CN112718909B - Short-flow preparation method of Ti-Al-Nb-Zr-Mo alloy seamless pipe - Google Patents

Short-flow preparation method of Ti-Al-Nb-Zr-Mo alloy seamless pipe Download PDF

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CN112718909B
CN112718909B CN202011323764.6A CN202011323764A CN112718909B CN 112718909 B CN112718909 B CN 112718909B CN 202011323764 A CN202011323764 A CN 202011323764A CN 112718909 B CN112718909 B CN 112718909B
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electron gun
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CN112718909A (en
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张玉勤
邓亚杰
黄海广
张浩泽
史亚鸣
李志敏
蒋业华
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Kunming University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C37/00Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
    • B21C37/06Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of tubes or metal hoses; Combined procedures for making tubes, e.g. for making multi-wall tubes
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/08Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for tubular bodies or pipes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/03Making non-ferrous alloys by melting using master alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C14/00Alloys based on titanium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • C22F1/183High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon

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  • Crystallography & Structural Chemistry (AREA)
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Abstract

本发明提供一种Ti‑Al‑Nb‑Zr‑Mo合金无缝管的短流程制备方法,其特征在于包括下列各步骤:1)备料,2)混料、压块,3)将料放于电子束枪EB炉内,4)真空熔炼得Ti‑Al‑Nb‑Zr‑Mo合金圆锭,5)在锭的两端打定心孔、送二辊斜轧机斜轧穿孔,6)送三辊连轧机连轧,7)加热定径得无缝管材,8)退火处理得Ti‑Al‑Nb‑Zr‑Mo合金无缝管。所获管材成分和组织均匀、高低密度夹杂少、高纯净,且工艺流程短,力学性能优于现有技术水平,综合成材率提高到85%左右,生产成本降低20~30%,具有明显的市场应用前景。

The invention provides a short-process preparation method for Ti-Al-Nb-Zr-Mo alloy seamless pipes, which is characterized by including the following steps: 1) preparing materials, 2) mixing and briquetting, 3) placing the materials in In the EB furnace of the electron beam gun, 4) Ti-Al-Nb-Zr-Mo alloy round ingot is obtained by vacuum melting, 5) centering holes are drilled at both ends of the ingot, and the two-roller cross-rolling machine is used for cross-rolling and perforation, 6) three-way Continuous rolling by roller rolling mill, 7) heating and sizing to obtain seamless pipes, 8) annealing treatment to obtain Ti‑Al‑Nb‑Zr‑Mo alloy seamless pipes. The obtained pipe has uniform composition and structure, few high and low density inclusions, high purity, short process flow, and better mechanical properties than the existing technical level. The comprehensive yield rate is increased to about 85%, and the production cost is reduced by 20 to 30%. It has obvious advantages. market application prospects.

Description

一种Ti-Al-Nb-Zr-Mo合金无缝管的短流程制备方法A short-process preparation method of Ti-Al-Nb-Zr-Mo alloy seamless pipe

技术领域Technical field

本发明涉及一种Ti-Al-Nb-Zr-Mo合金无缝管的短流程制备方法,属于有色金属轧制技术领域。The invention relates to a short-process preparation method of Ti-Al-Nb-Zr-Mo alloy seamless pipe and belongs to the technical field of non-ferrous metal rolling.

背景技术Background technique

Ti-6Al-3Nb-2Zr-1Mo钛合金(即TA31钛合金)不仅密度小、比强度高、塑性和耐蚀性好,而且还具有较高的断裂韧性、应力腐蚀断裂韧性、冲击韧性及可焊性等,特别是其突出的耐海水、耐海洋大气腐蚀性能,适用于油井管、通海管路系统、热交换器等部件的优异轻型结构材料。加工成无缝管材后,在海洋石油钻井平台、海洋工程装备、舰船、潜艇、深潜器及离岸设施等领域具有广阔的应用前景。Ti-6Al-3Nb-2Zr-1Mo titanium alloy (ie TA31 titanium alloy) not only has low density, high specific strength, good plasticity and corrosion resistance, but also has high fracture toughness, stress corrosion fracture toughness, impact toughness and Weldability, etc., especially its outstanding resistance to seawater and marine atmospheric corrosion, it is an excellent lightweight structural material suitable for oil well pipes, sea pipeline systems, heat exchangers and other components. After being processed into seamless pipes, it has broad application prospects in the fields of offshore oil drilling platforms, marine engineering equipment, ships, submarines, deep submersibles and offshore facilities.

现有技术制备TA31钛合金无缝管的工艺流程如下:先将海绵钛与合金原料进行混料后,压制、焊接成电极,经2~3次真空自耗电弧炉(VAR)熔炼成圆锭,然后将圆锭进行锻造加工后,再进行钻孔挤压或斜轧穿孔,最后再通过轧制、拉拔、旋压等工艺,制备出不同规格和用途的TA31钛合金无缝管。显然现有技术存在工艺流程长、综合成材率低、难以获得超长管材等不足,致使TA31钛合金无缝管的成本居高不下,应用受到极大限制。因此,有必要对现有技术加以改进。The process flow of preparing TA31 titanium alloy seamless pipes using the existing technology is as follows: first, mix titanium sponge with alloy raw materials, press and weld them into electrodes, and then smelt them into round shapes in a vacuum consumable electric arc furnace (VAR) 2 to 3 times. The round ingot is then forged, then drilled, extruded or cross-rolled and pierced, and finally through rolling, drawing, spinning and other processes to prepare TA31 titanium alloy seamless pipes of different specifications and uses. Obviously, the existing technology has shortcomings such as long process flow, low overall yield, and difficulty in obtaining ultra-long pipes. As a result, the cost of TA31 titanium alloy seamless pipes remains high and its application is greatly restricted. Therefore, it is necessary to improve the existing technology.

