阅读说明：本技术 一种铌锆合金粉末及其制备方法 (Niobium-zirconium alloy powder and preparation method thereof ) 是由 白掌军 黄云红 聂全新 牟东 陈飞 王强 颉维平 于 2020-06-29 设计创作，主要内容包括：本申请提供的铌锆合金粉末及其制备方法,以氢化后的铌粉和锆粉为原料制备混合粉末,控制混合粉末中铌元素与锆元素的含量比以及氧碳比,充分混料后再装入球磨机中进行机械合金化处理,之后将粉末压制成型,在高温真空下分段烧结,之后将合金条氢化处理,对氢化处理后的合金条采用球磨机进行破碎磨筛制粉,在一定的温度下将粉末的氢气脱除,合金粉末经除杂后处理后,制备出满足产品要求的铌锆合金粉末。该方法中由于原料均采用氢化铌粉和氢化锆粉,在制备混合粉末时能够充分混合且元素含量易控制,避免了采用纯铌与纯锆金属通过高温熔炼的方式进行合金化过程中,由于合金化的过程是熔融扩散完成的,扩散过程缓慢,存在的合金元素分布不均匀问题。(The application provides niobium-zirconium alloy powder and a preparation method thereof, hydrogenated niobium powder and zirconium powder are used as raw materials to prepare mixed powder, the content ratio and the oxygen-carbon ratio of niobium elements and zirconium elements in the mixed powder are controlled, the mixed powder is fully mixed and then is put into a ball mill to be subjected to mechanical alloying treatment, then the powder is pressed and molded, segmented sintering is carried out under high-temperature vacuum, then alloy strips are subjected to hydrogenation treatment, the alloy strips subjected to hydrogenation treatment are crushed, ground and sieved by the ball mill to prepare powder, hydrogen of the powder is removed at a certain temperature, and the niobium-zirconium alloy powder meeting the product requirements is prepared after impurity removal and treatment of the alloy powder. In the method, because the raw materials are the niobium hydride powder and the zirconium hydride powder, the niobium hydride powder and the zirconium hydride powder can be fully mixed when preparing the mixed powder, the element content is easy to control, and the problems that the alloying process is completed by melting and diffusion in the process of alloying pure niobium and pure zirconium metal in a high-temperature smelting mode, the diffusion process is slow, and the distribution of alloy elements is not uniform are solved.)

1. The niobium-zirconium alloy powder is characterized by comprising the following components in percentage by weight: 9 to 11 percent of zirconium, less than or equal to 0.01 percent of carbon, less than or equal to 0.15 percent of oxygen, less than or equal to 0.01 percent of iron, less than or equal to 0.01 percent of silicon, and the balance of niobium and other inevitable impurities.

2. A method for the preparation of a niobium zirconium alloy powder, wherein the method is used for the preparation of a niobium zirconium alloy powder according to claim 1, the method comprising the steps of:

fully mixing niobium hydride powder and zirconium hydride powder with the purity of more than 99.5 percent according to a certain proportion to prepare mixed niobium-zirconium powder, controlling the content ratio of niobium element to zirconium element in the mixed niobium-zirconium powder to be 8.1-10, controlling the oxygen-carbon ratio to be 6-10, and sieving the niobium hydride powder and the zirconium hydride powder by a 200-mesh sieve with the sieving rate of more than or equal to 98 percent;

putting the mixed niobium-zirconium powder after fully mixing into a ball mill for mechanical alloying treatment, and after the treatment is finished, pressing and forming the powder to obtain a formed niobium-zirconium alloy strip;

carrying out staged sintering alloying reaction on the niobium-zirconium alloy strip under high-temperature vacuum by adopting a temperature programming mode, and carrying out hydrogenation treatment on the niobium-zirconium alloy strip after sintering is finished to obtain a hydrogenated niobium-zirconium alloy strip;

crushing, grinding and screening the niobium-zirconium alloy strip subjected to hydrogenation treatment by using a ball mill pulverizer to prepare powder, and performing dehydrogenation treatment after the powder preparation is finished to obtain alloy powder subjected to dehydrogenation treatment;

and removing impurities from the alloy powder after dehydrogenation treatment, obtaining a finished product after treatment, and screening and grading the finished product.

