CN102965541A - Ti80 titanium alloy standard substance and preparation method thereof - Google Patents
Ti80 titanium alloy standard substance and preparation method thereof Download PDFInfo
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- CN102965541A CN102965541A CN2012105212680A CN201210521268A CN102965541A CN 102965541 A CN102965541 A CN 102965541A CN 2012105212680 A CN2012105212680 A CN 2012105212680A CN 201210521268 A CN201210521268 A CN 201210521268A CN 102965541 A CN102965541 A CN 102965541A
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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
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 contain the nearly alpha titanium alloy of beta stable element Nb, Mo and neutral element Zr, be that aim at ship design a kind of has the easily titanium alloy trade mark of the high-quality performances such as weldering of high strength anti-corrosion.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.
For reliability and the stability that ensures titanium alloy product, must carry out accurately component measurement to its material, need corresponding titanium alloy reference material that analytical procedure, Analytical equipment and analytical results are calibrated.The 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 to be used 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, is used for tester, estimates measuring method or to material or the material of material assignment.Reference material is a kind of as measurement instrument, and it can reappear, and preserves and the transmission value, guarantees 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) be used for the 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) be used for Laboratory Accreditation and Laboratory Ability Confirmation.
The development of Ti80 titanium alloy series standard material mainly contains following two difficult points:
(1) how to control 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 satisfy the use needs of reference material.Because reference material need to be drawn the analytical work curve, each analytical element content of reference material should be reasonably Gradient distribution, because each element chemistry component concentration narrow range of Ti80 titanium alloy will satisfy 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 two content point, and wherein the lower limit of the upper limit of low component and higher composition only differs 0.1%, 6 content and is difficult to distribution gradient.Need the unit of quantitative analysis to have the elements such as Al, Nb, Zr, Mo, Si, Fe, C in the Ti80 material, the saturation vapour pressure of each element is different, volatilization is asynchronous in the fusion process, wherein the saturation vapour pressure of Al, Fe, Si element is higher than the matrix titanium, it is more serious to volatilize, and the minimum content of Si, Fe, C impurity element has often surpassed Si, Fe, C foreign matter content that body material titanium sponge and various master alloy are brought into, and the impurity composition content distribution is inhomogeneous in the starting material, be difficult to accurately its component of control, and make it satisfy 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 guarantee the homogeneity of each element.According to national metallurgic product spectroscopic standard material technology standard relevant regulations: the content range of main ingredient element, outwards suitably extend by the upper and lower limit (especially lower limit) of product technology condition.Content extends 5% ~ 15% 10% above person; Content extends 15% ~ 30% 10% following person.The 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 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 surpassed the solid solubility of this element in body material, and homogeneity is difficult to guarantee.For example, the high-content of Ti80 titanium alloy standard ingredient Al element is 6.5%, and the high-content of Al element is 7.0% in the reference material, and the Al constituent content surpasses 6.0% with precipitating metal compound Ti
3Al produce segregation, and in the titanium alloy process of setting, α stable element (mainly being Al) is easily in the crystal boundary enrichment, and beta stable element Mo, Nb are easily in the 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, does not all have 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, with accurate control and assurance Ti80 titanium alloy product quality.
Summary of the invention
The purpose of this invention is to provide a kind of Ti80 titanium alloy reference material, be used for the proximate analysis of each element of Ti80 titanium alloy.
