CN108893652A - A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy and preparation method thereof - Google Patents
A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy 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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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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Abstract
A kind of preparation method of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy, the titanium alloy contain the component of following mass percents:4.5~6.7% Al, 0.5~4.5% Nb, 1.0~4.0% Zr, 0.5~2.0% Mo surplus are Ti.Preparation method includes:The cleaning of raw material Ti, Al, Nb, Zr, Mo and accurate weighing;Melting in vacuum non-consumable arc furnace, to guarantee that alloying component is uniform, equal melting 5 times of each alloy;It is heat-treated, in high temperature high vacuum tube furnace, 900 DEG C of heat preservation 2h, furnace cooling.Experimental considerations:By characterizing Room-Temperature Fracture Toughness, compressive strength, compression limit dependent variable and the etch resistant properties of alloy, and orthogonal calculation is carried out, it is determined that optimal alloying component is:Ti-5.5Al-3.0Nb-3.0Zr-1.5Mo.High strength anti-corrosion titanium alloy in the present invention is a kind of novel nearly alpha titanium alloy, have both excellent Room-Temperature Fracture Toughness, higher room temperature compressive strength, compression limit dependent variable and good etch resistant properties are expected to be applied to marine engineering equipment, have a good application prospect.
Description
Technical field
The invention belongs to titanium alloy preparation technical fields, and in particular to a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy
And preparation method thereof.
Background technique
The high development of today's society be unable to do without the support of the natural energy sources such as petroleum, natural gas, but explores exploitation and be easier to
Land natural energy source increasingly reducing, the correlative study of fungible energy source is also still immature, and energy problem is current at limitation
The major reason of social and economic development.Many countries have concentrated one's gaze on sight the ocean of ABUNDANT NATUREAL RESOURSES in this case,
Start to greatly develop ocean engineering.Special due to Service Environment, the selection of material is most important for each ocean engineering.
In view of Service Environment, marine engineering equipment material therefor need high intensity, high tenacity, it is anticorrosive the features such as.Titanium
And titanium alloy has the characteristics that density is low, specific strength is high, corrosion resistance is strong, it is especially non-to the immunocompetence of naval air environment erosion
It is often outstanding, it is a kind of good lightweight structural material, referred to as " marine metal ", is important strategy metal material.Wherein
Ti80 (Ti-6Al-3Nb-2Zr-1Mo) alloy is the novel nearly alpha titanium alloy of one kind of China's independent research, is had high-strength, high
The excellent comprehensive performance such as tough, anti-corrosion, is currently used primarily in the pressure hull on bathyscaph and naval vessel.However, current ocean engineering
Using intensity, corrosion resistance to high strength anti-corrosion titanium alloy etc., more stringent requirements are proposed, so needing to carry out alloying component excellent
Change, develop a kind of novel high-strength corrosion resistant Ti alloy, promotes its intensity and corrosion resisting property further to cope with deepwater field exploitation
The harsher ocean engineering of equal service conditions.
CN102965541A discloses a kind of Ti80 titanium alloy standard substance and preparation method thereof, belongs to analysis test neck
Domain is not related to the mechanical property and corrosion resisting property of specific composition alloy.CN108251695A discloses a kind of titanium aluminium
The preparation method of niobium zirconium molybdenum alloy, mainly uses PM technique to prepare alloy, does not characterize the corrosion resisting property of alloy.
Summary of the invention
The purpose of the present invention is to solve intensity, the corrosion resistances of existing high strength anti-corrosion titanium alloy to be unable to further satisfaction
The problem of ocean engineering service condition, provides a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy and preparation method thereof, passes through
The performance for characterizing the Ti-Al-Nb-Zr-Mo titanium alloy of heterogeneity, it is high-strength to obtain the optimal Ti-Al-Nb-Zr-Mo of comprehensive performance
Corrosion resistant Ti alloy.
To achieve the above object, the technical solution adopted by the present invention is as follows:
A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy, the titanium alloy is by mass percentage by following raw material groups
At:4.5~6.7% Al, 0.5~4.5% Nb, 1.0~4.0% Zr, 0.5~2.0% Mo, surplus Ti.
A kind of preparation method of above-mentioned Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy, the method includes following steps
Suddenly:
Step 1: purity is selected to be above 99% Ti, Al, Nb, Zr, Mo as raw material, above-mentioned raw materials surface is polished
Then scale removal cleans 5min, ultrasonic power 0.3W/cm using industrial alcohol ultrasonic oscillation2;
Step 2: the raw material after cleaning step 1 is placed on water jacketed copper crucible using vacuum non-consumable arc furnace melting
In, furnace body vacuum degree is evacuated to 5Pa hereinafter, being then turned on automatic vacuum using mechanical pump, vacuum degree is evacuated to 5 × 10-3Pa with
Under, automatic vacuum is closed, being subsequently charged with air pressure in the argon gas to furnace body as protective atmosphere is 0.05MPa, and it is non-certainly to open vacuum
Consume electric arc furnaces power supply, by tungsten electrode drop to from material 1~2mm place, starting striking, slowly by melting current boost to 450A~
Electric current is kept after between 500A, after raw material is completely melt as liquid, is continued 2~3min of melting, electric current is then shut off, to alloy
After natural cooling 10s, overturn;
Step 3: the alloy after overturning is reentered into melting in water jacketed copper crucible, after alloy is completely melt as liquid,
Maintenance 2~3min of melting, is then shut off electric current, after alloy natural cooling 10s, is overturn;
Step 4: repeating step 35 times, the Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy button ingot of as cast condition is obtained;
Step 5: the resulting alloy button ingot of step 4 is placed in high temperature high vacuum atmosphere tube type furnace, 900 DEG C of heat preservations
The preparation of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy is completed in 2h, furnace cooling.
