CN102965541B - Ti80 titanium alloy standard substance and preparation method thereof - Google Patents

Ti80 titanium alloy standard substance and preparation method thereof Download PDF

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CN102965541B
CN102965541B CN201210521268.0A CN201210521268A CN102965541B CN 102965541 B CN102965541 B CN 102965541B CN 201210521268 A CN201210521268 A CN 201210521268A CN 102965541 B CN102965541 B CN 102965541B
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component
weight percent
electrode
titanium alloy
impurity
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CN201210521268.0A
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CN102965541A (en
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赵教育
张亚娟
袁满
巩红涛
张卫国
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中国船舶重工集团公司第十二研究所
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Abstract

The invention provides a Ti80 titanium alloy standard substance. The Ti80 titanium alloy standard substance comprises the following main elements in percentage by weight: 4.3 to 7.2wt% of Al, 1.85 to 4.15wt% of Nb, 0.15 to 2.05wt% of Mo, 0.85 to 3.15wt% of Zr, 0.00 to 0.27wt% of Si, 0.00 to 0.40wt% of Fe, 0.00 to 0.14wt% of C, and the balance of Ti and other impurity elements, wherein the sum of the weight percentages of all components is a hundred percent. The preparation method comprises the following steps in sequence: compounding; pressing to form an electrode by a vertical type horizontal press machine; welding the electrode in a vacuum argon filling box; smelting and casting into ingots at the first time through a vacuum consumable electrode arc furnace; smelting and casting into the ingots at the second time through a vacuum consumable electrode arc skull furnace; smelting and casting into the ingots at the third time through the vacuum consumable electrode arc furnace; uniformly annealing; uniformly deforming and processing; thermally processing; and mechanically processing, thus obtaining the titanium alloy standard substance. The Ti80 titanium alloy standard substance is high in uniformity of the components, and can be used for analyzing the components of the Ti80 titanium alloy to precisely control and ensure the quality of Ti80 titanium alloy products.

Description

Ti80 titanium alloy reference material and preparation method thereof
Technical field
The invention belongs to technical field of analysis and detection, relate to a kind of reference material of Measuring and testing titanium alloy material, be specifically related to a kind of Ti80 titanium alloy reference material, also relate to the preparation method of this reference material.
Background technology
The nominal component of Ti80 titanium alloy is Ti-6Al-3Nb-2Zr-1Mo, that a kind of aluminium content is higher, and the nearly alpha titanium alloy that contains beta stable element Nb, Mo and neutral element Zr, be a kind of titanium alloy trade mark with high-quality performances such as the easy welderings of high strength anti-corrosion that aims at ship design.This alloy has higher specific tenacity, belongs to 786MPa level titanium alloy, has very strong erosion resistance and good welding property, is widely used in primary structure member, bolt, axle and the withstand voltage anti-corrosion housing of boats and ships.
In order to ensure reliability and the stability of titanium alloy product, must carry out component accurately to its material and measure, need corresponding titanium alloy reference material to calibrate analytical procedure, Analytical equipment and analytical results.Titanium alloy analytical procedure is except the chemical analysis method of wet method at present, and advanced person efficiently instrument analytical method has: (1) X-ray fluorescence spectra analytical method; (2) photoelectric direct reading spectrometry method; (3) atomic absorption spectrometry; (4) ICP plasma spectroscopy etc., these analytical procedures all need corresponding reference material for setting up working standard, and instrument is calibrated.
Reference material is to have one or more enough all even fine characteristic values of having determined, for tester, evaluates measuring method or material or material to material assignment.Reference material is as the one of measurement instrument, and it can reappear, and preserves and transmits value, ensures comparability and consistence at different time and space value.The effect of titanium alloy reference material can be summarized as the following aspects: the preci-sion and accuracy of (1) evaluation analysis testing method; (2) for calibration analyte instrument; (3) measure working standard as the analysis of setting up titanium alloy; (4) the analysis quality of control titanium alloy material; (5) for Laboratory Accreditation and laboratory proficiency testing.
The development of Ti80 titanium alloy series standard material mainly contains following two difficult points:
(1) how to control the each elementary composition content of Ti80 titanium alloy reference material, make it cover Ti80 titanium alloy standard ingredient content range, and make each constituent content distribution gradient, to meet the use needs of reference material.Because reference material need to be drawn analytical work curve, the each analytical element content of reference material should be reasonably Gradient distribution, due to the each element chemistry component concentration of Ti80 titanium alloy narrow range, meet 6 content point Gradient distribution, fusion process has larger difficulty to the accurate control of component content.For example the content range of principal element Nb only differs 2.0%, adjacent 2 content points, and wherein the upper limit of lower component and the lower limit of higher composition only differ 0.1%, 6 content and are difficult to distribution gradient.In Ti80 material, need the unit of quantitative analysis to have the elements such as Al, Nb, Zr, Mo, Si, Fe, C, the saturation vapour pressure difference of each element, in fusion process, volatilize asynchronous, wherein the saturation vapour pressure of Al, Fe, Si element is higher than matrix titanium, volatilize more serious, and the minimum content of Si, Fe, C impurity element has often exceeded Si, Fe, C foreign matter content that body material titanium sponge and various master alloy are brought into, and in starting material, impurity composition content distribution is inhomogeneous, be difficult to accurately control its component, and make it meet 6 component gradient distributions.