Another object of the present invention provides 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 comprised 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, may further comprise the 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 each the constituent content requirement of titanium alloy reference material, and it is for subsequent use to take by weighing respectively above-mentioned raw materials;
(2) electrode block compacting: adopt titanium sponge and master alloy monolithic electrode method for mixing, for preventing that some granularities are less in the electrode pressing process master alloy and pure metal additive are scattered in mold bottom, first an amount of titanium sponge is layered on mold bottom, mixture with titanium sponge and master alloy places mould to suppress in the lump again, realizes the even distribution of alloying element in consumable electrode;
(3) electrode welding: the electrode that suppresses is put into the welding case successively, when vacuum tightness is evacuated to 1.33x10
-1During Pa, be filled with argon gas, with the plasma weldering electrode be welded into the electrode group;
(4) melting: the electrode group is put into vaccum consumable electrode electric arc furnace carry out the melting first time; With an ingot casting as second electrode, at vacuum consumable electrode electric arc skull melting secondary ingot, then with the secondary ingot as three sub-electrodes, at three ingots of vaccum consumable electrode electric arc furnace melting as the finished product ingot casting;
(5) homogenizing annealing: ingot casting is carried out homogenizing annealing, and the dendritic segregation that exists in the elimination ingot casting and regional segregation etc. make ingot casting component and microstructure homogenization, prevent ingot casting cracking in the 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: at first adopt machined into to remove the titanium alloy bar surface scale, then carry out the car bits, and to titanium bits pulverize, sieve, clean, dry, the operation such as bottling, finally obtain the bits shape titanium alloy reference material of 0.5mm * 1 ~ 2mm, can be used for the instruments such as ICP plasma spectrum;
(9) processing lumpy sample: adopt the 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 guarantee 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 be prepared the Ti80 titanium alloy reference material that meets service requirements.
Embodiment
The present invention is described in detail below in conjunction with embodiment.
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 (such 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 comprised 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 (such as N, H, O etc.), the weight percent sum of each component is absolutely;
(2) weight percent of 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 (such as N, H, O etc.), and the weight percent sum of each component is absolutely;
(3) weight percent of 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 (such as N, H, O etc.), and the weight percent sum of each component is absolutely;
(4) weight percent of 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 (such as N, H, O etc.), and the weight percent sum of each component is absolutely;
(5) weight percent of 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 (such as N, H, O etc.), and the weight percent sum of each component is absolutely;
(6) weight percent of 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 (such 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 implement according to following steps:
(1) batching: carry out charge calculation by each the constituent content requirement of Ti80 titanium alloy reference material, take by weighing 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 the 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 ℃, density is 4.51g/cm
3The fusing point of metallic aluminium is 600 ℃, and density is 2.70g/cm
3The fusing point of metal molybdenum is 2610 ℃, and density is 10.2g/cm
32468 ℃ of the fusing points of metal niobium, density is 8.57g/cm
3The fusing point of nonmetal silicon is 1410 ℃, 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, produce easily 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 the matrix metal titanium to carry out melting as raw material, can improve the 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, and be reasonably combined, and the particle of master alloy and pure metal should be as far as possible tiny, is beneficial to the even distribution of master alloy in electrode, improves simultaneously electrode block intensity.Guarantee that master alloy and metal titanium melt synchronously when melting, avoid improper in the fusion process to fall piece, overcome the alloying element dilution segregation that causes therefrom.
(2) electrode block compacting: the present invention adopts the method for titanium sponge and master alloy monolithic electrode batch mixing, and is even in order to make chemical ingredients before the electrode pressing piece, and it is mixed to adopt rotary mixer that titanium sponge and various alloy addition are carried out homogenizing.For preventing that some granularities are less in the electrode pressing process master alloy and pure metal additive are scattered in mold bottom, first an amount of titanium sponge is layered on mold bottom, mixture with titanium sponge and master alloy places mould again, adopts 2000 tons of pressing machine electrode pressings, obtains specification and is
Electrode.
