CN109207795A - A kind of Zr, Y2O3The Ti-4Si/5TiO of alloying2Alloy and preparation method thereof - Google Patents
A kind of Zr, Y2O3The Ti-4Si/5TiO of 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
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Abstract
A kind of Zr, Y2O3The Ti-4Si/5TiO of alloying2Alloy and preparation method thereof, it is characterised in that: its raw material for preparing is Ti powder, Si powder, Zr powder, nano-TiO2Powder and nanometer Y2O3Powder；Preparation method is firstly, by Ti powder, Si powder, Zr powder, nano-TiO2Powder and nanometer Y2O3Powder carries out high-energy ball milling after mixing, keeps its partially-alloyed, then the resulting powder of ball milling is sieved, dry, and briquetting then is made by compression molding in dry powder, finally by vacuum non-pressure sintering, makes its abundant alloying.Ti-4Si-1.3Zr-0.3Y provided by the invention2O3/5TiO2Compactness, comprehensive mechanical property, high temperature oxidation resistance, heat/corrosion resistance and wearability of alloy 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, especially Zr, Y2O3The Ti-4Si/5TiO of alloying2The preparation of alloy
A kind of method, specifically, being its compactness of raising, comprehensive mechanical property, high temperature oxidation resistance, hot corrosion resistance and rubbing
Wipe the preparation method of the titanium silicon systems metal alloy compositions of polishing machine.
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-
High-temperature oxydation, thermophilic corrosion-resistance etc. 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.It reduces
Si content can make material be provided simultaneously with preferable high temperature resistance and higher toughness.Therefore the present invention selects 4wt.%Si to contain
The Ti-4Si series composite materials of amount are basic sample.And nano-TiO2Addition can form the solid solution of resistance to high temperature oxidation
Body improves the high temperature oxidation resistance of material.Zr plays solution strengthening effect, and wherein Ti-Si-Zr solid solution can be improved compound
The creep-resistant property of material.It is influenced on Ti-Si system α phase with β phase small, certain solution strengthening effect can be played, and study
It was found that (Ti, Zr)5Si3It is advantageous to the creep-resistant property of high-temperature titanium alloy.Further, since rare earth element or rare earth oxide tool
There is active rare-earth effect, the function of definitely refining crystal grain can be played；The distribution of rare earth element or its dispersed oxide simultaneously
In material, dislocation is hindered, dispersion-strengthened action is played, improves the service performance of alloy.
So far, there has been no a kind of a kind of Zr, Y with independent intellectual property rights2O3The Ti-4Si/5TiO of alloying2It closes
The preparation method of gold is available, this constrains the development of China's aerospace engine to a certain extent.
Summary of the invention
Aiming at the problem that purpose of the present invention high temperature poor toughness existing for the existing Ti-Si, invent a kind of high temperature resistance with
Toughness and strong Zr, the Y of creep resisting ability2O3The Ti-4Si/5TiO of alloying2Alloy, while a kind of " high-energy ball milling-molding being provided
Molding-vacuum non-pressure sintering " preparation method, it passes through addition metallic element Zr and rare earth oxide Y2O3, synthesis is prepared
Better performances, the high titanium alloy material of titanium-silicon compound content.
Technical solution of the present invention first is that:
A kind of Zr, Y2O3The Ti-4Si/5TiO of alloying2The preparation method of alloy, it is characterised in that the Ti-4Si- of preparation
xZr-yY2O3/5TiO2The component of alloy powder is to calculate by percentage to the quality, wherein Ti powder: (91-x-y) wt.%, Si powder:
4wt.%, Zr powder: xwt.%, nano TiO 2 powder: 5wt.%, nanometer Y2O3Powder: ywt.%, the sum of mass percent of each component
It is 100%, wherein the value range of x is 1-1.5, and the value range of y is 0.1-0.5.