3. The method of claim 2, wherein the mixed niobium zirconium powder has a ratio of niobium content to zirconium content of 9 and an oxygen to carbon content of 8.

4. The method for preparing niobium-zirconium alloy powder according to claim 2, wherein the mixed niobium-zirconium powder after being fully mixed is put into a ball mill for mechanical alloying treatment, the ball mill adopts a stirring ball mill, the ball milling medium is quenched steel balls, the ball milling time is 40-60h, the ball-to-material ratio is 10-15, and the loading ratio is 1: 2, the ball milling atmosphere is argon, the argon filling pressure of the ball milling tank is 0.02Mpa, and the ball milling speed is 125r/min-200 r/min.

5. The method of claim 2, wherein the step of compacting the niobium zirconium alloy powder after the step of treating is performed to obtain a shaped niobium zirconium alloy strip comprises: and under the condition that the forming pressure is more than or equal to 200MPa, pressing and forming the powder in an isostatic pressing or mould pressing mode to prepare the niobium-zirconium alloy strip.

6. The method for preparing niobium-zirconium alloy powder according to claim 2, wherein the step of crushing, grinding and screening the hydrogenated niobium-zirconium alloy strip by using a ball mill pulverizer comprises the steps of: adopting a stirring ball milling crusher, wherein quenching steel balls are used as a ball milling medium, the ball milling time is 20-30h, the ball material ratio is 10-15, and the filling ratio is 1: 2, the ball milling atmosphere is argon, the argon filling pressure of a ball milling tank is 0.02Mpa, and the ball milling speed is 125r/min-200 r/min.

7. The method for preparing niobium zirconium alloy powder according to claim 2, wherein the alloy powder after dehydrogenation is subjected to impurity removal post-treatment, and the impurity removal post-treatment comprises acid washing and water washing;

the pickling solution comprises hydrochloric acid with the mass fraction of 37%, nitric acid with the mass fraction of 65% and hydrofluoric acid with the mass fraction of 40%, wherein the volume ratio of the hydrochloric acid to the nitric acid to the hydrofluoric acid is 10%: 6.5%: 0.3 percent, and the pickling time is 1 to 3 hours;

the water washing includes rinsing the powder with deionized water until the pH of the alloy powder is neutral.

8. The method of claim 7, wherein the washed powder is dried in a vacuum oven at a vacuum level greater than 5 × 10^-2Pa, the drying temperature is 130-150 ℃, and the drying time is 7-10 h.

Technical Field

The application relates to the technical field of metallurgical materials, in particular to niobium-zirconium alloy powder and a preparation method thereof.

Background

The niobium-zirconium alloy is an alloy in which metal zirconium is added to metal niobium. The strength of the alloy can be improved after the zirconium is added into the niobium, the plasticity and the processing performance of the alloy can not be influenced, and the oxidation resistance and the alkali metal corrosion resistance of the alloy can be improved by the zirconium. The niobium-zirconium alloy is a functional niobium alloy proposed by commercial European users, is mainly used for the production and processing of magnetron sputtering targets, and can be used for the vapor phase coating of materials as the magnetron sputtering targets.

In the melting and casting manufacturing method of niobium-zirconium alloy, a method of melting and casting refractory metal and lower melting point metal into an alloy ingot by using an electron beam furnace and a vacuum consumable arc furnace is usually involved, and the conventional method is to alloy pure niobium and pure zirconium metal by a high-temperature melting method, but the alloying process of the preparation method is completed by melting and diffusion, the diffusion process is slow, and the problem of uneven distribution of alloy elements exists.

