CN109022871A - A kind of Ti-4Si/5TiO of Zr alloying2Alloy and preparation method thereof - Google Patents
A kind of Ti-4Si/5TiO of Zr alloying2Alloy and preparation method thereof Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C14/00—Alloys based on titanium
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
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Abstract
A kind of Ti-4Si/5TiO of Zr alloying2Alloy and preparation method thereof, it is characterised in that: its raw material for preparing is Ti, Si, Zr and TiO2；Preparation method is firstly, by Ti, Si, Zr and TiO2High-energy ball milling is carried out after mixing, keeps its partially-alloyed, then the resulting powder of ball milling is sieved, it is dry, briquetting then is made by compression molding in dry powder, finally by vacuum non-pressure sintering, makes its abundant alloying.Ti-4Si-1.3Zr/5TiO provided by the invention2Alloy comprehensive mechanical property, high temperature oxidation resistance and wearability etc. are improved to some extent, and are with a wide range of applications in aerospace engine art.
Description
Technical field
The present invention relates to Ti-4Si/5TiO2Alloy, the especially Ti-4Si/5TiO of Zr alloying2The preparation method of alloy,
Specifically, being a kind of titanium silicon systems metal conjunction for improving its comprehensive mechanical property, high temperature oxidation resistance and friction and wear behavior
The preparation method of golden material.
Background technique
Since titanium alloy has many advantages, such as that corrosion-resistant, high temperature resistant, specific strength are high, specific stiffness is high, prepares high performance titanium and close
Gold researching value with higher.Titanium alloy has broad application prospects in fields such as science and techniques of defence, Medical treatment device, ocean engineerings.
Titanium alloy is mainly used in aerospace field at present, and under high temperature environment, titanium alloy has superior comprehensive performance, such as anti-
The performances such as high-temperature oxydation, thermophilic corrosion-resistance are the important feature materials of aerial motor spare part.
Nowadays, for traditional high-temperature titanium alloy, 650 DEG C are still limited in using temperature hereinafter, corresponding material
The performances such as performance, mechanical property, resistance to high temperature oxidation, anticorrosive are expected there is no improving significantly, and this is mainly due to the height of material
The limitation for the problems such as temperature stability, effectively reinforcing and obdurability match.
Ti-Si composite material relies on the advantages of high-melting-point, high rigidity to be widely used in numerous areas, has outstanding grind
Study carefully value.Simple substance Si, oxide S iO are added in titanium composite material2Fine and close oxidation film can be formed on the surface of the material,
Oxidation rate is reduced, significantly improves the antioxygenic property of composite material, while the work of dispersion-strengtherning and refined crystalline strengthening can be played
With significantly improving the intensity of material.Although current existing Ti-8Si alloy high temperature resistance is outstanding, toughness is low.
So far, there has been no a kind of Ti-4Si/5TiO of Zr alloying with independent intellectual property rights2The preparation of alloy
Method is available, this constrains the development of China's aerospace engine to a certain extent.
Summary of the invention
The purpose of the present invention is not adapting to use under high temperature for the problem that the low difference of existing Ti-Si alloy ductility, send out
A kind of Ti-4Si/5TiO of bright Zr alloying2Alloy and preparation method thereof passes through selection " high-energy ball milling-compression molding-vacuum
Pressureless sintering " method prepares a kind of titanium silicon, and by addition metallic element Zr, and it is preferable to prepare a kind of comprehensive performance, titanium
The high titanium alloy material of silicon compound content.
The technical solution used in the present invention first is that:
A kind of Ti-4Si/5TiO of Zr alloying2Alloy, it is characterized in that: Ti-4Si-xZr/5TiO2The component of alloy be with
Mass percent calculates, wherein Ti:(91-x) wt.%, Si:4wt.%, Zr:xwt.%, TiO2: 5wt.%, the matter of each component
Measuring the sum of percentage is 100%, and wherein the value of x is 1-1.5..