发明内容Contents of the invention

为克服现有TA31钛合金无缝管制备方法存在的上述不足,本发明提供一种Ti-Al-Nb-Zr-Mo合金无缝管的短流程制备方法,其特征在于包括下列各步骤:In order to overcome the above-mentioned shortcomings of the existing TA31 titanium alloy seamless pipe preparation method, the present invention provides a short-process preparation method of Ti-Al-Nb-Zr-Mo alloy seamless pipe, which is characterized by including the following steps:

(1)按下列质量比备料:(1) Prepare materials according to the following mass ratio:

铝铌合金 5.7~6.3wt.%Aluminum niobium alloy 5.7~6.3wt.%

铝豆 4.05~4.77wt.%Aluminum beans 4.05~4.77wt.%

海绵锆 1.5~2.5wt.%Zirconium sponge 1.5~2.5wt.%

铝钼合金 1.5~1.7wt.%Aluminum-molybdenum alloy 1.5~1.7wt.%

海绵钛 余量Titanium sponge balance

上述各组分总和为100 wt.%;The sum of the above components is 100 wt.%;

(2)将步骤(1)的备料进行混料后,取适量混合料作为散装料,其余混合料均压制成块后,于100~120℃烘干5~6h,随炉冷却,得压块料;(2) After mixing the materials prepared in step (1), take an appropriate amount of the mixture as bulk material, and press the remaining mixture into blocks, dry them at 100-120°C for 5-6 hours, and then cool them with the furnace to obtain briquettes. material;

(3)将步骤(2)的散装料铺放在装有七杆电子枪的EB炉的冷床内,再将步骤(2)的适量压块料放入该EB炉进料区;(3) Place the bulk material from step (2) in the cooling bed of an EB furnace equipped with seven electron guns, and then place an appropriate amount of briquettes from step (2) into the feeding area of the EB furnace;

(4)在真空度为1.8×10-3~3.5×10-3torr时,开启1~5号电子枪对冷床内的散装料进行熔炼,控制1~5号电子枪的电压均为29.5~30.5KV,电流均为3.3~4.3A,熔炼100~120min后,关闭电子枪,冷却20~40min后,将进料区的压块料推入熔炼区,同时开启1~7号电子枪继续熔炼,控制1~7号电子枪的电压均为29.5~30.5KV,1~2号电子枪电流为2.3~3.0A,3~4号电子枪电流为5.3~6A,5号电子枪电流为3.6~4.6A,6~7号电子枪电流为1.6~2.6A,同时保持12~18mm/min的拉锭速度,如此持续推料、熔化和拉锭,直至熔炼完成,之后冷却至80~100℃,将铸锭从结晶器中取出,冷却至室温,经表面扒皮打磨处理后,得Ti-Al-Nb-Zr-Mo合金圆锭;(4) When the vacuum degree is 1.8×10 -3 ~ 3.5×10 -3 torr, turn on the No. 1 to 5 electron guns to melt the bulk materials in the cooling bed, and control the voltage of the No. 1 to 5 electron guns to be 29.5 to 30.5 KV and current are both 3.3~4.3A. After 100~120 minutes of melting, turn off the electron gun. After cooling for 20~40 minutes, push the briquettes in the feed area into the smelting area. At the same time, turn on the electron guns No. 1 to 7 to continue melting. Control 1 ~The voltage of electron gun No. 7 is 29.5~30.5KV, the current of electron gun No. 1~2 is 2.3~3.0A, the current of electron gun No. 3~4 is 5.3~6A, the current of electron gun No. 5 is 3.6~4.6A, the current of electron gun No. 6~7 The current of the electron gun is 1.6~2.6A, while maintaining the ingot pulling speed of 12~18mm/min. Continue to push, melt and pull the ingot until the melting is completed. Then cool to 80~100℃ and take the ingot out of the crystallizer. , cooled to room temperature, and after surface peeling and polishing, a Ti-Al-Nb-Zr-Mo alloy ingot was obtained;

(5)在步骤(4)的Ti-Al-Nb-Zr-Mo合金圆锭两端打定心孔,送入加热炉加热至1100~1200℃,保温6~8h,送入二辊斜轧机上进行斜轧穿孔,并控制:总压下率为10~15%、顶前压下率为6~8%、椭圆度系数为1.11~1.18、穿孔速度为0.15~0.4m/s、温度为1080~1120℃,得穿孔管材;(5) Drill centering holes at both ends of the Ti-Al-Nb-Zr-Mo alloy round ingot in step (4), send it to the heating furnace, heat it to 1100~1200℃, keep it warm for 6~8 hours, and send it to the two-roller cross-rolling machine Perform cross-rolling and piercing on the top, and control: the total reduction rate is 10 to 15%, the reduction rate before the top is 6 to 8%, the ovality coefficient is 1.11 to 1.18, the piercing speed is 0.15 to 0.4m/s, and the temperature is 1080~1120℃, perforated pipe is required;

