CN104120325B - Low thermal expansion coefficient NaMxAlySiz high entropy alloy and preparation method thereof - Google Patents
Low thermal expansion coefficient NaMxAlySiz high entropy alloy and preparation method thereof Download PDFInfo
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- CN104120325B CN104120325B CN201410319113.8A CN201410319113A CN104120325B CN 104120325 B CN104120325 B CN 104120325B CN 201410319113 A CN201410319113 A CN 201410319113A CN 104120325 B CN104120325 B CN 104120325B
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Abstract
The invention relates to a low thermal expansion coefficient NaMxAlySiz high entropy alloy and a preparation method thereof, the chemical components of the alloy are as follows: 75 <= a <= 100%, 0 <= x <= 10%, 0<= y<= 10%, 0<= z<= 5%, N is arbitrary three or more than three of Ta, Nb, Hf, Zr, Ti, Mo and W, and M is any one or more than one of V, Mn, Fe, Co, Ni and Cr. The alloy phase structure is as follows: a body centered cubic solid solution and an intermetallic compound. The alloy is prepared by arc melting method in three stages. The NaMxAlySiz high entropy alloy has a low thermal expansion coefficient at the temperature in the range of room temperature to 1000 DEG C, the change rate is less than 20%, and the alloy has a broad application prospect in the high temperature industrial field.
Description
Technical field
The invention belongs to high-temperature alloy material field is and in particular to a kind of low thermal coefficient of expansion namxalysizHigh-entropy alloy
And preparation method thereof.
Background technology
The expansion principle of metal and its alloy is the raw anharmonic vibration of lattice-site paroxysm, and the composition by material,
The impact of structure and phase transformation etc..Expansion characteristics linear expansion coefficient or the coefficient of volume expansion represent.Common metal be heated after with temperature
Degree raises the coefficient of volume expansion and almost ramps, within the temperature range of 20-800 DEG C, the linear expansion coefficient α of ordinary metallic material
It is about 10-20 × 10-6/ DEG C.French physician c.e.guialme in 1896 finds when studying 36ni-fe alloy, its
(α is about 1. 2 × 10 to have very little thermal coefficient of expansion near room temperature-6/ DEG C), this alloy is referred to as low-expansion alloy.Boat
The fast development of empty cause and the outburst of energy crisis, cause jumping up of fuel price, have promoted commercial low bulk
The appearance of high temperature alloy.The high temperature alloy of low expansion character can strictly control the gap between engine rotation part and stationary parts
And tolerance, greatly improve energy output and fuel efficiency, be widely used in aerospace field.As certain electromotor outer shroud, by
Other alloys are changed to ni-fe-co system low expansion superalloy, only use this part instead, and oil consumption rate just have dropped about 2%.This
Outward, aerospace field also commonly uses the ceramic material of high temperature resistance, with the connection with more low-expansion ceramic material
Low expansion superalloy need to be used.
For meeting required various low-expansion alloy under different temperatures, people have developed large quantities of low bulks or fixed expansion is closed
Gold, from earliest commercial low bulk fe-ni alloy to ni-co-fe series low-expansion alloy again to the in738 being recently developed etc..
But, the deficiency of three aspects of these low-expansion alloy presence at present:
1) thermal expansion rates are not little
2) because the heat stability of microstructure is not enough, the coefficient of expansion improves with temperature and increases too fast
3) because fusing point is not high, service temperature is too low
Due to above reason, it is unfavorable for controlling between engine rotation part and stationary parts using existing low-expansion alloy
Gap and tolerance.Further, since the use temperature of conventional Lo-Ex close to its fusion temperature it is impossible to meet
Inlet temperature before higher turbine, hinders raising engine fuel efficiency further.Therefore research and development can be used for high temperature, larger
Temperature range can keep more low-expansion novel alloy to become the recent studies on direction in this field.
Content of the invention
The use temperature that present invention is directed to current high temperature low-expansion alloy presence is limited, and expansion rate is larger, and swollen
The shortcomings of swollen curve is precipitous is it is proposed that a kind of low-thermal-expansion namxalysizHigh-entropy alloy, alloy and preparation method thereof.
