阅读说明：本技术 一种钽合金、铌合金管坯的制备方法 (Preparation method of tantalum alloy and niobium alloy tube blank ) 是由 李积贤 张九海 杜领会 李小平 宿康宁 谢新普 于 2020-06-18 设计创作，主要内容包括：本申请提供了一种钽合金、铌合金管坯的制备方法,包括以下步骤：在钽合金或铌合金铸锭中心加工直径为Φ40～Φ120mm的通孔,得到空心圆锭；对空心圆锭进行室温锻造或者加热锻造,得到直径为Φ90～Φ150mm的粗管坯；对粗管坯进行表面酸洗、热处理、机加、修料,得到成品钽合金或铌合金管坯成品。该方法中锻造工艺可以采用室温或者加热锻造的方式,使得锻造成材后的管坯表面质量好,后期处理简单,成品率高；同时,锻造加工可以实现对部分强度高、塑性差的材料管坯的制备。本申请中提供的钽合金、铌合金管坯的制备方法,能够获得表面缺陷、缩尾缺陷少的管坯表面,可以有效控制缺陷的产生,提高材料利用率。(The application provides a preparation method of a tantalum alloy and niobium alloy tube blank, which comprises the following steps: processing a through hole with the diameter of phi 40-phi 120mm in the center of a tantalum alloy or niobium alloy ingot to obtain a hollow round ingot; carrying out room-temperature forging or heating forging on the hollow round ingot to obtain a thick tube blank with the diameter phi of 90-phi 150 mm; and (3) carrying out surface acid washing, heat treatment, machining and material repairing on the rough pipe blank to obtain a finished product of the tantalum alloy or niobium alloy pipe blank. In the method, the forging process can adopt a room temperature or heating forging mode, so that the surface quality of the forged pipe blank is good, the post-treatment is simple, and the yield is high; meanwhile, forging can realize the preparation of a material pipe blank with high strength and poor plasticity in part. The preparation method of the tantalum alloy tube blank and the niobium alloy tube blank can obtain the tube blank surface with few surface defects and tail shrinkage defects, can effectively control the generation of the defects, and improves the material utilization rate.)

1. A preparation method of a tantalum alloy and niobium alloy tube blank is characterized by comprising the following steps:

processing a through hole with the diameter of phi 40-phi 120mm in the center of a tantalum alloy or niobium alloy ingot to obtain a hollow round ingot;

carrying out room-temperature forging or heating forging on the hollow round ingot to obtain a thick tube blank with the diameter phi of 90-phi 150 mm;

and carrying out surface pickling, heat treatment, machining and material repairing on the rough tube blank to obtain a finished product of the tantalum alloy or niobium alloy tube blank.

2. A method for preparing a tantalum alloy and niobium alloy tube blank according to claim 1, wherein the step of machining a through hole with the diameter phi of 40-120 mm in the center of the tantalum alloy or niobium alloy ingot comprises the step of drilling a hole in the center of the tantalum alloy or niobium alloy ingot by adopting a linear cutting or machining mode.

3. A method for preparing a tantalum alloy tube blank and a niobium alloy tube blank as claimed in claim 1, wherein the method comprises the step of performing heat treatment on the hollow round ingot at 800-.

4. A method for preparing a tantalum alloy and niobium alloy tube blank according to claim 1, wherein before the heat-treated hollow round ingot is subjected to room temperature forging or heating forging, the method comprises the steps of selecting room temperature forging or heating forging according to the plasticity of the hollow round ingot material, forging pure metal at room temperature and heating forging alloy.

5. A method for producing a tantalum alloy and niobium alloy tube blank according to claim 4, wherein said heating forging comprises:

and (3) loading the steel bar into the through hole, reserving a gap of not less than 1mm between the steel bar and the through hole, forging at the temperature of 350-1300 ℃ for 10-150min, and taking out the steel bar after forging.

6. A method for preparing a tantalum alloy and niobium alloy tube blank according to claim 1, wherein the acid solution in the acid pickling is an acidic mixed solution with a volume ratio of nitric acid to hydrofluoric acid of 40: 1-3.

7. A method for preparing a tantalum alloy and niobium alloy tube blank according to claim 1, wherein the tantalum alloy comprises the following components in percentage by mass:

0.001 to 42 percent of niobium, 0.001 to 13.5 percent of tungsten, 0.001 to 1.2 percent of zirconium, 0.001 to 1.1 percent of hafnium, and the balance of tantalum and impurity components.

