CN110408815B - Low-elasticity-modulus and high-strength spinodal decomposition type Zr-Nb-Ti alloy material and preparation method thereof - Google Patents
Low-elasticity-modulus and high-strength spinodal decomposition type Zr-Nb-Ti alloy material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an AM decomposition type Zr-Nb-Ti alloy material with low elastic modulus and high strength and a preparation method thereof. The Zr-Nb-Ti alloy material comprises the following components in atomic percentage: 20-50%; nb: 15-45%; the balance being Zr. The preparation method comprises the following steps: preparing a titanium source, a niobium source and a zirconium source according to a designed proportion; the Zr-Nb-Ti alloy material has higher strength and low elastic modulus, wherein the strength can reach 1130.8 +/-8.5 MPa to the maximum, and the elastic modulus is kept between 40 and 50GPa and is close to the elastic modulus of a human body.
Description
Technical Field
The invention belongs to the technical field of medical zirconium alloy, and particularly relates to an amplitude modulation decomposition type Zr-Nb-Ti alloy material with low elastic modulus and high strength and a preparation method thereof.
Technical Field
In recent years, with the development of society and the improvement of human living standard, people have increasingly demanded safe and reliable biological graft materials, and thus extensive researchers have conducted intensive research on implantable biological hard tissue materials. To develop an alloy for a human implant, the alloy is first required to have excellent biocompatibility. The biocompatible alloy elements applied to biomedical metal materials at present mainly comprise Ti, Zr, Nb, Ta, Mo, Sn, Mg, Zn and the like. Secondly, such alloys need to have high strength and excellent corrosion resistance. On the basis, the alloy also needs to have a low elastic modulus so as to be matched with the elastic modulus (15-30 GPa) of human bones. If the elastic modulus of the implant is too high, a "stress shielding effect" will result, leading to premature failure or fracture of the implant, which ultimately has a serious impact on human health. Therefore, the mismatch of mechanical properties of the implant alloy materials is a problem to be solved.
Therefore, the design and development of safe and reliable human body transplantation metal materials must be based on good biocompatibility and biomechanical compatibility. In order to provide good biomechanical compatibility, the alloy should have high strength and low elastic modulus, i.e., high (. sigma.). degreeysThe value of/E). Currently, there are two main approaches to achieve this: first, the modulus of elasticity is reduced. The scholars at home and abroad design and prepare the low-elasticity-modulus alloy by optimizing the alloy components. In addition, another effective way to reduce the elastic modulus of the alloy is to introduce a pore structure into the alloy to prepare a porous alloy. For example, patent (CN 109847110a) provides a porous Ti-Nb-Zr composite artificial bone implant material, and a preparation method and application thereof, which can significantly reduce the elastic modulus of the alloy through the introduction of a large number of pores, but also greatly reduce the strength of the alloy. For compact alloy materials, the method for improving the alloy strength is mainly to refine grains or precipitate a fine second phase through thermomechanical treatment so as to achieve the purpose of fine-grain strengthening or second-phase strengthening. However, high elastic modulus phases such as alpha phase and omega phase are precipitated during the heat treatment of the alloy, so that the alloy shows high elastic modulus. Therefore, how to solve the contradiction between high strength and low elastic modulus has become a hot issue in this research field.
Spinodal decomposition refers to a homogeneous phase transition in which a solid solution is destabilized due to infinitesimal fluctuations in infinitesimal/non-local regions or decomposes into two phases with different components and the same structure. Thermodynamically, phase separation occurs in the alloy system when the second derivative of the Gibbs free energy as a function of composition is negative. Compared with the traditional phase change, when amplitude modulation decomposition occurs, nucleation is not generated, and fine two phases with different components and the same structure are quickly formed. The unique phase change mode of amplitude modulation decomposition enables the crystal to have a plurality of excellent performances compared with the traditional nucleation, growth and precipitation strengthening mode. The amplitude modulation structure is uniform, the corrosion resistance of the alloy is higher, and the over-aging or the grain growth cannot be generated in the normal aging process; excessive accumulation of dislocation does not occur in the amplitude modulation decomposition process, so that the sensitivity of crack generation can be reduced, and the crack propagation can be delayed. Therefore, it has become an effective means for toughening some engineering materials. More importantly, the amplitude modulation structure with small component difference and the same structure can ensure the low elastic modulus of the alloy and obviously improve the strength.
