition temperature.In addition, in annealing or process of cooling, utilize between carbon and oxygen strong in conjunction with energy, carbon can also suppress oxygen to the segregation of crystal boundary, thus reduce further the impact of impurity element oxygen on molybdenum plasticity.When carbon Sauerstoffatom is than during at more than 2:1, alloy molybdenum can show good plasticity.
Relevant the technology used in the present invention, means and effect thereof, hereby lift a preferred embodiment and after coordinating graphic being described in more detail in, believe object, structure and feature that the present invention is above-mentioned, when can by a deeply concrete understanding.
Accompanying drawing explanation
Fig. 1: the schema of the method for making of molybdenum alloy target of the present invention.
Fig. 2: the excellent bending property measuring principle figure of molybdenum niobium carbon (MoNb-C) of the present invention.
Fig. 3: longitudinal metallographic microstructure analysis chart of molybdenum niobium carbon (MoNb-C) of the present invention.
Fig. 4: sweep electron microscope (Scanning Electron Microscope, the SEM) sectional view of known molybdenum alloy target.
Embodiment
First, as shown in Figure 1, preferred embodiment of the present invention, only these embodiments are only for explanation, restriction not by this structure in patent application.
The method for making of this molybdenum alloy target described, the steps include:
Step (1) 10 by quantitative molybdenum powder be selected from titanium, chromium, niobium and tantalum group the powder of at least one metallic element be respectively divided at least three parts, then every part of molybdenum powder be selected from titanium, chromium, niobium and at least one metallic element of tantalum group and the powder of carbon is mixed into aliquot powder mix more respectively, after at least dividing three groups every aliquot powder mix, mix respectively again and be finally combined, then more all powder mixs are mixed into uniform alloy powder;
This alloy powder inserts in pressurizing vessel by step (2) 20, under vacuo pressurizing vessel is carried out degasification processing procedure, and sealing is except pore;
Step (3) 30 uses the pressurization of hot isostatic pressing (hot isostatic pressing, HIP) machine, heats, and is added into oxygen in this pressurizing vessel.Hot isostatic pressing machine operation is divided into three humidity provinces; 0 degree to 800 degree Celsius Celsius, 800 degree to 1600 degree Celsius Celsius, 1600 degree to 2000 degree Celsius Celsius, and each humidity province at least sinters 3 hours, operating pressure be often 10,000 ten thousand handkerchiefs to 20,000 ten thousand handkerchiefs, make this alloy powder become alloy embryo;
This alloy embryo is annealed in 1500 degree Celsius to 1600 degree of High Temperature Furnaces Heating Apparatuss Celsius by step (4) 40;
This alloy embryo of step (5) 50 becomes molybdenum alloy target finished product through cutting, fine grinding, mechanical workout, and wherein the shape of this molybdenum alloy target finished product can be flat board or pipe.
Wherein be selected from this titanium, chromium, niobium and tantalum group the atomic percent of at least one elemental metalpowder be that one of percentage is to 50 percent;
The present invention studies discovery, in the impurity elements such as oxygen, carbon, nitrogen, the impact of carbon on molybdenum intensity is minimum, but it is very large on the impact of its unit elongation, if table one is that display carbon content is on the impact of molybdenum niobium alloy unit elongation, when carbon content increases to 20 mgs/kg from 10 mgs/kg, the unit elongation of molybdenum alloy is increased to rapidly 45 percent from 10, and sufficient proof carbon is conducive to the plasticity improving molybdenum alloy; And when carbon content continues to increase, the extension of molybdenum alloy slows down again.The molybdenum alloy that oxygen level is higher, it moulds-and crisp transition temperature is also higher.Equally with the increase of nitrogen content, the critical yield stress of molybdenum alloy sharply declines, and it moulds-and crisp transition temperature also sharply rises, and illustrates that the existence of high-content oxygen and nitrogen in molybdenum alloy can have a strong impact on the mechanical property of molybdenum alloy.