(3) electrode welding: grid for welding in the vacuum argon filling case, a plurality of electrodes that the upper step obtains are put into the welding case successively, when vacuum tightness is evacuated to 1.33x10
-1During Pa, be filled with purity and be not less than 99.95% argon gas, with the plasma weldering a plurality of electrodes are welded into the electrode group that length is 150 ± 5cm, straight behind the assurance 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 that welds is put into vaccum consumable electrode electric arc furnace carry out melting.With the vacuum degree control in the stove at 6.65x10
-2Pa ~ 1.33x10
-2In the Pa scope, melting vacuum tightness is high, be conducive to reduce the content of obnoxious flavour O, N, H in the burner hearth, the come-up of gas and discharge when being conducive to melting of metal simultaneously, can reach gas and non-metallic inclusion in effective removal metal, accurately the control chemical composition reduces the purposes such as alloying element oxidization burning loss.But too high vacuum tightness can cause again the element that saturated vapour pressure is higher in the alloy (normally low melting point element) volatilization more serious, makes component uniformity wayward.Control melting voltage is 28 ~ 36V, the melting electric current is 3500～5000A, less melting electric current can make the molten bath be in than melting under the tranquility, the disturbance that effectively prevents the molten bath is washed away the crystallization forward position, also is conducive to reduce speed of melting simultaneously, reduces pool depth and bath temperature gradient, keep the molten bath flat, for axial crystallization creates good conditions, improve the alloy homogeneity, reduce segregation.Suitably improve the melting electric current, the molten titanium amount of droplets is increased, particle diminishes, and its surface-area increases, and is conducive to the removal of nonmetallic impurity and gaseous impurities in the molten metal, improves the alloy refining effect.Therefore, during melting once, suitably large melting electric current should be adopted, when secondary, three meltings, less melting electric current should be adopted.The gap that guarantees 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 purpose of control metal liquid solidification rate, at the melting initial stage, consider the chill effect of heelpiece and crucible, the ingot solidification speed, speed of melting is also wanted corresponding quickening, set up rapidly the molten bath, and stable as early as possible, in the melting, later stage, pool depth to be controlled in the suitable scope, slowly reduce speed of melting, stop to put forearc 60～90min, speed of melting is subtracted, reduce successively molten bath thermal capacity, latent heat of solidification and pool depth, thereby the raising solidification rate suppresses the enrichment of the elements such as Fe, prevents segregation.By regulating at any time galvanic size of current in the crucible external coil, current control at 3000～15000A, is adjusted the intensity in stabilising arc magnetic field, guarantee that arc column is controlled, burning can be played sufficient stirring action to the molten bath, makes alloy compositions even, grain refining.The water coolant flow velocity of control crucible guarantees that leaving water temperature(LWT) at 40 ° below the C, imports and exports water temperature difference and be no more than 10 ° of C.Melting is treated to come out of the stove in ° C scope of ingot casting drop in temperature to 200 ~ 400 after finishing.
Vacuum consumable electrode electric arc skull melting secondary ingot casting, an ingot casting of arc melting is carried out machining, remove surface scale and top and emit notch portion, sampling check chemical composition and foreign matter content, when satisfying the component requirement, change in the vacuum consumable electrode electric arc skull crucible and carry out melting, vacuum tightness is evacuated to 1.33x10
-1Pa, regulating melting voltage after the starting the arc is that 30 ~ 35V, current density are 0.4 ~ 0.6A/cm
2The diameter ratio of electrode and crucible is 0.45 ~ 0.88, the gap of electrode and crucible inwall is the water coolant flow velocity of 30 ~ 40mm, control crucible, guarantee that leaving water temperature(LWT) is at 35 ° below the C, import and export water temperature difference and be no more than 10 ° of C, controlling the duration of pouring during cast graphite casting mould is 3 ~ 6s, the centrifugal pan rotating speed is 200 ~ 500r/min, pours to treat that ingot casting is cooled to 400 ° of C and comes out of the stove when following.
Three ingot castings of vaccum consumable electrode electric arc furnace melting, the secondary ingot casting of skull melting is carried out machining, remove surface scale and top and emit notch portion, sampling check chemical composition and foreign matter content, when satisfying the component requirement, change over to and carry out melting in the vaccum consumable electrode electric arc furnace, vacuum tightness is 6.65x10
-2～1.33x10
-2Pa, the 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, the water coolant flow velocity of control crucible guarantees that leaving water temperature(LWT) at 40 ° below the C, imports and exports water temperature difference and be no more than 10 ° of C.Melting is treated to come out of the stove in ° C scope of ingot casting drop in temperature to 200 ~ 400 after finishing.