The beneficial effect of the present invention compared with the existing technology is:The present invention by design orthogonal experiment, explore it is a variety of not
The tissue and performance of congruent Ti-Al-Nb-Zr-Mo alloy, specific and comprehensive, the Ti-5.5Al-3.0Nb-3.0Zr- of optimization
1.5Mo alloy has both excellent Room-Temperature Fracture Toughness, and higher room temperature compressive strength and good etch resistant properties, the alloy have
It hopes and is applied to marine engineering equipment, have a good application prospect.Alloy of the present invention is that conventional titanium alloy vacuum is non-
Consumable smelting obtains, and preparation method is simple.
Detailed description of the invention
Fig. 1 is the micro-organization chart of as cast condition A-1 alloy;
Fig. 2 is the micro-organization chart of heat treatment state A-1 alloy;
Fig. 3 is the micro-organization chart of as cast condition A-2 alloy;
Fig. 4 is the micro-organization chart of heat treatment state A-2 alloy;
Fig. 5 is the micro-organization chart of as cast condition A-3 alloy;
Fig. 6 is the micro-organization chart of heat treatment state A-3 alloy;
Fig. 7 is the micro-organization chart of as cast condition A-4 alloy;
Fig. 8 is the micro-organization chart of heat treatment state A-4 alloy;
Fig. 9 is the micro-organization chart of as cast condition A-5 alloy;
Figure 10 is the micro-organization chart of heat treatment state A-5 alloy;
Figure 11 is the micro-organization chart of as cast condition A-6 alloy;
Figure 12 is the micro-organization chart of heat treatment state A-6 alloy;
Figure 13 is the micro-organization chart of as cast condition A-7 alloy;
Figure 14 is the micro-organization chart of heat treatment state A-7 alloy;
Figure 15 is the micro-organization chart of as cast condition A-8 alloy;
Figure 16 is the micro-organization chart of heat treatment state A-8 alloy;
Figure 17 is the micro-organization chart of as cast condition A-9 alloy;
Figure 18 is the micro-organization chart of heat treatment state A-9 alloy;
Figure 19 is the micro-organization chart of as cast condition A-10 alloy;
Figure 20 is the micro-organization chart of heat treatment state A-10 alloy;
Figure 21 is the micro-organization chart of as cast condition A-11 alloy;
Figure 22 is the micro-organization chart of heat treatment state A-11 alloy;
Figure 23 is the micro-organization chart of as cast condition A-12 alloy;
Figure 24 is the micro-organization chart of heat treatment state A-12 alloy;
Figure 25 is the micro-organization chart of as cast condition A-13 alloy;
Figure 26 is the micro-organization chart of heat treatment state A-13 alloy;
Figure 27 is the micro-organization chart of as cast condition A-14 alloy;
Figure 28 is the micro-organization chart of heat treatment state A-14 alloy;
Figure 29 is the micro-organization chart of as cast condition A-15 alloy;
Figure 30 is the micro-organization chart of heat treatment state A-15 alloy;
Figure 31 is the micro-organization chart of as cast condition A-16 alloy;
Figure 32 is the micro-organization chart of heat treatment state A-16 alloy;
Figure 33 is the micro-organization chart of as cast condition Ti80 alloy;
Figure 34 is the micro-organization chart of heat treatment state Ti80 alloy;
Figure 35 is the XRD diffracting spectrum of A-1 alloy;
Figure 36 is the XRD diffracting spectrum of A-2 alloy;
Figure 37 is the XRD diffracting spectrum of A-3 alloy;
Figure 38 is the XRD diffracting spectrum of A-4 alloy;
Figure 39 is the XRD diffracting spectrum of A-5 alloy;
Figure 40 is the XRD diffracting spectrum of A-6 alloy;
Figure 41 is the XRD diffracting spectrum of A-7 alloy;
Figure 42 is the XRD diffracting spectrum of A-8 alloy;
Figure 43 is the XRD diffracting spectrum of A-9 alloy;
Figure 44 is the XRD diffracting spectrum of A-10 alloy;
Figure 45 is the XRD diffracting spectrum of A-11 alloy;
Figure 46 is the XRD diffracting spectrum of A-12 alloy;
Figure 47 is the XRD diffracting spectrum of A-13 alloy;
Figure 48 is the XRD diffracting spectrum of A-14 alloy;
Figure 49 is the XRD diffracting spectrum of A-15 alloy;
Figure 50 is the XRD diffracting spectrum of A-16 alloy;
Figure 51 is test room temperature fracture toughness specimen figure;
Figure 52 is three-point bending stress diagram, wherein PQIt is sample thickness for breaking load N, B, L is three-point bending mould
Has span, W is specimen width, and a is precrack notch depth, L0For specimen length;
Figure 53 is A-1~A-4 component alloy three point bending test load-displacement curves figure;
Figure 54 is A-5~A-8 component alloy three point bending test load-displacement curves figure;
Figure 55 is A-9~A-12 component alloy three point bending test load-displacement curves figure;
Figure 56 is A-13~A-16 and Ti80 component alloy three point bending test load-displacement curves figure;
Figure 57 is each component Alloy At Room Temperature fracture toughness KICIt is worth schematic diagram;
Figure 58 is that each component alloy is heat-treated front and back compression yield strength value comparison line chart;
Figure 59 is that each component alloy is heat-treated front and back compression limit dependent variable comparison line chart;
Figure 60 is Tafel linear extrapolation method schematic diagram;
Figure 61 is A-1~A-6 component alloy Tafel curve comparison figure;
Figure 62 is A-7~A-12 component alloy Tafel curve comparison figure;
Figure 63 is A-13~A-16+Ti80 component alloy Tafel curve comparison figure.
Specific embodiment
Further description of the technical solution of the present invention with reference to the accompanying drawings and examples, and however, it is not limited to this,
It is all that modifying or equivalently replacing the technical solution of the present invention, without departing from the spirit and scope of the technical solution of the present invention,
It should all cover within the protection scope of the present invention.