Technical solution of the present invention second is that:
A kind of Zr, Y2O3The Ti-4Si/5TiO of alloying2The preparation method of alloy, it is characterized in that it mainly includes following several
A step:
(1) high-energy ball milling mixes powder: first preparing Ti-4Si-xZr-yY by composition2O3/5TiO2Mixed-powder is put into ball grinder,
It is placed in ball mill with certain ball milling parameter ball milling, so that tri- kinds of elemental powders of Ti, S, Zr, nano-TiO2Powder and nanometer
Y2O3Powder is partially-alloyed, and 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: carrying out vacuum non-pressure sintering for the briquetting of step (2) compression moulding so that Ti, Si, Zr,
TiO2And Y2O3Further alloying.
Described Zr, the Y2O3The Ti-4Si/5TiO of alloying2Step (1) ball-milling technology in the preparation method of alloy
Are as follows: ratio of grinding media to material 8:1,300r/min ball milling 48h, ball milling 1h shut down 15min.
Described Zr, the Y2O3The Ti-4Si/5TiO of alloying2Step (1) drying means in the preparation method of alloy
Are as follows: 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.
Described Zr, the Y2O3The Ti-4Si/5TiO of alloying2Step (2) mould pressing process in the preparation method of alloy
Are as follows: for the operating pressure used when compacting for 550MPa, briquetting is the round block of φ=30mm, 3~5mm of thickness.
Described Zr, the Y2O3Step (3) sintering process in the preparation method of the Ti-4Si/5TiO2 alloy of alloying
Are as follows: it is evacuated 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 tri- kinds of elemental powders of Ti, Si, Zr, nano-TiO by high-energy ball milling in the mixed powder stage2Powder and nanometer Y2O3Powder portion
Division aurification, during the sintering process, further alloying, compared with ordinary powder metallurgical technology, this technique makes four kinds of mixing
Powder metallurgyization is more abundant, for titanium provide it is a kind of can industrialized production preparation method.
(2) Zr, Y provided by the invention2O3The Ti-4Si/5TiO of alloying2The preparation method of alloy is easy to operate, Yi Shi
It is existing, economical.
(3) Zr, Y prepared by the present invention2O3The Ti-4Si/5TiO of alloying2Alloy material is compared to common Ti-4Si/
5TiO2Metal alloy compositions, compactness, comprehensive mechanical property, high temperature oxidation resistance, heat/corrosion resistance and rub resistance abrasiveness
Energy etc. has different degrees of raising.
(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.
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-0.3Y after ball milling in the embodiment of the present invention2O3/5TiO2The XRD diagram of powder；
Fig. 4 is Ti-4Si-1.3Zr-0.3Y after ball milling in the embodiment of the present invention2O3/5TiO2The 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-0.3Y after being sintered in the embodiment of the present invention2O3/5TiO2The XRD diagram of alloy；
Fig. 8 is Ti-4Si-1.3Zr-0.3Y after being sintered in the embodiment of the present invention2O3/5TiO2The 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；
Figure 10 is that the embodiment of the present invention and comparative example corrode 30h in 750 DEG C of 25%NaCl+75%Na2SO4 fused salt
Kinetic curve.
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 Zr, Y2O3The Ti-4Si/5TiO of alloying2Alloy, Ti-4Si-1.3Zr-0.3Y2O3/5TiO2Preparation side
Method:
Firstly, preparing Ti, Si, Zr elemental powders of 30g, nano-TiO2Powder and nanometer Y2O3The mixed-powder of powder,
Wherein Ti powder 89.4wt.% (26.82g), Si powder 4wt.% (1.2g), Zr powder 1.3wt.% (0.39g), Y2O3Powder 0.3wt.%
(0.09g), TiO2Mixed-powder is placed in a beaker by powder 5wt.% (1.5g) 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 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.