Technical solution of the present invention second is that:
A kind of Ti-4Si/5TiO of Zr alloying2The preparation method of alloy, it is characterized in that it mainly includes following step
It is rapid:
(1) high-energy ball milling mixes powder: first preparing Ti-4Si-xZr/5TiO by composition2Mixed-powder is put into ball grinder, is placed in
With certain ball milling parameter ball milling in ball mill, so that tri- kinds of elemental powders of Ti, Si, Zr and TiO2Nanometer powder alloy part
Change, gained mixed-powder after ball milling is sieved, drying in vacuum oven is placed in；
(2) conventional compression molding: mixed-powder prepared by step (1) is pressed, briquetting is obtained；
(3) vacuum non-pressure sintering: the briquetting of step (2) compression moulding is subjected to vacuum non-pressure sintering, so that Ti, Si, Zr
And TiO2Further alloying.
The Ti-4Si/5TiO of the Zr alloying2Step (1) ball-milling technology in the preparation method of alloy are as follows: ball
Material shuts down 15min than 8:1,300r/min ball milling 48h, ball milling 1h.
The Ti-4Si/5TiO of the Zr alloying2Step (1) drying means in the preparation method of alloy are as follows: will
Composite powder is placed in vacuum oven, is warming up to after 60 DEG C with drying box and keeps the temperature 4h, crosses 300 meshes.
The Ti-4Si/5TiO of the Zr alloying2Step (2) mould pressing process in the preparation method of alloy are as follows: pressure
For the operating pressure used when processed for 550MPa, briquetting is the round block of φ=30mm, 3~5mm of thickness.
The Ti-4Si/5TiO of the Zr alloying2Step (3) sintering process in the preparation method of alloy are as follows: take out
Vacuum is to 1 × 10-1Pa, heating rate are 10 DEG C/min, and sintering process is 600 ± 10 DEG C × 2h+800 ± 10 DEG C × 2h+1000
± 10 DEG C × 2h+1250 ± 10 DEG C × 2h, last furnace cooling.
The beneficial effects of the present invention are:
(1) present invention innovatively proposes a kind of " high-energy ball milling-compression molding-vacuum non-pressure sintering " powder metallurgy work
Skill makes Ti, tri- kinds of elemental powders of Si, Zr and TiO by high-energy ball milling in the mixed powder stage2Nanometer powder is partially-alloyed,
In sintering process, further alloying, compared with ordinary powder metallurgical technology, this technique makes four kinds of mixed-powder alloyings more
Add sufficiently, for titanium provide one kind can industrialized production preparation method.
(2) Ti-4Si/5TiO of Zr alloying provided by the invention2The preparation method of alloy is easy to operate, easy realization, warp
Ji property is excellent.
(3) Zr alloying Ti-4Si/5TiO prepared by the present invention2It is metal alloy compositions compared to common Ti-4Si/
5TiO2Metal alloy compositions, comprehensive mechanical property, high temperature oxidation resistance, wear resistance etc. have different degrees of
It improves.
(4) high-temperature titanium alloy has been well solved to be difficult to break through the problem of 650 DEG C of application environment.
(5) present invention is applicable not only to Ti-4Si/5TiO2The preparation of series titanium alloy applies also for various model titaniums
Preparation, provides more information and theoretical foundation for the invention of titanium alloy material.
Reducing Si content can make material be provided simultaneously with preferable high temperature resistance and higher toughness.Therefore present invention choosing
It is basic sample with the Ti-4Si series composite materials of 4wt.%Si content.And nano-TiO2Addition can be formed it is resistant to high temperatures
The solid solution of oxidation improves the high temperature oxidation resistance of material.Zr plays solution strengthening effect, and wherein Ti-Si-Zr solid solution can
To improve the creep-resistant property of composite material.It is influenced on Ti-Si system α phase with β phase small, certain solution strengthening can be played and made
With, and study discovery (Ti, Zr)5Si3It is advantageous to the creep-resistant property of high-temperature titanium alloy.
