CN102230100B - Method for preparing Ti-Nb-Zr-Sn alloy by using powder metallurgical process - Google Patents
Method for preparing Ti-Nb-Zr-Sn alloy by using powder metallurgical process Download PDFInfo
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Abstract
The invention provides a method for preparing a Ti-Nb-Zr-Sn alloy by using a powder metallurgical process and belongs to the technical field of powder metallurgy. The method comprises the following steps of: (a) preparing TiH2 powder, Nb powder, Zr powder and Sn powder wherein the mass ratio of TiH2:Nb:Zr:Sn is 66.1:24:4:7.9; (b) dry-mixing the prepared powders for 5 hours; (c) pressing for forming the powder mixture obtained by dry mixing in a universal material testing machine under such conditions that the pressing pressure is 350 MPa and the pressure maintaining time is 7 to 8 seconds; and (d) sintering the formed sample in a vacuum sintering furnace. Compared with the prior art, the preparation method provided by the invention has the advantages that the sintering temperature is low, the sintering time is short, and the obtained product has a high density and a small and uniform crystal grain size, low impurity content, high tensile strength and high hardness.
Description
Technical field
The invention belongs to powder metallurgical technology, particularly a kind of method of preparing Ti-Nb-Zr-Sn alloy by using powder metallurgical process.
Background technology
Titanium and titanium alloy thereof have low density, high specific strength, good hot strength, the remarkable excellent properties such as erosion resistance, are widely used in the fields such as automobile, biotechnology and aerospace.But the machinability of titanium and alloy thereof is poor, and hardness is the special difficulty of machining during greater than HB350, sticking cutter phenomenon then easily appears during less than HB300, also be difficult to cutting, become the obstacle of a large amount of production complicated shape parts, thereby produce titanium part with powder metallurgic method and enjoy and gaze at.
Titanium is nontoxic, light weight, intensity is high and have good biocompatibility, is ideal medical metal material, can be used as the implant of implant into body etc.At present, widely usedly in medical field be still Ti-6Al-4V ELI alloy, but can separate out vanadium and the aluminum ion of denier, reduced its cell adaptation and might work the mischief to human body.The U.S. as far back as 20th century the mid-80 just begin to develop without aluminium, without vanadium, have the titanium alloy of biocompatibility, use it for orthopaedy.A large amount of research work is also being done by Japan, Britain etc. aspect this, and obtains some new progresses.For example, Japan has developed a series of alpha+beta titanium alloys with good biocompatibility, and the corrosion strength of these alloys, fatigue strength and corrosion resistance all are better than Ti-6Al-4V ELI.Compare with alpha+beta titanium alloys, beta-titanium alloy has higher strength level, and better otch performance and toughness, is more suitable for as the implant implant into body.
Beta titanium alloy is titanium alloy priority research areas in recent years, Japan TKK company adopts Ti powder and 39Al-26V-17.5Fe-17.5Mo master alloyed powder, pass through batch mixing, mold pressing and vacuum sintering have prepared the SP-700 titanium alloy, Ti-15Mo-3Nb is a kind of novel low elastic modulus that American TI MET company develops on the Ti-15Mo-3Nb-3Al basis, high strength and a kind of metastable beta-type biological titanium alloy with better corrosion resistance, the Ti-24Nb-4Zr-7.9Sn alloy is the special beta titanium alloy of a class, (associating) laboratory Yang Rui of engineering alloy research department of Shenyang Materials science country of metal institute of the Chinese Academy of Sciences, the experts such as Hao Yulin adopt fusion casting to succeed in developing and in clinic trial, this method is to experiment material, experimental situations etc. require higher, and it is simple because of its preparation technology to adopt powder metallurgic method to prepare the Ti-24Nb-4Zr-7.9Sn alloy, cost is low, has become in recent years one of focus of titanium matrix composite research field.
Powder metallurgy be produce metal or with metal-powder (or mixture of metal-powder and non-metal powder) as raw material, through being shaped and sintering, make the Technology of metallic substance, compound and all kinds goods.Powder metallurgic method has similar place to the production pottery, and therefore, a series of New Technologies In Powder Metallu Rgies also can be used for the preparation of stupalith.