Disclosure of Invention
Aiming at the problem that the zirconium alloy in the prior art cannot realize low elastic modulus and high strength at the same time, the invention aims to provide an AM decomposition type Zr-Nb-Ti alloy material with low elastic modulus and high strength and a preparation method thereof.
In order to achieve the above object, the present invention adopts the following technical solutions. The invention relates to an AM decomposition type Zr-Nb-Ti alloy material with low elastic modulus and high strength, which comprises the following components in atomic percent: 20-50%; nb: 15-45%; the balance being Zr.
Aiming at the problem that the conventional zirconium alloy cannot realize low elastic modulus and high strength at the same time, the invention provides an amplitude modulation decomposition type zirconium alloy: a Zr-Nb-Ti alloy material having an spinodal decomposition region within the above composition range; the AM decomposition does not need nucleation, but quickly forms two phases with fine and uniform tissues, same crystal structures and different components. Therefore, the alloy can ensure low elastic modulus while improving the strength of the alloy.
In a preferable scheme, the Zr-Nb-Ti alloy material comprises the following components in atomic percentage: 30-35%; nb: 30-35%; the balance being Zr.
Within the preferred ranges above, spinodal decomposition must be present.
The invention relates to a preparation method of an AM decomposition type Zr-Nb-Ti alloy material with low elastic modulus and high strength, which comprises the following steps: preparing a titanium source, a niobium source and a zirconium source according to a designed proportion; smelting for multiple times to obtain a zirconium alloy ingot, carrying out suction casting on the zirconium alloy ingot to obtain a zirconium alloy rod, and sequentially carrying out solid solution treatment and aging treatment on the zirconium alloy rod to obtain the Zr-Nb-Ti alloy material.
According to the preparation method, the zirconium alloy ingot with prepared and uniform components is obtained through multiple times of smelting, however, the uniformity is further improved through suction casting, then the supersaturated solid solution of the zirconium alloy rod is obtained through solid solution treatment, and the material is subjected to homogeneous phase transformation through aging treatment to obtain the amplitude-modulated decomposition phase. The solid solution and aging treatment in the invention can not precipitate other phases with higher elastic modulus, such as alpha phase and omega phase, but do not need nucleation, and two phases with different components and the same structure are rapidly formed. Therefore, the over-aging or the grain growth is not generated in the normal aging process, but the amplitude modulation structure with small component difference and the same structure is adopted, so that the strength of the alloy can be obviously improved while the low elastic modulus is ensured.
Preferably, the titanium source is selected from titanium particles with the purity of not less than 99.99 percent; the niobium source is selected from niobium particles with a purity of not less than 99.99 percent, and the zirconium source is selected from zirconium particles with a purity of not less than 99.99 percent.
In the preferable scheme, the smelting current is 200-250A, the single-time smelting suspension time is 60-90 s, and the smelting times are more than or equal to 4 times. More preferably 6 times.
By carrying out multiple times of smelting in the process range, the zirconium alloy ingot with accurate and uniform components can be obtained.
In the actual operation process, smelting and suction casting are carried out in a vacuum electric arc smelting furnace.
The suction casting process can ensure better uniformity of the zirconium alloy, if cast ingots are directly adopted, dendritic materials still exist, so that the components of the material are not uniform, and in order to solve the non-uniformity, the time of solid solution treatment needs to be increased, so that crystal grains are enlarged, and the performance of the material is influenced.