Detailed description of the invention
Fig. 1 is Ti-4Si/5TiO after ball milling in comparative example of the present invention2The XRD diagram of powder；
Fig. 2 is Ti-4Si/5TiO after ball milling in comparative example of the present invention2The SEM of powder schemes；
Fig. 3 is Ti-4Si-1.3Zr/5TiO after ball milling in the embodiment of the present invention2The XRD diagram of powder；
Fig. 4 is Ti-4Si-1.3Zr/5TiO after ball milling in the embodiment of the present invention2The SEM of powder schemes；
Fig. 5 is Ti-4Si/5TiO after being sintered in comparative example of the present invention2The XRD diagram of alloy；
Fig. 6 is Ti-4Si/5TiO after being sintered in comparative example of the present invention2The SEM of alloy schemes；
Fig. 7 is Ti-4Si-1.3Zr/5TiO after being sintered in the embodiment of the present invention2The XRD diagram of alloy；
Fig. 8 is Ti-4Si-1.3Zr/5TiO after being sintered in the embodiment of the present invention2The SEM of alloy schemes；
Fig. 9 is the oxidizing dynamics curve of the embodiment of the present invention and comparative example at 900 DEG C, 1000 DEG C and 1100 DEG C.
Specific embodiment
Specific embodiments of the present invention will be described in detail with reference to the accompanying drawings and examples, but the present invention not only limits
In embodiment.
Embodiment 1.
A kind of Ti-4Si/5TiO of Zr alloying2Alloy, Ti-4Si-1.3Zr/5TiO2Preparation method:
Firstly, preparing Ti, Si, Zr elemental powders and TiO of 30g2The mixed-powder of nanometer powder, wherein Ti powder
89.7wt.% (26.91g), Si powder 4wt.% (1.2g), Zr powder 1.3wt.% (0.39g), TiO2Powder 5wt.% (1.5g) will be mixed
Conjunction powder, which is placed in a beaker, to stir evenly；
It is placed in 500ml nylon ball grinder secondly, first weighing 240g agate ball according to ratio of grinding media to material 8:1, then will weigh and mix
It closes uniform mixed-powder to be placed in nylon ball grinder, seal；
Then, ball grinder is mounted on planetary ball mill, starts ball milling, ball milling parameter is set as 300r/min, ball milling
1h shuts down 15min, after seeking mill 48h, takes out the powder in ball grinder；
Further, the mixed-powder of taking-up is crossed into 300 meshes, after obtaining the powder of uniform granularity, placed it in true
120 ± 10 DEG C of vacuum drying 2h, obtain required powder in empty drying box；
Later, gained powder is pressed in the powder compact forming method unidirectionally to be pressurizeed using mold, in mold
Diameter is φ=30mm, operating pressure 550MPa, and the round block of φ=30mm, 3~5mm of thickness is made；
Vacuum non-pressure sintering is carried out finally, gained briquetting is placed in two-chamber vacuum sintering furnace, first will be evacuated to 1 in furnace
×10-1Pa, heating rate be 10 DEG C/min, sintering process be 600 ± 10 DEG C × 2h+800 ± 10 DEG C × 2h+1000 ± 10 DEG C ×
2h+1250 ± 10 DEG C × 2h, last furnace cooling.