The technical scheme is that: a kind of low thermal coefficient of expansion namxalysizHigh-entropy alloy, the atom hundred of this alloying component
Dividing than expression formula is namxalysiZ,Wherein, 75≤a < 100 at%, 0≤x≤10 at %, 0≤y≤10 at %, 0≤z
≤5at %.
Further, described n is 99% for purity tantalum ta, niobium nb, hafnium hf, zirconium zr, titanium ti, three kinds in molybdenum mo, tungsten w with
On.
Further, one of described m is 99% for purity vanadium v, manganese mn, ferrum fe, cobalt co, nickel ni, chromium cr element or many
Kind.
In alloy, the effect of essential element: n is high-melting point alloy element, is also to promote to form body-centered cubic structure simultaneously
Element;The interpolation of si can form siliceous oxide on surface, puies forward heavy alloyed non-oxidizability, promote shape between crystal boundary simultaneously
Become silicide;The aluminium oxide that the interpolation surface of al forms densification puies forward heavy alloyed non-oxidizability.
The hot expansibility of alloy, in addition to the composition influence by alloy, is also affected by the organizational structure of alloy.This
Bright low heat expansion alloy adopts vacuum arc melting furnace melting, direct pouring molding, and technique is very simple.
It is a further object of the present invention to provide above-mentioned low thermal coefficient of expansion namxalysizThe preparation method of high-entropy alloy, bag
Include following steps:
Step 1: first the atomic percent expression formula of design alloying component is namxalysiZ,The atom of raw material after determining again
Percentage ratio is converted into mass ratio and weighs each raw material respectively;
Step 2: in the range of the n that step 1 is weighed, two kinds of metals of raw metal are one group of addition vacuum arc melting furnace,
It is placed in crucible and the angle horizontal by 20 ° -40 °, melt back 2 times, obtain the prealloy ingot of two kinds of metals, then by institute
The prealloy ingot having two kinds of metals melts together, obtains the prealloy ingot containing n;
Step 3: the prealloy ingot containing n that in the range of the m that step 1 is weighed, raw metal and step 2 obtain together is put
Enter vacuum melting furnace, will the initial alloy ingot that be formed after fusing, be placed in crucible and horizontal by 20 ° -40 ° angle repeatedly
Melting 3 times, obtains prealloy ingot;
Step 4: si and al that weigh step 1 and step 3 obtain prealloy ingot and together put into vacuum melting furnace, will melt
The initial alloy ingot being formed after change, is placed in crucible and the angle melt back 5 times horizontal by 20 ° -40 °, smelting and pouring
Become alloy pig, this alloy pig average coefficient of linear expansion between room temperature is to 1000 DEG C is not more than 12 × 10-6/ DEG C, and thermal expansion system
Number rate of change is less than 20%, and this alloy is mainly body center cubic solid solution and a small amount of intermetallic compound for structure.
The low-thermal-expansion n that the preparation method of the present invention is madeamxalysizHigh-entropy alloy is average between room temperature is to 1000 DEG C
Linear expansion coefficient is not more than 12 × 10-6/DEG C, thermal coefficient of expansion rate of change is less than 20%.The low bulk high-entropy alloy of the present invention is suitable
It is applied to the part working under hot conditionss.
The present invention is compared with prior art had an advantage in that
(1) alloy melting point of the present invention is higher than 1600 DEG C, and more existing low-expansion alloy at least improves 300 DEG C using temperature;
(2) with existing low expansion superalloy, the thermal coefficient of expansion of alloy of the present invention reduces 3-10 × 10-6/DEG C model
Enclose, and thermal coefficient of expansion rate of change reduces 10%-20%.
(3) by the xrd spectral line in the range of 50 DEG C -1000 DEG C of thermal dilatometry and Fig. 9 embodiment 2 of Fig. 8 embodiment 2
Find out, in temperature-rise period, alloy structure does not undergo phase transition, alloy of the present invention is described, and microstructure is highly stable at high temperature.
Specific embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
1. alloying component
The alloying component of embodiment 1 is ta5nb17.5hf17.5zr17.5ti17.5mo5w5al10si5.