(2) homogeneity of reference material characteristic value, stability and accuracy are important quality index, thus high to the uniformity requirement of reference material ingot casting, how to solve the segregation problem of ingot casting, to ensure the homogeneity of each element.According to national metallurgic product spectroscopic standard material technology specification relevant regulations: the content range of main ingredient element, outwards suitably extends by the upper and lower limit of product technology condition (especially lower limit).Content, 10% above person, extends 5% ~ 15%; Content is person below 10%, extends 15% ~ 30%.Impurity content scope, should comprise the upper limit of this trade mark or product technology conditional request, and be unlikely to produce under the prerequisite of interelement effect, and maximum can reach the more than 5 times of Schwellenwert.Because reference material component concentration scope is than standard ingredient wide ranges, the high-content of each element has often exceeded the solid solubility of this element in body material, and homogeneity is difficult to ensure.For example, the high-content of Ti80 titanium alloy standard ingredient Al element is 6.5%, and in reference material, the high-content of Al element is 7.0%, and Al constituent content exceedes 6.0% by precipitating metal compound Ti 3al, produce segregation, and in titanium alloy process of setting, α stable element (being mainly Al) is easily in crystal boundary enrichment, and beta stable element Mo, Nb are easily in crystal boundary dilution, and homogeneity is difficult to reach the requirement of reference material.
Because Ti80 titanium alloy series standard material development difficulty is very large, so up to now, all there is no Ti80 titanium alloy series standard material both at home and abroad.Therefore, in the urgent need to developing a kind of Ti80 titanium alloy material proximate analysis reference material, accurately to control and to ensure Ti80 titanium alloy product quality.
Summary of the invention
The object of this invention is to provide a kind of Ti80 titanium alloy reference material, for the proximate analysis of the each element of Ti80 titanium alloy.
Another object of the present invention is to provide the preparation method of above-mentioned reference material.
The object of the present invention is achieved like this, Ti80 titanium alloy reference material, each principal element content range is: Al:4.3wt%~7.2wt%, Nb:1.85wt% ~ 4.15wt%, Mo:0.15wt%~2.05wt%, Zr:0.85wt%~3.15wt%, Si:0.00wt%~0.27wt%, Fe:0.00wt%~0.40wt%, C:0.00wt%~0.14wt%, all the other are Ti and other impurity element, and the weight percent sum of each component is absolutely.
Ti80 titanium alloy reference material of the present invention is made up of following 6 kinds of reference materials:
(1) Ti80-1, the weight percent of each component is: Al:4.5 ± 0.2wt%, Nb:4.00 ± 0.15wt%, Mo:0.10 ± 0.05wt%, Zr:3.00 ± 0.15wt%, Si:0.01 ± 0.02wt%, Fe:0.35 ± 0.05wt%, C:0.12 ± 0.02wt%, all the other are Ti and other impurity element, the weight percent sum of each component is absolutely;
(2) Ti80-2, the weight percent of each component is: Al:5.0 ± 0.2wt%, Nb:3.70 ± 0.15wt%, Mo:0.30 ± 0.05wt%, Zr:2.70 ± 0.15wt%, Si:0.05 ± 0.02wt%, Fe:0.30 ± 0.05wt%, C:0.08 ± 0.02wt%, all the other are Ti and other impurity element, the weight percent sum of each component is absolutely;
(3) Ti80-3, the weight percent of each component is: Al:5.5 ± 0.2wt%, Nb:3.30 ± 0.15wt%, Mo:0.60 ± 0.05wt%, Zr:2.30 ± 0.15wt%, Si:0.10 ± 0.02wt%, Fe:0.24 ± 0.05wt%, C:0.06 ± 0.02wt%, all the other are Ti and other impurity element, the weight percent sum of each component is absolutely;
(4) Ti80-4, the weight percent of each component is: Al:6.0 ± 0.2wt%, Nb:2.80 ± 0.15wt%, Mo:1.00 ± 0.05wt%, Zr:1.90 ± 0.15wt%, Si:0.15 ± 0.02wt%, Fe:0.18 ± 0.05wt%, C:0.04 ± 0.02wt%, all the other are T i and other impurity element, the weight percent sum of each component is absolutely;
(5) Ti80-5, the weight percent of each component is: Al:6.5 ± 0.2wt%, Nb:2.40 ± 0.15wt%, Mo:1.50 ± 0.05wt%, Zr:1.50 ± 0.15wt%, Si:0.20 ± 0.02wt%, Fe:0.12 ± 0.05wt%, C:0.02 ± 0.02wt%, all the other are Ti and other impurity element, the weight percent sum of each component is absolutely;
(6) Ti80-6, the weight percent of each component is: Al:7.0 ± 0.2wt%, Nb:2.00 ± 0.15wt%, Mo:2.00 ± 0.05wt%, Zr:1.00 ± 0.15wt%, Si:0.25 ± 0.02wt%, Fe:0.05 ± 0.05wt%, C:0.01 ± 0.02wt%, all the other are Ti and other impurity element, the weight percent sum of each component is absolutely.
Another object of the present invention is achieved in that the preparation method of above-mentioned Ti80 titanium alloy reference material, comprises the following steps:
(1) batching: adopt 0 grade of titanium sponge, AlMo50 master alloy, AlNb50 master alloy, AlSi24 master alloy, zirconium sponge, pure iron, fine aluminium and graphite as raw material, carry out charge calculation by the each constituent content requirement of titanium alloy reference material, and it is for subsequent use to take respectively above-mentioned raw materials;
(2) electrode block compacting: adopt titanium sponge and master alloy monolithic electrode method for mixing, for preventing that master alloy and pure metal additive that in electrode pressing process, some granularities are less are scattered in mold bottom, first appropriate titanium sponge is layered on to mold bottom, again the mixture of titanium sponge and master alloy is placed in to mould and suppresses in the lump, realize alloying element being uniformly distributed in consumable electrode;
(3) electrode welding: the electrode suppressing is put into welding case successively, when vacuum tightness is evacuated to 1.33x10 -1when Pa, be filled with argon gas, weld electrode is welded into electrode group with plasma;
(4) melting: electrode group is put into vaccum consumable electrode electric arc furnace and carry out melting for the first time; Using an ingot casting as second electrode, at vacuum consumable electrode electric arc skull melting secondary ingot, then using secondary ingot as three sub-electrodes, at three ingots of vaccum consumable electrode electric arc furnace melting as finished product ingot casting;
(5) homogenizing annealing: ingot casting is carried out to homogenizing annealing, eliminate the dendritic segregation and the regional segregation etc. that exist in ingot casting, make ingot casting component and microstructure homogenization, prevent ingot casting cracking in forging process;
(6) homogenizing deformation processing: adopt interactive pier to pull out deformation processing technique obtain the meeting the requirements titanium alloy rod bar of size to ingot casting;
(7) recrystallization annealing: carry out recrystallization annealing to forging rod, further crystal grain thinning, stabilizing tissue;
(8) processing bits shape sample: first adopt machined into remove titanium alloy bar surface scale, then carry out car bits, and to titanium bits pulverize, sieve, clean, dry, the operation such as bottling, the bits shape titanium alloy reference material that finally obtains 0.5mm × 1 ~ 2mm, can be used for the instruments such as ICP plasma spectrum;
(9) processing lumpy sample: adopt machined into titanium alloy bar extremely obtain block titanium alloy reference material, can be used for the instruments such as photoelectric direct reading spectrometry.