(5) homogenizing annealing: adopt vacuum annealing furnace that ingot casting is carried out homogenizing annealing, the dendritic segregation that exists in the elimination ingot casting and regional segregation etc. make ingot casting component and homogeneous microstructure, and prevent ingot casting cracking in the forging process.Annealing temperature is: 950 ℃, soaking time is 10h, treats that drop in temperature to 200 ° comes out of the stove below the C.
(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 ℃ of coggings forges, adopt the 3T hammer to carry out repeatedly pier and pull out, adopt at last the 1T flat-die hammer that titanium alloy rod bar is changed and forge 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 ℃, and soaking time is 2h, treats that drop in temperature to 200 ° comes out of the stove below the C.
(8) processing bits shape sample: at first adopt machined into to remove the titanium alloy bar surface scale, then carry out the car bits, and to titanium bits pulverize, sieve, clean, dry, the operation such as bottling, finally obtain the bits shape titanium alloy reference material of 0.5mm * 1 ~ 2mm, can be used for the instruments such as ICP plasma spectrum.
(9) processing lumpy sample: adopt the 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 sees Table 1,
Concrete batching sees Table 2.
One, preparation Ti80-1
Concrete preparation process is as follows:
(1) batching: calculate by the 100kg that feeds intake, take by weighing 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 the 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 ℃, density is 4.51g/cm
3The fusing point of metallic aluminium is 600 ℃, and density is 2.70g/cm
3The fusing point of metal molybdenum is 2610 ℃, and density is 10.2g/cm
32468 ℃ of the fusing points of metal niobium, density is 8.57g/cm
3The fusing point of nonmetal silicon is 1410 ℃, 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, produce easily 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 the matrix metal titanium to carry out melting as raw material, can improve the 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, and be reasonably combined, and the particle of master alloy and pure metal should be as far as possible tiny, is beneficial to the even distribution of master alloy in electrode, improves simultaneously electrode block intensity.Guarantee that master alloy and metal titanium melt synchronously when melting, avoid improper in the fusion process to fall piece, overcome the alloying element dilution segregation that causes therefrom.
(2) electrode block compacting: the present invention adopts the method for titanium sponge and master alloy monolithic electrode batch mixing, and is even in order to make chemical ingredients before the electrode pressing piece, and it is mixed to adopt rotary mixer that titanium sponge and various alloy addition are carried out homogenizing.For preventing that some granularities are less in the electrode pressing process master alloy and pure metal additive are scattered in mold bottom, first an amount of titanium sponge is layered on mold bottom, mixture with titanium sponge and master alloy places mould again, adopts 2000 tons of pressing machine electrode pressings, obtains specification and is
Electrode.
(3) electrode welding: grid for welding in the vacuum argon filling case, a plurality of electrodes that the upper step obtains are put into the welding case successively, when vacuum tightness is evacuated to 1.33x10
-1During Pa, be filled with purity and be not less than 99.95% argon gas, with the plasma weldering a plurality of electrodes are welded into the electrode group that length is 150 ± 5cm, straight behind the assurance 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 that welds is put into vaccum consumable electrode electric arc furnace carry out melting.With the vacuum degree control in the stove at 6.65x10
-2Pa ~ 1.33x10
-2In the Pa scope, melting vacuum tightness is high, be conducive to reduce the content of obnoxious flavour O, N, H in the burner hearth, the come-up of gas and discharge when being conducive to melting of metal simultaneously, can reach gas and non-metallic inclusion in effective removal metal, accurately the control chemical composition reduces the purposes such as alloying element oxidization burning loss.But too high vacuum tightness can cause again the element that saturated vapour pressure is higher in the alloy (normally low melting point element) volatilization more serious, makes component uniformity wayward.Control melting voltage is 28 ~ 36V, the melting electric current is 3500～5000A, less melting electric current can make the molten bath be in than melting under the tranquility, the disturbance that effectively prevents the molten bath is washed away the crystallization forward position, also is conducive to reduce speed of melting simultaneously, reduces pool depth and bath temperature gradient, keep the molten bath flat, for axial crystallization creates good conditions, improve