In the traditional technology, the preparation method of the niobium-zirconium alloy comprises the steps of pressing 89.5-90.5% of hydrogenated-dehydrogenated niobium powder into an electrode, purifying the electrode, and smelting the electrode into a niobium ingot in a vacuum consumable arc furnace; removing impurities from 9.5-10.5% atomic level sponge zirconium, cleaning, vacuum drying, purifying, forming into ingots, forging, hot rolling and cold rolling to form zirconium plates; then, shearing the zirconium plate into zirconium strips with the same length as the niobium ingot, tightly attaching the zirconium strips to the niobium ingot, and welding the zirconium strips and the niobium ingot together in a vacuum argon-filled welding box to prepare a niobium-zirconium composite ingot; and finally melting the niobium-zirconium composite ingot into an electrode, and cooling the electrode after twice melting to obtain the niobium-zirconium alloy. However, the niobium-zirconium alloy prepared by the smelting method cannot solve the problem of uneven distribution of the alloy elements, and the powder metallurgy method is an effective method for effectively solving the problem of uneven distribution of the alloy elements, so that the alloy powder is prepared by alloying the niobium-zirconium alloy by the smelting method and then by adopting the hydrogenation dehydrogenation method in the prior art, but the method still has the inherent problem of uneven distribution of the zirconium element, so that the problem of uneven distribution of the alloy elements cannot be completely solved.

Disclosure of Invention

The application provides niobium-zirconium alloy powder and a preparation method thereof, which aim to solve the problem that the inherent zirconium element is not uniformly distributed in the traditional method of preparing niobium-zirconium alloy powder by alloying the powder by a smelting method and then adopting a hydrogenation dehydrogenation mode.

The technical scheme adopted by the application for solving the technical problems is as follows:

niobium-zirconium alloy powder consisting of the following constituents in percentage by weight: 9 to 11 percent of zirconium, less than or equal to 0.01 percent of carbon, less than or equal to 0.15 percent of oxygen, less than or equal to 0.01 percent of iron, less than or equal to 0.01 percent of silicon, and the balance of niobium and other inevitable impurities.

A method for the preparation of a niobium zirconium alloy powder, said method being used for the preparation of the niobium zirconium alloy powder as described above, said method comprising the steps of:

fully mixing niobium hydride powder and zirconium hydride powder with the purity of more than 99.5 percent according to a certain proportion to prepare mixed niobium-zirconium powder, controlling the content ratio of niobium element to zirconium element in the mixed niobium-zirconium powder to be 8.1-10, controlling the oxygen-carbon ratio to be 6-10, and sieving the niobium hydride powder and the zirconium hydride powder by a 200-mesh sieve with the sieving rate of more than or equal to 98 percent;

putting the mixed niobium-zirconium powder after fully mixing into a ball mill for mechanical alloying treatment, and after the treatment is finished, pressing and forming the powder to obtain a formed niobium-zirconium alloy strip;

carrying out staged sintering alloying reaction on the niobium-zirconium alloy strip under high-temperature vacuum by adopting a temperature programming mode, and carrying out hydrogenation treatment on the niobium-zirconium alloy strip after sintering is finished to obtain a hydrogenated niobium-zirconium alloy strip;

crushing, grinding and screening the niobium-zirconium alloy strip subjected to hydrogenation treatment by using a ball mill pulverizer to prepare powder, and performing dehydrogenation treatment after the powder preparation is finished to obtain alloy powder subjected to dehydrogenation treatment;

and removing impurities from the alloy powder after dehydrogenation treatment, obtaining a finished product after treatment, and screening and grading the finished product.

Optionally, the ratio of the niobium element content to the zirconium element content in the mixed niobium-zirconium powder is 9, and the ratio of the oxygen-carbon content is 8.

Optionally, the mixed niobium-zirconium powder after being fully mixed is put into a ball mill for mechanical alloying treatment, the ball mill adopts a stirring ball mill, the ball milling medium is quenching steel balls, the ball milling time is 40-60 hours, the ball-material ratio is 10-15, and the filling ratio is 1: 2, the ball milling atmosphere is argon, the argon filling pressure of the ball milling tank is 0.02Mpa, and the ball milling speed is 125r/min-200 r/min.

Optionally, after the treatment, the powder is pressed and molded to obtain a molded niobium-zirconium alloy strip, including: and under the condition that the forming pressure is more than or equal to 200MPa, pressing and forming the powder in an isostatic pressing or mould pressing mode to prepare the niobium-zirconium alloy strip.