The present invention has following beneficial effect:
1. Ti80 titanium alloy reference material of the present invention can be used in the spectroscopic analysis of Ti80 titanium alloy, can accurately control and ensure Ti80 titanium alloy product quality.
2. the reliable easily row of the preparation method of Ti80 titanium alloy reference material of the present invention, can prepare the Ti80 titanium alloy reference material that meets service requirements.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
Ti80 titanium alloy reference material of the present invention, each principal element content range is: Al:4.3wt%~7.2wt%, Nb:1.85wt% ~ 4.15wt%, Mo:0.15wt%~2.05wt%, Zr:0.85wt%~3.15wt%, Si:0.00wt%~0.27wt%, Fe:0.00wt%~0.40wt%, C:0.00wt%~0.14wt%, all the other are Ti and other impurity element (as N, H, O etc.), the weight percent sum of each component is absolutely.
Designed the reference material of 6 kinds of component gradients according to full system of elements method of design, that is this cover reference material is made up of following 6 kinds of reference materials:
(1) Ti80-1, the weight percent of each component is: Al:4.5 ± 0.2wt%, Nb:4.00 ± 0.15wt%, Mo:0.10 ± 0.05wt%, Zr:3.00 ± 0.15wt%, Si:0.01 ± 0.02wt%, Fe:0.35 ± 0.05wt%, C:0.12 ± 0.02wt%, all the other are Ti and other impurity element (as N, H, O etc.), the weight percent sum of each component is absolutely;
(2) weight percent of the each component of Ti80-2 is: Al:5.0 ± 0.2wt%, Nb:3.70 ± 0.15wt%, Mo:0.30 ± 0.05wt%, Zr:2.70 ± 0.15wt%, Si:0.05 ± 0.02wt%, Fe:0.30 ± 0.05wt%, C:0.08 ± 0.02wt%, all the other are Ti and other impurity element (as N, H, O etc.), and the weight percent sum of each component is absolutely;
(3) weight percent of the each component of Ti80-3 is: Al:5.5 ± 0.2wt%, Nb:3.30 ± 0.15wt%, Mo:0.60 ± 0.05wt%, Zr:2.30 ± 0.15wt%, Si:0.10 ± 0.02wt%, Fe:0.24 ± 0.05wt%, C:0.06 ± 0.02wt%, all the other are Ti and other impurity element (as N, H, O etc.), and the weight percent sum of each component is absolutely;
(4) weight percent of the each component of Ti80-4 is: Al:6.0 ± 0.2wt%, Nb:2.80 ± 0.15wt%, Mo:1.00 ± 0.05wt%, Zr:1.90 ± 0.15wt%, Si:0.15 ± 0.02wt%, Fe:0.18 ± 0.05wt%, C:0.04 ± 0.02wt%, all the other are T i and other impurity element (as N, H, O etc.), and the weight percent sum of each component is absolutely;
(5) weight percent of the each component of Ti80-5 is: Al:6.5 ± 0.2wt%, Nb:2.40 ± 0.15wt%, Mo:1.50 ± 0.05wt%, Zr:1.50 ± 0.15wt%, Si:0.20 ± 0.02wt%, Fe:0.12 ± 0.05wt%, C:0.02 ± 0.02wt%, all the other are Ti and other impurity element (as N, H, O etc.), and the weight percent sum of each component is absolutely;
(6) weight percent of the each component of Ti80-6 is: Al:7.0 ± 0.2wt%, Nb:2.00 ± 0.15wt%, Mo:2.00 ± 0.05wt%, Zr:1.00 ± 0.15wt%, Si:0.25 ± 0.02wt%, Fe:0.05 ± 0.05wt%, C:0.01 ± 0.02wt%, all the other are Ti and other impurity element (as N, H, O etc.), and the weight percent sum of each component is absolutely.
The preparation method of Ti80 titanium alloy reference material of the present invention, specifically implements according to following steps:
(1) batching: carry out charge calculation by the each constituent content requirement of Ti80 titanium alloy reference material, take diameter and be 0 grade of titanium sponge, AlMo50 master alloy, AlNb50 master alloy, AlSi24 master alloy, zirconium sponge, pure iron, fine aluminium and the graphite of 3 ~ 5mm as raw material.Adopt 0 grade of titanium sponge can avoid the impact of impurity in titanium sponge, selecting diameter is that 3 ~ 5mm titanium sponge can make being more evenly distributed of titanium sponge.Because the fusing point of titanium sponge is 1668 ± 4 DEG C, density is 4.51g/cm 3; The fusing point of metallic aluminium is 600 DEG C, and density is 2.70g/cm 3; The fusing point of metal molybdenum is 2610 DEG C, and density is 10.2g/cm 3; 2468 DEG C of the fusing points of metal niobium, density is 8.57g/cm 3; The fusing point of nonmetal silicon is 1410 DEG C, and density is 2.33g/cm 3, fusing point or the density variation of the fusing point of these elements or density and metal titanium are larger, directly add and carry out melting, easily produce being mingled with and segregation of high-melting-point, high-density constituent element, and the segregation of low density constituent element.Therefore, adopt density, specific heat capacity, Al-Mo, Al-Nb, Al-Si master alloy that the latent heat of fusion is close with matrix metal titanium to carry out melting as raw material, can improve alloying condition, overcome segregation and do not melt and the metallurgical imperfection such as be mingled with.And master alloy, pure metal and titanium sponge granularity should be controlled within the specific limits, reasonably combined, the particle of master alloy and pure metal should be as far as possible tiny, is beneficial to master alloy being uniformly distributed in electrode, improves electrode block intensity simultaneously.Ensure that master alloy is synchronizeed and melted with metal titanium in the time of melting, avoid in fusion process improper fall piece, overcome the alloying element dilution segregation causing therefrom.