Specific embodiment one:What present embodiment was recorded is a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy, institute
The titanium alloy stated is made of following raw materials by mass percentage:4.5~6.7% Al, 0.5~4.5% Nb, 1.0~4.0%
Zr, 0.5~2.0% Mo, surplus Ti, calculated by orthogonal experiment and determining be optimized to be divided into Ti-5.5Al-3.0Nb-
3.0Zr-1.5Mo。
Specific embodiment two:A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy described in specific embodiment one,
The titanium alloy is made of following raw materials by mass percentage:4.5% Al, 0.5% Nb, 1.0% Zr, 0.5%
Mo, surplus Ti.
Specific embodiment three:A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy described in specific embodiment one,
The titanium alloy is made of following raw materials by mass percentage:4.5% Al, 1.5% Nb, 2.0% Zr, 1.0%
Mo, surplus Ti.
Specific embodiment four:A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy described in specific embodiment one,
The titanium alloy is made of following raw materials by mass percentage:4.5% Al, 3.0% Nb, 3.0% Zr, 1.5%
Mo, surplus Ti.
Specific embodiment five:A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy described in specific embodiment one,
The titanium alloy is made of following raw materials by mass percentage:4.5% Al, 4.5% Nb, 4.0% Zr, 2.0%
Mo, surplus Ti.
Specific embodiment six:A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy described in specific embodiment one,
The titanium alloy is made of following raw materials by mass percentage:5.3% Al, 0.5% Nb, 2.0% Zr, 2.0%
Mo, surplus Ti.
Specific embodiment seven:A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy described in specific embodiment one,
The titanium alloy is made of following raw materials by mass percentage:5.3% Al, 1.5% Nb, 3.0% Zr, 0.5%
Mo, surplus Ti.
Specific embodiment eight:A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy described in specific embodiment one,
The titanium alloy is made of following raw materials by mass percentage:5.3% Al, 3.0% Nb, 4.0% Zr, 1.0%
Mo, surplus Ti.
Specific embodiment nine:A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy described in specific embodiment one,
The titanium alloy is made of following raw materials by mass percentage:5.3% Al, 4.5% Nb, 1.0% Zr, 1.5%
Mo, surplus Ti.
Specific embodiment ten:A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy described in specific embodiment one,
The titanium alloy is made of following raw materials by mass percentage:6.0% Al, 0.5% Nb, 3.0% Zr, 1.5%
Mo, surplus Ti.
Specific embodiment 11:A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium conjunction described in specific embodiment one
Gold, the titanium alloy are made of following raw materials by mass percentage:6.0% Al, 1.5% Nb, 4.0% Zr, 1.0%
Mo, surplus Ti.
Specific embodiment 12:A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium conjunction described in specific embodiment one
Gold, the titanium alloy are made of following raw materials by mass percentage:6.0% Al, 3.0% Nb, 1.0% Zr, 0.5%
Mo, surplus Ti.
Specific embodiment 13:A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium conjunction described in specific embodiment one
Gold, the titanium alloy are made of following raw materials by mass percentage:6.0% Al, 4.5% Nb, 2.0% Zr, 2.0%
Mo, surplus Ti.
Specific embodiment 14:A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium conjunction described in specific embodiment one
Gold, the titanium alloy are made of following raw materials by mass percentage:6.7% Al, 0.5% Nb, 4.0% Zr, 1.0%
Mo, surplus Ti.
Specific embodiment 15:A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium conjunction described in specific embodiment one
Gold, the titanium alloy are made of following raw materials by mass percentage:6.7% Al, 1.5% Nb, 1.0% Zr, 1.5%
Mo, surplus Ti.
Specific embodiment 16:A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium conjunction described in specific embodiment one
Gold, the titanium alloy are made of following raw materials by mass percentage:6.7% Al, 3.0% Nb, 2.0% Zr, 2.0%
Mo, surplus Ti.
Specific embodiment 17:A kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium conjunction described in specific embodiment one
Gold, the titanium alloy are made of following raw materials by mass percentage:6.7% Al, 4.5% Nb, 3.0% Zr, 0.5%
Mo, surplus Ti.
Specific embodiment 18:Ti-Al- described in a kind of any specific embodiment of specific embodiment one to 17
The preparation method of Nb-Zr-Mo high strength anti-corrosion titanium alloy, the described method comprises the following steps:
Step 1: purity is selected to be above 99% Ti, Al, Nb, Zr, Mo as raw material, above-mentioned raw materials surface is polished
Then scale removal cleans 5min, ultrasonic power 0.3W/cm using industrial alcohol ultrasonic oscillation2;
Step 2: using vacuum non-consumable arc furnace, (model JVAM -1B type, producer are that Shenyang gold grinds new material preparation
Technology Co., Ltd.) melting, the raw material after step 1 is cleaned is placed in water jacketed copper crucible, using mechanical pump by furnace body vacuum
Degree is evacuated to 5Pa hereinafter, being then turned on automatic vacuum, and vacuum degree is evacuated to 5 × 10-3Pa is subsequently charged with hereinafter, closing automatic vacuum
It is 0.05MPa as air pressure in the argon gas to furnace body of protective atmosphere, opens the power supply of vacuum non-consumable arc furnace, tungsten electrode is declined
To at from 1~2mm of material, start striking, melting current boost is slowly kept into electric current to after between 450A~500A, it is complete in raw material
After fine melt turns to liquid, continues 2~3min of melting, be then shut off electric current, after alloy natural cooling 10s, overturn;
Step 3: the alloy after overturning is reentered into melting in water jacketed copper crucible, after alloy is completely melt as liquid,
Maintenance 2~3min of melting, is then shut off electric current, after alloy natural cooling 10s, is overturn;
Step 4: repeating step 35 times, the Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy button ingot of as cast condition is obtained;
Step 5: the resulting alloy button ingot of step 4 is placed in high temperature high vacuum atmosphere tube type furnace, (producer Shanghai is entirely large
Electric furnace Co., Ltd;Model:QSH-VTF-1700T in), 900 DEG C of heat preservation 2h, furnace cooling, i.e. completion Ti-Al-Nb-Zr-Mo
The preparation of high strength anti-corrosion titanium alloy.