In the preferable scheme, the temperature of the solution treatment is 850-950 ℃, and the heat preservation time is 1-10 h.
Preferably, the temperature of the solution treatment is 860-900 ℃, and the heat preservation time is 3-6 h.
Preferably, the solution treatment is performed in a vacuum environment.
In a preferred scheme, after the solution treatment and heat preservation are finished, the zirconium alloy bar is placed in ice brine for quenching.
In the invention, the solution treatment temperature has certain influence on the performance of the material, if the solution treatment is too high, the crystal grains can grow rapidly to influence the performance of the material, and if the solution treatment is too low, the solution time can be prolonged, and the rapid homogenization cannot be realized. In addition, rapid cooling quenching in ice brine can ensure that beta phase is retained, and if the cooling speed is too slow, alpha phase and omega phase with higher elastic modulus are separated out.
Preferably, the solution treatment comprises the following specific processes: sealing the zirconium alloy bar by adopting a vacuum quartz tube, putting the sealed zirconium alloy bar into a heat treatment furnace for solution treatment, taking out the zirconium alloy bar, and putting the zirconium alloy bar into ice brine for quenching.
In the actual operation process, after the solution treatment and heat preservation are finished, the vacuum quartz tube is taken out and quickly crushed, so that the bar falls into ice brine for quenching.
In the preferable scheme, the temperature of the aging treatment is 500-600 ℃, and the heat preservation time is 4-24 h.
Preferably, the temperature of the aging treatment is 500-560 ℃, and the heat preservation time is 4-14 h.
Preferably, the aging treatment is performed in a vacuum environment.
In the preferable scheme, after the aging treatment and heat preservation are finished, the zirconium alloy bar is placed in ice brine for cooling.
The aging treatment temperature has great influence on the performance of the material, if the aging temperature is out of the range of the invention, the AM decomposition phase can not be separated out, and meanwhile, the material needs to be cooled in ice brine, otherwise, the separated AM decomposition phase can not be reserved.
Preferably, the aging treatment process comprises the steps of sealing the zirconium alloy rod subjected to the solution treatment by adopting a vacuum quartz tube, placing the sealed zirconium alloy rod in a heat treatment furnace for aging treatment, taking out the zirconium alloy rod, and placing the zirconium alloy rod in ice brine for cooling.
In the actual operation process, after the aging treatment and heat preservation are completed, the vacuum quartz tube is taken out and quickly crushed, so that the bar falls into ice brine for cooling.
Has the advantages that:
the invention provides a zirconium alloy material with an amplitude-modulated decomposition phase for the first time, on one hand, the range of the components of the material with the amplitude-modulated decomposition phase is obtained through thermodynamic calculation and a large number of experiments, and simultaneously, the process is combined to ensure that the amplitude-modulated decomposition phase is formed in the preparation process of the material. The spinodal decomposition does not need nucleation, but quickly forms two phases with fine and uniform tissues, same crystal structures and different components. Therefore, the alloy material provided by the invention can ensure low elastic modulus while improving the alloy strength.
The zirconium alloy material obtained by the invention has higher strength and low elastic modulus, wherein the strength can reach 1130.8 +/-8.5 MPa at most, and the elastic modulus is kept between 40-50 GPa and is closer to the elastic modulus of a human body.
The zirconium alloy material obtained by the invention is a Zr-Nb-Ti ternary alloy material, compared with pure titanium, the zirconium alloy has the advantages of good ductility, wear resistance, lower magnetic susceptibility, harmonious elastic modulus and the like, and is expected to replace the titanium-based implant which is used more at present to become a novel bone substitute material in the next stage.
Drawings
FIG. 1 is an XRD pattern of samples at various stages in example 1;
FIG. 2 is a TEM bright field image and selected area diffraction pattern of the aged sample in example 1;
FIG. 3 is a graph of the compressive stress strain of the samples at various stages in example 1;
FIG. 4 is a TEM bright field image of the aged sample in example 2;
FIG. 5 is a plot of the compressive stress strain of the sample after aging treatment of example 2;
FIG. 6 is a TEM bright field image of the aged sample in example 3;
FIG. 7 is a plot of the compressive stress strain of the samples after aging treatment of example 3.
