CN102230100A - 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 powder metallurgic method prepares the method for Ti-Nb-Zr-Sn alloy.
Background technology
Titanium and titanium alloy thereof have the excellent properties such as erosion resistance of low density, high specific strength, good high-temperature intensity, brilliance, are widely used in fields such as automobile, biotechnology and aerospace.But the machinability of titanium and alloy thereof is poor, and hardness is machining difficulty especially during greater than HB350, sticking cutter phenomenon then appears during less than HB300 easily, also be difficult to cutting, become the obstacle of mass production complicated shape part, thereby produce titanium part with powder metallurgic method and enjoy and gaze at.
Titanium is nontoxic, light weight, intensity high and have good biocompatibility, is unusual 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 the vanadium and the aluminum ion of denier, reduced its cell adapted property and might work the mischief human body.The U.S. as far back as 20th century the mid-80 just begin to develop no aluminium, do not have vanadium, have the titanium alloy of biocompatibility, use it for orthopaedy.Number of research projects 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 a 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, the Yang Rui of laboratory engineering alloy research department of Shenyang Materials science country of metal institute of the Chinese Academy of Sciences (associating), 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 than 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 one of focus of titanium matrix composite research field in recent years.
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 powder metallurgy new technologies also can be used for the preparation of stupalith.
The powder metallurgy new technology is different from the characteristics of conventional sintering method:
(1) can to reduce alloying constituent to greatest extent poly-partially for powder metallurgy technology, eliminates thick, uneven 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 (as Al-Li alloy, heat-resisting Al alloy, superalloy, powder corrosion resisting stainless steel, powder rapid steel, 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 over-saturation sosoloid, 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 material with special construction and performance and the goods that common smelting process can't be produced, 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, the resource and the energy consumption of production can be reduced effectively.
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 defective such as the space is more.
Summary of the invention
For solving the above-mentioned technical problem that existing Ti-Nb-Zr-Sn alloy preparation method exists, the invention provides the method that a kind of powder metallurgic method prepares the Ti-Nb-Zr-Sn alloy, preparation method provided by the present invention has the advantage that sintering temperature is low, sintering time is short, products therefrom density height, grain-size are 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 are pressed mass ratio TiH
2: the Nb:Zr:Sn=66.1:24:4:7.9 configuration; B. the powder that configures is done and mixed 5 hours; C. will do the powder press forming in universal testing machine after mixing, wherein pressing pressure is 350 Mpa, and 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 with heating-up time 30min, vacuum sintering furnace power be the speed of 70KW power to be warming up to sintering temperature be 1150 ℃-1350 ℃, 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 for preparing of powder metallurgical reaches as high as 97.7%, and grain-size is about 48 μ m, and microtexture is good, hole seldom, alloy possesses the tensile strength height, the advantage that hardness is big.
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
By embodiment the present invention is further detailed below, but the present invention is not limited only to following examples, can not limits scope of the present invention with this.