8. A method for manufacturing a tube blank of tantalum alloy and niobium alloy according to claim 7, wherein the impurity components comprise metal elements of iron, silicon, titanium, molybdenum, nickel and aluminum and gas elements of carbon, nitrogen, oxygen and hydrogen.

9. A method for preparing a tantalum alloy and niobium alloy tube blank according to claim 1, wherein the niobium alloy comprises the following components in percentage by mass:

0.001-58% of tantalum, 0.001-5.5% of tungsten, 0.001-1.2% of zirconium, 0.001-2.3% of molybdenum, and the balance of niobium and impurity elements.

10. A method for manufacturing a tube blank of tantalum alloy and niobium alloy according to claim 9, wherein the impurity elements comprise metal elements of iron, silicon, titanium, molybdenum, nickel and aluminum and gas elements of carbon, nitrogen, oxygen and hydrogen.

Technical Field

The application relates to the technical field of alloy pipe blank processing, in particular to a preparation method of a tantalum alloy and niobium alloy pipe blank.

Background

The tantalum, niobium and alloys thereof have good high-temperature corrosion resistance and good thermal expansion coefficient. Tantalum, niobium and their alloy pipes are used as main materials for chemical corrosion prevention, aerospace, semiconductors, electric light sources and the like, and have been widely applied to the manufacture of acid guns, acid liquor conveying equipment, high-pressure sodium lamps and missiles.

At present, the production process of tube blanks for tantalum-niobium and tantalum-niobium alloy tubes is mainly an extrusion method, namely a mode of pushing an ingot into a mold with a hole through extrusion equipment and performing plastic deformation to obtain a blank with a smaller size. However, the extrusion method needs heating, so that the energy consumption is high, the material is greatly deformed due to insufficient lubrication, the produced tube blank has the defects of wrinkles and peeling on the surface, the material consumption in post-treatment is high, and the yield is low; and the extrusion method is difficult to realize the preparation of the tube blank for materials with high part strength and poor plasticity.

Disclosure of Invention

The application provides a preparation method of a tantalum alloy and niobium alloy tube blank, which aims to solve the problems of high energy consumption, wrinkle and peeling defects on the surface of the produced tube blank and the like of the traditional extrusion method adopted by the tube blank for the alloy tube.

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

a preparation method of tantalum alloy and niobium alloy tube blanks comprises the following steps:

processing a through hole with the diameter of phi 40-phi 120mm in the center of a tantalum alloy or niobium alloy ingot to obtain a hollow round ingot;

carrying out room-temperature forging or heating forging on the hollow round ingot to obtain a thick tube blank with the diameter phi of 90-phi 150 mm;

and carrying out surface pickling, heat treatment, machining and material repairing on the rough tube blank to obtain a finished product of the tantalum alloy or niobium alloy tube blank.

Optionally, the step of machining a through hole with the diameter phi of 40-120 mm in the center of the tantalum alloy or niobium alloy ingot comprises the step of drilling a hole in the center of the tantalum alloy or niobium alloy ingot in a linear cutting or machining mode.

Optionally, before the hollow round ingot is forged at room temperature or heated to obtain a rough tube blank with the diameter of phi 90-phi 150mm, the method further comprises the step of performing heat treatment on the hollow round ingot, wherein the heat treatment condition is that the temperature is 1450 ℃ at 800-phi for 30-150 min.

Optionally, before performing room-temperature forging or heating forging on the hollow round ingot after heat treatment, the method includes selecting room-temperature forging or heating forging according to the plasticity of the hollow round ingot material, forging pure metal at room temperature, and heating and forging alloy.

Optionally, the heating forging comprises:

and (3) loading the steel bar into the through hole, reserving a gap of not less than 1mm between the steel bar and the through hole, forging at the temperature of 350-1300 ℃ for 10-150min, and taking out the steel bar after forging.

Optionally, the acid solution in the acid washing is an acidic mixed solution with a volume ratio of nitric acid to hydrofluoric acid of 40: 1-3.

Optionally, the tantalum alloy consists of the following components in percentage by mass:

0.001 to 42 percent of niobium, 0.001 to 13.5 percent of tungsten, 0.001 to 1.2 percent of zirconium, 0.001 to 1.1 percent of hafnium, and the balance of tantalum and impurity components.

Optionally, the impurity component includes metal elements of iron, silicon, titanium, molybdenum, nickel and aluminum, and gas elements of carbon, nitrogen, oxygen and hydrogen.

Optionally, the niobium alloy consists of the following components in percentage by mass:

0.001-58% of tantalum, 0.001-5.5% of tungsten, 0.001-1.2% of zirconium, 0.001-2.3% of molybdenum, and the balance of niobium and impurity elements.