Using Ti-4Si-1.3Zr-0.3Y made from above-mentioned steps2O3/5TiO2Mixed-powder mechanical alloying phenomenon is bright
Aobvious, Fig. 3 is resulting Ti-4Si-1.3Zr-0.3Y after the present embodiment high-energy ball milling2O3/5TiO2The XRD diagram of powder, through analyzing,
Contain Ti after mixed-powder high-energy ball milling5Si3、Ti5Si4, TiSi and TiSi2Equal titaniums silicon object phase and Ti2Zr and Zr3Si2Deng change
Object is closed, does not occur Ti, Si element.Comparison diagram 1 is it is found that addition Zr and Y2O3It can promote the reaction of Ti, Si element；Fig. 7 is vacuum
The XRD diagram obtained after pressureless sintering, comparison diagram 5 is it is found that composite material contains Ti5Si4、Ti5Si3Equal objects phase and Ti2Zr、
Zr3Si2Equal solid solution, nothing detect TiSi2, the objects phase such as TiSi, illustrate TiSi2, TiSi compound is in vacuum non-pressure sintering process
In be converted into stable Ti-Si compound；Ti-4Si-1.3Zr-0.3Y2O3/5TiO2The apparent porosity 2.9% of alloy, it is micro- hard
Degree is 1478HV, elasticity modulus 120.68GPa, fracture toughness 8.68MPa.m1/2, the average oxidation speed of 100h at 900 DEG C
Spend K+Value is 0.206gm-2/ h, the average oxidation speed K of 100h at 1000 DEG C+Value is 0.383gm-2/ h, at 1100 DEG C
The average oxidation speed K of 100h+Value is 0.711gm-2/ h, the unit area corrosion after corroding 30h under 750 DEG C of isoperibols
Weight gain is 0.6856mg/cm2, wear scar width is 222 μm.
Comparative example
Ti-4Si/5TiO2The preparation method of composite material:
This comparative example and embodiment 1 are similar, the difference is that not adding Zr powder and nanometer Y2O3Powder, only 91wt.%
The Ti powder of (27.3g), the Si powder of 4wt.% (1.2g) and the TiO of 5wt.% (1.5g)2Nano powder；
Fig. 1 be high energy ask mill after Ti-4Si/5TiO2 powder XRD diagram, 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,
Exist simultaneously 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, by
Figure is it is found that powder is not apparent from refinement after high-energy ball milling, and the phenomenon that reunion occurs；Fig. 5 is Ti-4Si/ after vacuum non-pressure sintering
5TiO2The XRD diagram of alloy, composite sample is mainly by Ti5Si3、Ti5Si4In addition to this object phase composition also detects Ti member
Element does not occur Si element, is to generate titanium-silicon compound during vacuum non-pressure sintering due to Ti, Si element, comparison diagram 1 can
Know, Ti5Si4The enhancing of object phase peak, unstable TiSi2Phase object inversion of phases is stable Ti5Si3Phase, Ti5Si4Phase；Fig. 6 is comparison
Ti-4Si/5TiO after being sintered in example2The SEM of powder schemes, and as seen from the figure, microstructure of composite is fine and close, does not occur obvious shortcoming.It is right
Than Fig. 2 it is found that composite alloy effect after sintering is obvious；Ti-4Si/5TiO2The apparent porosity of alloy is 5.8%,
Microhardness is 672HV, elasticity modulus 89.88GPa, fracture toughness 5.53MPa.m1/2, the averaged oxygen of 100h at 900 DEG C
Change speed K+Value is 0.311gm-2/ h, the average oxidation speed K of 100h at 1000 DEG C+Value is 0.781gm-2/ h, 1100 DEG C
The average oxidation speed K of lower 100h+Value is 1.375gm-2/ h, wear scar width are 500 μm.