Using Ti-4Si-1.3Zr/5TiO made from above-mentioned steps2Mixed-powder mechanical alloying phenomenon is obvious, and Fig. 3 is
Resulting Ti-4Si-1.3Zr/5TiO after the present embodiment high-energy ball milling2The XRD diagram of powder, through analysis it is found that except detect Ti,
Si element and Ti5Si4、Ti5Si3、TiSi2, outside the titanium-silicon compounds such as TiSi, there are also Ti2Zr、Zr3Si2The solid solution of equal zirconiums,
Ti, Si, Zr simple substance are element activated to be increased, and solid solution diffusion rate improves, and it is solid to generate stable titanium silicon solid solution and titanium silicon zirconium
Solution has a small amount of Si element to have neither part nor lot in reaction.Comparison diagram 1 is it is found that in Ti-4Si/5TiO2Basic components add simple substance element
After Zr, compound Ti5Si3The enhancing of object phase diffraction maximum, and Ti5Si4、TiSi2Compound diffraction peak intensity weakens, and is converted into stable
Ti5Si3Compound, stability improve, and alloying effect is obvious；Fig. 7 is obtained XRD diagram after vacuum non-pressure sintering, sintered
Composite material is mainly by Ti element, Ti5Si3、Ti5Si4Equal Ti-Si compound and Zr3Si2、Ti2The Ti-Zr, Zr-Siization such as Zr
Object composition is closed, Ti additionally occurs2Zr3Si3Titanium silicon zirconium solid solution, the TiSi after not finding ball milling2, TiSi object phase.Comparison diagram 5
It is found that Ti5Si3The enhancing of object phase diffraction maximum, Ti5Si4Object phase diffraction maximum weakens.Zr element promotes titanium-silicon compound to be converted into stabilization
Ti5Si3Compound, while simple substance elements Si participates in reaction during vacuum non-pressure sintering and generates Ti-Si compound；Fig. 8 is
The SEM figure of Ti-4Si-1.3Zr/5TiO2 alloy after being sintered in embodiment, by pattern it is found that sintered material surface quality is good
Good, surface texture even compact, comparison diagram 6 is it is found that Ti-4Si-1.3Zr/5TiO2Alloy, alloying effect are obvious；Ti-4Si-
1.3Zr/5TiO2The microhardness of alloy is 1048HV, elasticity modulus 108.71GPa, fracture toughness 6.25MPa.m1/2,
The average oxidation speed K of 100h at 900 DEG C+Value is 0.292gm-2/ h, the average oxidation speed K of 100h at 1000 DEG C+Value is
0.555g·m-2/ h, the average oxidation speed K of 100h at 1100 DEG C+Value is 0.858gm-2/h；Wear scar width is 388 μm.
Comparative example
Ti-4Si/5TiO2The preparation method of composite material:
This comparative example and embodiment 1 are similar, the difference is that Zr powder is not added, the Ti of only 91wt.% (27.3g)
Powder, the Si powder of 4wt.% (1.2g) and the TiO of 5wt.% (1.5g)2Nano powder；
Fig. 1 is that high energy seeks Ti-4Si/5TiO after mill2The XRD diagram of powder, powder include Ti, Si simple substance object phase and TiSi2、
Ti5Si3、Ti5Si4Compound, the obvious alloying of powder known to diffraction maximum, and there is stable Ti5Si3Object phase, is deposited simultaneously
In a small amount of non-alloying of Ti, Si element；Fig. 2 is Ti-4Si/5TiO after ball milling in comparative example2The SEM of powder schemes, can by figure
Know, powder is not apparent from refinement after high-energy ball milling, and the phenomenon that reunion occurs；Fig. 5 is Ti-4Si/5TiO after vacuum non-pressure sintering2
The XRD diagram of alloy, composite sample is mainly by Ti5Si3、Ti5Si4In addition to this object phase composition also detects Ti element, not
Occur Si element, be to generate titanium-silicon compound during vacuum non-pressure sintering due to Ti, Si element, comparison diagram 1 it is found that
Ti5Si4The enhancing of object phase peak, unstable TiSi2Phase object inversion of phases is stable Ti5Si3Phase, Ti5Si4Phase；Fig. 6 is in comparative example
Ti-4Si/5TiO after sintering2The SEM of powder schemes, and as seen from the figure, microstructure of composite is fine and close, does not occur obvious shortcoming.Comparison diagram
2 it is found that composite alloy effect after sintering is obvious.Ti-4Si/5TiO2The microhardness of alloy is 672HV, elasticity
Modulus is 89.88GPa, fracture toughness 5.53MPa.m1/2；The average oxidation speed K of 100h at 900 DEG C+Value is 0.311gm-2/ h, the average oxidation speed K of 100h at 1000 DEG C+Value is 0.781gm-2/ h, the average oxidation speed K of 100h at 1100 DEG C+
Value is 1.375gm-2/h；Wear scar width is 500 μm.