(6)将步骤(5)的穿孔管材送入三辊连轧机上进行连轧,并控制:总压下率为12~18%、椭圆度系数为1.05~1.15、穿孔速度为0.3~0.6m/s、温度为950~1000℃,得连轧管材;(6) Send the perforated pipe in step (5) to the three-roll rolling mill for continuous rolling, and control: the total reduction rate is 12 to 18%, the ovality coefficient is 1.05 to 1.15, and the perforation speed is 0.3 to 0.6m /s, the temperature is 950~1000℃, continuous rolling pipes are obtained;

(7)将步骤(6)的连轧管材送入加热炉中,加热至800~900℃后,送入定径机上进行定径,同时控制定径速率为0.4~0.8m/s,得无缝管材;(7) Send the continuously rolled pipe in step (6) into the heating furnace. After heating to 800~900°C, send it to the sizing machine for sizing. At the same time, control the sizing speed to 0.4~0.8m/s to obtain no sizing. seam pipes;

(8)将步骤(7)的无缝管材于850~900℃温度下退火2~3h,冷却至室温,得Ti-Al-Nb-Zr-Mo合金无缝管。(8) Anneal the seamless pipe in step (7) at 850 to 900°C for 2 to 3 hours, and then cool to room temperature to obtain a Ti-Al-Nb-Zr-Mo alloy seamless pipe.

所述步骤(5)中,Ti-Al-Nb-Zr-Mo合金圆锭加热完毕后,在进入斜轧机前需要在靠近顶头的一端涂抹玻璃粉润滑剂,同时在定心孔内塞入用锡纸包裹的玻璃粉润滑剂,以防止穿孔过程中管材内壁产生缺陷。In step (5), after the Ti-Al-Nb-Zr-Mo alloy ingot is heated, it is necessary to apply glass powder lubricant on the end near the head before entering the cross-rolling machine, and at the same time insert it into the centering hole. Glass powder lubricant wrapped in tin foil to prevent defects in the inner wall of the pipe during the perforation process.

所述步骤(8)的Ti-Al-Nb-Zr-Mo合金无缝管的成分为:Al:5.5 wt.%~6.5wt.%,Nb:2.5 wt.%~3.5wt.%,Zr:1.5 wt.%~2.5wt.%,Mo:0.6 wt.%~1.5wt.%,余量为Ti。The composition of the Ti-Al-Nb-Zr-Mo alloy seamless pipe in step (8) is: Al: 5.5 wt.%~6.5wt.%, Nb: 2.5 wt.%~3.5wt.%, Zr: 1.5 wt.%~2.5wt.%, Mo: 0.6 wt.%~1.5wt.%, the balance is Ti.

本发明具有下列优点和有益效果:采用上述技术方案获得的Ti-Al-Nb-Zr-Mo合金无缝管,其成分和组织均匀、高低密度夹杂少、高纯净,且在加工过程中无需进行锻造,直接将熔炼后的铸锭送入二辊斜轧穿孔机上制备出穿孔无缝管材,再经三辊连轧、定径、退火即得产品,不仅缩短了该钛合金无缝管的工艺流程,而且力学性能优于现有技术制备的水平。本发明工艺简单、操作方便,工艺流程短,使无缝管的综合成材率提高到85%左右,生产成本降低20~30%,具有明显的市场应用前景。The invention has the following advantages and beneficial effects: the Ti-Al-Nb-Zr-Mo alloy seamless pipe obtained by using the above technical solution has uniform composition and structure, few high and low density inclusions, high purity, and no need for processing during processing. Forging is carried out, and the smelted ingot is directly sent to a two-roller cross-rolling piercing machine to prepare a perforated seamless pipe. The product is then obtained by three-roller continuous rolling, sizing and annealing. This not only shortens the length of the titanium alloy seamless pipe. process, and its mechanical properties are superior to those prepared by existing technologies. The invention has simple process, convenient operation and short process flow, which increases the comprehensive yield of the seamless pipe to about 85%, reduces the production cost by 20 to 30%, and has obvious market application prospects.

附图说明Description of the drawings

图1为本发明工艺流程图。Figure 1 is a process flow diagram of the present invention.

图2为本发明实施例1所得管材金相组织图。Figure 2 is a diagram of the metallographic structure of the pipe obtained in Example 1 of the present invention.

图3为本发明实施例2所得管材金相组织图。Figure 3 is a diagram of the metallographic structure of the pipe obtained in Example 2 of the present invention.

图4为本发明实施例3所得管材金相组织图。Figure 4 is a diagram of the metallographic structure of the pipe obtained in Example 3 of the present invention.

图5为本发明实施例1所得管材的力学性能图。Figure 5 is a graph showing the mechanical properties of the pipe obtained in Example 1 of the present invention.

图6为本发明实施例2所得管材的力学性能图。Figure 6 is a graph showing the mechanical properties of the pipe obtained in Example 2 of the present invention.

图7为本发明实施例3所得管材的力学性能图。Figure 7 is a graph showing the mechanical properties of the pipe obtained in Example 3 of the present invention.

具体实施方式Detailed ways

下面结合具体实施方式对本发明作进一步详细说明,但本发明的保护范围并不限于所述内容。The present invention will be further described in detail below in conjunction with specific embodiments, but the protection scope of the present invention is not limited to the content described.