New Technologies In Powder Metallu Rgy is different from the characteristics of conventional sintering method:
(1) powder metallurgy technology can reduce the alloying constituent segregation to greatest extent, eliminates thick, inhomogeneous cast structure.Has important effect at preparation high-performance rare-earth permanent magnet material, rare earth hydrogen storage material, rare earth luminescent material, rare earth catalyst, high temperature superconducting materia, new metallic material (such as Al-Li alloy, heat-resisting Al alloy, superalloy, powder corrosion resisting stainless steel, Powder High-speed Steels, intermetallic compound high-temperature structural material etc.).
(2) can prepare the non-equilibrium materials of a series of high-performance such as amorphous, crystallite, accurate brilliant, nanocrystalline and supersaturated solid solution, these materials have electricity, magnetics, optics and the mechanical property of excellence.
(3) can easily realize polytype compoundly, give full play to each group element material characteristic separately, be the Technology of a kind of low cost production high-performance metal base and ceramic composite.
(4) can produce the material with special construction and performance and the goods that common smelting process can't be produced, such as novel porous biomaterial, porous diffusion barrier material, high performance structure ceramic grinding tool and ceramic material etc.
(5) can realize nearly clean shape and the automatic batch production of forming, thereby, resource and the energy consumption of production can effectively be reduced.
Because the advantage of powder metallurgy technology, it has become the key that solves the novel material problem, plays a part very important in the development of novel material.But existing powder metallurgy technology exists also that sintering temperature is higher, and sintering time is longer, and prepared Ti-Nb-Zr-Sn alloy impurity is more, and grain-size is inhomogeneous under microscopic observation, and the defective such as the space is more.
Summary of the invention
The above-mentioned technical problem that exists for solving existing Ti-Nb-Zr-Sn alloy preparation method, the invention provides a kind of method of preparing Ti-Nb-Zr-Sn alloy by using powder metallurgical process, preparation method provided by the present invention has advantages of that sintering temperature is low, sintering time is short, the products therefrom density is high, grain-size is more tiny evenly, and impurity is few.
The technical scheme that the present invention solves the problems of the technologies described above may further comprise the steps: a. is with TiH
2Powder, Nb powder, Zr powder and Sn powder be TiH in mass ratio
2: the Nb:Zr:Sn=66.1:24:4:7.9 configuration; B. the powder that configures is dry mixed 5 hours; C. the powder press forming in universal testing machine after will being dry mixed, wherein pressing pressure is 350 Mpa, the dwell time is 7～8 s; D. with sample sintering in vacuum sintering furnace of press forming.
Sintering process step among the above-mentioned steps d is: at first with heating-up time 60min, vacuum sintering furnace power is that the speed of 30KW power is warming up to 300 ℃, under this temperature, be incubated 30min, again with heating-up time 90min, vacuum sintering furnace power is that the speed of 50KW power is warming up to 750 ℃, under this temperature, be incubated 20min, then with heating-up time 20min, vacuum sintering furnace power is that the speed of 60KW power is warming up to 1000 ℃, under this temperature, be incubated 20min, at last with heating-up time 30min, vacuum sintering furnace power is that the speed of 70KW power is warming up to sintering temperature, furnace cooling after being incubated 1-4 hour under this temperature.
Furthermore, in the sintering process step among the above-mentioned steps d, at last be warming up to sintering temperature as 1150 ℃-1350 ℃ take heating-up time 30min, vacuum sintering furnace power as the speed of 70KW power, at the furnace cooling after 1-4 hour of insulation under this temperature.
Technique effect of the present invention is:
1) with common smelting process relatively, adopt powder metallurgic method to prepare fertile material and goods with special construction and performance, and the sintering densification time significantly reduce, sintering temperature also significantly reduces.
2) the Ti-Nb-Zr-Sn alloy density of powder metallurgic method preparation preparation reaches as high as 97.7%, and grain-size is about 48 μ m, and microtexture is good, hole seldom, it is high that alloy possesses tensile strength, the advantage that hardness is large.
Description of drawings
Fig. 1 is the fracture apperance of embodiment 1 prepared Ti-Nb-Zr-Sn alloy.
Fig. 2 is the fracture apperance of embodiment 2 prepared Ti-Nb-Zr-Sn alloys.
Fig. 3 is the fracture apperance of embodiment 3 prepared Ti-Nb-Zr-Sn alloys.
Fig. 4 is the fracture apperance of embodiment 4 prepared Ti-Nb-Zr-Sn alloys.