Optionally, the niobium-zirconium alloy strip after hydrogenation treatment is crushed, milled and sieved by a ball mill pulverizer to prepare powder, which includes: adopting a stirring ball milling crusher, wherein quenching steel balls are used as a ball milling medium, the ball milling time is 20-30h, the ball material ratio is 10-15, and the filling ratio is 1: 2, the ball milling atmosphere is argon, the argon filling pressure of a ball milling tank is 0.02Mpa, and the ball milling speed is 125r/min-200 r/min.

Optionally, in the impurity removal post-treatment of the alloy powder after dehydrogenation treatment, the impurity removal post-treatment includes acid washing and water washing;

the pickling solution comprises hydrochloric acid with the mass fraction of 37%, nitric acid with the mass fraction of 65% and hydrofluoric acid with the mass fraction of 40%, wherein the volume ratio of the hydrochloric acid to the nitric acid to the hydrofluoric acid is 10%: 6.5%: 0.3 percent, and the pickling time is 1 to 3 hours;

the water washing includes rinsing the powder with deionized water until the pH of the alloy powder is neutral.

Optionally, drying the alloy powder after washing in a vacuum oven with the vacuum degree of the oven being more than 5 × 10^-2Pa, the drying temperature is 130-150 ℃, and the drying time is 7-10 h.

The technical scheme provided by the application comprises the following beneficial technical effects:

the application provides a niobium-zirconium alloy powder and a preparation method thereof, niobium hydride powder and zirconium hydride powder are used as raw materials to prepare mixed powder, the content ratio and the oxygen-carbon ratio of niobium element and zirconium element in the mixed powder are controlled, the mixed powder is fully mixed and then is put into a ball mill to be subjected to mechanical alloying treatment, then the powder is pressed and molded, the powder is sintered in sections under high-temperature vacuum, then alloy strips are subjected to hydrogenation treatment, the alloy strips subjected to hydrogenation treatment are crushed, ground and screened by the ball mill to prepare powder, hydrogen of the powder is removed at a certain temperature, and the alloy powder is subjected to impurity removal post-treatment and then is screened and classified according to product requirements. By adopting the preparation method of the niobium-zirconium alloy powder, because the niobium hydride powder and the zirconium hydride powder are adopted as raw materials, the niobium hydride powder and the zirconium hydride powder can be uniformly mixed when the mixed powder is prepared, the element content is easy to control, and the problem of nonuniform distribution of alloy elements due to the fact that the alloying process is completed by melting and diffusion and the diffusion process is slow in the alloying process of pure niobium and pure zirconium metal in a high-temperature smelting mode is avoided; meanwhile, according to the technical scheme, the powder formed by pressing is subjected to high-temperature sectional sintering, so that gas impurities can be more fully released in the sintering process, the prepared niobium-zirconium alloy powder is uniform in distribution of zirconium elements and low in content of gas impurity elements, and the niobium-zirconium alloy powder is suitable for thermal spraying repair of failed targets or is directly prepared into niobium-zirconium alloy targets by adopting a hot pressing mode.

Drawings

In order to more clearly explain the technical solution of the present application, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious to those skilled in the art that other drawings can be obtained according to the drawings without any creative effort.

FIG. 1 is a flow chart of a method for preparing niobium zirconium alloy powder according to an embodiment of the present disclosure;

FIG. 2 is the surface morphology of sintered niobium-zirconium alloy block;

FIG. 3 is a graph showing the distribution of the surface of the zirconium element in FIG. 2;

FIG. 4 is a diagram showing the surface distribution of the element niobium in FIG. 2.

Detailed Description

In order to make the technical solutions in the present application better understood by those skilled in the art, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application; it is to be understood that the embodiments described are only a few embodiments of the present application and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.

In the traditional preparation method of the niobium-zirconium alloy, niobium ingots and zirconium plates are used as raw materials, a series of forging procedures are carried out to prepare niobium-zirconium composite ingots, then the niobium-zirconium composite ingots are melted into electrodes, and the electrodes are melted twice and then cooled to obtain the niobium-zirconium alloy.