实施例1Example 1

一种Ti-Al-Nb-Zr-Mo合金无缝管的短流程制备方法,其特征在于包括下列各步骤:A short-process preparation method for Ti-Al-Nb-Zr-Mo alloy seamless pipes, which is characterized by including the following steps:

(1)按下列质量比备料:(1) Prepare materials according to the following mass ratio:

铝铌合金 5.7wt.%Aluminum niobium alloy 5.7wt.%

铝豆 4.05wt.%Aluminum beans 4.05wt.%

海绵锆 1.5wt.%Zirconium sponge 1.5wt.%

铝钼合金 1.5wt.%Aluminum-molybdenum alloy 1.5wt.%

海绵钛 87.25wt.%;Titanium sponge 87.25wt.%;

(2)将步骤(1)的备料进行混料后,取适量混合料作为散装料,其余混合料均压制成块后,于100℃烘干6h,随炉冷却,得压块料;(2) After mixing the materials prepared in step (1), take an appropriate amount of the mixture as bulk material, and press the rest of the mixture into blocks, dry them at 100°C for 6 hours, and cool them with the furnace to obtain briquettes;

(3)将步骤(2)的散装料铺放在装有七杆电子枪的EB炉的冷床内,再将步骤(2)的适量压块料放入该EB炉进料区;(3) Place the bulk material from step (2) in the cooling bed of an EB furnace equipped with seven electron guns, and then place an appropriate amount of briquettes from step (2) into the feeding area of the EB furnace;

(4)在真空度为1.8×10-3torr时,开启1~5号电子枪对冷床内的散装料进行熔炼,控制1~5号电子枪的电压均为29.5KV,电流均为3.3A,熔炼100min后,关闭电子枪,冷却20min后,将进料区的压块料推入熔炼区,同时开启1~7号电子枪继续熔炼,控制1~7号电子枪的电压均为29.5KV,1号~2号电子枪电流为2.3A,3号~4号电子枪电流为5.3A,5号电子枪电流为3.6A,6号~7号电子枪电流为1.6A,同时保持12mm/min的拉锭速度,如此持续推料、熔化和拉锭,直至熔炼完成,之后冷却至80℃,将铸锭从结晶器中取出,冷却至室温,经表面扒皮打磨处理后,得Ti-Al-Nb-Zr-Mo合金圆锭;(4) When the vacuum degree is 1.8×10 -3 torr, turn on the No. 1 to 5 electron guns to melt the bulk materials in the cooling bed. Control the voltage of the No. 1 to 5 electron guns to be 29.5KV and the current to be 3.3A. After 100 minutes of smelting, turn off the electron gun. After cooling for 20 minutes, push the briquettes in the feed area into the smelting area. At the same time, turn on the electron guns No. 1 to 7 to continue melting. Control the voltage of the electron guns No. 1 to 7 to be 29.5KV. The current of electron gun No. 2 is 2.3A, the current of electron gun No. 3 to No. 4 is 5.3A, the current of electron gun No. 5 is 3.6A, the current of electron gun No. 6 to No. 7 is 1.6A, while maintaining the ingot pulling speed of 12mm/min, and so on. Push, melt and pull the ingot until the smelting is completed, then cool to 80°C, take the ingot out of the crystallizer, cool to room temperature, and after surface peeling and polishing, the Ti-Al-Nb-Zr-Mo alloy round is obtained ingot;

(5)在步骤(4)的Ti-Al-Nb-Zr-Mo合金圆锭两端打定心孔后,送入加热炉加热至1100℃,保温8h,出炉后迅速在靠近顶头的一端涂抹适量玻璃粉润滑剂,同时在定心孔内塞入用锡纸包裹的玻璃粉润滑剂,以防止穿孔过程中管材内壁产生缺陷,之后送入二辊斜轧机上进行斜轧穿孔,并控制:总压下率为10%、顶前压下率为6%、椭圆度系数为1.11、穿孔速度为0.15m/s、温度为1080℃,得穿孔管材;(5) After drilling centering holes at both ends of the Ti-Al-Nb-Zr-Mo alloy round ingot in step (4), send it to the heating furnace to be heated to 1100°C and kept for 8 hours. After coming out of the furnace, quickly apply it on the end near the top. Appropriate amount of glass powder lubricant, and at the same time, stuff the glass powder lubricant wrapped with tin foil into the centering hole to prevent defects in the inner wall of the pipe during the perforation process, and then send it to the two-roller cross-rolling machine for cross-rolling and perforation, and control: The perforated pipe is obtained with a reduction rate of 10%, a reduction rate before top of 6%, an ellipticity coefficient of 1.11, a perforation speed of 0.15m/s, and a temperature of 1080°C;

(6)将步骤(5)的穿孔管材送入三辊连轧机上进行连轧,并控制:总压下率为12%、椭圆度系数为1.05、穿孔速度为0.3m/s、温度为950℃,得连轧管材;(6) Send the perforated pipe in step (5) to the three-roll rolling mill for continuous rolling, and control: the total reduction rate is 12%, the ovality coefficient is 1.05, the perforation speed is 0.3m/s, and the temperature is 950 ℃, continuous rolling pipes;

(7)将步骤(6)的连轧管材送入加热炉中,加热至800℃后,送入定径机上进行定径,同时控制定径速率为0.4m/s,得无缝管材;(7) Send the continuously rolled pipe in step (6) into the heating furnace. After heating to 800°C, send it to the sizing machine for sizing. At the same time, control the sizing rate to 0.4m/s to obtain seamless pipes;

(8)将步骤(7)的无缝管材于850℃温度下退火3h,冷却至室温,得Ti-Al-Nb-Zr-Mo合金无缝管;(8) Anneal the seamless pipe in step (7) at 850°C for 3 hours and cool to room temperature to obtain a Ti-Al-Nb-Zr-Mo alloy seamless pipe;

