CN109182839A - A kind of Y2O3The Ti-4Si/5TiO of alloying2The preparation method of alloy - Google Patents
A kind of Y2O3The Ti-4Si/5TiO of alloying2The preparation method of alloy Download PDFInfo
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- 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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- B22F9/00—Making metallic powder or suspensions thereof
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- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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Abstract
A kind of Y2O3The Ti-4Si-0.3Y of alloying2O3/5TiO2The preparation method of alloy, it is characterised in that: its raw material for preparing is Ti powder, Si powder, nano-TiO2Powder and nanometer Y2O3Powder;Preparation method is firstly, by Ti powder, Si 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-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 Y2O3The Ti-4Si/5TiO of alloying2The preparation side of alloy
Method, specifically, being a kind of raising its compactness, comprehensive mechanical property, high temperature oxidation resistance, hot corrosion resistance and friction
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.Due to rare earth element or rare earth oxide Y2O3It, can with active rare-earth effect
To play the function of definitely refining crystal grain;Rare earth element or its oxide Y simultaneously2O3Disperse is distributed in material, is changed brilliant
Lattice put in order, and hinder dislocation, play dispersion-strengthened action, effectively improve the mechanical property of material.
So far, there has been no a kind of Y with independent intellectual property rights2O3The Ti-4Si/5TiO of alloying2The system of alloy
Preparation Method is available, this constrains the development of China's aerospace engine to a certain extent.
Summary of the invention
The present invention selects " high-energy ball milling-compression molding-vacuum non-pressure sintering " to prepare a kind of titanium silicozirconium, and by adding
Plus nano Y2O3Powder, prepares that a kind of comprehensive performance is preferable, the high titanium alloy material of titanium-silicon compound content.
Technical solution of the present invention first is that:
A kind of Y2O3The Ti-4Si/5TiO of alloying2The preparation method of alloy, it is characterised in that the Ti-4Si- of preparation
xY2O3/5TiO2The component of alloy powder is to calculate by percentage to the quality, wherein Ti powder: (91-x) wt.%, Si powder: 4wt.%,
Nano-TiO2Powder: 5wt.%, nanometer Y2O3Powder: xwt.%, the sum of mass percent of powder are the value range of 100%, x
For 0.1-0.5.
Technical solution of the present invention second is that:
A kind of Y2O3The Ti-4Si/5TiO of alloying2The preparation method of alloy, it is characterized in that it including the following steps:
(1) high-energy ball milling mixes powder: first preparing Ti-4Si-xY by composition2O3/5TiO2Mixed-powder is put into ball grinder, is placed in
With certain ball milling parameter ball milling in ball mill, so that Ti, Si, nano-TiO2Powder and nanometer Y2O3It closes four kinds of powder parts of powder
Gained mixed-powder after ball milling is sieved, is placed in drying in vacuum oven by aurification;
(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, receiving
Rice TiO2Powder and 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.
Composite powder after the ball milling is placed in vacuum oven, is warming up to after 60 ± 5 DEG C with drying box and keeps the temperature 4h, mistake
300 meshes.
The technique of the compression moulding are as follows: the operating pressure used when compacting for 550MPa, obtained round briquetting
The ratio between diameter and thickness are 6-10.
Briquetting is placed in vacuum oven before the sintering, keeps the temperature 6h after being warming up to 100 ± 5 DEG C with drying box.
The technique of the vacuum non-pressure sintering are as follows: be evacuated to 1 × 10-1Pa, heating rate are 10 DEG C/min, agglomerant
Skill 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, Si, nano-TiO by high-energy ball milling in the mixed powder stage2Powder and nanometer Y2O3Four kinds of powder of powder are partially-alloyed,
During the sintering process, further alloying, compared with ordinary powder metallurgical technology, this technique makes four kinds of powder metallurgyizatioies more
Sufficiently, for titanium provide it is a kind of can industrialized production preparation method.
(2) Y provided by the invention2O3The Ti-4Si/5TiO of alloying2The preparation method of alloy is easy to operate, it is easy realize,
Economical.