Detailed Description
The present invention will be described in further detail below with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
Example 1
(1) Weighing: weighing raw materials: the alloy is prepared from 30% of Ti, 30% of Nb and the balance of Zr according to the element atomic percentage, and high-purity titanium particles, high-purity niobium particles and high-purity zirconium particles are respectively weighed. The purities of the high-purity titanium particles, the high-purity niobium particles and the high-purity zirconium particles are not less than 99.99 percent.
(2) Smelting: and (2) putting the raw materials weighed in the step (1) into a vacuum arc melting furnace for melting, wherein the melting current is 220A, and the melting suspension time is 65 s. In order to improve the accuracy and uniformity of the components, the ingot needs to be repeatedly smelted for six times to obtain the ingot.
(3) Suction casting: and (3) putting the cast ingot obtained in the step (2) into a vacuum arc melting furnace for suction casting to obtain a zirconium alloy rod.
(4) And (3) regulating and controlling the microstructure: and (3) carrying out solution treatment on the suction-cast bar obtained in the step (3), carrying out solution treatment, namely sealing the bar obtained by suction casting by using a vacuum quartz tube, putting the bar into a tube type heat treatment furnace, heating to 900 ℃ and preserving heat for 3 hours, taking out the quartz tube and quickly crushing the quartz tube to enable the bar to fall into ice brine for quenching, carrying out aging treatment on a sample subjected to solution treatment, sealing the sample subjected to solution treatment by using the vacuum quartz tube, putting the sample into a tube type furnace, heating to 500 ℃ and preserving heat for 4 hours, taking out the quartz tube and quickly crushing the quartz tube to enable the bar to fall into the ice brine for cooling.
FIG. 1 is XRD patterns of samples of example 1 after solution treatment and solution aging, and it can be seen from FIG. 1 that the phases of the alloy after solution treatment and aging treatment are both beta-phase, but from the enlarged view, a side band peak appears after the alloy aging treatment, indicating that the alloy has an AM decomposition structure. FIG. 2 is a bright field image of transmission electron microscope of the sample treated with aging during solid solution, and a significant amplitude-modulated structure can be seen, wherein the size of the structure is in the nanometer level. As can be seen from the diffraction of the selected area of the sample after the solution and aging treatment in FIG. 2, obvious satellite diffraction spots exist. FIG. 2 shows that the samples aged in example 1 have amplitude-modulated decomposition phases. The samples at each stage in this example were subjected to a compression test, and the compressive stress strain curve is shown in FIG. 3. As can be seen from the curve, the compressive yield strength of the sample after the solution treatment is 795 +/-8.5 MPa, the elastic modulus is 40.8 +/-1.3 GPa, and the value is 0.019; the compressive yield strength of the sample after the solution and aging treatment is 1130.8 +/-8.5 MPa, the elastic modulus is 45.5 +/-2.8 GPa, the value is 0.025, and the value is obviously improved compared with that of the sample subjected to the solution treatment; it can be seen that the yield strength of the aged samples is significantly increased, while the elastic modulus remains in the lower range.
Example 2
(1) Weighing the following components: weighing raw materials: the alloy is prepared from 33% of Ti, 31% of Nb and the balance of Zr according to the element atomic percentage, and high-purity titanium particles, high-purity niobium particles and high-purity zirconium particles are respectively weighed. The purities of the high-purity titanium particles, the high-purity niobium particles and the high-purity zirconium particles are not less than 99.99 percent.
(2) Smelting: and (2) putting the raw materials weighed in the step (1) into a vacuum arc melting furnace for melting, wherein the melting current is 200A, and the melting suspension time is 90 s. In order to improve the accuracy and uniformity of the components, the ingot needs to be repeatedly smelted for six times to obtain the ingot.