Fig. 5 is the fracture apperance of embodiment 5 prepared Ti-Nb-Zr-Sn alloys.
Fig. 6 is the fracture apperance of embodiment 5 prepared Ti-Nb-Zr-Sn alloys.
Fig. 7 is the fracture apperance of embodiment 5 prepared Ti-Nb-Zr-Sn alloys.
Fig. 8 is the fracture apperance of embodiment 5 prepared Ti-Nb-Zr-Sn alloys.
Embodiment
The below is further detailed the present invention by embodiment, but the present invention is not limited only to following examples, can not limit scope of the present invention with this.
Embodiment 1
With TiH
2Powder, Nb powder, Zr powder and Sn powder be TiH in mass ratio
2: the Nb:Zr:Sn=66.1:24:4:7.9 configuration, the powder that configures is dry mixed 5 hours in four tank blenders, adopt universal testing machine, under pressing pressure 350 Mpa, pressurize 7～8 s are with sample sintering in the vacuum molybdenum wire furnace.Sintering process is: at first with heating-up time 60min, vacuum molybdenum wire furnace power is that the speed of 30KW power is warming up to 300 ℃, under this temperature, be incubated 30min, again with heating-up time 90min, vacuum molybdenum wire furnace power is that the speed of 50KW power is warming up to 750 ℃, under this temperature, be incubated 20min, then with heating-up time 20min, vacuum molybdenum wire furnace power is that the speed of 60KW power is warming up to 1000 ℃, under this temperature, be incubated 20min, at last with heating-up time 30min, vacuum molybdenum wire furnace power is that the speed of 70KW power is warming up to 1150 ℃ of sintering temperatures, furnace cooling behind insulation 2h under this temperature, obtaining density is 93.5%, and average grain size is the Ti-Nb-Zr-Sn alloy of 45 μ m.As seen from Figure 1, the fracture of the Ti-Nb-Zr-Sn alloy of preparation is particulate state, and hole is more, and dimple is arranged.
Embodiment 2
Not existing together of the present embodiment and embodiment 1 only is, in the sintering process step last take the heating-up time as 30min, vacuum molybdenum wire furnace power is warming up to 1200 ℃ of sintering temperatures as the speed of 70KW power, furnace cooling behind insulation 2h under this temperature, obtaining density is 95.7%, and average grain size is the Ti-Nb-Zr-Sn alloy of 47 μ m.As seen from Figure 2, the Ti-Nb-Zr-Sn fracture of preparation is particulate state, and a small amount of hole is arranged, and dimple is arranged.
Embodiment 3
Not existing together of the present embodiment and embodiment 1 only is, in the sintering process step last take the heating-up time as 30min, vacuum molybdenum wire furnace power is warming up to 1250 ℃ of sintering temperatures as the speed of 70KW power, furnace cooling behind insulation 2h under this temperature, obtaining density is 97.2%, and average grain size is the Ti-Nb-Zr-Sn alloy of 50 μ m.As seen from Figure 3, the Ti-Nb-Zr-Sn Alloy Fracture of preparation is particulate state, and a small amount of hole is arranged, and has a large amount of dimples to exist.
Embodiment 4
Not existing together of the present embodiment and embodiment 1 only is, in the sintering process step last take the heating-up time as 30min, vacuum molybdenum wire furnace power is warming up to 1300 ℃ of sintering temperatures as the speed of 70KW power, furnace cooling behind insulation 2h under this temperature, obtaining density is 97.5%, and average grain size is the Ti-Nb-Zr-Sn alloy of 55 μ m.As seen from Figure 4, the Ti-Nb-Zr-Sn Alloy Fracture of preparation is particulate state, and a small amount of hole is arranged, and has a large amount of dimples to exist.
Embodiment 5
Not existing together of the present embodiment and embodiment 1 only is, in the sintering process step last take the heating-up time as 30min, vacuum molybdenum wire furnace power is warming up to 1350 ℃ of sintering temperatures as the speed of 70KW power, furnace cooling behind insulation 2h under this temperature, obtaining density is 97.7%, and average grain size is the Ti-Nb-Zr-Sn alloy of 60 μ m.As seen from Figure 5, the Ti-Nb-Zr-Sn Alloy Fracture of preparation is particulate state, and a small amount of hole is arranged, and has dimple to exist, and crystal grain has a little growing up.