the alloy homogeneity, reduce segregation.Suitably improve the melting electric current, the molten titanium amount of droplets is increased, particle diminishes, and its surface-area increases, and is conducive to the removal of nonmetallic impurity and gaseous impurities in the molten metal, improves the alloy refining effect.Therefore, during melting once, suitably large melting electric current should be adopted, when secondary, three meltings, less melting electric current should be adopted.The gap that guarantees 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 purpose of control metal liquid solidification rate, at the melting initial stage, consider the chill effect of heelpiece and crucible, the ingot solidification speed, speed of melting is also wanted corresponding quickening, set up rapidly the molten bath, and stable as early as possible, in the melting, later stage, pool depth to be controlled in the suitable scope, slowly reduce speed of melting, stop to put forearc 60～90min, speed of melting is subtracted, reduce successively molten bath thermal capacity, latent heat of solidification and pool depth, thereby the raising solidification rate suppresses the enrichment of the elements such as Fe, prevents segregation.By regulating at any time galvanic size of current in the crucible external coil, current control at 3000～15000A, is adjusted the intensity in stabilising arc magnetic field, guarantee that arc column is controlled, burning can be played sufficient stirring action to the molten bath, makes alloy compositions even, grain refining.The water coolant flow velocity of control crucible guarantees that leaving water temperature(LWT) at 40 ° below the C, imports and exports water temperature difference and be no more than 10 ° of C.Melting is treated to come out of the stove in ° C scope of ingot casting drop in temperature to 200 ~ 400 after finishing.
Vacuum consumable electrode electric arc skull melting secondary ingot casting, an ingot casting of arc melting is carried out machining, remove surface scale and top and emit notch portion, sampling check chemical composition and foreign matter content, when satisfying the component requirement, change in the vacuum consumable electrode electric arc skull crucible and carry out melting, vacuum tightness is evacuated to 1.33x10
-1Pa, regulating melting voltage after the starting the arc is that 30 ~ 35V, current density are 0.4 ~ 0.6A/cm
2The diameter ratio of electrode and crucible is 0.45 ~ 0.88, the gap of electrode and crucible inwall is the water coolant flow velocity of 30 ~ 40mm, control crucible, guarantee that leaving water temperature(LWT) is at 35 ° below the C, import and export water temperature difference and be no more than 10 ° of C, controlling the duration of pouring during cast graphite casting mould is 3 ~ 6s, the centrifugal pan rotating speed is 200 ~ 500r/min, pours to treat that ingot casting is cooled to 400 ° of C and comes out of the stove when following.
Three ingot castings of vaccum consumable electrode electric arc furnace melting, the secondary ingot casting of skull melting is carried out machining, remove surface scale and top and emit notch portion, sampling check chemical composition and foreign matter content, when satisfying the component requirement, change over to and carry out melting in the vaccum consumable electrode electric arc furnace, vacuum tightness is 6.65x10
-2～1.33x10
-2Pa, the 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, the water coolant flow velocity of control crucible guarantees that leaving water temperature(LWT) at 40 ° below the C, imports and exports water temperature difference and be no more than 10 ° of C.Melting is treated to come out of the stove in ° C scope of ingot casting drop in temperature to 200 ~ 400 after finishing.
(5) homogenizing annealing: adopt vacuum annealing furnace that ingot casting is carried out homogenizing annealing, the dendritic segregation that exists in the elimination ingot casting and regional segregation etc. make ingot casting component and homogeneous microstructure, and prevent ingot casting cracking in the forging process.Annealing temperature is: 950 ℃, soaking time is 10h, treats that drop in temperature to 200 ° comes out of the stove below the C.
(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 ℃ of coggings forges, adopt the 3T hammer to carry out repeatedly pier and pull out, adopt at last the 1T flat-die hammer that titanium alloy rod bar is changed and forge 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 ℃, and soaking time is 2h, treats that drop in temperature to 200 ° comes out of the stove below the C.
(8) processing bits shape sample: at first adopt machined into to remove the titanium alloy bar surface scale, then carry out the car bits, and to titanium bits pulverize, sieve, clean, dry, the operation such as bottling, finally obtain the bits shape titanium alloy reference material of 0.5mm * 1 ~ 2mm, can be used for the instruments such as ICP plasma spectrum.