(3) Suction casting: and (3) putting the cast ingot obtained in the step (2) into a vacuum arc melting furnace for suction casting to obtain a zirconium alloy rod.
(4) And (3) regulating and controlling the microstructure: and (3) carrying out solution treatment on the suction-cast bar obtained in the step (3), carrying out solution treatment, namely sealing the bar obtained by suction casting by using a vacuum quartz tube, putting the bar into a tube type heat treatment furnace, heating to 860 ℃ and preserving heat for 6 hours, taking out the quartz tube and quickly crushing the quartz tube to enable the bar to fall into ice brine for quenching, carrying out aging treatment on a sample subjected to solution treatment, carrying out aging treatment, namely sealing the sample subjected to solution treatment by using the vacuum quartz tube, putting the sample into a tube type furnace, heating to 560 ℃ and preserving heat for 14 hours, taking out the quartz tube and quickly crushing the quartz tube to enable the bar to fall into the ice brine for cooling.
The TEM bright field image after aging treatment of this example is shown in FIG. 4, which shows that AM-modulated structure exists, and the compressive stress strain curve of the sample after aging treatment is shown in FIG. 5, and it is clear from FIG. 5 that the compressive yield strength of the sample after aging treatment is 998.9 + -8.5 MPa, the elastic modulus is 46.3 + -2.1 GPa, and the value is 0.022.
Example 3
(1) Weighing the following components: weighing raw materials: the alloy is prepared from 30% of Ti, 30% of Nb and the balance of Zr according to the element atomic percentage, and high-purity titanium particles, high-purity niobium particles and high-purity zirconium particles are respectively weighed. The purities of the high-purity titanium particles, the high-purity niobium particles and the high-purity zirconium particles are not less than 99.99 percent.
(2) Smelting: and (2) putting the raw materials weighed in the step (1) into a vacuum arc melting furnace for melting, wherein the melting current is 230A, and the melting suspension time is 85 s. In order to improve the accuracy and uniformity of the components, the ingot needs to be repeatedly smelted for six times to obtain the ingot.
(3) Suction casting: and (3) putting the cast ingot obtained in the step (2) into a vacuum arc melting furnace for suction casting to obtain a zirconium alloy rod.
(4) And (3) regulating and controlling the microstructure: and (3) carrying out solution treatment on the suction-cast bar obtained in the step (3), carrying out solution treatment, namely sealing the bar obtained by suction casting by using a vacuum quartz tube, putting the bar into a tube type heat treatment furnace, heating to 950 ℃ for heat preservation for 2 hours, taking out the quartz tube, quickly crushing the quartz tube to enable the bar to fall into ice brine for quenching, carrying out aging treatment on a sample subjected to solution treatment, carrying out aging treatment, namely sealing the sample subjected to solution treatment by using the vacuum quartz tube, putting the sample into a tube type furnace, heating to 500 ℃ for heat preservation for 24 hours, taking out the quartz tube, quickly crushing the quartz tube to enable the bar to fall into the ice brine for cooling.
The TEM bright field image after aging treatment of this example is shown in FIG. 6, which shows that there is an AM decomposition phase, and the compressive stress strain curve of the sample after aging treatment is shown in FIG. 7, and it can be seen from FIG. 7 that the compressive yield of the sample after aging treatment is 899.6 + -8.5 MPa, the elastic modulus is 48.4 + -1.9 GPa, and the value is 0.018, and it is likely that the structure in the alloy grows coarse due to long-time heat preservation, which causes strength reduction, and thus the value is slightly reduced compared with the value of the solid solution treatment sample.
Comparative example 1
(1) Weighing: weighing raw materials: the alloy is prepared from 10% of Ti, 10% of Nb and the balance of Zr according to the element atomic percentage, and high-purity titanium particles, high-purity niobium particles and high-purity zirconium particles are respectively weighed. The purities of the high-purity titanium particles, the high-purity niobium particles and the high-purity zirconium particles are not less than 99.99 percent.
