CN103849803B - Tantalum alloy and method for preparing tantalum alloy tube - Google Patents
Tantalum alloy and method for preparing tantalum alloy tube Download PDFInfo
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- CN103849803B CN103849803B CN201410114933.3A CN201410114933A CN103849803B CN 103849803 B CN103849803 B CN 103849803B CN 201410114933 A CN201410114933 A CN 201410114933A CN 103849803 B CN103849803 B CN 103849803B
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Abstract
The invention provides a tantalum alloy comprising at least one of the following components in percentage by weight: 1.5-45% of Nb, 1.8-17.5% of W, 0.7-1.2% of Zr, 0.5-3.0% of Hf, 0.7-3.5% of Rb, 0.015-0.025% of C, 0.015-0.025% of N and 0.015-0.025% of Y, and the balance of Ta. The invention also provides a method for preparing a tantalum alloy tube. In the preparation process, the processing procedures of wire cutting, preheating, coating of an oxidation resistant coating, heating, extruding, vacuum heat treatment, rolling and vacuum heat treatment are performed in sequence so as to ensure that the surface of the tantalum alloy tube is relatively good in quality, relatively high in mechanical property and excellent in corrosion resistance and high in temperature resistant performance.
Description
Technical field
The present invention relates to technical field of metal, particularly relate to the preparation method of tantalum alloy and tantalum alloy pipe.
Background technology
Tantalum is primarily present in tantalite, and the quality of tantalum is the hardest, is rich in ductility, and the advantage of tantalum metal maximum is tool
There is high corrosion resistance, no matter under conditions of cold or heat, hydrochloric acid, concentrated nitric acid and chloroazotic acid are not reacted.Tantalum almost exists
Can form layer of surface oxide-film under any environment rapidly, this layer of oxide-film is the most thin and dense, almost to all of Jie
Matter all has impermeability, and once damage can also spontaneous recovery immediately.Tantalum alloy is the alloy adding other element with tantalum for base, tantalum
Alloy have high temperature resistant, intensity is high, chemical stability good, the feature such as corrosion-resistant, is aerospace industry, atomic energy industry, height
The material that the field such as temperature technique and chemical anticorrosion is indispensable.Therefore, tantalum alloy be prepared as the focus in order to study.
Such as, the Chinese patent of Application No. 200910304529.1 discloses the vacuum annealing method of tantalum pipe, tantalum pipe
Tantalum pipe, particularly as follows: first cleaned up by tantalum pipe inside and outside wall, is inserted in heat-resisting sleeve by preparation method, sends into vacuum annealing furnace
In, then carrying out evacuation annealing, after cooling, i.e. obtain tantalum pipe, tantalum pipe prepared by the method disclosed in the patent is carried out in a vacuum
Annealing, decreases the environmental factors impact on tantalum pipe, and the combination property making finally prepd tantalum pipe is preferable.Application No.
The Chinese patent of 200610156332.4 discloses strengthens tantalum and the method for tantalum alloy material a kind of preparation, is specially tantalum and tantalum
Alloy powder carries out surface oxygen supplement process under the conditions of low oxygen partial pressure；Tantalum powder after processing again carries out high temperature insostatic pressing (HIP) solidification, obtains
Obtain fine and close block materials；Finally carry out vacuum heat, obtain tantalum and tantalum alloy material, use tantalum and tantalum prepared by the method
Alloy material good percentage elongation, intensity are high.Therefore present invention provides the preparation side of a kind of tantalum alloy material and tantalum alloy material
Method.
Summary of the invention
Present invention solves the technical problem that the preparation method being to provide a kind of tantalum alloy pipe, the tantalum making the present invention prepare closes
Gold tube-surface quality preferably and has higher mechanical property.
In view of this, this application provides a kind of tantalum alloy, described tantalum alloy include 1.5wt%～45wt% Nb,
The Rb of Hf, 0.7wt%～3.5wt% of Zr, 0.5wt%～3.0wt% of W, 0.7wt%～1.2wt% of 1.8wt%～17.5wt%,
In the Y of N Yu 0.015wt%～0.025wt% of C, 0.015wt%～0.025wt% of 0.015wt%～0.025wt% at least one
Kind, and the Ta of surplus.