该Ti-Al-Nb-Zr-Mo合金无缝管的成分为:Al:58wt.%,Nb:2.98wt.%,Zr:2.00wt.%,Mo:1.02wt.%,余量为Ti;The composition of the Ti-Al-Nb-Zr-Mo alloy seamless pipe is: Al: 58wt.%, Nb: 2.98wt.%, Zr: 2.00wt.%, Mo: 1.02wt.%, and the balance is Ti;

经力学性能检测,退火态无缝管各处的力学性能均能达到要求,获得的无缝管尺寸为Ф180×12×11452mm(外径×壁厚×长度)。After mechanical property testing, the mechanical properties of the annealed seamless pipe can meet the requirements. The obtained seamless pipe size is Ф180×12×11452mm (outer diameter×wall thickness×length).

力学性能见表1、图5:The mechanical properties are shown in Table 1 and Figure 5:

表1Table 1

试样编号Sample No Rm/MPaR m /MPa Rp0.2/MPaR p0.2 /MPa A/%A/% 11 902902 793793 12.812.8 22 910910 806806 12.412.4 33 896896 801801 13.213.2 44 906906 794794 12.112.1 55 914914 812812 12.912.9 66 903903 793793 13.213.2 平均值average value 905905 799799 12.712.7

金相组织见图2。The metallographic structure is shown in Figure 2.

实施例2Example 2

一种Ti-Al-Nb-Zr-Mo合金无缝管的短流程制备方法,其特征在于包括下列各步骤:A short-process preparation method for Ti-Al-Nb-Zr-Mo alloy seamless pipes, which is characterized by including the following steps:

(1)按下列质量比备料:(1) Prepare materials according to the following mass ratio:

铝铌合金 6.3wt.%Aluminum niobium alloy 6.3wt.%

铝豆 4.77wt.%Aluminum beans 4.77wt.%

海绵锆 2.5wt.%Zirconium sponge 2.5wt.%

铝钼合金 1.7wt.%Aluminum-molybdenum alloy 1.7wt.%

海绵钛 84.73wt.%;Titanium sponge 84.73wt.%;

(2)将步骤(1)的备料进行混料后,取适量混合料作为散装料,其余混合料均压制成块后,于120℃烘干5h,随炉冷却,得压块料;(2) After mixing the materials prepared in step (1), take an appropriate amount of the mixture as bulk material, and press the remaining mixture into blocks, dry them at 120°C for 5 hours, and cool them with the furnace to obtain briquettes;

(3)将步骤(2)的散装料铺放在装有七杆电子枪的EB炉的冷床内,再将步骤(2)的适量压块料放入该EB炉进料区;(3) Place the bulk material from step (2) in the cooling bed of an EB furnace equipped with seven electron guns, and then place an appropriate amount of briquettes from step (2) into the feeding area of the EB furnace;

(4)在真空度为3.5×10-3torr时,开启1~5号电子枪对冷床内的散装料进行熔炼,控制1~5号电子枪的电压均为30.5KV,电流均为4.3A,熔炼120min后,关闭电子枪,冷却40min后,将进料区的压块料推入熔炼区,同时开启1~7号电子枪继续熔炼,控制1~7号电子枪的电压均为30.5KV,1~2号电子枪电流为3.0A,3~4号电子枪电流为6A,5号电子枪电流为4.6A,6~7号电子枪电流为2.6A,同时保持18mm/min的拉锭速度,如此持续推料、熔化和拉锭,直至熔炼完成,之后冷却至100℃,将铸锭从结晶器中取出,冷却至室温,经表面扒皮打磨处理后,得Ti-Al-Nb-Zr-Mo合金圆锭;(4) When the vacuum degree is 3.5×10 -3 torr, turn on the No. 1 to 5 electron guns to melt the bulk materials in the cooling bed. Control the voltage of the No. 1 to 5 electron guns to be 30.5KV and the current to be 4.3A. After 120 minutes of smelting, turn off the electron gun. After cooling for 40 minutes, push the briquettes in the feed area into the smelting area. At the same time, turn on the electron guns No. 1 to 7 to continue melting. Control the voltage of the electron guns No. 1 to 7 to be 30.5KV, 1 to 2 The current of electron gun No. 3 is 3.0A, the current of electron gun No. 3 to 4 is 6A, the current of electron gun No. 5 is 4.6A, and the current of electron gun No. 6 to 7 is 2.6A. At the same time, the ingot pulling speed is maintained at 18mm/min, and the material is continuously pushed and melted. and pull the ingot until the smelting is completed, then cool it to 100°C, take the ingot out of the crystallizer, cool it to room temperature, and grind the surface to obtain a Ti-Al-Nb-Zr-Mo alloy round ingot;

(5)在步骤(4)的Ti-Al-Nb-Zr-Mo合金圆锭两端打定心孔后,送入加热炉加热至1200℃,保温6h,出炉后迅速在靠近顶头的一端涂抹适量玻璃粉润滑剂,同时在定心孔内塞入用锡纸包裹的玻璃粉润滑剂,以防止穿孔过程中管材内壁产生缺陷,之后送入二辊斜轧机上进行斜轧穿孔,并控制:总压下率为15%、顶前压下率为8%、椭圆度系数为1.18、穿孔速度为0.4m/s、温度为1120℃,得穿孔管材;(5) After drilling centering holes at both ends of the Ti-Al-Nb-Zr-Mo alloy round ingot in step (4), send it to the heating furnace to be heated to 1200°C and kept for 6 hours. After coming out of the furnace, quickly apply it on the end near the top. Appropriate amount of glass powder lubricant, and at the same time, stuff the glass powder lubricant wrapped with tin foil into the centering hole to prevent defects in the inner wall of the pipe during the perforation process, and then send it to the two-roller cross-rolling machine for cross-rolling and perforation, and control: The reduction rate is 15%, the reduction rate before top is 8%, the ellipticity coefficient is 1.18, the perforation speed is 0.4m/s, and the temperature is 1120°C, the perforated pipe is obtained;