(2) electrode block compacting: the present invention adopts the method for titanium sponge and master alloy monolithic electrode batch mixing, before electrode pressing piece, in order to make chemical composition even, adopts rotary mixer to carry out homogenizing to titanium sponge and various alloy addition mixed.For preventing that master alloy and pure metal additive that in electrode pressing process, some granularities are less are scattered in mold bottom, first appropriate titanium sponge is layered on to mold bottom, again the mixture of titanium sponge and master alloy is placed in to mould, adopts 2000 tons of pressing machine electrode pressings, obtain specification and be electrode.
(3) electrode welding: grid for welding in vacuum argon filling case, multiple electrodes that upper step is obtained are put into welding case successively, when vacuum tightness is evacuated to 1.33x10 -1when Pa, be filled with purity and be not less than 99.95% argon gas, weld multiple electrodes are welded into the electrode group that length is 150 ± 5cm with plasma, straight after guarantee electrode welding, non-oxidation is polluted, and tensile strength is not less than 10Mpa;
(4) melting: ingot casting of vaccum consumable electrode electric arc furnace melting, the electrode group welding is put into vaccum consumable electrode electric arc furnace and carry out melting.By the vacuum degree control in stove at 6.65x10 -2pa ~ 1.33x10 -2within the scope of Pa, melting vacuum tightness is high, be conducive to reduce the content of obnoxious flavour O, N, H in burner hearth, the floating of gas and discharge while being conducive to melting of metal simultaneously, can reach gas and non-metallic inclusion in effective removal metal, accurately control chemical composition, reduce the objects such as alloying element oxidization burning loss.But too high vacuum tightness can cause again the element that in alloy, saturation vapour pressure is higher (normally low melting point element) volatilization more serious, makes component uniformity wayward.Controlling melting voltage is 28 ~ 36V, melting electric current is 3500~5000A, less melting electric current can make molten bath melting under compared with tranquility, the disturbance that effectively prevents molten bath is washed away crystallization forward position, is also conducive to reduce speed of melting simultaneously, reduces pool depth and bath temperature gradient, keep molten bath flat, for axial crystallization creates good conditions, improve alloy homogeneity, reduce segregation.Suitably improve melting electric current, can make molten titanium amount of droplets increase, particle diminishes, and its surface-area increases, and is conducive to the removal of nonmetallic impurity and gaseous impurities in molten metal, improves alloy refining effect.Therefore, when melting once, suitably large melting electric current should be adopted, in the time of secondary, three meltings, less melting electric current should be adopted.The gap that ensures electrode and crucible inwall is 30 ~ 40mm, electrode is 0.5 ~ 0.9 with the diameter ratio of crucible, regulating electrode melting speed is 12~30g/s, control the degree of depth in molten bath by the variation of this burn-off rate, thereby reach the object of controlling metal liquid solidification rate, at the melting initial stage, consider the chill effect of heelpiece and crucible, ingot solidification speed, speed of melting is also wanted corresponding quickening, set up rapidly molten bath, and stable as early as possible, in melting, later stage, pool depth to be controlled in suitable scope, slowly reduce speed of melting, stop putting forearc 60~90min, speed of melting is subtracted, reduce successively molten bath thermal capacity, latent heat of solidification and pool depth, thereby raising solidification rate, suppress the enrichment of the elements such as Fe, prevent segregation.By regulating at any time galvanic size of current in crucible external coil, current control, at 3000~15000A, is adjusted to the intensity in stabilising arc magnetic field, guarantee that arc column is controlled, burning, can play sufficient stirring action to molten bath, makes alloy compositions even, grain refining.Control the water coolant flow velocity of crucible, guarantee leaving water temperature(LWT), is imported and exported water temperature difference and is no more than 10 ° of C below C at 40 °.After melting finishes, treat that ingot casting temperature drops within the scope of 200 ~ 400 ° of C to come out of the stove.
Vacuum consumable electrode electric arc skull melting secondary ingot casting, an ingot casting of arc melting is carried out to machining, remove surface scale and top and emit notch portion, sampling check chemical composition and foreign matter content, while meeting component requirement, proceed in vacuum consumable electrode electric arc skull crucible and carry out melting, vacuum tightness is evacuated to 1.33x10 -1pa, after the starting the arc, regulating melting voltage is that 30 ~ 35V, current density are 0.4 ~ 0.6A/cm 2electrode and the diameter ratio of crucible are 0.45 ~ 0.88, the gap of electrode and crucible inwall is 30 ~ 40mm, the water coolant flow velocity of controlling crucible, ensure that leaving water temperature(LWT) is at 35 ° below C, import and export water temperature difference and be no more than 10 ° of C, when cast graphite casting mould, controlling the duration of pouring is 3 ~ 6s, centrifugal pan rotating speed is 200 ~ 500r/min, pours to be cooled to 400 ° until ingot casting and to come out of the stove below C time.