(9) processing lumpy sample: adopt the 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, and therefore, the reference material that embodiment is prepared carries out uniformity testing.According to GB/T15000 " standard model work guide rule " and YS/T409 " standard model technical specifications " regulation, stochastic sampling adopts one-way analysis of variance method (F method) to carry out uniformity testing.
The one-way analysis of variance method is in same heat (batch) number, randomly draws m sample, and each analyzes n time, and (general m＞15 n=3), namely are divided into m data set, and every group of data n is individual, obtain first the inner variance S of group
e 2With variance between laboratories S
A 2, compute statistics F value again is with the threshold value F of statistic F
0Make comparisons and judge: if F＜F
0, then 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:
f
e=m (n-1) ... the group internal degree of freedom
f
A=m-1 ... ... .. ... .. degree of freedom between organizing
Be x in the formula
IjI organizes the j time analytical data,
Be the mean value of i group data,
Population mean for whole data.
Respectively extract at random 20 reference material Ti80-1 ~ Ti80-6, test 3 times, calculate F value (seeing table 3 for details) according to following formula, with threshold value F for every
0Compare, all less than threshold value F
0, show that the Certified Reference Material Homogeneity that embodiment prepares is good.
Table 3 embodiment Ti80 titanium alloy Certified Reference Material Homogeneity
Definite value is analyzed: original value data is adopted 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, respectively organize data with the inspection of Cochran method again and whether wait precision, on inspection without the 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 cover reference material, select top condition to excite with ARL4460 type Photoelectric Spectrometer and gather its light intensity, with standard value and light intensity drawing curve.The contact ratio of working curve all (is seeing table 4 for details) more than 0.99, can satisfy the spectroscopic analysis needs fully.
The working curve contact ratio of the reference material of table 4 embodiment of the invention preparation
| Element | Al | Nb | Zr | Mo | Fe | Si | C |
| Ti80 | 0.993 | 0.995 | 0.993 | 0.991 | 0.995 | 0.995 | 0.992 |
Claims (3)
1. 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.
2. Ti80 titanium alloy reference material as claimed in claim 1 is characterized in that, is comprised 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.
3. the preparation method of Ti80 titanium alloy reference material as claimed in claim 1 or 2 is characterized in that, may further comprise the 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 each the constituent content requirement of titanium alloy reference material, and take by weighing 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 some granularities are less in the electrode pressing process master alloy and pure metal additive are scattered in mold bottom, first an amount of titanium sponge is layered on mold bottom, mixture with titanium sponge and master alloy places mould to suppress in the lump again, realizes the even distribution of alloying element in consumable electrode;
(3) electrode welding: the electrode that suppresses is put into the welding case successively, when vacuum tightness is evacuated to 1.33x10
-1During Pa, be filled with argon gas, with the plasma weldering electrode be welded into the electrode group;
(4) melting: the electrode group is put into vaccum consumable electrode electric arc furnace carry out the melting first time; With an ingot casting as second electrode, at vacuum consumable electrode electric arc skull melting secondary ingot, then with the secondary ingot as three sub-electrodes, at three ingots of vaccum consumable electrode electric arc furnace melting as the finished product ingot casting;
(5) homogenizing annealing: ingot casting is carried out homogenizing annealing, and the dendritic segregation that exists in the elimination ingot casting and regional segregation etc. make ingot casting component and microstructure homogenization, prevent ingot casting cracking in the 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: at first adopt machined into to remove the titanium alloy bar surface scale, then carry out the car bits, and to titanium bits pulverize, sieve, clean, dry, the operation such as bottling, finally obtain the bits shape titanium alloy reference material of 0.5mm * 1 ~ 2mm, can be used for the instruments such as ICP plasma spectrum;
(9) processing lumpy sample: adopt the machined into titanium alloy bar extremely
Obtain block titanium alloy reference material, can be used for the instruments such as photoelectric direct reading spectrometry.
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