(6)将步骤(5)的穿孔管材送入三辊连轧机上进行连轧,并控制:总压下率为18%、椭圆度系数为1.15、穿孔速度为0.6m/s、温度为1000℃,得连轧管材;(6) Send the perforated pipe in step (5) to the three-roller for continuous rolling, and control: the total reduction rate is 18%, the ovality coefficient is 1.15, the perforation speed is 0.6m/s, and the temperature is 1000 ℃, continuous rolling pipes;

(7)将步骤(6)的连轧管材送入加热炉中,加热至900℃后,送入定径机上进行定径,同时控制定径速率为0.8m/s,得无缝管材;(7) Send the continuously rolled pipe in step (6) into the heating furnace. After heating to 900°C, send it to the sizing machine for sizing. At the same time, control the sizing rate to 0.8m/s to obtain seamless pipes;

(8)将步骤(7)的无缝管材于900℃温度下退火2h,冷却至室温,得Ti-Al-Nb-Zr-Mo合金无缝管;(8) Anneal the seamless pipe in step (7) at 900°C for 2 hours and cool to room temperature to obtain a Ti-Al-Nb-Zr-Mo alloy seamless pipe;

该Ti-Al-Nb-Zr-Mo合金无缝管的成分为:Al:6.12wt.%,Nb: 3.02wt.%,Zr:2.03wt.%,Mo:1.00wt.%,余量为Ti;The composition of the Ti-Al-Nb-Zr-Mo alloy seamless pipe is: Al: 6.12wt.%, Nb: 3.02wt.%, Zr: 2.03wt.%, Mo: 1.00wt.%, the balance is Ti ;

力学性能见表2、图6:The mechanical properties are shown in Table 2 and Figure 6:

表2Table 2

试样编号Sample No Rm/MPaR m /MPa Rp0.2/MPaR p0.2 /MPa A/%A/% 11 921921 806806 12.912.9 22 916916 814814 13.213.2 33 909909 806806 12.412.4 44 913913 816816 13.013.0 55 915915 807807 12.612.6 66 920920 812812 12.812.8 平均值average value 916916 810810 12.812.8

经力学性能检测,各处的力学性能均能达到要求,获得的无缝管尺寸为Ф180×12×11802mm(外径×壁厚×长度)。After mechanical property testing, the mechanical properties of all parts can meet the requirements. The size of the seamless pipe obtained is Ф180×12×11802mm (outer diameter×wall thickness×length).

金相组织见图3。The metallographic structure is shown in Figure 3.

实施例3Example 3

一种Ti-Al-Nb-Zr-Mo合金无缝管的短流程制备方法,其特征在于包括下列各步骤:A short-process preparation method for Ti-Al-Nb-Zr-Mo alloy seamless pipes, which is characterized by including the following steps:

(1)按下列质量比备料:(1) Prepare materials according to the following mass ratio:

铝铌合金 6.0wt.%Aluminum niobium alloy 6.0wt.%

铝豆 4.62wt.%Aluminum beans 4.62wt.%

海绵锆 2.00wt.%Zirconium sponge 2.00wt.%

铝钼合金 1.6wt.%Aluminum-molybdenum alloy 1.6wt.%

海绵钛 58.78wt.%;Titanium sponge 58.78wt.%;

(2)将步骤(1)的备料进行混料后,取适量混合料作为散装料,其余混合料均压制成块后,于110℃烘干5h,随炉冷却,得压块料;(2) After mixing the materials prepared in step (1), take an appropriate amount of the mixture as bulk material, and press the remaining mixture into blocks, dry them at 110°C for 5 hours, and then cool them with the furnace to obtain briquettes;

(3)将步骤(2)的散装料铺放在装有七杆电子枪的EB炉的冷床内,再将步骤(2)的适量压块料放入该EB炉进料区;(3) Place the bulk material from step (2) in the cooling bed of an EB furnace equipped with seven electron guns, and then place an appropriate amount of briquettes from step (2) into the feeding area of the EB furnace;