The application provides a preparation method of niobium-zirconium alloy powder, the principle is that niobium hydride powder and zirconium hydride powder are adopted as raw materials, physical alloying treatment is firstly carried out, then niobium-zirconium alloy strips are prepared through compression molding and staged sintering alloying reaction, finally crushing, grinding and screening are carried out through a ball-milling pulverizer, after the whole process, the raw materials can be fully fused with each other, the prepared niobium-zirconium alloy strips are uniform in texture, and then the niobium-zirconium alloy powder with uniform texture is obtained through ball milling.

The preparation method of the niobium-zirconium alloy powder provided by the embodiment of the application comprises the following steps:

s1: fully mixing niobium hydride powder and zirconium hydride powder with the purity of more than 99.5 percent according to a certain proportion to prepare mixed niobium-zirconium powder, controlling the content ratio of niobium element to zirconium element in the mixed niobium-zirconium powder to be 8.1-10, controlling the oxygen-carbon ratio to be 6-10, and sieving the niobium hydride powder and the zirconium hydride powder by a 200-mesh sieve with the sieving rate of more than or equal to 98 percent;

s2: putting the fully mixed niobium-zirconium powder into a ball mill for mechanical alloying treatment, namely a physical alloying treatment stage, and after the treatment is finished, pressing and forming the powder to obtain a formed niobium-zirconium alloy strip;

s3: carrying out staged sintering alloying reaction on the niobium-zirconium alloy strip under high-temperature vacuum by adopting a temperature programming mode, and carrying out hydrogenation treatment on the niobium-zirconium alloy strip after sintering is finished to obtain a hydrogenated niobium-zirconium alloy strip;

s4: crushing, grinding and screening the niobium-zirconium alloy strip subjected to hydrogenation treatment by using a ball mill pulverizer to prepare powder, and performing dehydrogenation treatment after the powder preparation is finished to obtain alloy powder subjected to dehydrogenation treatment;

s5: and removing impurities from the alloy powder after dehydrogenation treatment, obtaining a finished product after treatment, and screening and grading the finished product.

In the above preparation method, the niobium powder and zirconium powder after hydrogenation treatment are used as raw materials, and because the niobium powder and zirconium powder have high reactivity and are in a powder state, the niobium powder and zirconium powder have low safety performance. Meanwhile, when the niobium-zirconium alloy strip is subjected to staged sintering alloying reaction under high-temperature vacuum, the niobium-zirconium alloy strip is subjected to sintering treatment in stages by adopting a temperature programming mode, so that gas impurities can be more fully released in the sintering process, and the prepared niobium-zirconium alloy powder is uniform in zirconium element distribution and low in gas impurity element content.

As an embodiment, the ratio of the content of the niobium element to the content of the zirconium element in the mixed niobium-zirconium powder is preferably 9; the ratio of the oxygen to carbon contents is preferably 8.

As an embodiment, the method comprises the steps of loading the fully mixed niobium-zirconium powder into a ball mill for mechanical alloying treatment, wherein the ball mill adopts an agitating ball mill, the ball milling medium is quenching steel balls, the ball milling time is 40-60h, the ball-to-material ratio is 10-15, and the loading ratio is 1: 2, the ball milling atmosphere is argon, the argon filling pressure of the ball milling tank is 0.02Mpa, and the ball milling speed is 125r/min-200 r/min.

And after the treatment is finished, the powder is pressed and molded to obtain a molded niobium-zirconium alloy strip, which comprises the following steps: and (3) under the condition that the forming pressure is more than or equal to 200MPa, pressing and forming the powder in an isostatic pressing or mould pressing mode to prepare the niobium-zirconium alloy strip or rod.

Adopt ball-milling rubbing crusher to carry out crushing mill sieve powder process to niobium zirconium alloy strip after the hydrotreating includes: adopting a stirring ball milling crusher, wherein quenching steel balls are used as a ball milling medium, the ball milling time is 20-30h, the ball material ratio is 10-15, and the filling ratio is 1: 2, the ball milling atmosphere is argon, the argon filling pressure of a ball milling tank is 0.02Mpa, and the ball milling speed is 125r/min-200 r/min.