Optionally, the impurity elements include metal elements of iron, silicon, titanium, molybdenum, nickel and aluminum, and gas elements of carbon, nitrogen, oxygen and hydrogen.

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

the application provides a preparation method of a tantalum alloy and niobium alloy tube blank, which comprises the following steps: processing a through hole with the diameter of phi 40-phi 120mm in the center of a tantalum alloy or niobium alloy ingot to obtain a hollow round ingot; carrying out room-temperature forging or heating forging on the hollow round ingot to obtain a thick tube blank with the diameter phi of 90-phi 150 mm; and (3) carrying out surface acid washing, heat treatment, machining and material repairing on the rough pipe blank to obtain a finished product of the tantalum alloy or niobium alloy pipe blank. In the method, the forging process can adopt a room temperature or heating forging mode, so that the surface quality of the forged pipe blank is good, the post-treatment is simple, and the yield is high; meanwhile, forging can realize the preparation of a material pipe blank with high strength and poor plasticity in part. The preparation method of the tantalum alloy tube blank and the niobium alloy tube blank can obtain the tube blank surface with few surface defects and tail shrinkage defects, can effectively control the generation of the defects, and improves the material utilization rate.

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 flowchart of a method for manufacturing a tantalum alloy tube blank and a niobium alloy tube blank according to an embodiment of the present application.

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.

Referring to fig. 1, fig. 1 is a flowchart of a method for manufacturing a tantalum alloy and niobium alloy tube blank according to an embodiment of the present disclosure, and as shown in the drawing, the method for manufacturing a tantalum alloy and niobium alloy tube blank according to the embodiment includes the following steps:

s1: and processing a through hole with the diameter of phi 40-phi 120mm in the center of the tantalum alloy or niobium alloy ingot to obtain a hollow round ingot.

S2: and carrying out room-temperature forging or heating forging on the hollow round ingot to obtain a rough pipe blank with the diameter phi of 90-phi 150 mm.

S3: and carrying out surface pickling, heat treatment, machining and material repairing on the rough tube blank to obtain a finished product of the tantalum alloy or niobium alloy tube blank.

According to the traditional extrusion method for producing the tube blank, a large amount of grooves and peeling defects are generated on the inner surface and the outer surface of the tube blank in the extrusion mode, and tail shrinkage defects are generated and need to be removed later, so that the material utilization rate is reduced. The technical scheme in the application can obtain good surface, and surface defect, tail-shrinking defect are few, can effectively control the production of defect, improve material utilization. In the method, the forging process can adopt a room temperature or heating forging mode, so that the surface quality of the forged pipe blank is good, the post-treatment is simple, and the yield is high; meanwhile, forging can realize the preparation of a material pipe blank with high strength and poor plasticity in part. The preparation method of the tantalum alloy tube blank and the niobium alloy tube blank can obtain the tube blank surface with few surface defects and tail shrinkage defects, can effectively control the generation of the defects, and improves the material utilization rate.

As an embodiment, the step of machining the through hole with the diameter of phi 40-phi 120mm in the center of the tantalum alloy or niobium alloy ingot comprises the step of drilling the center of the tantalum alloy or niobium alloy ingot by adopting a linear cutting or machining mode.

In the embodiment of the application, before the hollow round ingot is forged at room temperature or heated to obtain a thick tube blank with the diameter of phi 90-phi 150mm, the heat treatment is carried out on the hollow round ingot. After the hollow round ingot is subjected to heat treatment, the cast structure can be optimized, the hardness of the material is reduced, the subsequent forging resistance is reduced, and the plasticity of the material is improved. The heat treatment condition is that the temperature is 800-1450 ℃, and the time is 30-150 min.

As an embodiment, before the room-temperature forging or the heating forging is performed on the hollow round ingot after the heat treatment, the room-temperature forging or the heating forging is selected according to the plasticity of the hollow round ingot, the forging is performed under the condition of pure metal room temperature, and the alloy heating forging is performed.

If the steel bar is heated and forged, the operation mode is that a steel bar is arranged in the through hole, a gap with the diameter not less than 1mm is reserved between the steel bar and the through hole, the inner diameter size and the inner surface quality are ensured, the steel bar is forged under the conditions that the temperature is 350-1300 ℃ and the heat preservation time is 10-150min, and the steel bar is taken out after the forging is finished.