Specific embodiment 19:Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy described in specific embodiment 18
Preparation method, in step 2 and step 3, the electric current of the melting is 450~500A.
Embodiment 1:
Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy provided in this embodiment, specific preparation process is as follows:
(1) preparation of raw material
It selects purity to be above 99% Ti, Al, Nb, Zr, Mo as raw material, above-mentioned raw materials surface is polished and removes oxidation
Then skin cleans 5min, ultrasonic power 0.3W/cm using industrial alcohol ultrasonic oscillation2, then press each element mass fraction
Accurate weighing, for alloy melting use.Alloying component is shown in Table 2.
Each element ingredient section is determined according to the relevant designs criterion such as Al equivalent, Mo equivalent in Titanium Alloy Design, in this area
Interior interval water intaking level values, 16 groups of horizontal orthogonal experiment groups of four factor of composition four.The ingredient orthogonal design table of 16 groups of designs and
Element level factor is as shown in table 1.
Each factor level table of 1 orthogonal test of table (wt.%)
According to the principle of orthogonal test, the horizontal orthogonal components table of four factor four is as shown in table 2.
2 orthogonal experiment each component alloying component table of table
(2) melting of alloy
Using vacuum non-consumable arc furnace, the raw material after cleaning is placed in water jacketed copper crucible, and by one piece of pure titanium ingot
It is placed in one of crucible, furnace body vacuum degree is evacuated to 5Pa hereinafter, being then turned on automatic vacuum, by vacuum using mechanical pump
Degree is evacuated to 5 × 10-3Pa is hereinafter, close automatic vacuum.It is close to be then charged with air pressure in the argon gas to furnace body as protective atmosphere
0.05MPa or so to prevent metal charge to be oxidized, while also guaranteeing to discharge in fusion process.The pure titanium ingot of melting first
Tungsten electrode is then adjusted to start striking from raw material 1-2mm or so by 1min to eliminate oxygen remaining in furnace chamber, slowly by melting electricity
Stream keeps electric current after being promoted between 450A~500A, after raw material is completely melt as liquid, continues 2~3min of melting, then
Electric current is closed, is overturn after alloy is cooling;It is above repeatedly to operate 5 times to obtain the uniform alloy of ingredient.
(2) heat treatment of alloy
The intensity of cast titanium alloy is higher and corrosion resisting property is good, therefore is widely used in aerospace and navigation chemical industry
Etc. industries, but the problems such as cast titanium alloy usually there will be casting stress and nonuniform organization in casting process.It solves
These problems, usual cast titanium alloy before application can by annealing with eliminate the casting stress generated in casting process with
And make tissue stabilization to obtain uniform performance.
Heat treatment mode used by this patent is:Resulting alloy button ingot is placed in high temperature high vacuum atmosphere tube type
In furnace, 900 DEG C of heat preservation 2h, furnace cooling.
The alloy obtained to the present embodiment is analyzed as follows:
(1) microscopic structure and XRD analysis of Ti-Al-Nb-Zr-Mo system alloy
Position intercepts 6 × 6 × 3mm among the button ingot of as cast condition and heat treatment state3Sheet specimens, inlayed through tooth shedding
240#, 600#, 800#, 1000#, 1200#, 1500#, 2000# liquid honing are used after embedding, then use Cr2O3Solution is polished to light
It learns under microscope without scratches visible, by the sample after polishing in HF:HNO3:H2O=1:2:50 corrosive liquid (Kroll ' s reagent)
It is rinsed with water after middle placement 5s or so.Then the sample after corrosion is placed in the beaker for filling dehydrated alcohol, corrosion is face-up
It is placed in ultrasonic cleaning instrument, the alcohol of electricity consumption blowing drying tested surface, completes sample preparation after ultrasonic vibration 5min.It is scanned in Flied emission
Electric microscopic observation as cast condition is distributed with the tissue topography of heat treatment state each component alloy and mutually.
For the phase composition in determining microscopic structure, XRD material phase analysis is made to heat treatment state each component alloy, heat treatment state
Uniformly position passes through 6 × 6 × 3mm of wire cutting interception among button ingot3Thin slice, be placed in after gradually being polished and polished with sand paper
On Empyrean smart X-ray diffractometer objective table, voltage is set as 40KV, electric current 40mA, scanning angle is 20~100 °,
Scanning speed is 10 °/min.Diffracting spectrum is obtained by X-ray diffraction, PDF card is compareed to appearing in figure according to diffracting spectrum
Diffraction maximum in spectrum is demarcated the type to determine compound phase in alloy structure, and according to each corresponding diffraction maximum quantity
And intensity determines the relative amount of each phase.
Fig. 1~34 are respectively A-1~A-16 and Ti80 alloy casting state and heat treatment state tissue SEM image, for convenience of right
Than summarizing as shown in table 3.