Three ingot castings of vaccum consumable electrode electric arc furnace melting, the secondary ingot casting of skull melting is carried out to machining, remove surface scale and top and emit notch portion, sampling check chemical composition and foreign matter content, while meeting component requirement, proceed in vaccum consumable electrode electric arc furnace and carry out melting, vacuum tightness is 6.65x10 -2~1.33x10 -2pa, melting electric current is 2500~4000A, the gap of electrode and crucible inwall is 30~38mm, electrode is 0.45~0.85 with the diameter ratio of crucible, electrode melting speed is 12~30g/s, control the water coolant flow velocity of crucible, guarantee leaving water temperature(LWT), is imported and exported water temperature difference and is no more than 10 ° of C below C at 40 °.After melting finishes, treat that ingot casting temperature drops within the scope of 200 ~ 400 ° of C to come out of the stove.
(5) homogenizing annealing: adopt vacuum annealing furnace to carry out homogenizing annealing to ingot casting, eliminate the dendritic segregation and the regional segregation etc. that exist in ingot casting, make ingot casting component and homogeneous microstructure, and prevent ingot casting cracking in forging process.Annealing temperature is: 950 DEG C, soaking time is 10h, treats that temperature drops to 200 ° of C and comes out of the stove below.
(6) homogenizing deformation processing: adopt interactive pier to pull out deformation processing technique refinement ingot structure to ingot casting, further improve the component uniformity of ingot casting.Ingot casting is heated to 1150 DEG C of coggings and forges, adopt 3T hammer to carry out repeatedly pier and pull out, finally adopt 1T flat-die hammer that titanium alloy rod bar is changed and forges 50 ~ 55mm to Ф.
(7) recrystallization annealing: adopt vacuum annealing furnace to carry out recrystallization annealing to forging rod, further crystal grain thinning, stabilizing tissue.Annealing temperature is 900 DEG C, and soaking time is 2h, treats that temperature drops to 200 ° of C and comes out of the stove below.
(8) processing bits shape sample: first adopt machined into remove titanium alloy bar surface scale, then carry out car bits, and to titanium bits pulverize, sieve, clean, dry, the operation such as bottling, the bits shape titanium alloy reference material that finally obtains 0.5mm × 1 ~ 2mm, can be used for the instruments such as ICP plasma spectrum.
(9) processing lumpy sample: adopt machined into titanium alloy bar extremely obtain block titanium alloy reference material, can be used for the instruments such as photoelectric direct reading spectrometry.
Embodiment, Ti80 titanium alloy reference material and preparation method thereof, preparation Ti80 titanium alloy reference material Ti80-1, Ti80-2, Ti80-3, Ti80-4, Ti80-5 and Ti80-6.Its components by weight percent is in table 1,
Specifically prepare burden in table 2.
One, preparation Ti80-1
Concrete preparation process is as follows:
(1) batching: calculate by the 100kg that feeds intake, take titanium sponge 87.5kg, AlMo50 master alloy 0.19kg, AlNb50 master alloy 8.08kg, zirconium sponge 3.03kg, pure iron 0.36kg, fine aluminium 0.71kg and graphite 0.13kg as raw material.Adopt 0 grade of titanium sponge can avoid the impact of impurity in titanium sponge, selecting diameter is that 3 ~ 5mm titanium sponge can make being more evenly distributed of titanium sponge.Because the fusing point of titanium sponge is 1668 ± 4 DEG C, density is 4.51g/cm 3; The fusing point of metallic aluminium is 600 DEG C, and density is 2.70g/cm 3; The fusing point of metal molybdenum is 2610 DEG C, and density is 10.2g/cm 3; 2468 DEG C of the fusing points of metal niobium, density is 8.57g/cm 3; The fusing point of nonmetal silicon is 1410 DEG C, and density is 2.33g/cm 3, fusing point or the density variation of the fusing point of these elements or density and metal titanium are larger, directly add and carry out melting, easily produce being mingled with and segregation of high-melting-point, high-density constituent element, and the segregation of low density constituent element.Therefore, adopt density, specific heat capacity, Al-Mo, Al-Nb, Al-Si master alloy that the latent heat of fusion is close with matrix metal titanium to carry out melting as raw material, can improve alloying condition, overcome segregation and do not melt and the metallurgical imperfection such as be mingled with.And master alloy, pure metal and titanium sponge granularity should be controlled within the specific limits, reasonably combined, the particle of master alloy and pure metal should be as far as possible tiny, is beneficial to master alloy being uniformly distributed in electrode, improves electrode block intensity simultaneously.Ensure that master alloy is synchronizeed and melted with metal titanium in the time of melting, avoid in fusion process improper fall piece, overcome the alloying element dilution segregation causing therefrom.
(2) electrode block compacting: the present invention adopts the method for titanium sponge and master alloy monolithic electrode batch mixing, before electrode pressing piece, in order to make chemical composition even, adopts rotary mixer to carry out homogenizing to titanium sponge and various alloy addition mixed.For preventing that master alloy and pure metal additive that in electrode pressing process, some granularities are less are scattered in mold bottom, first appropriate titanium sponge is layered on to mold bottom, again the mixture of titanium sponge and master alloy is placed in to mould, adopts 2000 tons of pressing machine electrode pressings, obtain specification and be electrode.