And after the forging is finished, carrying out surface acid washing, heat treatment, machining and material repairing on the rough tube blank to obtain a finished product of the tantalum alloy or niobium alloy tube blank. The acid liquid in the acid cleaning adopts an acid mixed liquid with the volume ratio of nitric acid to hydrofluoric acid being 40:1-3, and oil stains and foreign matters on the surface are removed. The acid-washed rough pipe blank is subjected to heat treatment and machining to remove the surface defects of the inner hole and the outer hole, and the acid-washed rough pipe blank is used for producing tantalum-niobium and alloy pipes thereof after partial defects are removed.

As an embodiment, the tantalum alloy comprises the following components in percentage by mass:

0.001-42% of niobium, 0.001-13.5% of tungsten, 0.001-1.2% of zirconium, 0.001-1.1% of hafnium and the balance of tantalum and impurity components, wherein the impurity components comprise metal elements of iron, silicon, titanium, molybdenum, nickel and aluminum and gas elements of carbon, nitrogen, oxygen and hydrogen.

As an embodiment, the niobium alloy comprises the following components in percentage by mass:

0.001-58% of tantalum, 0.001-5.5% of tungsten, 0.001-1.2% of zirconium, 0.001-2.3% of molybdenum, and the balance of niobium and impurity elements, wherein the impurity elements comprise metal elements of iron, silicon, titanium, molybdenum, nickel and aluminum and body elements of carbon, nitrogen, oxygen and hydrogen.

In the embodiment, the production of the tantalum-niobium and alloy pipe blanks thereof is realized by adopting a forging method, and the tantalum-niobium and alloy pipe blanks thereof with the outer circle diameter phi of 90-phi 150mm and the inner hole diameter phi of 40-phi 120mm can be processed on the premise of simple process and no need of manufacturing and heating. The method adopts a forging method to process the outer diameter phi of 90-phi 150mm and the inner hole diameter phi of 40-phi 120mm, and controls the effective deformation of the material in the forging process by controlling the forging reduction and the striking speed, thereby reducing the generation of surface defects; the inner diameter of the tube blank is ensured to keep the required size by lining the steel rod, and the quality of the inner surface can also be ensured.

The ingot for tantalum alloy or niobium alloy raw tube in the present example has a large diameter of 150mm or more, preferably 150mm to 285 mm.

In order to make the technical solution in the present application more clear to those skilled in the art, this embodiment also provides a specific operation mode, whether it is tantalum alloy or niobium alloy, which is implemented by the following steps:

s10: drilling holes on the tantalum-niobium and alloy cast ingots with the aperture ofObtaining the hollow cast ingot.

S11: and (4) carrying out homogenization heat treatment on the hollow ingot obtained in the step S10: carrying out heat treatment on the cast ingot with the prepared holes, wherein the heat treatment temperature is different according to different alloys, the temperature range is 700-; such as: tantalum 2.5 tungsten alloy, the homogenization heat treatment system is as follows: 1250-; the niobium-zirconium alloy comprises the following homogenized heat treatment system: the temperature is kept at 1100-1200 ℃ for 60-150 min.

S12: and (4) preheating the hollow cast ingot obtained in the step (S11), wherein preheating treatment is performed on a part of materials with high strength and poor plasticity, such as tantalum alloy or niobium alloy, before forging, the preheating can be performed by adopting a box-type resistance furnace or a medium-frequency induction furnace, the preheating temperature is 350-800 ℃, the heat preservation time is 10-150min, the tantalum is 10 tungsten, the preheating temperature is 800 ℃, and the heat preservation time is 60-150 min. And (3) carrying out heat preservation on the niobium-zirconium alloy for 60-150min at the preheating temperature of 410 ℃. The material with low strength and good plasticity, such as pure tantalum metal or niobium metal, can be directly forged.

S13: and (5) penetrating the hollow ingot obtained in the step (S12) into a steel bar which is coated with a lubricant in advance, wherein the diameter of the steel bar is smaller than that of the inner hole of the ingot. Repeatedly striking the outer circular die or directly striking the outer surface of the cast ingot, and timely rotating the outer circular die or the cast ingot to ensure that the shape of the forging material is nearly circular or round all the time. Eventually reaching the desired outer diameter dimension. And after the forging is finished, removing the steel bar.

S14: the pipe blank obtained in step S13 is pickled and heat-treated. Removing grease and impurities by acid washing, and eliminating processing stress by heat treatment.

S15: and (4) machining and repairing the tube blank obtained in the step (S14). The defects of the outer surface of the tube blank are removed through a handheld grinder, and the defects of the inner surface of the tube blank are removed through boring and turning.

S16: and (5) transferring the tube blank obtained in the step S15 to tube rolling production.

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.