(3) Y prepared by the present invention2O3The Ti-4Si/5TiO of alloying2It is metal alloy compositions compared to common Ti-
4Si/5TiO2Metal alloy compositions, compactness, comprehensive mechanical property, high temperature oxidation resistance, heat/corrosion resistance and antifriction scouring
Damage performance 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-0.3Y after ball milling in the embodiment of the present invention2O3/5TiO2The XRD diagram of powder;
Fig. 4 is Ti-4Si-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-0.3Y after being sintered in the embodiment of the present invention2O3/5TiO2The XRD diagram of alloy;
Fig. 8 is Ti-4Si-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
The present invention is further illustrated with reference to the accompanying drawings and examples, but the present invention is not limited only to listed implementation
Example.
Embodiment one.
A kind of Y2O3The Ti-4Si/5TiO of alloying2Alloy, that is, Ti-4Si-0.3Y2O3/5TiO2Preparation method:
Firstly, preparing Ti, Si, the nano-TiO of 30g2Powder and nanometer Y2O3The mixed-powder of powder, wherein Ti powder
90.7wt.% (27.21g), Si powder 4wt.% (1.2g), nano-TiO2Powder 5wt.% (1.5g), nanometer Y2O3Powder 0.3wt.%
Mixed-powder is placed in a beaker by (0.09g) 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;The mixed-powder of taking-up is crossed into 300 meshes, obtains granularity
After uniform powder, 120 DEG C of vacuum drying 2h in vacuum oven are placed it in, when it is implemented, can also will mix after ball milling
Powder is placed in a vacuum drying oven, and is warming up to after 60 ± 5 DEG C with vacuum oven and is kept the temperature 4h, is crossed 300 meshes, is obtained required powder
Material;
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-0.3Y made from above-mentioned steps2O3/5TiO2Mixed-powder mechanical alloying phenomenon is obvious, and Fig. 3 is
Resulting Ti-4Si-0.3Y after the present embodiment high-energy ball milling2O3/5TiO2The XRD diagram of powder is matched after high-energy ball milling through analyzing
Fang Fenmo is mainly by simple substance object phase Ti and compound TiSi2、Ti5Si3、Ti5Si4Equal objects phase composition.With Fig. 1 compare it is found that
Ti-4Si/5TiO2Basic components add Y2O3Object phase composition later is similar, however TiSi2The object phase diffraction peak intensity ratio of compound
Ti5Si4The object phase diffraction peak intensity of compound is weak, illustrates Y2O3Oxide can promote TiSi2Object inversion of phases is Ti5Si4, finally
It is converted into stable Ti5Si3Object phase, alloying effect is obvious, and Si element is furthermore not detected, illustrates Y2O3Si can be promoted first
Element and Ti element reaction.Due to Y2O3Content is low, will form the solid solution of package in mechanical milling process, so the change of yttrium is not detected
Close object;Fig. 7 is obtained Ti-4Si-0.3Y after vacuum non-pressure sintering2O3/5TiO2The XRD diagram of alloy is obtained with Fig. 5 comparative analysis,
Object phase composition and Ti-4Si-5TiO2Composite-material formula is similar, contains simple substance element ti and Ti5Si4、Ti5Si3Equal compounds
Object phase, does not find TiSi2Object phase illustrates to add rare earth oxide Y2O3Titanium-silicon compound can be promoted to be converted into stable Ti5Si3
Object phase;In addition simple substance Si is not detected, and Ti Elemental Diffraction peak intensity reduces, and shows Y2O3Compound can improve Ti, Si element
Reaction efficiency, promote between each other reaction.Moreover, composite wood material phase Ti5Si3Compound diffraction peak intensity highest, shows to press
Alloying effect is excellent after embryo passes through vacuum non-pressure sintering;Ti-4Si-0.3Y2O3/5TiO2The apparent porosity of alloy is
3.8%, microhardness 859HV, elasticity modulus 95.85GPa, fracture toughness 5.89MPa.m1/2, 100h at 900 DEG C
Average oxidation speed K+Value is 0.267gm-2/ h, the average oxidation speed K of 100h at 1000 DEG C+Value is 0.359gm-2/ h,
The average oxidation speed K of 100h at 1100 DEG C+Value is 0.797gm-2/ h corrodes the unit after 30h under 750 DEG C of isoperibols
Area surrosion is 0.7852mg/cm2, wear scar width is 416 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 a nanometer Y2O3Powder, only 91wt.% (27.3g)
Ti 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 apparent porosity of alloy is 5.8%, micro-
Hardness is 672HV, elasticity modulus 89.88GPa, fracture toughness 5.53MPa.m1/2;The average oxidation speed of 100h at 900 DEG C
Spend K+Value is 0.311gm-2/ h, the average oxidation speed K of 100h at 1000 DEG C+Value is 0.781gm-2/ h, at 1100 DEG C
The average oxidation speed K of 100h+Value is 1.375gm-2/h;Unit area corrosion after corroding 30h under 750 DEG C of isoperibols
Weight gain is 0.9846mg/cm2, wear scar width is 500 μm.