(4)在真空度为2.6×10-3torr时,开启1~5号电子枪对冷床内的散装料进行熔炼,控制1~5号电子枪的电压均为30KV,电流均为3.8A,熔炼110min后,关闭电子枪,冷却30min后,将进料区的压块料推入熔炼区,同时开启1~7号电子枪继续熔炼,控制1~7号电子枪的电压均为30KV,1~2号电子枪电流为2.8A,3~4号电子枪电流为5.8A,5号电子枪电流为4.1A,6~7号电子枪电流为1.9A,同时保持15mm/min的拉锭速度,如此持续推料、熔化和拉锭,直至熔炼完成,之后冷却至90℃,将铸锭从结晶器中取出,冷却至室温,经表面扒皮打磨处理后,得Ti-Al-Nb-Zr-Mo合金圆锭;(4) When the vacuum degree is 2.6×10 -3 torr, turn on the No. 1 to 5 electron guns to melt the bulk materials in the cooling bed. Control the voltage of the No. 1 to 5 electron guns to be 30KV and the current to be 3.8A. Melting After 110 minutes, turn off the electron gun. After cooling for 30 minutes, push the briquettes in the feeding area into the melting area. At the same time, turn on the electron guns No. 1 to 7 to continue melting. Control the voltage of the electron guns No. 1 to 7 to be 30KV, and the voltage of the electron guns No. 1 to 2 to be 30KV. The current is 2.8A, the current of electron gun No. 3 to 4 is 5.8A, the current of electron gun No. 5 is 4.1A, and the current of electron gun No. 6 to 7 is 1.9A. At the same time, the ingot pulling speed is maintained at 15mm/min, so as to continuously push, melt and Pull the ingot until the smelting is completed, then cool it to 90°C, take the ingot out of the crystallizer, cool it to room temperature, and grind the surface to obtain a Ti-Al-Nb-Zr-Mo alloy round ingot;

(5)在步骤(4)的Ti-Al-Nb-Zr-Mo合金圆锭两端打定心孔后,送入加热炉加热至1150℃,保温7h,出炉后迅速在靠近顶头的一端涂抹适量玻璃粉润滑剂,同时在定心孔内塞入用锡纸包裹的玻璃粉润滑剂,以防止穿孔过程中管材内壁产生缺陷,之后送入二辊斜轧机上进行斜轧穿孔并控制:总压下率为13%、顶前压下率为7%、椭圆度系数为1.15、穿孔速度为0.2m/s、温度为1100℃,得穿孔管材;(5) After drilling centering holes at both ends of the Ti-Al-Nb-Zr-Mo alloy round ingot in step (4), send it to the heating furnace to be heated to 1150°C and kept for 7 hours. After coming out of the furnace, quickly apply it on the end near the top. Appropriate amount of glass powder lubricant, and at the same time, stuff the glass powder lubricant wrapped with tin foil into the centering hole to prevent defects in the inner wall of the pipe during the perforation process, and then send it to the two-roller cross-rolling machine for cross-rolling and perforation and control: total pressure The perforated pipe is obtained when the reduction rate is 13%, the reduction rate before top is 7%, the ellipticity coefficient is 1.15, the perforation speed is 0.2m/s, and the temperature is 1100°C;

(6)将步骤(5)的穿孔管材送入三辊连轧机上进行连轧,并控制:总压下率为15%、椭圆度系数为1.09、穿孔速度为0.5m/s、温度为980℃,得连轧管材;(6) Send the perforated pipe in step (5) to the three-roller for continuous rolling, and control: the total reduction rate is 15%, the ovality coefficient is 1.09, the perforation speed is 0.5m/s, and the temperature is 980 ℃, continuous rolling pipes;

(7)将步骤(6)的连轧管材送入加热炉中,加热至850℃后,送入定径机上进行定径,同时控制定径速率为0.6m/s,得无缝管材;(7) Send the continuously rolled pipe in step (6) into the heating furnace. After heating to 850°C, send it to the sizing machine for sizing. At the same time, control the sizing rate to 0.6m/s to obtain seamless pipes;

(8)将步骤(7)的无缝管材于880℃温度下退火2h,冷却至室温,得Ti-Al-Nb-Zr-Mo合金无缝管;(8) Anneal the seamless pipe in step (7) at 880°C for 2 hours and cool to room temperature to obtain a Ti-Al-Nb-Zr-Mo alloy seamless pipe;

该Ti-Al-Nb-Zr-Mo合金无缝管的成分为:Al:6.03wt.%,Nb:3.0wt.%,Zr:2.01wt.%,Mo:0.98wt.%,余量为Ti;The composition of the Ti-Al-Nb-Zr-Mo alloy seamless pipe is: Al: 6.03wt.%, Nb: 3.0wt.%, Zr: 2.01wt.%, Mo: 0.98wt.%, and the balance is Ti ;

经力学性能检测,各处的力学性能均能达到要求,获得的无缝管尺寸为Ф180×12×12542mm(外径×壁厚×长度)。After mechanical property testing, the mechanical properties of all parts can meet the requirements. The size of the seamless pipe obtained is Ф180×12×12542mm (outer diameter×wall thickness×length).

金相组织见图4。The metallographic structure is shown in Figure 4.

力学性能为见表3、图7。The mechanical properties are shown in Table 3 and Figure 7.

表3table 3

试样编号Sample No Rm/MPaR m /MPa Rp0.2/MPaR p0.2 /MPa A/%A/% 11 914914 806806 12.812.8 22 906906 801801 12.412.4 33 910910 810810 12.612.6 44 908908 807807 13.413.4 55 912912 809809 13.113.1 66 915915 812812 12.812.8 平均值average value 911911 807807 12.912.9

从图2、图3、图4的三个实施例的金相显微组织可以看出,三个实施例均为片层状组织,且有大量的α相集束相互交错。It can be seen from the metallographic microstructure of the three embodiments in Figures 2, 3 and 4 that the three embodiments are all lamellar structures, and there are a large number of α phase bundles interlaced with each other.