Preferably, described tantalum alloy includes: the Hf of W, 2.0wt%～the 3.0wt% of 9.0wt%～11.0wt%, 180ppm～
The C of 200ppm and the Ta of surplus.
Preferably, described tantalum alloy includes: the Hf of W, 0.6wt%～the 1.2wt% of 13.0wt%～15.0wt%, 150ppm～
The N of Rb, 150ppm～the 200ppm of C, 0.7wt%～the 1.5wt% of 200ppm and the Ta of surplus.
Present invention also provides the preparation method of tantalum alloy pipe, comprise the following steps:
A) tantalum alloy ingot casting is carried out line cutting and draws hole, obtain hollow cast ingot；
B) hollow cast ingot that step a) obtains is preheated, the hollow cast ingot surface-coated antioxidation after preheating
Coating；
C) hollow cast ingot step b) obtained heats again, is extruded by the hollow cast ingot after heating again；
D) pipe step c) obtained carries out vacuum heat, is rolled by the pipe after vacuum heat；
E) pipe step d) obtained carries out vacuum heat, obtains tantalum alloy pipe；Described tantalum alloy ingot casting includes
The Hf of Zr, 0.5wt%～3.0wt% of W, 0.7wt%～1.2wt% of Nb, 1.8wt%～17.5wt% of 1.5wt%～45wt%,
N Yu 0.015wt% of C, 0.015wt%～0.025wt% of Rb, 0.015wt%～the 0.025wt% of 0.7wt%～3.5wt%～
At least one in the Y of 0.025wt%, and the Ta of surplus.
Preferably, the cutting of line described in step a) also includes after drawing hole:
Hollow cast ingot after line cutting is drawn hole carries out surface process.
Preferably, preheat described in step b) and carry out in chamber type electric resistance furnace or intermediate frequency furnace, pre-warmed temperature
It it is 120 DEG C～180 DEG C.
Preferably, again heat described in step c) and carry out in intermediate frequency furnace, the temperature of described heating be 750 DEG C～
1350℃。
Preferably, the temperature of vacuum heat described in step d) is the 30%～50% of tantalum alloy fusing point, the time be 60～
180min, vacuum≤1.6 × 10-3Pa。
Preferably, also include after rolling described in step d): the pipe after rolling is used chamber type electric resistance furnace or well formula
Resistance furnace carries out surface oxidation treatment, and the heating-up temperature of described surface oxidation treatment is 180～700 DEG C, the time be 2min～
70min。
Preferably, pipe also includes after carrying out surface oxidation treatment:
Using vacuum annealing furnace that the pipe of surface oxidation treatment is carried out calcination, the temperature of described calcination is 450 DEG C～550
DEG C, the time is 20min～60min.
The invention provides the preparation method of tantalum alloy pipe, first tantalum alloy ingot casting carries out line cutting and draws hole, line cuts
Technology can improve the inner surface quality of tantalum alloy hollow cast ingot after processing, coaxiality of inner hole and reduction wall thickness deviation；To obtain
Hollow cast ingot preheat, it is ensured that ORC is at hollow cast ingot surface even application；Then on hollow cast ingot surface
Coating ORC, effectively prevent tantalum alloy hollow cast ingot in the course of processing with air contact, improve hollow cast ingot
The generation of the brittle cracking tendency rising problem that the suction of surface quality and reduction gap gas element causes；Then coating is resisted
The hollow cast ingot of oxide covering carries out heating and extruding again, tantalum alloy hollow cast ingot deform upon so as to get tantalum close
Gold pipe uniform small grains；Then the pipe through crimp being carried out vacuum heat, this heat treatment mode can carry
The purity of high pipe, structure property, and reduce surface contamination；Pipe after vacuum heat is rolled, it is ensured that rolling
The size of pipe and surfaces externally and internally quality, and make the deformation of pipe uniformly, finally carry out vacuum heat, effectively eliminated
Residual stress in the pipe course of processing and obtain the most tiny recrystallized structure, finally makes the mechanical property of tantalum alloy pipe
Preferably.