The as cast condition and heat treatment state tissue of each orthogonal experiment component alloy of table 3 and Ti80 alloy composition
It can be seen that each component As-cast Microstructure is mainly in mesh basket shape from micro-organization chart, α phase mainly with it is needle-shaped with
The form of sheet exists.The present invention relates to Ti-Al-Nb-Zr-Mo system alloy in, main is mutually α phase, is only existed few
Measure β phase.For the XRD diffracting spectrum of alloy as shown in Figure 35~50, the phase composition detected is main phase α phase+a small amount of β phase, is had
The alloy of a little ingredients coincide even without the presence for detecting β phase with the phase observed in micro-organization chart substantially.It can from figure
Substantially to see that the promotion alloy structure with aluminium content has refinement trend, this is because Al element can be by promoting α phase nucleation rate
Refine alloy structure, the influence of Nb and Zr to tissue is unobvious, and A-4 (Ti-4.5Al- is organized in each component alloy
4.5Nb-4.0Zr-2.0Mo)、A-5(Ti-5.3Al-0.5Nb-2.0Zr-2.0Mo)、A-14(Ti-6.7Al-1.5Nb-1.0Zr-
1.5Mo), the as-cast structure of A-15 (Ti-6.7Al-3.0Nb-2.0Zr-2.0Mo) is the finest and closely woven, the common ground of this several groups of alloys
It is that Mo constituent content is higher, crystal grain can be refined, while promoting the generation of β phase, refines tissue more.Each group division after heat treatment
Nascent irregular phase in gold completely disappears, and acicular structure evolves into lamellar structure, and tissue is whole to become uniformly coarse, or even meeting
There is a small amount of streaky structure.
(2) Room-Temperature Fracture Toughness of Ti-Al-Nb-Zr-Mo system alloy
Unilateral Notched Izod beam method will be taken to test each component alloy to obtain the fracture toughness of each component alloy.
Sample is that the method that relatively uniform position uses wire cutting among the button ingot after Overheating Treatment intercepts 2 × 4 × 20mm3's
Cuboid sample, and in intermediate prefabricated 2mm deep torn grain, surface is polishing to without obvious wire cutting scratch, as shown in figure 51.Test is set
Standby is Instron5569 electronic universal tester.Installed on electronic universal tester place after three-point bending fixture sample in
Centre makes above pressure head face crackle, then controls pressure head and slowly pushes, loading speed 0.2mm/min, until breaking (load
Sharply decline) stop.Three-point bending stress diagram is as shown in figure 50.
The test data that breaking load is in median in test three times is taken to draw each component displacement-load curves.Such as figure
Shown in 53~56.The room temperature fracture that material can be calculated in maximum load substitution formula (1) and (2) during this is tough
Property KICValue.
The fracture toughness K of sampleICValue is calculated by formula (1) and (2):
Wherein,It is for independent variableFunction, value can calculate with following formula:
In formula, PQFor breaking load N;B is sample thickness, 2mm;L is three-point bending mold span, 16mm;W is that sample is wide
Degree, 4mm;A is precrack notch depth, 2mm.
By every group of alloy K that experiment calculation obtains three timesICValue is averaged, and is determined as the K of the component alloyICValue, table 3 are
For each component alloy and the Fracture Toughness of Ti80 alloy.
The fracture toughness of 4 each component alloy of table
As can be seen from Table 4, the average Fracture Toughness of each component alloy is in 48MPam1/2More than, illustrate each component
Alloy fracture toughness is all better.On the other hand, it can be seen that the average Fracture Toughness of each component alloy is distributed in 48.93
~60.95MPam1/2Between, very poor is 12.02MPam1/2, this illustrates in Ti-Al-Nb-Zr-Mo system alloy, Al, Nb,
The content of tetra- kinds of main alloying elements of Zr, Mo has a certain impact to the Room-Temperature Fracture Toughness of material.In 16 groups of alloys of experiment,
The best component of toughness is A-10 alloy (Ti-6.0Al-1.5Nb-4.0Zr-1.0Mo), KICValue is 60.95MPam1/2;Toughness
That worst is A-1 alloy (Ti-4.5Al-0.5Nb-1.0Zr-0.5Mo), KICValue is 48.93MPam1/2.For more intuitive table
Above data is shown as Figure 57 with bar chart by the toughness value gap of bright each component alloy.
From Figure 57 it can be seen that each component Alloy At Room Temperature Fracture Toughness is not much different, wherein showing relatively good has A-
4 alloys (Ti-4.5Al-4.5Nb-4.0Zr-2.0Mo), A-9 alloy (Ti-6.0Al-0.5Nb-3.0Zr-1.5Mo), A-10 are closed
Golden (Ti-6.0Al-1.5Nb-4.0Zr-1.0Mo) and A-16 alloy (Ti-6.7Al-4.5Nb-3.0Zr-0.5Mo).Performance is opposite
Poor has A-1 alloy (Ti-4.5Al-0.5Nb-1.0Zr-0.5Mo), A-2 alloy (Ti-4.5Al-1.5Nb-2.0Zr-
1.0Mo), A-6 (Ti-5.3Al-1.5Nb-3.0Zr-0.5Mo) and A-11 alloy (Ti-6.0Al-3.0Nb-1.0Zr-0.5Mo).
It is analyzed in conjunction with above-mentioned alloy fracture toughness value with its ingredient, is seen between Al and the constituent content and alloy fracture toughness value of Zr
Do not go out direct relation, but more it is evident that higher (the A-4 of content of the preferable alloy Mo element of fracture toughness or Nb element:
4.5Nb-2.0Mo,A-10:1.5Nb-1.0Mo), Fracture Toughness lower alloy Nb and the then relatively fewer (A-1 of Mo content:
0.5Nb-0.5Mo,A-2:1.5Nb-1.0Mo,A-6:1.5Nb-0.5Mo).It can be considered that compared to main alloying element Al and
Zr, Nb and Mo are larger to the fracture toughness contribution of Ti-Al-Nb-Zr-Mo system alloy.Nb with Mo element can promote β phase to generate,
And β crystal boundary energy effectively hinders the extension of crackle to make alloy fracture toughness get a promotion.In addition Nb and Mo content is lesser
The fracture toughness performance of A-16 alloy preferably may be related with its lamellar structure, and correlative study shows that titanium alloy lamella is bigger, increases
Tough effect is more obvious.