The alloy powder after dehydrogenation treatment is subjected to impurity removal post-treatment comprising acid washing and water washing;

the pickling solution comprises hydrochloric acid with the mass fraction of 37%, nitric acid with the mass fraction of 65% and hydrofluoric acid with the mass fraction of 40%, wherein the volume ratio of the hydrochloric acid to the nitric acid to the hydrofluoric acid is 10%: 6.5%: 0.3 percent, and the pickling time is 1 to 3 hours;

the water washing includes rinsing the powder with deionized water until the pH of the alloy powder is neutral.

Drying the alloy powder after washing in a vacuum oven with the vacuum degree of the oven being more than 5 × 10^-2Pa, drying temperature of 130The temperature is between 150 ℃ below zero and the drying time is between 7 and 10 hours.

The finished niobium-zirconium alloy powder meeting the following conditions can be obtained by the preparation method. Namely, the finished niobium-zirconium alloy powder consists of the following components in percentage by weight: 9 to 11 percent of zirconium, less than or equal to 0.01 percent of carbon, less than or equal to 0.15 percent of oxygen, less than or equal to 0.01 percent of iron, less than or equal to 0.01 percent of silicon, and the balance of niobium and other inevitable impurities.

In order to make the technical solutions in the present application more clear to those skilled in the art, this embodiment further provides a specific experimental example, which is as follows:

s101: preparing a powder material: firstly, adding zirconium hydride powder into the niobium hydride powder, wherein C is required to be less than or equal to 0.01 percent in the zirconium hydride powder, Zr is required to be 8.1-10, the mass ratio of Nb to Zr is preferably 9, the granularity of all the powder is preferably below 200 meshes, the sieving rate is more than or equal to 98 percent, the purity is more than 99.5 percent, the C is less than or equal to 0.05 percent, O is less than or equal to 0.3 percent, and the O/C ratio is between 6 and 10.

S102: ball milling and alloying: preliminarily mixing the prepared materials in a V-shaped mixing system for 8-10h, then putting the materials into a stirring ball mill for ball milling, wherein the ball milling medium is quenching steel balls, the ball milling time is 40-60h, the ball-material ratio is 10-15, and the filling ratio is 1: 2, the ball milling atmosphere is argon, the ball milling tank is filled with argon to 0.02Mpa, and the ball milling speed is 125r/min-200 r/min.

S103: pressing materials: and pressing the ball-milled materials into strips or rods by adopting an isostatic pressing or mould pressing mode, wherein the forming pressure is more than or equal to 200 MPa.

S104: vacuum and high-temperature sintering: the pressed materials are loaded into a high-temperature vacuum furnace sintering furnace, a radiation type electric heating mode is adopted, the quantity of the loaded materials is less than or equal to 500Kg at one time, and the temperature rise condition is shown in table 1. The vacuum high-temperature sintering process is a gradual alloying sintering process, so that impurity gas in the formed alloy strip can be fully released.

TABLE 1 sintering conditions

S105: and (3) hydrogenation treatment:

after the materials are sintered at high temperature in vacuum, blocky alloy blanks are prepared, the blocky materials are directly put into a hydrogenation degassing furnace for treatment, and the hydrogenation treatment process conditions are shown in table 2. In this embodiment, X-ray energy spectrum analysis (EDS) is performed on the sintered block, fig. 2 shows the surface morphology of the sintered niobium-zirconium alloy block, and fig. 3 and 4 are respectively a graph of the surface distribution of zirconium element and niobium element in fig. 2; as can be seen in fig. 2, the sintered alloy block had a relatively flat surface and no porosity due to impurities, indicating that the alloy blocks prepared by the method of the present application had a uniform texture. Fig. 3 and 4 show the distribution of the zirconium element and the niobium element in fig. 2, respectively, and it can be seen that the distribution of either the zirconium element or the niobium element in the alloy block is relatively uniform, which illustrates the alloy material prepared by the method provided in the present application, which is free from the problem of non-uniform distribution of the alloy elements in the finished product.