Two embodiments and comparative example comparison are found, metal nano Y is added2O3Made from powder carries out after alloying
Ti-4Si-0.3Y2O3/5TiO2The alloying effect of alloy is obvious, and comprehensive performance ratio Ti-4Si/5TiO2It is good.Wherein, Ti-
4Si-0.3Y2O3/5TiO2The apparent porosity ratio Ti-4Si/5TiO of alloy2Alloy reduces about 34.5% (3.8%VS
5.8%), microhardness ratio Ti-4Si/5TiO2Alloy improves about 27.8% (859HV VS 672HV), modular ratio Ti-
4Si/5TiO2Alloy improves 6.6% (95.85Gpa VS 89.88Gpa), fracture toughness ratio Ti-4Si/5TiO2It improves about
6.5% (5.89MPa.m1/2VS 5.53MPa.m1/2), the average oxidation speed K of 100h at 900 DEG C+Value ratio Ti-4Si/5TiO2It closes
Gold reduces 14.1% (0.267gm-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 54.03% (0.359gm-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 42.03% (0.797gm-2/h VS 1.375g·m-2/ h),
Corrode the unit area surrosion ratio Ti-4Si/5TiO after 30h under 750 DEG C of isoperibols2Alloy reduces 20.3%
(0.7852mg/cm2VS 0.9846mg/cm2), wear scar width ratio Ti-4Si/5TiO2Alloy reduces 16.8% (416 μm of VS
500μm)。
Embodiment two.
The difference of the present embodiment and embodiment one is Y2O3Content it is different, the Y of the present embodiment2O3Content be 0.1, i.e.,
Preparing resulting alloy is Ti-4Si-0.1Y2O3/5TiO2, it is similar with embodiment one to survey indices.
Embodiment three.
The difference of the present embodiment and embodiment one is Y2O3Content it is different, the Y of the present embodiment2O3Content be 0.5, i.e.,
Preparing resulting alloy is Ti-4Si-0.5Y2O3/5TiO2, it is also similar with embodiment one to survey indices.
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 Y2O3The Ti-4Si/5TiO of alloying2Alloy, it is characterized in that: Ti-4Si-xY2O3/5TiO2The group of alloy powder
Dividing is to calculate by percentage to the quality, wherein Ti powder: (91-x) wt.%, Si powder: 4wt.%, nano-TiO2Powder: 5wt.%, nanometer
Y2O3Powder: xwt.%, the value range that the sum of mass percent of powder is 100%, x is 0.1-0.5.
2. Y as described in claim 12O3The Ti-4Si/5TiO of alloying2The preparation method of alloy, it is characterized in that according to following
Step carries out:
(1) high-energy ball milling mixes powder: first preparing Ti-4Si-xY by composition2O3/5TiO2Mixed-powder is put into ball grinder, is placed in ball milling
With certain ball milling parameter ball milling in machine, so that Ti, Si, nano-TiO2Powder and nanometer Y2O3Four kinds of powder of powder are partially-alloyed,
By gained mixed-powder sieving after ball milling, it 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, nano-TiO2
Powder and 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 ± 5 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, the ratio between diameter and thickness of obtained round briquetting are 6-10.
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 ± 5 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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CN111347048A (en) * | 2020-03-17 | 2020-06-30 | 苏勇君 | Low-cost titanium alloy indirect additive manufacturing method |
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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 |
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CN111347048A (en) * | 2020-03-17 | 2020-06-30 | 苏勇君 | Low-cost titanium alloy indirect additive manufacturing method |
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Application publication date: 20190111 |