2. the melting of alloy
The melting of alloy comprises the following steps:
Step 1: design alloying component atomic percent expression formula be
ta5nb17.5hf17.5zr17.5ti17.5mo5w5al10si5, then the atomic percent of raw material is converted into mass ratio and claims respectively after determining
Take each raw material;
Step 2: mo, ti are set to one group, w, hf are set to one group, ta, nb, zr are set to one group, are separately added into vacuum electric
Arc smelting furnace, is placed in crucible and the angle horizontal by 20 ° -40 °, melt back 2 times, obtains the prealloy of two kinds of metals
Ingot, then the prealloy ingot of all two kinds of metals is melted together, obtain the prealloy ingot containing n;
Step 3: si, the al that weigh step 1 and step 2 obtain prealloy ingot and together put into vacuum melting furnace, will melt
The initial alloy ingot being formed after change, is placed in crucible and the angle melt back 5 times horizontal by 20 ° -40 °, smelting and pouring
Become alloy pig.
3. the tissue signature of alloy
Prepared by tissue topography's figure of the as cast condition of Fig. 1 embodiment 1 and the as cast condition xrd figure of Fig. 2 embodiment 1 can be seen that
The alloy microstructure of embodiment, wherein dendrite are body center cubic solid solution, and intercrystalline is distributed intermetallic compound on a small quantity.
Embodiment 2
1. alloying component
The alloying component of embodiment 2 is ta10nb19hf5zr5ti7mo8w35v10si1.
2. the melting of alloy
The melting of alloy comprises the following steps:
Step 1: the atomic percent expression formula of design alloying component is ta10nb19hf5zr5ti7mo8w35v10si1, then will
After determination, the atomic percent of raw material is converted into mass ratio and weighs each raw material respectively;
Step 2: mo, ti are set to one group, w, hf are set to one group, ta, nb, zr are set to one group, are separately added into vacuum electric
Arc smelting furnace, is placed in crucible and the angle horizontal by 20 ° -40 °, melt back 2 times, obtains the prealloy of two kinds of metals
Ingot, then the prealloy ingot of all two kinds of metals is melted together, obtain the prealloy ingot containing n;
Step 3: vacuum melting furnace together put into by the prealloy ingot containing n that the v that step 1 is weighed is obtained with step 2, will
The initial alloy ingot being formed after fusing, is placed in crucible and the angle melt back 3 times horizontal by 20 ° -40 °, obtains pre-
Alloy pig;
Step 4: si, the al that weigh step 1 and step 3 obtain prealloy ingot and together put into vacuum melting furnace, will melt
The initial alloy ingot being formed after change, is placed in crucible and the angle melt back 5 times horizontal by 20 ° -40 °, smelting and pouring
Become alloy pig.
3. the tissue signature of alloy
The alloy microstructure of prepared embodiment be can be seen that by tissue topography's figure of Fig. 3 embodiment alloy 2 as cast condition,
Wherein dendrite is body center cubic solid solution, and intercrystalline is distributed intermetallic compound on a small quantity.Fig. 8,9 can be seen that alloy of the present invention is high
The lower microstructure of temperature is highly stable.
Embodiment 3
1. alloying component
The alloying component of embodiment 3 is ta8nb5hf35zr12ti5mo15w15co1al1si3.
2. the melting of alloy
The melting of alloy comprises the following steps:
Step 1: the atomic percent expression formula of design alloying component is ta8nb5hf35zr12ti5mo15w15co1al1si3, then
After determining, the atomic percent of raw material is converted into mass ratio and weighs each raw material respectively;
Step 2: mo, ti are set to one group, w, hf are set to one group, ta, nb, zr are set to one group, are separately added into vacuum electric
Arc smelting furnace, is placed in crucible and the angle horizontal by 20 ° -40 °, melt back 2 times, obtains the prealloy of two kinds of metals
Ingot, then the prealloy ingot of all two kinds of metals is melted together, obtain the prealloy ingot containing n;
Step 3: the prealloy ingot containing n that the co that step 1 is weighed is obtained with step 2 together puts into vacuum melting furnace,
Will the initial alloy ingot that be formed after fusing, be placed in crucible and the angle melt back 3 times horizontal by 20 ° -40 °, obtain
Prealloy ingot;
Step 4: si, the al that weigh step 1 and step 3 obtain prealloy ingot and together put into vacuum melting furnace, will melt
The initial alloy ingot being formed after change, is placed in crucible and the angle melt back 5 times horizontal by 20 ° -40 °, smelting and pouring
Become alloy pig.