(3) the room temperature compression performance of Ti-Al-Nb-Zr-Mo system alloy
It compares to progress room temperature compression test after the button ingot sample preparation after vacuum annealing and with as-cast specimen, is heat-treated
The room temperature compression performance of state sample and as-cast specimen is shown in Table 5.
5 each component alloy of table heat treatment front and back compression yield strength and the limit prolong dependent variable
In order to more intuitively show the variation of heat treatment front and back each component alloy compression performance, the data in upper table are rolled over
Line chart is indicated, as shown in Figure 58,59.From in line chart as can be seen that each component alloy after carrying out vacuum annealing process
Compression yield strength has different degrees of decline, and compression limit dependent variable then has different degrees of promotion.From each component
The tissue contrast of alloy heat treatment front and back schemes (Fig. 1~32) it can be seen that each component alloy is after vacuum annealing process, α phase
It is sufficiently grown, tissue becomes thick and uniform, and tissue can be such that alloy strength declines after becoming thick, and organizes to become equal
The plasticity of alloy can be made to improve after even, so each component alloy strength is lower and plasticity improves after vacuum annealing.
(4) electrochemical corrosion performance of Ti-Al-Nb-Zr-Mo system alloy
Using dynamic method to each component alloy carry out three-electrode system electrochemical test, the system mainly by working electrode,
Reference electrode and auxiliary electrode composition, wherein each component alloy is saturated sweet as working electrode, platinum black electrode as auxiliary electrode
Mercury electrode is as reference electrode.Corrosion test is carried out using potentiostatic scanning method in electrochemical workstation, sample is sanding and polishing
Φ 8 × 2mm disk to optical microscopy lower surface without scratches visible, corrosive liquid are the 1mol/L hydrochloric acid containing 3.0wt.%NaCl
Solution, corrosive liquid volume are about 250mL.First time of repose is set as 300s before scanning, and test sweep speed is 0.01V/s, surveys
Amount current potential is -2.0~+2.0V.
The polarization curve measured can acquire each corrosive nature parameter, as shown in figure 60, root by Tafel linear extrapolation method
According to the slope b of the straightway of polarization curveAAnd bC, the corresponding electric current of the intersection point postponed outside is icorr, characterization corrosion speed
Rate, icorrIt is slower to be worth smaller expression corrosion, it is more big, indicate that corrosion is faster, the corresponding ordinate of intersection point is corrosion potential Ecorr,
The complexity that characterization corrosion occurs, EcorrThe bigger expression corrosion of value is more difficult to occur, smaller, indicates that corrosion is more easy to happen.One
As use icorrValue indicates corrosion rate.
Using Tafel curve such as Figure 61~63 institute of dynamic linear scanning voltammetric method measurement heat treatment state each component alloy
Show, each component alloy corrosion current potential E obtained by Tafel linear extrapolation methodcorrValue and corrosion current value IcorrIt is shown in Table 6.
6 each component alloy corrosion current potential E of tablecorrWith corrosion current Icorr
Alloy serial number | Alloying component | Ecorr/V | Icorr/×10-7A |
A-1 | Ti-4.5Al-0.5Nb-1.0Zr-0.5Mo | -0.455 | 31.63 |
A-2 | Ti-4.5Al-1.5Nb-2.0Zr-1.0Mo | -0.403 | 16.05 |
A-3 | Ti-4.5Al-3.0Nb-3.0Zr-1.5Mo | -0.140 | 3.00 |
A-4 | Ti-4.5Al-4.5Nb-4.0Zr-2.0Mo | -0.488 | 82.65 |
A-5 | Ti-5.3Al-0.5Nb-2.0Zr-2.0Mo | -0.420 | 32.32 |
A-6 | Ti-5.3Al-1.5Nb-3.0Zr-0.5Mo | -0.584 | 1.94 |
A-7 | Ti-5.3Al-3.0Nb-4.0Zr-1.0Mo | -0.652 | 1.22 |
A-8 | Ti-5.3Al-4.5Nb-1.0Zr-1.5Mo | -0.406 | 25.35 |
A-9 | Ti-6.0Al-0.5Nb-3.0Zr-1.5Mo | -0.428 | 9.92 |
A-10 | Ti-6.0Al-1.5Nb-4.0Zr-1.0Mo | -0.400 | 1.80 |
A-11 | Ti-6.0Al-3.0Nb-1.0Zr-0.5Mo | -0.396 | 0.26 |
A-12 | Ti-6.0Al-4.5Nb-2.0Zr-2.0Mo | -0.465 | 44.11 |
A-13 | Ti-6.7Al-0.5Nb-4.0Zr-1.0Mo | -0.477 | 7.48 |
A-14 | Ti-6.7Al-1.5Nb-1.0Zr-1.5Mo | -0.460 | 7.53 |
A-15 | Ti-6.7Al-3.0Nb-2.0Zr-2.0Mo | -0.486 | 9.48 |
A-16 | Ti-6.7Al-4.5Nb-3.0Zr-0.5Mo | -0.501 | 4.13 |
Ti80 | Ti-6.0Al-3.0Nb-2.0Zr-1.0Mo | -0.493 | 8.25 |
Rise with aluminium content, downward trend is integrally presented in each component alloy corrosion electric current, illustrates Al element to promotion Ti-
The electrochemical corrosion performance of Al-Nb-Zr-Mo system alloy is advantageous.This is because although Al is unfavorable for titanium alloy passivation, but Al2O3Energy
Stablize TiO2Passivating film promotes the corrosive nature of titanium alloy.The corrosion current Icorr value of most of component alloy concentrates on 10
×10-7A is hereinafter, only a small amount of alloy (such as A-1:Ti-4.5Al-0.5Nb-1.0Zr-0.5Mo,A-4:Ti-4.5Al-4.5Nb-
4.0Zr-2.0Mo,A-5:Ti-5.3Al-0.5Nb-2.0Zr-2.0Mo,A-12:Ti-6.0Al-4.5Nb-2.0Zr-2.0Mo etc.)