(2) Smelting: and (2) putting the raw materials weighed in the step (1) into a vacuum arc melting furnace for melting, wherein the melting current is 220A, and the melting suspension time is 65 s. In order to improve the accuracy and uniformity of the components, the ingot needs to be repeatedly smelted for six times to obtain the ingot.
(3) Suction casting: and (3) putting the cast ingot obtained in the step (2) into a vacuum arc melting furnace for suction casting to obtain a zirconium alloy rod.
(4) And (3) regulating and controlling the microstructure: and (3) carrying out solution treatment on the suction-cast bar obtained in the step (3), carrying out solution treatment, namely sealing the bar obtained by suction casting by using a vacuum quartz tube, putting the bar into a tube type heat treatment furnace, heating to 900 ℃ and preserving heat for 3 hours, taking out the quartz tube and quickly crushing the quartz tube to enable the bar to fall into ice brine for quenching, carrying out aging treatment on a sample subjected to solution treatment, sealing the sample subjected to solution treatment by using the vacuum quartz tube, putting the sample into a tube type furnace, heating to 500 ℃ and preserving heat for 4 hours, taking out the quartz tube and quickly crushing the quartz tube to enable the bar to fall into the ice brine for cooling.
The composition of the material in comparative example 1 is out of the corresponding range, so that the zirconium alloy material obtained after the solution treatment and the aging treatment has no spinodal decomposition phase, the compressive yield is 780.6 +/-5.5 MPa, the elastic modulus is 55.7 +/-2.3 GPa, and the value is 0.014
Comparative example 2
(1) Weighing: weighing raw materials: the alloy is prepared from 30% of Ti, 30% of Nb and the balance of Zr according to the element atomic percentage, and high-purity titanium particles, high-purity niobium particles and high-purity zirconium particles are respectively weighed. The purities of the high-purity titanium particles, the high-purity niobium particles and the high-purity zirconium particles are not less than 99.99 percent.
(2) Smelting: and (2) putting the raw materials weighed in the step (1) into a vacuum arc melting furnace for melting, wherein the melting current is 220A, and the melting suspension time is 65 s. In order to improve the accuracy and uniformity of the components, the ingot needs to be repeatedly smelted for six times to obtain the ingot.
(3) Suction casting: and (3) putting the cast ingot obtained in the step (2) into a vacuum arc melting furnace for suction casting to obtain a zirconium alloy rod.
(4) And (3) regulating and controlling the microstructure: and (3) carrying out solution treatment on the suction-cast bar obtained in the step (3), carrying out solution treatment, namely sealing the bar obtained by suction casting by using a vacuum quartz tube, putting the bar into a tube type heat treatment furnace, heating to 900 ℃ and preserving heat for 3 hours, taking out the quartz tube and quickly crushing the quartz tube to enable the bar to fall into ice brine for quenching, carrying out aging treatment on a sample subjected to solution treatment, sealing the sample subjected to solution treatment by using the vacuum quartz tube, putting the sample into a tube type furnace, heating to 400 ℃ and preserving heat for 4 hours, taking out the quartz tube and quickly crushing the quartz tube to enable the bar to fall into the ice brine for cooling.
In the comparative example 2, because the aging treatment is not carried out in the corresponding temperature range, the spinodal decomposition phase transformation can not occur, the zirconium alloy material obtained after the solid solution and the aging treatment has no spinodal decomposition phase, and the alpha phase and the omega phase with higher elastic modulus can be precipitated at lower temperature and the aging treatment is carried out, so that the elastic modulus is obviously improved. The compressive yield is 950.9 +/-7.3 MPa, the elastic modulus is 77.6 +/-1.2 GPa, and the value is 0.012
Comparative example 3
(1) Weighing: weighing raw materials: the alloy is prepared from 30% of Ti, 30% of Nb and the balance of Zr according to the element atomic percentage, and high-purity titanium particles, high-purity niobium particles and high-purity zirconium particles are respectively weighed. The purities of the high-purity titanium particles, the high-purity niobium particles and the high-purity zirconium particles are not less than 99.99 percent.