3. the tissue signature of alloy
The alloy microstructure of prepared embodiment be can be seen that by tissue topography's figure of Fig. 4 embodiment alloy 3 as cast condition,
Wherein dendrite is body center cubic solid solution, and intercrystalline is distributed intermetallic compound on a small quantity.
Embodiment 4
1. alloying component
The alloying component of embodiment 4 is ta35nb5.2hf5.2zr5.2ti5.2mo35w5.2fe2si2.
2. the melting of alloy
The melting of alloy comprises the following steps:
Step 1: design alloying component atomic percent expression formula be
ta35nb5.2hf5.2zr5.2ti5.2mo35w5.2fe2si2, then the atomic percent of raw material is converted into mass ratio and claims respectively after determining
Take each raw material;
Step 2: mo, ti are set to one group, w, hf are set to one group, ta, nb, zr are set to one group, are separately added into vacuum electric
Arc smelting furnace, is placed in crucible and the angle horizontal by 20 ° -40 °, melt back 2 times, obtains the prealloy of two kinds of metals
Ingot, then the prealloy ingot of all two kinds of metals is melted together, obtain the prealloy ingot containing n;
Step 3: the prealloy ingot containing n that the fe that step 1 is weighed is obtained with step 2 together puts into vacuum melting furnace,
Will the initial alloy ingot that be formed after fusing, be placed in crucible and the angle melt back 3 times horizontal by 20 ° -40 °, obtain
Prealloy ingot;
Step 4: the si step 3 that step 1 is weighed obtains prealloy ingot and together puts into vacuum melting furnace, shape after melting
The initial alloy ingot becoming, is placed in crucible and the angle melt back 5 times horizontal by 20 ° -40 °, smelting and pouring becomes alloy
Ingot.
3. the tissue signature of alloy
The alloy microstructure of prepared embodiment be can be seen that by tissue topography's figure of Fig. 5 embodiment alloy 4 as cast condition,
Wherein dendrite is body center cubic solid solution, and intercrystalline is distributed intermetallic compound on a small quantity.
Embodiment 5
1. alloying component
The alloying component of embodiment 5 is ta8nb11hf15zr35ti15mo15w15al4ni2.
2. the melting of alloy
The melting of alloy comprises the following steps:
Step 1: the atomic percent expression formula of design alloying component is ta8nb11hf15zr35ti15mo15w15al4ni2, then
After determining, the atomic percent of raw material is converted into mass ratio and weighs each raw material respectively;
Step 2: mo, ti are set to one group, w, hf are set to one group, ta, nb, zr are set to one group, are separately added into vacuum electric
Arc smelting furnace, is placed in crucible and the angle horizontal by 20 ° -40 °, melt back 2 times, obtains the prealloy of two kinds of metals
Ingot, then the prealloy ingot of all two kinds of metals is melted together, obtain the prealloy ingot containing n;
Step 3: the prealloy ingot containing n that the ni that step 1 is weighed is obtained with step 2 together puts into vacuum melting furnace,
Will the initial alloy ingot that be formed after fusing, be placed in crucible and the angle melt back 3 times horizontal by 20 ° -40 °, obtain
Prealloy ingot;
Step 4: the si step 3 that step 1 is weighed obtains prealloy ingot and together puts into vacuum melting furnace, shape after melting
The initial alloy ingot becoming, is placed in crucible and the angle melt back 5 times horizontal by 20 ° -40 °, smelting and pouring becomes alloy
Ingot.
3. the tissue signature of alloy
By tissue topography's figure of Fig. 6 embodiment 5 it can be seen that the phase structure of alloy of prepared embodiment is: body-centered cubic is solid
Solution.