Two embodiments and comparative example comparison are found, metal Zr powder and nanometer Y are added2O3Powder carry out alloying it
Ti-4Si-1.3Zr-0.3Y obtained afterwards2O3/5TiO2The alloying effect of alloy is obvious, and comprehensive performance ratio Ti-4Si/
5TiO2It is good.Wherein, Ti-4Si-1.3Zr-0.3Y2O3/5TiO2The apparent porosity ratio Ti-4Si/5TiO of alloy2Alloy reduces
50% (29%VS 5.8%), microhardness ratio Ti-4Si/5TiO2Alloy improves about 1.2 times (1478HV VS 672HV),
Modular ratio Ti-4Si/5TiO2Alloy improves 34.27% (120.68Gpa VS 89.88Gpa), fracture toughness ratio Ti-
4Si/5TiO2Improve about 36.29% (8.68MPa.m1/2VS 5.53MPa.m1/2), the average oxidation speed of 100h at 900 DEG C
K+Value ratio Ti-4Si/5TiO2Alloy reduces 33.76% (0.206gm-2/h VS 0.311g·m-2/ h), at 1000 DEG C
The average oxidation speed K of 100h+Value ratio Ti-4Si/5TiO2Alloy reduces 50.96% (0.383gm-2/h VS
0.781g·m-2/ h), the average oxidation speed K of 100h at 1100 DEG C+Value ratio Ti-4Si/5TiO2Alloy reduces 48.29%
(0.711g·m-2/h VS 1.375g·m-2/ h), corrode the unit area surrosion after 30h under 750 DEG C of isoperibols
Compare Ti-4Si/5TiO2Alloy reduces 30.4% (0.6856mg/cm2VS 0.9846mg/cm2) wear scar width ratio Ti-4Si/
5TiO2Alloy reduces 55.6% (222 μm of 500 μm of VS).
Embodiment 2.
This implementation the difference from embodiment 1 is that alloying Zr, Y2O3Component it is different, Zr, Y of the present embodiment2O3
Component be respectively 1 and 0.1, resulting alloy is Ti-4Si-Zr-0.1Y2O3/5TiO2, remaining each component and preparation method with
Embodiment 1 is identical.
Embodiment 3.
This implementation the difference from embodiment 1 is that alloying Zr, Y2O3Component it is different, Zr, Y of the present embodiment2O3
Component be respectively 1.5 and 0.5, resulting alloy is Ti-4Si-1.5Zr-0.5Y2O3/5TiO2, remaining each component and preparation side
Method is same as Example 1.
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 Zr, Y2O3The Ti-4Si/5TiO of alloying2Alloy, it is characterized in that: Ti-4Si-xZr-yY2O3/5TiO2Alloyed powder
The component at end is to calculate by percentage to the quality, wherein Ti powder: (91-x-y) wt.%, Si powder: 4wt.%, Zr powder: xwt.% receives
Rice TiO2Powder: 5wt.%, nanometer Y2O3Powder: ywt.%, the sum of mass percent of each component are 100%, wherein the value model of x
It encloses for 1-1.5, the value range of y is 0.1-0.5.
2. a kind of Zr, Y described in claim 12O3The Ti-4Si/5TiO of alloying2The preparation method of alloy, it is characterized in that it
The following steps are included:
(1) high-energy ball milling mixes powder: first preparing Ti-4Si-xZr-yY by composition2O3/5TiO2Mixed-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, nano-TiO2Powder and nanometer Y2O3Powder
Gained mixed-powder after ball milling is sieved, is placed in drying in vacuum oven by end part alloying；
(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,
Y2O3Further alloying.
3. preparation method as claimed in claim 2, it is characterized in that the ball-milling technology of 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 ball milling is placed in vacuum oven, with drying
Case keeps the temperature 4h after being warming up to 60 DEG C, cross 300 meshes.
5. preparation method as claimed in claim 2, it is characterized in that the technique of compression moulding are as follows: the operating pressure used when compacting
For 550MPa, 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 green compact 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 vacuum non-pressure sintering are as follows: be evacuated 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.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105274375A (en) * | 2015-10-29 | 2016-01-27 | 江苏大学 | Method for compounding and preparing high-elastic-modulus Ti-based material based on nano ceramic particles |
| 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 |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105274375A (en) * | 2015-10-29 | 2016-01-27 | 江苏大学 | Method for compounding and preparing high-elastic-modulus Ti-based material based on nano ceramic particles |
| 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 |
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