(3) electrode welding: grid for welding in vacuum argon filling case, multiple electrodes that upper step is obtained are put into welding case successively, when vacuum tightness is evacuated to 1.33x10 -1when Pa, be filled with purity and be not less than 99.95% argon gas, weld multiple electrodes are welded into the electrode group that length is 150 ± 5cm with plasma, straight after guarantee electrode welding, non-oxidation is polluted, and tensile strength is not less than 10Mpa;
(4) melting: ingot casting of vaccum consumable electrode electric arc furnace melting, the electrode group welding is put into vaccum consumable electrode electric arc furnace and carry out melting.By the vacuum degree control in stove at 6.65x10 -2pa ~ 1.33x10 -2within the scope of Pa, melting vacuum tightness is high, be conducive to reduce the content of obnoxious flavour O, N, H in burner hearth, the floating of gas and discharge while being conducive to melting of metal simultaneously, can reach gas and non-metallic inclusion in effective removal metal, accurately control chemical composition, reduce the objects such as alloying element oxidization burning loss.But too high vacuum tightness can cause again the element that in alloy, saturation vapour pressure is higher (normally low melting point element) volatilization more serious, makes component uniformity wayward.Controlling melting voltage is 28 ~ 36V, melting electric current is 3500~5000A, less melting electric current can make molten bath melting under compared with tranquility, the disturbance that effectively prevents molten bath is washed away crystallization forward position, is also conducive to reduce speed of melting simultaneously, reduces pool depth and bath temperature gradient, keep molten bath flat, for axial crystallization creates good conditions, improve alloy homogeneity, reduce segregation.Suitably improve melting electric current, can make molten titanium amount of droplets increase, particle diminishes, and its surface-area increases, and is conducive to the removal of nonmetallic impurity and gaseous impurities in molten metal, improves alloy refining effect.Therefore, when melting once, suitably large melting electric current should be adopted, in the time of secondary, three meltings, less melting electric current should be adopted.The gap that ensures electrode and crucible inwall is 30 ~ 40mm, electrode is 0.5 ~ 0.9 with the diameter ratio of crucible, regulating electrode melting speed is 12~30g/s, control the degree of depth in molten bath by the variation of this burn-off rate, thereby reach the object of controlling metal liquid solidification rate, at the melting initial stage, consider the chill effect of heelpiece and crucible, ingot solidification speed, speed of melting is also wanted corresponding quickening, set up rapidly molten bath, and stable as early as possible, in melting, later stage, pool depth to be controlled in suitable scope, slowly reduce speed of melting, stop putting forearc 60~90min, speed of melting is subtracted, reduce successively molten bath thermal capacity, latent heat of solidification and pool depth, thereby raising solidification rate, suppress the enrichment of the elements such as Fe, prevent segregation.By regulating at any time galvanic size of current in crucible external coil, current control, at 3000~15000A, is adjusted to the intensity in stabilising arc magnetic field, guarantee that arc column is controlled, burning, can play sufficient stirring action to molten bath, makes alloy compositions even, grain refining.Control the water coolant flow velocity of crucible, guarantee leaving water temperature(LWT), is imported and exported water temperature difference and is no more than 10 ° of C below C at 40 °.After melting finishes, treat that ingot casting temperature drops within the scope of 200 ~ 400 ° of C to come out of the stove.
Vacuum consumable electrode electric arc skull melting secondary ingot casting, an ingot casting of arc melting is carried out to machining, remove surface scale and top and emit notch portion, sampling check chemical composition and foreign matter content, while meeting component requirement, proceed in vacuum consumable electrode electric arc skull crucible and carry out melting, vacuum tightness is evacuated to 1.33x10 -1pa, after the starting the arc, regulating melting voltage is that 30 ~ 35V, current density are 0.4 ~ 0.6A/cm 2electrode and the diameter ratio of crucible are 0.45 ~ 0.88, the gap of electrode and crucible inwall is 30 ~ 40mm, the water coolant flow velocity of controlling crucible, ensure that leaving water temperature(LWT) is at 35 ° below C, import and export water temperature difference and be no more than 10 ° of C, when cast graphite casting mould, controlling the duration of pouring is 3 ~ 6s, centrifugal pan rotating speed is 200 ~ 500r/min, pours to be cooled to 400 ° until ingot casting and to come out of the stove below C time.
Three ingot castings of vaccum consumable electrode electric arc furnace melting, the secondary ingot casting of skull melting is carried out to machining, remove surface scale and top and emit notch portion, sampling check chemical composition and foreign matter content, while meeting component requirement, proceed in vaccum consumable electrode electric arc furnace and carry out melting, vacuum tightness is 6.65x10 -2~1.33x10 -2pa, melting electric current is 2500~4000A, the gap of electrode and crucible inwall is 30~38mm, electrode is 0.45~0.85 with the diameter ratio of crucible, electrode melting speed is 12~30g/s, control the water coolant flow velocity of crucible, guarantee leaving water temperature(LWT), is imported and exported water temperature difference and is no more than 10 ° of C below C at 40 °.After melting finishes, treat that ingot casting temperature drops within the scope of 200 ~ 400 ° of C to come out of the stove.
(5) homogenizing annealing: adopt vacuum annealing furnace to carry out homogenizing annealing to ingot casting, eliminate the dendritic segregation and the regional segregation etc. that exist in ingot casting, make ingot casting component and homogeneous microstructure, and prevent ingot casting cracking in forging process.Annealing temperature is: 950 DEG C, soaking time is 10h, treats that temperature drops to 200 ° of C and comes out of the stove below.
(6) homogenizing deformation processing: adopt interactive pier to pull out deformation processing technique refinement ingot structure to ingot casting, further improve the component uniformity of ingot casting.Ingot casting is heated to 1150 DEG C of coggings and forges, adopt 3T hammer to carry out repeatedly pier and pull out, finally adopt 1T flat-die hammer that titanium alloy rod bar is changed and forges 50 ~ 55mm to Ф.
(7) recrystallization annealing: adopt vacuum annealing furnace to carry out recrystallization annealing to forging rod, further crystal grain thinning, stabilizing tissue.Annealing temperature is 900 DEG C, and soaking time is 2h, treats that temperature drops to 200 ° of C and comes out of the stove below.
(8) processing bits shape sample: first adopt machined into remove titanium alloy bar surface scale, then carry out car bits, and to titanium bits pulverize, sieve, clean, dry, the operation such as bottling, the bits shape titanium alloy reference material that finally obtains 0.5mm × 1 ~ 2mm, can be used for the instruments such as ICP plasma spectrum.
(9) processing lumpy sample: adopt machined into titanium alloy bar extremely obtain block titanium alloy reference material, can be used for the instruments such as photoelectric direct reading spectrometry.
Two, preparation Ti80-2 ~ Ti80-6
Preparation process is identical with preparation Ti80-1.