FIG. 4 is a diagram showing the surface distribution of the element niobium in FIG. 2.

TABLE 2 hydrotreating conditions

S106: powder preparation and dehydrogenation treatment:

stirring and ball milling to prepare powder, wherein a ball milling medium is quenching steel balls, the ball milling time is 20-30h, the ball material ratio is 10-15, the filling ratio is 1/2, the ball milling atmosphere is argon, a ball milling tank is filled with argon to 0.02Mpa, the ball milling speed is 125r/min-200r/min, the alloy powder after being milled and sieved is filled into a heat-resistant stainless steel disc and is filled into a hydrogenation degassing furnace, and the dehydrogenation process is continuously evacuated to maintain negative pressure. The dehydrogenation process is shown in Table 3, and the alloy powder analysis results are shown in Table 4.

TABLE 3 dehydrogenation conditions

Parameter (. degree. C.)	Time of temperature rise (h)	Incubation time (h)
			Room temperature-450-	2-6	2-4
450-600-700-800	2-4	To vacuum of not less than 60Pa

TABLE 4NbZr alloy powder analysis results in percentage by mass

Element(s)

C

O

N

H

Ta

Fe

Cr

Si

Zr

1#

0.0063

0.136

0.027

0.001

<0.01

<0.01

<0.01

<0.01

9.73

2#

0.0033

0.119

0.02

0.001

<0.01

<0.01

<0.01

<0.01

9.62

The mass percentages of the elements in table 4 above satisfy the ranges of the zirconium content 9% -11%, the carbon content less than or equal to 0.01%, the oxygen content less than or equal to 0.15%, the iron content less than or equal to 0.01%, the silicon content less than or equal to 0.01%, and the balance of the elements of niobium and other unavoidable impurities in the finished niobium-zirconium alloy powder. As can be shown from the data in table 4 above, the niobium-zirconium alloy powder satisfying the content requirement of the specific element can be obtained by the preparation method in the present application.

To sum up, the niobium-zirconium alloy powder and the preparation method thereof provided by the embodiment of the application are characterized in that firstly, zirconium hydride powder is added into niobium hydride powder, the content ratio of each element in the mixed powder is controlled, the mixed powder is fully mixed and then put into a ball mill for mechanical alloying treatment, then the powder is pressed and molded, sintering is carried out under high temperature and vacuum for further alloying, alloy strips are hydrogenated, a ball mill is adopted for crushing and grinding to prepare powder, hydrogen of the powder is removed at a certain temperature, the alloy powder is pickled, washed by water and dried, and finally, screening and grading are carried out according to the product requirements. By adopting the preparation method of the niobium-zirconium alloy powder in the embodiment, because the niobium hydride powder and the zirconium hydride powder are adopted as raw materials, the niobium hydride powder and the zirconium hydride powder can be uniformly mixed when the mixed powder is prepared, the element content is easy to control, and the problem of nonuniform distribution of alloy elements caused by slow diffusion process because the alloying process is completed by melting diffusion in the alloying process of pure niobium and pure zirconium metal by a high-temperature smelting mode is avoided; meanwhile, according to the technical scheme, the powder formed by pressing is subjected to high-temperature sectional sintering, so that gas impurities can be more fully released in the sintering process, the prepared niobium-zirconium alloy powder is uniform in distribution of zirconium elements and low in content of gas impurity elements, and the niobium-zirconium alloy powder is suitable for thermal spraying repair of failed targets or is directly prepared into niobium-zirconium alloy targets by adopting a hot pressing mode.

It is noted that relational terms such as "first" and "second," and the like, may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that an article or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.

The above description is merely exemplary of the present application and is presented to enable those skilled in the art to understand and practice the present application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

It will be understood that the present application is not limited to what has been described above and shown in the accompanying drawings, and that various modifications and changes can be made without departing from the scope thereof. The scope of the application is limited only by the appended claims.