Corrosion current value be significantly higher than other components alloy.The Mo of these alloy component analysis discovery A-4, A-5, A-12 alloy is contained
Amount is in highest level value.This is because Mo element can promote the generation of β phase as beta stable element, and Mo element is in α
Content in phase is less than the content in β phase, this meeting has significant alternate potential difference so that α phase is alternate with β, then containing Mo member
The low α phase surface passivating film of element can be more easily rupturable, makes α phase that the preferential dissolution of selectivity occur, to show poor corrosion resistance
Energy.A-1 alloy (Ti-4.5Al-0.5Nb-1.0Zr-0.5Mo) also shows poor electrochemical corrosion performance, this is because
Nb, Zr, Mo can promote the passivation ability of titanium alloy, and Nb can also form Nb by oxidation2O5, play stable titanium alloy surface film
Effect.And these types of constituent content is in floor level in A-1 alloy, therefore corrosion resisting property is poor.
(5) orthogonal calculation of Ti-Al-Nb-Zr-Mo system alloy
Comprehensive scoring method or synthesis necessary technology are generally used for the data processing of multi-index orthogonal test.Here, using
Synthesis necessary technology handles orthogonal experiment data, and each index is first carried out range analysis by single index respectively, obtains each
Then the optimal ingredient of performance indicator and each factor analyze each performance Index Calculation the influence degree of the performance indicator
As a result overall balance is carried out, so that it is determined that each factor level optimal or transferring to combine.
As shown in table 7 to each component Alloy At Room Temperature fracture toughness range analysis process, calculated result is shown for single finger
The mark optimal alloy compositions of Room-Temperature Fracture Toughness are Ti-6.0Al-4.5Nb-4.0Zr-2.0Mo.Very poor calculated result shows, respectively
Main alloying element is ordered as the influence degree of material Room-Temperature Fracture Toughness:Zr>Nb>Al>Mo.
The orthogonal range analysis of 7 each component Alloy At Room Temperature fracture toughness of table
It is as shown in table 8 to the test result range analysis process of each component Alloy At Room Temperature compressive strength and limiting strain amount,
Calculated result shows that the optimal alloy group to single index compression yield strength is divided into Ti-6.7Al-4.5Nb-4.0Zr-1.0Mo,
Ti-5.3Al-3.0Nb-3.0Zr-1.5Mo is divided into the optimal alloy group of single index compression limit dependent variable.By very poor size
Sequence is it is found that each main alloying element is ordered as the influence degree of usable material chamber temperature compressive strength:Al>Zr>Mo>Nb, to usable material chamber
The influence degree of temperature and pressure contracting limiting strain amount is ordered as:Al>Zr>Nb>Mo.
The orthogonal range analysis of 8 heat treatment state each component alloy compression performance of table
It is as shown in table 9 to the orthogonal range analysis of each component alloy electrochemical corrosion performance.Due to corrosion current value Icorr
Smaller expression material corrosion is slower, and corrosion resistance is better, therefore smaller certain element of expression of Ki (i=1,2,3 or 4) value is in the water
Corrosion resisting property under flat is better, which is the preferred levels of element thus.And corrosion potential is then that more just, corrosion resistance is got over
It is good.As can be seen from the table, Ti-6.7Al-3.0Nb-3.0Zr- is divided into the optimal alloy group of single index corrosion current
1.0Mo.According to very poor size, each main alloying element is ordered as the influence degree of electrochemical current:Nb>Mo > Al >
Zr.To corrosion potential EcorrFor optimal alloy group be divided into Ti-4.5Al-3.0Nb-3.0Zr-1.5Mo.Each main alloying element
The influence degree of electrochemical corrosion potential is ordered as:Al>Mo > Zr > Nb.
The orthogonal range analysis of 9 heat treatment state each component alloy electrochemical corrosion performance of table
Overall balance is carried out to the calculated result of above-mentioned each performance indicator, the alloy pressure when Al content is 6.0% and 5.3%
Contracting performance, fracture toughness and electrochemical corrosion performance are preferable, and compromise takes 5.5%;When Nb content is 3.0%, compression limit is answered
Variable and electrochemical corrosion performance are best, and compressive strength is also preferable with fracture toughness, therefore optimize component Nb constituent content and take
3.0%;Zr content is at 3.0%, while fracture toughness and yield strength keep good, compression limit dependent variable and electrochemistry
Corrosive nature is best, therefore Zr content also selects 3.0%;For Mo content at 1.5%, compression limit dependent variable is best, other each property
Energy index is also preferable.So being optimized to be divided into Ti-5.5Al-3.0Nb-3.0Zr-1.5Mo, marine titanium alloy is generally with nearly α titanium
Based on alloy, it is therefore necessary to consider the problems of Al equivalent and Mo equivalent, and according to China's industry titanium alloy selecting experience, nearly α titanium
The molybdenum equivalent of alloy is usually within 2.5.
According to [Mo]eq(molybdenum equivalent) calculation formula:
[Mo]eq=%Mo+%Ta/4.5+%Nb/3.6+%W/2+%V/1.4+%Cr/0.63+%Ni/0.8+%Mn/
0.65+%Fe/0.35+%Co/0.9.
[Mo] of Ti-5.5Al-3.0Nb-3.0Zr-1.5Moeq=2.333 < 2.5 meet the nearly alpha titanium alloy design in China
When [Mo]eqRequirement.
From the above analysis:Excellent room temperature is had both by the Ti-Al-Nb-Zr-Mo alloy of orthogonal experiment optimization design
Fracture toughness, higher room temperature compressive strength, compression limit dependent variable and good etch resistant properties are expected to using Yu Haiyang work
Journey equipment, has a good application prospect.