Two embodiments and comparative example comparison are found, addition metal Zr powder carries out Ti- obtained after alloying
4Si-1.3Zr/5TiO2The alloying effect of alloy is obvious, and comprehensive performance ratio Ti-4Si/5TiO2It is good.Wherein, Ti-4Si-
1.3Zr/5TiO2The microhardness ratio Ti-4Si/5TiO of alloy2Alloy improves about 56% (1048HV VS 672HV), elasticity
Modular ratio Ti-4Si/5TiO2Alloy improves 21% (108.71Gpa VS 89.88Gpa), fracture toughness ratio Ti-4Si/5TiO2
Improve about 13% (6.25MPa.m1/2VS5.53MPa.m1/2), the average oxidation speed K of 100h at 900 DEG C+Value ratio Ti-4Si/
5TiO2Alloy reduces 6% (0.292gm-2/h VS 0.311g·m-2/ h), the average oxidation speed K of 100h at 1000 DEG C+
Value ratio Ti-4Si/5TiO2Alloy reduces 29% (05552gm-2/h VS 0.781g·m-2/ h), 100h's is flat at 1100 DEG C
Equal oxidation rate K+Value ratio Ti-4Si/5TiO2Alloy reduces 38% (0.858gm-2/h VS 1.375g·m-2/ h), polishing scratch
Width ratio Ti-4Si/5TiO2Alloy reduces 22.4% (388 μm of 500 μm of VS).
Embodiment 2.
The present embodiment and implement 1 difference be x value 1 (i.e. alloy be Ti-4Si-Zr/5TiO2), remaining with reality
Apply that example 1 is identical, the mixed-powder mechanical alloying phenomenon for preparing resulting material is obvious, resulting Ti-4Si- after high-energy ball milling
1Zr/5TiO2The XRD diagram of powder is similar with Fig. 3, through analysis it is found that except Ti, Si element and Ti is detected5Si4、Ti5Si3、
TiSi2, outside the titanium-silicon compounds such as TiSi, there are also Ti2Zr、Zr3Si2The solid solution of equal zirconiums, Ti, Si, Zr simple substance are element activated to be risen
Height, solid solution diffusion rate improve, generate stable titanium silicon solid solution and titanium silicon zirconium solid solution, have a small amount of Si element to have neither part nor lot in
Reaction.Comparison diagram 1 is it is found that in Ti-4Si/5TiO2After basic components add simple substance element Zr, compound Ti5Si3Object phase diffraction maximum
Enhancing, and Ti5Si4、TiSi2Compound diffraction peak intensity weakens, and is converted into stable Ti5Si3Compound, stability improve, and close
Aurification effect is obvious；The XRD diagram obtained after vacuum non-pressure sintering is also approximate with Fig. 7, and sintered composite material is mainly by Ti member
Element, Ti5Si3、Ti5Si4Equal Ti-Si compound and Zr3Si2、Ti2Ti-Zr, Zr-Si compound such as Zr composition, additionally occur
Ti2Zr3Si3Titanium silicon zirconium solid solution, the TiSi after not finding ball milling2, TiSi object phase.Comparison diagram 5 is it is found that Ti5Si3Object phase diffraction maximum
Enhancing, Ti5Si4Object phase diffraction maximum weakens.Zr element promotes titanium-silicon compound to be converted into stable Ti5Si3Compound, at the same it is single
Prime element Si participates in reaction during vacuum non-pressure sintering and generates Ti-Si compound；Ti-4Si-Zr/5TiO2 alloy after sintering
SEM figure it is similar with Fig. 8, by pattern it is found that sintered material surface quality is good, surface texture even compact, compare
Fig. 6 is it is found that Ti-4Si-Zr/5TiO2Alloy, alloying effect are obvious；Ti-4Si-Zr/5TiO2The microhardness of alloy, elasticity
Modulus, fracture toughness, the average oxidation speed K of 100h at 900 DEG C+It is worth, the average oxidation speed K of 100h at 1000 DEG C+Value,
The average oxidation speed K of 100h at 1100 DEG C+Value is that wear scar width etc. is similar with embodiment 1.It similarly can also be by this reality
The x value for applying example is changed to 1.5, and (i.e. alloy is Ti-4Si-1.5Zr/5TiO2), alloying effect and performance indexes and this
Embodiment is same or similar seemingly.
Part that the present invention does not relate to is the same as those in the prior art or can be realized by using the prior art.