图5、图6、图7分别为三个实施例的力学性能图,可看出其力学性能的均匀性,相比于现有技术即:多次VAR熔炼的铸锭、锻造后斜轧穿孔得到的无缝管,其力学性能如表4所示,三个实施例的力学性能,均优于表4现有技术得到的无缝管性能。Figure 5, Figure 6, and Figure 7 are the mechanical performance diagrams of the three embodiments respectively. It can be seen that the uniformity of the mechanical properties is compared with the existing technology, namely: multiple VAR melting ingots, cross-rolled piercing after forging The mechanical properties of the obtained seamless pipe are as shown in Table 4. The mechanical properties of the three embodiments are all better than those of the seamless pipes obtained by the existing technology in Table 4.

Ti-Al-Nb-Zr-Mo合金传统工艺下的无缝管性能见表4The seamless pipe properties of Ti-Al-Nb-Zr-Mo alloy under traditional technology are shown in Table 4

表4Table 4

合金alloy Rm/MPaR m /MPa Rp0.2/MPaR p0.2 /MPa A/%A/% TA31TA31 880880 785785 1212

以上所述,仅是本发明较佳的实施例,并非对本发明作任何限制,凡是根据本发明技术实质对以上实施例进行简单的修改、变更以及等效结构的变化,均仍属于本发明技术。The above are only preferred embodiments of the present invention and do not limit the present invention in any way. Any simple modifications, changes and equivalent structural changes to the above embodiments based on the technical essence of the present invention still belong to the technology of the present invention. .

Claims (2)

1. A short-flow preparation method of a Ti-Al-Nb-Zr-Mo alloy seamless pipe is characterized by comprising the following steps:
(1) The materials are prepared according to the following mass ratio:
5.7 to 6.3 weight percent of aluminum-niobium alloy
4.05 to 4.77 weight percent of aluminum beans
1.5 to 2.5 weight percent of sponge zirconium
1.5 to 1.7 weight percent of aluminum molybdenum alloy
Titanium sponge balance
The sum of the components is 100 wt percent;
(2) Mixing the prepared materials in the step (1), taking a proper amount of the mixture as bulk materials, uniformly pressing the rest of the mixture into blocks, drying at 100-120 ℃ for 5-6 h, and cooling along with a furnace to obtain pressed blocks;
(3) The bulk material in the step (2) is laid in a cooling bed of an EB furnace provided with a seven-rod electron gun, and then a proper amount of pressing blocks in the step (2) are put into a feeding area of the EB furnace;
(4) At a vacuum level of 1.8X10 -3 ~3.5×10 -3 When in torr, starting an electron gun 1-5 to smelt bulk materials in a cooling bed, controlling the voltage of the electron gun 1-5 to 29.5KV, the current of the electron gun 3.3-4.3A, smelting for 100-120 min, closing the electron gun, cooling for 20-40 min, pushing a briquetting material in a feeding area into a smelting area, simultaneously starting the electron gun 1-7 to continue smelting, controlling the voltage of the electron gun 1-7 to 29.5-30.5 KV, the current of the electron gun 1-2 to 2.3-3.0A, the current of the electron gun 3-4 to 5.3-6A, the current of the electron gun 5 to 3.6-4.6A, and the current of the electron gun 6-7 to 1.6-2.6A, simultaneously keeping the ingot pulling speed of 12-18 mm/min, continuously pushing, smelting and ingot pulling until smelting is completed, cooling to 80-100 ℃, taking out the ingot from a crystallizer, cooling to room temperature, and carrying out skin removing and polishing treatment on the ingot to obtain a round Ti-Al-Mo-Nb alloy;
(5) Punching centering holes at two ends of the Ti-Al-Nb-Zr-Mo alloy round ingot in the step (4), feeding the round ingot into a heating furnace to heat to 1100-1200 ℃, preserving heat for 6-8 h, feeding the round ingot into a two-roll diagonal mill to perform diagonal rolling perforation, and controlling: the total rolling reduction is 10-15%, the rolling reduction before top is 6-8%, the ellipticity coefficient is 1.11-1.18, the perforation speed is 0.15-0.4 m/s, and the temperature is 1080-1120 ℃, so as to obtain perforated pipe;
before the two-roller oblique rolling mill is sent, a glass powder lubricant is required to be smeared at one end close to the plug, and meanwhile, the glass powder lubricant wrapped by tinfoil is plugged into the centering hole, so that defects on the inner wall of the pipe in the perforation process are prevented;
(6) Feeding the perforated pipe in the step (5) into a three-roller continuous rolling mill for continuous rolling, and controlling: the total rolling reduction is 12-18%, the ellipticity coefficient is 1.05-1.15, the perforation speed is 0.3-0.6 m/s, and the temperature is 950-1000 ℃, so as to obtain the tandem rolling pipe;
(7) Feeding the continuous rolling pipe in the step (6) into a reheating furnace, heating to 800-900 ℃, feeding the pipe into a sizing mill for sizing, and controlling the sizing speed to be 0.4-0.8 m/s to obtain a seamless pipe;
(8) And (3) annealing the seamless pipe in the step (7) for 2-3 hours at the temperature of 850-900 ℃, and cooling to room temperature to obtain the Ti-Al-Nb-Zr-Mo alloy seamless pipe.
2. The short-flow preparation method of the Ti-Al-Nb-Zr-Mo alloy seamless pipe according to claim 1, wherein the Ti-Al-Nb-Zr-Mo alloy seamless pipe in the step (8) comprises the following components: al:5.5 wt.% to 6.5wt.%, nb:2.5 wt.% to 3.5wt.%, zr:1.5 0.6 to 1.5wt.% of Mo, and the balance of Ti.
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