The present invention during preparing tantalum alloy pipe, carried out successively line cutting-preheat-coat ORC-
The manufacturing procedure of heating-extruding-vacuum heat-rolling-vacuum heat, makes the deformation of tantalum alloy ingot casting uniformly, and avoids
The problem of material contamination in the course of processing, preferably and mechanical property is higher to make the surface quality of tantalum alloy pipe of preparation.
Detailed description of the invention
In order to be further appreciated by the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but
Should be appreciated that these describe simply as to further illustrate the features and advantages of the present invention rather than to the claims in the present invention
Limit.
The embodiment of the invention discloses a kind of tantalum alloy, described tantalum alloy include 1.5wt%～45wt% Nb, 1.8wt%～
The Rb of Hf, 0.7wt%～3.5wt% of Zr, 0.5wt%～3.0wt% of W, 0.7wt%～1.2wt% of 17.5wt%, 0.015wt%
～at least one in the Y of N Yu 0.015wt%～0.025wt% of C, 0.015wt%～0.025wt% of 0.025wt%, and surplus
Ta.
According to the present invention, described tantalum alloy is with tantalum as base and adds the alloy of other element, described tantalum alloy be niobium,
The alloy that one or more in tungsten, zirconium, hafnium, rubidium, carbon and nitrogen form with tantalum.Described tantalum is the material of a kind of excellent anti-corrosion performance
Material, adds other a small amount of element in tantalum material, and keeping it corrosion proof while, its mechanical property and other performance are also
Can be improved, thus expand the application of tantalum alloy.
Well known to those skilled in the art, tantalum itself has had the most excellent antiseptic property.And the application is by adding
Add other alloying element and be more beneficial for the raising of tantalum alloy combination property.According to the application, tantalum alloy adds tungsten and can enter
One step promotes the antiseptic property of tantalum alloy；The atom size of niobium, molybdenum, hafnium and tungsten approximates with tantalum, can form displacement when alloying
Solid solution, thus there is the effect making above-mentioned element have solution strengthening；The elements such as rubidium, carbon, nitrogen are secondary precipitation hardening constituent unit
Element, mainly puies forward heavy alloyed high-temperature behavior, particularly improves high temperature creep property, and improves the high temperature process of tantalum alloy
Energy；Yttrium is a kind of addition element in powder sintered tantalum, improves high temperature life and the element of regulation tissue of material.
Therefore, the application is by adding suitable element in tantalum alloy, it is possible to be effectively improved the antiseptic property of tantalum alloy, heat-resisting quantity
Energy and mechanical property.
Tantalum alloy described herein is owing to the addition of different elements, and has obtained different tantalum alloys.According to this Shen
Please, described tantalum alloy can be that Ta8W2Hf, described Ta8W2Hf include: the W of 7.0～9.0wt%, the Hf of 2.0～2.8wt% and
The Ta of surplus.
Described tantalum alloy can be that Ta10W2.5Hf0.015C, described Ta10W2.5Hf0.015C include 9.0～11.0wt%
W, the Hf of 2.0～3.0wt%, the C of 150～180ppm and the Ta of surplus.
Described tantalum alloy can be Ta7W3Rb, comprising: the W of 6.0～8.0wt%, the Rb of 2.5～3.5wt% and surplus
Ta。
Described tantalum alloy can be Ta8W1Rb1Hf0.025C, comprising: the W of 7.0～9.0wt%, 1.0～1.5wt%
Hf, the C of 200～300ppm, the Rb of 0.8～1.5wt% and the Ta of surplus.
Described tantalum alloy can be Ta12W1Rb0.7Hf0.25C, comprising: the W of 11.0～13.0wt%, 0.5～
The Hf of 1.2wt%, the C of 200～250ppm, the Rb of 0.9～1.5wt% and the Ta of surplus.