Claims (19)
1. a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy, it is characterised in that:The titanium alloy by mass percentage by
Following raw material compositions:4.5~6.7% Al, 0.5~4.5% Nb, 1.0~4.0% Zr, 0.5~2.0% Mo, surplus
For Ti.
2. a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy according to claim 1, it is characterised in that:The titanium
Alloy is made of following raw materials by mass percentage:4.5% Al, 0.5% Nb, 1.0% Zr, 0.5% Mo, surplus are
Ti。
3. a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy according to claim 1, it is characterised in that:The titanium
Alloy is made of following raw materials by mass percentage:4.5% Al, 1.5% Nb, 2.0% Zr, 1.0% Mo, surplus are
Ti。
4. a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy according to claim 1, it is characterised in that:The titanium
Alloy is made of following raw materials by mass percentage:4.5% Al, 3.0% Nb, 3.0% Zr, 1.5% Mo, surplus are
Ti。
5. a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy according to claim 1, it is characterised in that:The titanium
Alloy is made of following raw materials by mass percentage:4.5% Al, 4.5% Nb, 4.0% Zr, 2.0% Mo, surplus are
Ti。
6. a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy according to claim 1, it is characterised in that:The titanium
Alloy is made of following raw materials by mass percentage:5.3% Al, 0.5% Nb, 2.0% Zr, 2.0% Mo, surplus are
Ti。
7. a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy according to claim 1, it is characterised in that:The titanium
Alloy is made of following raw materials by mass percentage:5.3% Al, 1.5% Nb, 3.0% Zr, 0.5% Mo, surplus are
Ti。
8. a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy according to claim 1, it is characterised in that:The titanium
Alloy is made of following raw materials by mass percentage:5.3% Al, 3.0% Nb, 4.0% Zr, 1.0% Mo, surplus are
Ti。
9. a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy according to claim 1, it is characterised in that:The titanium
Alloy is made of following raw materials by mass percentage:5.3% Al, 4.5% Nb, 1.0% Zr, 1.5% Mo, surplus are
Ti。
10. a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy according to claim 1, it is characterised in that:Described
Titanium alloy is made of following raw materials by mass percentage:6.0% Al, 0.5% Nb, 3.0% Zr, 1.5% Mo, surplus
For Ti.
11. a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy according to claim 1, it is characterised in that:Described
Titanium alloy is made of following raw materials by mass percentage:6.0% Al, 1.5% Nb, 4.0% Zr, 1.0% Mo, surplus
For Ti.
12. a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy according to claim 1, it is characterised in that:Described
Titanium alloy is made of following raw materials by mass percentage:6.0% Al, 3.0% Nb, 1.0% Zr, 0.5% Mo, surplus
For Ti.
13. a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy according to claim 1, it is characterised in that:Described
Titanium alloy is made of following raw materials by mass percentage:6.0% Al, 4.5% Nb, 2.0% Zr, 2.0% Mo, surplus
For Ti.
14. a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy according to claim 1, it is characterised in that:Described
Titanium alloy is made of following raw materials by mass percentage:6.7% Al, 0.5% Nb, 4.0% Zr, 1.0% Mo, surplus
For Ti.
15. a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy according to claim 1, it is characterised in that:Described
Titanium alloy is made of following raw materials by mass percentage:6.7% Al, 1.5% Nb, 1.0% Zr, 1.5% Mo, surplus
For Ti.
16. a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy according to claim 1, it is characterised in that:Described
Titanium alloy is made of following raw materials by mass percentage:6.7% Al, 3.0% Nb, 2.0% Zr, 2.0% Mo, surplus
For Ti.
17. a kind of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy according to claim 1, it is characterised in that:Described
Titanium alloy is made of following raw materials by mass percentage:6.7% Al, 4.5% Nb, 3.0% Zr, 0.5% Mo, surplus
For Ti.
18. the preparation of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy described in a kind of claim 1~17 any claim
Method, it is characterised in that:It the described method comprises the following steps:
Step 1: purity is selected to be above 99% Ti, Al, Nb, Zr, Mo as raw material, above-mentioned raw materials surface is polished and is removed
Then oxide skin cleans 5min, ultrasonic power 0.3W/cm using industrial alcohol ultrasonic oscillation2;
Step 2: the raw material after cleaning step 1 is placed in water jacketed copper crucible using vacuum non-consumable arc furnace melting, make
Furnace body vacuum degree is evacuated to 5Pa hereinafter, being then turned on automatic vacuum with mechanical pump, vacuum degree is evacuated to 5 × 10-3Pa is hereinafter, close
Automatic vacuum is closed, being subsequently charged with air pressure in the argon gas to furnace body as protective atmosphere is 0.05MPa, opens vacuum non-consumable electric arc
Tungsten electrode is dropped to from 1~2mm of material, starts striking, slowly by melting current boost between 450A~500A by the power supply of furnace
After keep electric current, after raw material is completely melt as liquid, continue 2~3min of melting, electric current is then shut off, to alloy natural cooling
After 10s, overturn;
Step 3: the alloy after overturning is reentered into melting in water jacketed copper crucible, after alloy is completely melt as liquid, keep
Continue 2~3min of melting, is then shut off electric current, after alloy natural cooling 10s, is overturn;
Step 4: repeating step 35 times, the Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy button ingot of as cast condition is obtained;
Step 5: the resulting alloy button ingot of step 4 is placed in high temperature high vacuum atmosphere tube type furnace, 900 DEG C of heat preservation 2h, with
Furnace is cooling, that is, completes the preparation of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy.
19. the preparation method of Ti-Al-Nb-Zr-Mo high strength anti-corrosion titanium alloy according to claim 18, it is characterised in that:
In step 2 and step 3, the electric current of the melting is 450~500A.
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Application publication date: 20181127 |