Claims (7)
1. a kind of Ti-4Si/5TiO of Zr alloying2Alloy, it is characterized in that: Ti-4Si-xZr/5TiO2The component of alloy is with matter
Measure percentage to calculate, wherein Ti:(91-x) wt.%, Si:4wt.%, Zr:xwt.%, TiO2Nano powder: 5wt.%, each component
The sum of mass percent be 100%；Wherein the value of x is 1-1.5.
2. a kind of Ti-4Si/5TiO of the Zr alloying of claim 12The preparation method of alloy, it is characterized in that it includes following step
It is rapid:
(1) high-energy ball milling mixes powder: first preparing Ti-4Si-xZr/5TiO by composition2Mixed-powder is put into ball grinder, is placed in ball mill
Interior ball milling, so that tri- kinds of elemental powders of Ti, Si, Zr and TiO2Nanometer powder is partially-alloyed, by gained mixed powder after ball milling
End sieving is placed in drying in vacuum oven；
(2) conventional compression molding: mixed-powder prepared by step (1) is pressed, briquetting is obtained；
(3) vacuum non-pressure sintering: the briquetting of step (2) compression moulding is subjected to vacuum non-pressure sintering, so that Ti, Si, Zr, TiO2
Further alloying.
3. preparation method as claimed in claim 2, it is characterized in that the ball-milling technology of the high-energy ball milling are as follows: ratio of grinding media to material 8:1,
300r/min ball milling 48h, ball milling 1h shut down 15min.
4. preparation method as claimed in claim 2, it is characterized in that the composite powder after the ball milling is placed in vacuum oven,
It is warming up to after 60 DEG C with drying box and keeps the temperature 4h, cross 300 meshes.
5. preparation method as claimed in claim 2, it is characterized in that the technique of the compression moulding are as follows: the work used when compacting
Making pressure is 550MPa, and briquetting is the round block of φ=30mm, 3~5mm of thickness.
6. preparation method as claimed in claim 2, it is characterized in that briquetting is placed in vacuum oven before sintering, with drying box liter
Temperature is to keeping the temperature 6h after 100 DEG C.
7. preparation method as claimed in claim 2, it is characterized in that the technique of the vacuum non-pressure sintering are as follows: be evacuated to 1
×10-1Pa, heating rate be 10 DEG C/min, sintering process be 600 ± 10 DEG C × 2h+800 ± 10 DEG C × 2h+1000 ± 10 DEG C ×
2h+1250 ± 10 DEG C × 2h, last furnace cooling.
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| CN103556000A (en) * | 2013-11-11 | 2014-02-05 | 北京科技大学 | Ti-Si-Al-based alloy containing RE (rare earth) and intermetallic compound reinforcing phase |
| CN106119604A (en) * | 2016-08-18 | 2016-11-16 | 江苏大学 | A kind of Y2o3ti 8Si 1.4Zr alloy of alloying and preparation method thereof |
| CN106244852A (en) * | 2016-08-18 | 2016-12-21 | 江苏大学 | A kind of Ti 8Si alloy of Zr alloying and preparation method thereof |
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2018
- 2018-09-10 CN CN201811048240.3A patent/CN109022871B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003089831A (en) * | 2001-07-12 | 2003-03-28 | Komatsu Ltd | Copper-based sintered sliding material and multi-layer sintered sliding member |
| JP2008115419A (en) * | 2006-11-02 | 2008-05-22 | Nippon Steel Corp | Alpha-type titanium alloy material with excellent workability for exhaust system component, its manufacturing method, and exhaust system member using the alloy |
| CN103556000A (en) * | 2013-11-11 | 2014-02-05 | 北京科技大学 | Ti-Si-Al-based alloy containing RE (rare earth) and intermetallic compound reinforcing phase |
| CN106119604A (en) * | 2016-08-18 | 2016-11-16 | 江苏大学 | A kind of Y2o3ti 8Si 1.4Zr alloy of alloying and preparation method thereof |
| CN106244852A (en) * | 2016-08-18 | 2016-12-21 | 江苏大学 | A kind of Ti 8Si alloy of Zr alloying and preparation method thereof |
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