Implement to grin 6
1. alloying component
The alloying component of embodiment 2 is ta8nb35hf10zr10ti10mo10w10al4cr1si2.
2. the melting of alloy
The melting of alloy comprises the following steps:
Step 1: the atomic percent expression formula of design alloying component is ta8nb35hf10zr10ti10mo10w10al4cr1
si2, then the atomic percent of raw material is converted into mass ratio and weighs each raw material respectively after determining;
Step 2: mo, ti are set to one group, w, hf are set to one group, ta, nb, zr are set to one group, are separately added into vacuum electric
Arc smelting furnace, is placed in crucible and the angle horizontal by 20 ° -40 °, melt back 2 times, obtains the prealloy of two kinds of metals
Ingot, then the prealloy ingot of all two kinds of metals is melted together, obtain the prealloy ingot containing n;
Step 3: the prealloy ingot containing n that the cr that step 1 is weighed is obtained with step 2 together puts into vacuum melting furnace,
Will the initial alloy ingot that be formed after fusing, be placed in crucible and the angle melt back 3 times horizontal by 20 ° -40 °, obtain
Prealloy ingot;
Step 4: al, si step 3 that step 1 is weighed obtains prealloy ingot and together puts into vacuum melting furnace, will melt
The initial alloy ingot being formed afterwards, is placed in crucible and the angle melt back 5 times horizontal by 20 ° -40 °, smelting and pouring becomes
Alloy pig.
3. the tissue signature of alloy
Can be seen that the phase structure of alloy of prepared embodiment is: body-centered cubic by tissue topography's figure of Fig. 7 embodiment 6
Solid solution and a small amount of intermetallic compound.
7th, the hot expansibility of alloy of the present invention
The hot expansibility of alloy of the present invention is as shown in table 1:
The hot expansibility of table 1 alloy of the present invention
In sum, alloy of the present invention has high applicable temperature range, and thermal coefficient of expansion is not only low but also thermal expansion
Process is slow, stable.
Claims (1)
1. a kind of low thermal coefficient of expansion namxalysizThe preparation method of high-entropy alloy is it is characterised in that the atom of this alloying component
Percentage expression formula is namxalysiZ,Wherein, 75≤a < 100 at%, 0≤x≤10 at %, 0≤y≤10 at %, 0
Tantalum ta that≤z≤5at %, described n are 99% for purity, niobium nb, hafnium hf, zirconium zr, titanium ti, more than three kinds in molybdenum mo, tungsten w, institute
State one or more of the vanadium v that m is 99%, manganese mn, ferrum fe, cobalt co, nickel ni, chromium cr element it is characterised in that including following
Step:
Step 1: first the atomic percent expression formula of design alloying component is namxalysiZ,The atomic percent of raw material after determining again
Weigh each raw material than being converted into mass ratio respectively;
Step 2: in the range of the n that step 1 is weighed, two kinds of metals of raw metal are one group of addition vacuum arc melting furnace, are placed in
Angle in crucible and horizontal by 20 ° -40 °, melt back 2 times, obtain the prealloy ingot of two kinds of metals, then by all two
The prealloy ingot planting metal melts together, obtains the prealloy ingot containing n;
Step 3: the prealloy ingot containing n that in the range of the m that step 1 is weighed, raw metal and step 2 obtain together is put into very
Empty smelting furnace, will the initial alloy ingot that be formed after fusing, be placed in crucible and the angle melt back horizontal by 20 ° -40 °
3 times, obtain prealloy ingot;
Step 4: si and al that weigh step 1 and step 3 obtain prealloy ingot and together put into vacuum melting furnace, after melting
The initial alloy ingot being formed, is placed in crucible and the angle melt back 5 times horizontal by 20 ° -40 °, smelting and pouring becomes to close
Ingot, this alloy pig average coefficient of linear expansion between room temperature is to 1000 DEG C is not more than 12 × 10-6/ DEG C, and thermal coefficient of expansion change
Rate is less than 20%, and this alloy is mainly body center cubic solid solution and a small amount of intermetallic compound for structure.
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