Table 1 embodiment Ti80 titanium alloy reference material weight percentages of components (%)
Table 2 embodiment Ti80 titanium alloy reference material allocation sheet (kg)
Numbering Titanium sponge AlNb50 AlMo50 AlSi24 Zirconium sponge Fine aluminium Pure iron Graphite
Ti80-1 87.5 8.08 0.19 0 3.03 0.71 0.36 0.13
Ti80-2 87.4 7.47 0.58 0.22 2.73 1.21 0.31 0.08
Ti80-3 87.4 6.67 1.17 0.43 2.33 1.7 0.25 0.06
Ti80-4 87.4 5.66 1.94 0.65 1.92 2.21 0.18 0.04
Ti80-5 87.2 4.85 2.91 0.87 1.52 2.52 0.12 0.02
Ti80-6 87.1 4.04 3.89 1.09 1.01 2.83 0.05 0.01
Uniformity testing: the homogeneity of reference material is one of its most critical index, therefore, reference material prepared by embodiment carries out uniformity testing.According to GB/T15000 " standard model work directive/guide " and YS/T409 " standard model technical specifications " regulation, stochastic sampling adopts one-way analysis of variance method (F method) to carry out uniformity testing.
One-way analysis of variance method is in same heat (batch) number, randomly draws m sample, respectively analyzes n time (general m > 15, n=3), is divided into m data set, every group data n, first obtains the inner variance S of group e 2with variance between laboratories S a 2, then compute statistics F value, with the threshold value F of statistic F 0make comparisons and do and judge: if F < is F 0, sample is evenly, otherwise sample is inhomogeneous.F 0be and group between degree of freedom m-1, group internal degree of freedom m (n-1), and the relevant constant of level of significance α.Calculation formula is as follows:
Q e = &Sigma; i = 1 m &Sigma; j = 1 n ( x ij - x &OverBar; i ) 2 The sum of squares of deviations in group
Q A = &Sigma; i = 1 m &Sigma; j = 1 n ( x &OverBar; i - x = ) 2 ... the sum of squares of deviations between group
F e=m (n-1) ... the group internal degree of freedom
F a=m-1 ... ... .. ... .. degree of freedom between group
S e 2 = Q e / f e ... variance within laboratory
S A 2 = Q A / f A ... .... variance between laboratories
F = S A 2 / S e 2 .... ... .. statistic F
In formula, be x iji organizes the analytical data of the j time, be the mean value of i group data, for the population mean of whole data.
Random each 20 reference material Ti80-1 ~ Ti80-6 that extract, test 3 times, calculate F value (referring to table 3), with threshold value F according to above formula for every 0compare, be all less than threshold value F 0, show that Certified Reference Material Homogeneity prepared by embodiment is good.
Table 3 embodiment Ti80 titanium alloy Certified Reference Material Homogeneity
Definite value is analyzed: original value data is adopted to the Grubbs test criterion rejecting dubious value of testing, then investigate the normality of DATA DISTRIBUTION, assay all meets normal state or seemingly normal distribution, all select, check the each group of data precision such as whether by Cochran method again, on inspection without abnormal data group, then according to GB/T15000.3-2008, the value of settling the standard and uncertainty.
Working curve checks: in order to check the usable condition of this cover reference material, randomly draw a set of reference material, select top condition to excite and gather its light intensity, with standard value and light intensity drawing curve by ARL4460 type Photoelectric Spectrometer.The contact ratio of working curve all (refers to table 4) more than 0.99, can meet spectroscopic analysis needs completely.
The working curve contact ratio of reference material prepared by table 4 embodiment of the present invention
Element Al Nb Zr Mo Fe Si C
Ti80 0.993 0.995 0.993 0.991 0.995 0.995 0.992

Claims (2)

1. a Ti80 titanium alloy reference material, is characterized in that, is made up of following 6 kinds of reference materials:
(1) Ti80-1, the weight percent of each component is, Al:4.5 ± 0.2wt%, Nb:4.00 ± 0.15wt%, Mo:0.10 ± 0.05wt%, Zr:3.00 ± 0.15wt%, Si:0.01 ± 0.02wt%, Fe:0.35 ± 0.05wt%, C:0.12 ± 0.02wt%, all the other are Ti and other impurity element, and the weight percent sum of each component is absolutely;
(2) Ti80-2, the weight percent of each component is, Al:5.0 ± 0.2wt%, Nb:3.70 ± 0.15wt%, Mo:0.30 ± 0.05wt%, Zr:2.70 ± 0.15wt%, Si:0.05 ± 0.02wt%, Fe:0.30 ± 0.05wt%, C:0.08 ± 0.02wt%, all the other are Ti and other impurity element, and the weight percent sum of each component is absolutely;
(3) Ti80-3, the weight percent of each component is, Al:5.5 ± 0.2wt%, Nb:3.30 ± 0.15wt%, Mo:0.60 ± 0.05wt%, Zr:2.30 ± 0.15wt%, Si:0.10 ± 0.02wt%, Fe:0.24 ± 0.05wt%, C:0.06 ± 0.02wt%, all the other are Ti and other impurity element, and the weight percent sum of each component is absolutely;
(4) Ti80-4, the weight percent of each component is, Al:6.0 ± 0.2wt%, Nb:2.80 ± 0.15wt%, Mo:1.00 ± 0.05wt%, Zr:1.90 ± 0.15wt%, Si:0.15 ± 0.02wt%, Fe:0.18 ± 0.05wt%, C:0.04 ± 0.02wt%, all the other are T i and other impurity element, and the weight percent sum of each component is absolutely;
(5) Ti80-5, the weight percent of each component is, Al:6.5 ± 0.2wt%, Nb:2.40 ± 0.15wt%, Mo:1.50 ± 0.05wt%, Zr:1.50 ± 0.15wt%, Si:0.20 ± 0.02wt%, Fe:0.12 ± 0.05wt%, C:0.02 ± 0.02wt%, all the other are Ti and other impurity element, and the weight percent sum of each component is absolutely;
(6) Ti80-6, the weight percent of each component is, Al:7.0 ± 0.2wt%, Nb:2.00 ± 0.15wt%, Mo:2.00 ± 0.05wt%, Zr:1.00 ± 0.15wt%, Si:0.25 ± 0.02wt%, Fe:0.05 ± 0.05wt%, C:0.01 ± 0.02wt%, all the other are Ti and other impurity element, and the weight percent sum of each component is absolutely.