Embodiment 1
With TiH
2Powder, Nb powder, Zr powder and Sn powder are pressed mass ratio TiH
2: the Nb:Zr:Sn=66.1:24:4:7.9 configuration, the powder that configures was done in four jars of blenders mixed 5 hours, 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 present embodiment and embodiment 1 only is, last in the sintering process step is that 30min, vacuum molybdenum wire furnace power are that the speed of 70KW power is warming up to 1200 ℃ of sintering temperatures with the heating-up time, 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 present embodiment and embodiment 1 only is, last in the sintering process step is that 30min, vacuum molybdenum wire furnace power are that the speed of 70KW power is warming up to 1250 ℃ of sintering temperatures with the heating-up time, 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 present embodiment and embodiment 1 only is, last in the sintering process step is that 30min, vacuum molybdenum wire furnace power are that the speed of 70KW power is warming up to 1300 ℃ of sintering temperatures with the heating-up time, 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 present embodiment and embodiment 1 only is, last in the sintering process step is that 30min, vacuum molybdenum wire furnace power are that the speed of 70KW power is warming up to 1350 ℃ of sintering temperatures with the heating-up time, 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 present embodiment and embodiment 1 only is, last in the sintering process step is that 30min, vacuum molybdenum wire furnace power are that the speed of 70KW power is warming up to 1250 ℃ with the heating-up time, 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 present embodiment and embodiment 1 only is, last in the sintering process step is that 30min, vacuum molybdenum wire furnace power are that the speed of 70KW power is warming up to 1250 ℃ with the heating-up time, 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 present embodiment and embodiment 1 only is, last in the sintering process step is that 30min, vacuum molybdenum wire furnace power are that the speed of 70KW power is warming up to 1250 ℃ with the heating-up time, 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 (6)
1. a powder metallurgic method prepares the method for Ti-Nb-Zr-Sn alloy, and may further comprise the steps: a. is with TiH
2Powder, Nb powder, Zr powder and Sn powder are pressed mass ratio TiH
2: the Nb:Zr:Sn=66.1:24:4:7.9 configuration; B. the powder that configures is done and mixed 5 hours; C. will do the powder press forming in universal testing machine after mixing, wherein pressing pressure is 350 Mpa, and the dwell time is 7～8 s; D. with sample sintering in vacuum sintering furnace of press forming.
2. powder metallurgic method according to claim 1 prepares the method for Ti-Nb-Zr-Sn alloy, the sintering process step is in the described steps d: 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.
3. powder metallurgic method according to claim 2 prepares the method for Ti-Nb-Zr-Sn alloy, and described sintering temperature is 1150 ℃-1350 ℃, furnace cooling after being incubated 1-4 hour under this temperature.
4. powder metallurgic method according to claim 3 prepares the method for Ti-Nb-Zr-Sn alloy, under the described sintering temperature insulation 2 hours after furnace cooling.
5. powder metallurgic method according to claim 1 prepares the method for Ti-Nb-Zr-Sn alloy, and the vacuum sintering furnace in the described steps d is the vacuum molybdenum wire furnace.
6. powder metallurgic method according to claim 1 prepares the method for Ti-Nb-Zr-Sn alloy, does the powder that configures mixed in four jars of blenders among the described step b.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN103643066A (en) * | 2013-12-03 | 2014-03-19 | 天津大学 | Preparation method of high-damping titanium alloy |
| CN111992711A (en) * | 2019-05-10 | 2020-11-27 | 天津大学 | Method for improving tensile property of titanium alloy additive manufacturing by adding Nb powder |
| CN112475303A (en) * | 2020-11-23 | 2021-03-12 | 江南大学 | Based on TiH2Powder metallurgy preparation method of Ti-Nb-Sn bone repair alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1982504A (en) * | 2005-12-16 | 2007-06-20 | 中国科学院金属研究所 | Production of titanium and titanium-alloy glass ceramic coating |
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2011
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1982504A (en) * | 2005-12-16 | 2007-06-20 | 中国科学院金属研究所 | Production of titanium and titanium-alloy glass ceramic coating |
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| 喻岚等: "粉末冶金钛合金的制备", 《轻金属》 * |
| 张晗亮等: "锡钛合金的粉末冶金法制备", 《功能材料》 * |
| 赵瑶等: "粉末冶金钛合金SP-700的制备", 《粉末冶金材料科学与工程》 * |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111992711A (en) * | 2019-05-10 | 2020-11-27 | 天津大学 | Method for improving tensile property of titanium alloy additive manufacturing by adding Nb powder |
| CN112475303A (en) * | 2020-11-23 | 2021-03-12 | 江南大学 | Based on TiH2Powder metallurgy preparation method of Ti-Nb-Sn bone repair alloy |
| WO2022105438A1 (en) * | 2020-11-23 | 2022-05-27 | 江南大学 | Tih2-based preparation method for ti-nb-sn bone repair alloy by powder metallurgy |
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