Table one
In the manufacturing processed of molybdenum alloy target of the present invention, adjust appropriate carbon and be present in molybdenum alloy, effectively can improve the plasticity of molybdenum alloy material, reduce and mould crisp transition temperature.Its reason mainly can form the compounds such as two molybdenum carbon (Mo2C), molybdenum carbon (MoC) due to carbon in molybdenum alloy, two molybdenum carbon and Mo substrate have very strong bonding force, the existence of two molybdenum carbon can the relatively weak interface of efficient hardening polycrystalline bonding force, reduce intergranular flwrittle fracture trend, polycrystalline molybdenum materials plasticity is improved.In addition, in annealing or process of cooling, utilize between carbon and oxygen strong in conjunction with energy, carbon can also suppress oxygen to the segregation of crystal boundary, thus reduce further the impact of impurity element oxygen on molybdenum plasticity.As shown in table two, table three, be the impact of carbon oxygen content ratio of the present invention on molybdenum niobium alloy transverse bend unit elongation, when carbon Sauerstoffatom is than during at more than 2:1, molybdenum alloy can show good plasticity.
Table two
Table three
Transverse bend unit elongation enhancing rate (η) of the present invention, account form is as shown in formula 1 and Fig. 2.Wherein R is bending radius, millimeter (mm); D is thickness of sample, millimeter (mm).Be on the piece of stainless steel of 50 millimeters × 40 millimeters × 20 millimeters in 10 pieces of sizes (long × wide × high), cut out radius with Linear cut and be respectively 1000 millimeters, 400 millimeters, 200 millimeters, 133.33 millimeters, 100 millimeters, 66.67 millimeters, 50 millimeters, 33.33 millimeters, the circular arc of 25 millimeters and 20 millimeters.Cross-sectional cut growth × wide × height sample to be recorded being prolonged rod is the molybdenum bar of 10 millimeters × 4 millimeters × 2 millimeters, the punching block putting into R=1000 millimeter slowly pressurizes and molybdenum bar is bent, and then, puts into the less punching block of R successively and bends, until the fracture of molybdenum bar, write down radius during fracture.Because during sample bent, top dependent variable is maximum, so alloy plasticity is assessed by calculating maximum deformation quantity, and horizontal plastic property calculation formula is formula 1:
Formula 1:
As shown in Figure 3, add a certain proportion of carbon, Sauerstoffatom in molybdenum alloy, along with annealing temperature raises, molybdenum niobium carbon (MoNb-C) crystal boundary can gradually grow up as even perfect shape, as ellipse, when annealing for 1500 degree to 1600 degree Celsius Celsius, the transverse bend unit elongation of alloy is the highest, reaches 5 percent.
As Fig. 3, molybdenum alloy target of the present invention has following advantage:
1. crystal grain is comparatively fine and close, and thickness homogeneity (uniformity) more known (as shown in Figure 4) the circular crystal grain target after sputter (sputtering) film forming is good;
2. oval crystal grain is interspersed, and can prevent crystal boundary (grain boundary) from sliding, (such as Linear cut) target not easily broken (crack) when mechanical workout is shaped;
Effect of contrast prior art:
One, method for making system of the present invention by molybdenum powder be selected from titanium, chromium, niobium and tantalum group at least one metallic element mix with the powder of carbon after, directly utilize hot isostatic pressing to be heated by alloy powder, add and be pressed into alloy preform, pulverize again to manufacture secondary powder after not needing the method for making as known molybdenum alloy target alloy powder first need be utilized cold balancer pressurized feedstock powder to form raw embryo, and after sintering completes, target embryo does not need to carry out the multi-programs such as hot rolling again, not only few compared with the step of known molybdenum alloy target, and production cycle and the production cost of molybdenum alloy target can be reduced.Comparatively known techniques is fine and close for the crystal grain of molybdenum alloy target of the present invention, and the thickness homogeneity after forming sputtering film is better, and crystal grain is interspersed, and can prevent intercrystalline slip, and when mechanical workout is shaped, target is not easily broken.
In the manufacturing processed of two, molybdenum alloy target of the present invention, adjust appropriate carbon and be present in molybdenum alloy, effectively can improve the plasticity of molybdenum alloy material, reduce and mould crisp transition temperature.In addition, in annealing or process of cooling, utilize between carbon and oxygen strong in conjunction with energy, carbon can also suppress oxygen to the segregation of crystal boundary, thus reduce further the impact of impurity element oxygen on molybdenum plasticity.When carbon Sauerstoffatom is than during at more than 2:1, High-Purity Molybdenum can show good plasticity.