2. the preparation method of a Ti80 titanium alloy reference material, it is characterized in that, each principal element content range is: Al:4.3wt%~7.2wt%, Nb:1.85wt%~4.15wt%, Mo:0.15wt%~2.05wt%, Zr:0.85wt%~3.15wt%, Si:0.00wt%~0.27wt%, Fe:0.00wt%~0.40wt%, C:0.00wt%~0.14wt%, all the other are Ti and other impurity element, and the weight percent sum of each component is absolutely;
Each principal element is made up of following 6 kinds of reference materials:
(1) Ti80-1, the weight percent of each component is, Al:4.5 ± 0.2wt%, Nb:4.00 ± 0.15wt%, Mo:0.10 ± 0.05wt%, Zr:3.00 ± 0.15wt%, Si:0.01 ± 0.02wt%, Fe:0.35 ± 0.05wt%, C:0.12 ± 0.02wt%, all the other are Ti and other impurity element, and the weight percent sum of each component is absolutely;
(2) Ti80-2, the weight percent of each component is, Al:5.0 ± 0.2wt%, Nb:3.70 ± 0.15wt%, Mo:0.30 ± 0.05wt%, Zr:2.70 ± 0.15wt%, Si:0.05 ± 0.02wt%, Fe:0.30 ± 0.05wt%, C:0.08 ± 0.02wt%, all the other are Ti and other impurity element, and the weight percent sum of each component is absolutely;
(3) Ti80-3, the weight percent of each component is, Al:5.5 ± 0.2wt%, Nb:3.30 ± 0.15wt%, Mo:0.60 ± 0.05wt%, Zr:2.30 ± 0.15wt%, Si:0.10 ± 0.02wt%, Fe:0.24 ± 0.05wt%, C:0.06 ± 0.02wt%, all the other are Ti and other impurity element, and the weight percent sum of each component is absolutely;
(4) Ti80-4, the weight percent of each component is, Al:6.0 ± 0.2wt%, Nb:2.80 ± 0.15wt%, Mo:1.00 ± 0.05wt%, Zr:1.90 ± 0.15wt%, Si:0.15 ± 0.02wt%, Fe:0.18 ± 0.05wt%, C:0.04 ± 0.02wt%, all the other are T i and other impurity element, and the weight percent sum of each component is absolutely;
(5) Ti80-5, the weight percent of each component is, Al:6.5 ± 0.2wt%, Nb:2.40 ± 0.15wt%, Mo:1.50 ± 0.05wt%, Zr:1.50 ± 0.15wt%, Si:0.20 ± 0.02wt%, Fe:0.12 ± 0.05wt%, C:0.02 ± 0.02wt%, all the other are Ti and other impurity element, and the weight percent sum of each component is absolutely;
(6) Ti80-6, the weight percent of each component is, Al:7.0 ± 0.2wt%, Nb:2.00 ± 0.15wt%, Mo:2.00 ± 0.05wt%, Zr:1.00 ± 0.15wt%, Si:0.25 ± 0.02wt%, Fe:0.05 ± 0.05wt%, C:0.01 ± 0.02wt%, all the other are Ti and other impurity element, and the weight percent sum of each component is absolutely;
Concrete preparation method comprises the following steps:
(1) batching: adopt 0 grade of titanium sponge, AlMo50 master alloy, AlNb50 master alloy, AlSi24 master alloy, zirconium sponge, pure iron, fine aluminium and graphite as raw material, carry out charge calculation by the each constituent content requirement of titanium alloy reference material, and take respectively the raw material for standby of said components;
(2) electrode block compacting: adopt titanium sponge and master alloy monolithic electrode method for mixing, for preventing that master alloy and pure metal additive that in electrode pressing process, some granularities are less are scattered in mold bottom, first appropriate titanium sponge is layered on to mold bottom, again the mixture of titanium sponge and master alloy is placed in to mould and suppresses in the lump, realize alloying element being uniformly distributed in consumable electrode;
(3) electrode welding: the electrode suppressing is put into welding case successively, when vacuum tightness is evacuated to 1.33 х 10 -1when Pa, be filled with argon gas, weld electrode is welded into electrode group with plasma;
(4) melting: electrode group is put into vaccum consumable electrode electric arc furnace and carry out melting for the first time; Using an ingot casting as second electrode, at vacuum consumable electrode electric arc skull melting secondary ingot, then using secondary ingot as three sub-electrodes, at three ingots of vaccum consumable electrode electric arc furnace melting as finished product ingot casting;
(5) homogenizing annealing: ingot casting is carried out to homogenizing annealing, eliminate the dendritic segregation and the regional segregation that exist in ingot casting, make ingot casting component and microstructure homogenization, prevent ingot casting cracking in forging process;
(6) homogenizing deformation processing: adopt interactive pier to pull out deformation processing technique obtain the meeting the requirements titanium alloy rod bar of size to ingot casting;
(7) recrystallization annealing: carry out recrystallization annealing to forging rod, further crystal grain thinning, stabilizing tissue;
(8) processing bits shape sample: first adopt machined into remove titanium alloy bar surface scale, then carry out car bits, and titanium is considered to be worth doing to the operation of pulverizing, sieve, clean, dry, bottle, finally obtain the bits shape titanium alloy reference material of 0.5mm × 1~2mm, for ICP plasma spectrum instrument;
(9) processing lumpy sample: adopt machined into titanium alloy bar extremely obtain block titanium alloy reference material, for photo-electric direct reading spectrometer device.
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