(2) Smelting: and (2) putting the raw materials weighed in the step (1) into a vacuum arc melting furnace for melting, wherein the melting current is 220A, and the melting suspension time is 65 s. In order to improve the accuracy and uniformity of the components, the ingot needs to be repeatedly smelted for six times to obtain the ingot.
(3) Suction casting: and (3) putting the cast ingot obtained in the step (2) into a vacuum arc melting furnace for suction casting to obtain a zirconium alloy rod.
(4) And (3) regulating and controlling the microstructure: and (3) carrying out solution treatment on the suction-cast bar obtained in the step (3), carrying out solution treatment, namely sealing the bar obtained by suction casting by using a vacuum quartz tube, putting the bar into a tube type heat treatment furnace, heating to 900 ℃ and preserving heat for 3 hours, taking out the quartz tube and quickly crushing the quartz tube to enable the bar to fall into ice brine for quenching, carrying out aging treatment on a sample subjected to solution treatment, carrying out aging treatment, namely sealing the sample subjected to solution treatment by using the vacuum quartz tube, putting the sample into a tube type furnace, heating to 500 ℃ and preserving heat for 4 hours, taking out the quartz tube and crushing the quartz tube to enable the bar to be cooled in the air.
In comparative example 3, the material was air-cooled after aging treatment, and the α phase and ω phase having higher elastic modulus were similarly precipitated during the air-cooling, but some spinodal decomposition phases were also retained in the material, so that the elastic modulus was not increased so much, and the material had a compressive yield of 966.9 ± 7.3MPa, an elastic modulus of 64.6 ± 1.2GPa and a value of 0.014.
Claims (4)
1. An AM decomposition type Zr-Nb-Ti alloy material with low elastic modulus and high strength is characterized in that: the alloy comprises the following components in atomic percentage: 30-35%; nb: 30-35%; the balance being Zr; the preparation method comprises the following steps: preparing a titanium source, a niobium source and a zirconium source according to a designed proportion; smelting for multiple times to obtain a zirconium alloy ingot, performing suction casting on the zirconium alloy ingot to obtain a zirconium alloy rod, and sequentially performing solid solution treatment and aging treatment on the zirconium alloy rod to obtain a Zr-Nb-Ti alloy material; the temperature of the solution treatment is 860-900 ℃, the heat preservation time is 3-6 hours, and after the solution treatment and the heat preservation are finished, the zirconium alloy bar is placed in ice brine for quenching; the temperature of the aging treatment is 500-600 ℃, and the heat preservation time is 4-24 h; and after the aging treatment and heat preservation are finished, putting the zirconium alloy bar into ice brine for cooling.
2. The method for preparing the Zr-Nb-Ti alloy material according to claim 1, wherein: the smelting current is 200-250A, the single-time smelting suspension time is 60-90 s, and the smelting times are more than or equal to 4 times.
3. The method for preparing the Zr-Nb-Ti alloy material according to claim 1, wherein: the specific process of the solution treatment is as follows: sealing the zirconium alloy bar by adopting a vacuum quartz tube, putting the sealed zirconium alloy bar into a heat treatment furnace for solution treatment, taking out the zirconium alloy bar, and putting the zirconium alloy bar into ice brine for quenching.
4. The method for preparing the Zr-Nb-Ti alloy material according to claim 1, wherein: the aging treatment process comprises the steps of sealing the zirconium alloy rod subjected to the solution treatment by adopting a vacuum quartz tube, placing the sealed zirconium alloy rod in a heat treatment furnace for aging treatment, taking out the zirconium alloy rod, and placing the zirconium alloy rod in ice brine for cooling.
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