Be be that technical characteristic of the present invention is specifically described for preferred embodiment of the present invention above; Only, person skilled in the art is when carrying out changing and revise to the present invention not departing under spirit of the present invention and principle, and these changes and revising, and all should be covered by the category that following claim defines.
Claims (6)
1. a method for making for molybdenum alloy target, the steps include:
(1) by molybdenum powder be selected from titanium, chromium, niobium and tantalum group the powder of at least one metallic element be respectively divided at least three parts, then every part of molybdenum powder and every part are selected from titanium, chromium, the powder of at least one metallic element of niobium and tantalum group and the powder of carbon and are mixed into aliquot powder mix respectively again, after at least dividing three groups every aliquot powder mix, mix respectively again and be finally combined, then more all powder mixs are mixed into uniform alloy powder;
(2) this alloy powder is inserted in pressurizing vessel, under vacuo pressurizing vessel is carried out degasification processing procedure, and sealing is except pore;
(3) use hot isostatic press pressurization, heat, and be added into oxygen in this pressurizing vessel, this hot isostatic pressing machine operation is divided into three humidity provinces; Be respectively 0 degree to 800 degree Celsius Celsius, 800 degree to 1600 degree Celsius Celsius, 1600 degree to 2000 degree Celsius Celsius, each humidity province at least sinters 3 hours, operating pressure be 10,000 ten thousand handkerchiefs to 20,000 ten thousand handkerchiefs, make this alloy powder become alloy embryo;
(4) this alloy embryo is annealed in High Temperature Furnaces Heating Apparatus;
(5) this alloy embryo becomes molybdenum alloy target finished product through cutting, fine grinding, mechanical workout.
2. the method for making of molybdenum alloy target as claimed in claim 1, is characterized in that, be selected from this titanium, chromium, niobium and tantalum group the atomic percent of at least one elemental metalpowder be that one of percentage is to 50 percent.
3. the method for making of molybdenum alloy target as claimed in claim 1, it is characterized in that, this alloy preform utilizes High Temperature Furnaces Heating Apparatus to anneal, and the temperature of this High Temperature Furnaces Heating Apparatus is 1500 degree to 1600 degree Celsius Celsius.
4. the method for making of molybdenum alloy target as claimed in claim 1, is characterized in that, the shape of this molybdenum alloy target finished product is dull and stereotyped.
5. the method for making of molybdenum alloy target as claimed in claim 1, it is characterized in that, the shape of this molybdenum alloy target finished product is pipe.
6. the method for making of molybdenum alloy target as claimed in claim 1, is characterized in that, the crystal boundary of this molybdenum alloy target finished product is oval.
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| CN106378455A (en) * | 2015-07-31 | 2017-02-08 | 汉能新材料科技有限公司 | Molybdenum alloy rotary metal pipe material and preparation method thereof |
| CN108213440A (en) * | 2017-12-25 | 2018-06-29 | 安泰天龙钨钼科技有限公司 | A kind of preparation method of Mo Re alloys tubing |
| CN108611607A (en) * | 2016-12-09 | 2018-10-02 | 宁波江丰电子材料股份有限公司 | The forming method of powder metallurgy process and target |
| CN111636052A (en) * | 2019-03-01 | 2020-09-08 | 宁波江丰电子材料股份有限公司 | Preparation method of target material |
| CN113584366A (en) * | 2021-07-16 | 2021-11-02 | 洛阳高新四丰电子材料有限公司 | Niobium alloy sputtering target material and preparation method thereof |
| CN114934260A (en) * | 2022-05-23 | 2022-08-23 | 安泰天龙钨钼科技有限公司 | Molybdenum alloy target material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106378455A (en) * | 2015-07-31 | 2017-02-08 | 汉能新材料科技有限公司 | Molybdenum alloy rotary metal pipe material and preparation method thereof |
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| CN114934260A (en) * | 2022-05-23 | 2022-08-23 | 安泰天龙钨钼科技有限公司 | Molybdenum alloy target material and preparation method and application thereof |
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| CN114934260B (en) * | 2022-05-23 | 2024-02-13 | 安泰天龙钨钼科技有限公司 | Molybdenum alloy target material and preparation method and application thereof |
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Application publication date: 20150513 |