Embodiment 6
Not existing together of the present embodiment and embodiment 1 only is, in the sintering process step last take the heating-up time as 30min, vacuum molybdenum wire furnace power is warming up to 1250 ℃ as the speed of 70KW power, furnace cooling behind insulation 1h under this temperature, obtaining density is 97.7%, and average grain size is the Ti-Nb-Zr-Sn alloy of 47 μ m.As seen from Figure 6, the Ti-Nb-Zr-Sn Alloy Fracture of preparation is particulate state, and a small amount of hole is arranged, and has dimple to exist.
Embodiment 7
Not existing together of the present embodiment and embodiment 1 only is, in the sintering process step last take the heating-up time as 30min, vacuum molybdenum wire furnace power is warming up to 1250 ℃ as the speed of 70KW power, furnace cooling behind insulation 3h under this temperature, obtaining density is 97.7%, and average grain size is the Ti-Nb-Zr-Sn alloy of 52 μ m.As seen from Figure 7, the Ti-Nb-Zr-Sn Alloy Fracture of preparation is particulate state, and a small amount of hole is arranged, and has dimple to exist.
Embodiment 8
Not existing together of the present embodiment and embodiment 1 only is, in the sintering process step last take the heating-up time as 30min, vacuum molybdenum wire furnace power is warming up to 1250 ℃ as the speed of 70KW power, furnace cooling behind insulation 4h under this temperature, obtaining density is 97.7%, and average grain size is the Ti-Nb-Zr-Sn alloy of 56 μ m.As seen from Figure 8, the Ti-Nb-Zr-Sn Alloy Fracture of preparation is particulate state, and a small amount of hole is arranged, and has dimple to exist, and crystal grain has a little growing up.
The relevant performance perameter of the Ti-Nb-Zr-Sn alloy of embodiment 1-8 preparation is as shown in table 1.
Table 1
Claims (3)
1. the method for a preparing Ti-Nb-Zr-Sn alloy by using powder metallurgical process, may further comprise the steps: a. is with TiH
2Powder, Nb powder, Zr powder and Sn powder be TiH in mass ratio
2: the Nb:Zr:Sn=66.1:24:4:7.9 configuration; B. the powder that configures is dry mixed 5 hours; C. the powder press forming in universal testing machine after will being dry mixed, wherein pressing pressure is 350 MPa, the dwell time is 7～8 s; D. with sample sintering in vacuum sintering furnace of press forming, at first with heating-up time 60min, vacuum sintering furnace power is that the speed of 30kw power is warming up to 300 ℃, under this temperature, be incubated 30min, again with heating-up time 90min, vacuum sintering furnace power is that the speed of 50kw power is warming up to 750 ℃, under this temperature, be incubated 20min, then with heating-up time 20min, vacuum sintering furnace power is that the speed of 60kw power is warming up to 1000 ℃, under this temperature, be incubated 20min, at last with heating-up time 30min, vacuum sintering furnace power is that the speed of 70kw power is warming up to sintering temperature, furnace cooling after being incubated 1-4 hour under this temperature.
2. the method for preparing Ti-Nb-Zr-Sn alloy by using powder metallurgical process according to claim 1, described sintering temperature is 1150 ℃-1350 ℃, at the furnace cooling after 1-4 hour of insulation under this temperature.
3. the method for preparing Ti-Nb-Zr-Sn alloy by using powder metallurgical process according to claim 1, described soaking time is furnace cooling after 2 hours.
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| CN102732747A (en) * | 2012-02-14 | 2012-10-17 | 湘潭正和矫形器技术发展有限公司 | Method for preparing Ti-24Nb-8Sn alloy by using TiH2 powder as raw material though powder metallurgy |
| CN102719700A (en) * | 2012-06-04 | 2012-10-10 | 天津大学 | Ti-Nb-O high damping titanium alloy and powder metallurgy preparation method thereof |
| CN103643066A (en) * | 2013-12-03 | 2014-03-19 | 天津大学 | Preparation method of high-damping titanium alloy |
| CN111992711B (en) * | 2019-05-10 | 2022-08-16 | 天津大学 | Method for improving tensile property of titanium alloy additive manufacturing by adding Nb powder |
| CN112475303B (en) * | 2020-11-23 | 2022-03-08 | 江南大学 | Based on TiH2Powder metallurgy preparation method of Ti-Nb-Sn bone repair alloy |
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