Described tantalum alloy is Ta15W1Rb0.7Hf0.025C, comprising: the W of 14.0～16.0wt%, 0.5～1.2wt%
Hf, the C of 200～250ppm, the Rb of 0.7～1.5wt% and the Ta of surplus.
Described tantalum alloy can also be Ta14W2Rb0.7Hf0.02C, comprising: the W of 13.0～15.0wt%, 0.5～
The Hf of 1.2wt%, the C of 180～220ppm, the Rb of 1.5～3.0wt% and the Ta of surplus.
Described tantalum alloy can also be Ta16W3Rb0.7Hf0.023C, comprising: the W of 15.0～17.0wt%, 0.5～
The Hf of 1.2wt%, the C of 180～230ppm, the Rb of 2.5～3.2wt% and the Ta of surplus.
Described tantalum alloy also includes Ta14W1Rb0.9Hf0.018C0.018N, comprising: the W of 13.0～15.0wt%, 0.5
～the Hf of 1.2wt%, the C of 180～200ppm, the Rb of 0.8～1.5wt%, the N of 160～200ppm and the Ta of surplus.
Described tantalum alloy can also be Ta3W2Hf0.02C, comprising: the W of 2.0wt%～3.5wt%, 2.0wt%～
The C of Hf, 180ppm～the 200ppm of 3.0wt% and the Ta of surplus.
Present invention also offers the preparation method of a kind of tantalum alloy pipe, comprise the following steps:
A) tantalum alloy ingot casting is carried out line cutting and draws hole；
B) hollow cast ingot that step a) obtains is preheated, the hollow cast ingot surface-coated antioxidation after preheating
Coating；
C) hollow cast ingot step b) obtained heats again, is extruded by the hollow cast ingot after heating again；
D) pipe step c) obtained carries out vacuum heat, is rolled by the pipe after vacuum heat；
E) pipe step d) obtained carries out vacuum heat, obtains tantalum alloy pipe；Described tantalum alloy ingot casting includes
The Hf of Zr, 0.5wt%～3.0wt% of W, 0.7wt%～1.2wt% of Nb, 1.8wt%～17.5wt% of 1.5wt%～45wt%,
N Yu 0.015wt% of C, 0.015wt%～0.025wt% of Rb, 0.015wt%～0.025wt% of 0.7wt%～3.5wt%～
At least one in the Y of 0.025wt%, and the Ta of surplus.
Present invention firstly provides the ingot casting of tantalum alloy, the ingot casting of described tantalum alloy can melt in vacuum electron beam stove
Refining, it is also possible to melting in vacuum consumable electrode arc furnace, it is also possible to carry out melting in the smelting furnace that above two method combines, this
Application preferably employs vacuum electron beam melting.Tantalum alloy ingot casting is carried out line cutting and draws hole by the present invention, so that ingot casting formation can be real
The hollow ingot blank of existing extrusion process；Preferably employ spark puncher and wire cutting machine carries out linear cutter and goes out centre bore.This
Bright during ingot casting is processed into hollow cast ingot, have employed linear cutter, which can improve the utilization rate of material,
Improve the axiality of centre bore, reduce the deviation of tube wall thickness, improve the fineness of center bore inner wall, thus improve the interior of tubing
Endoporus bar after wall quality, and line cutting may be used for direct processing rod filament material, further increases combining of material
Close utilization rate.Described tantalum alloy ingot casting prepares hollow cast ingot by line cutting, and hollow cast ingot is by necessity of extrusion process
Condition.
After described tantalum alloy ingot casting carries out line cutting, obtain hollow cast ingot material.Preferably, will cut through line
The hollow cast ingot material cut carries out surface process, and line cutting process uses high current discharge until localized metallic instant melting or soft
Change, owing to tantalum alloy belongs to the metal that chemism is the strongest, so causing short time high temperature to aoxidize during shelf depreciation temperature rise
Air-breathing, causes contact layer to form oxidation gettering layer brittle, and the purpose using surface to process is the hardest for oxidation gettering layer crisp layer
Removed by mixed strong acids pickling or other mechanical means, and the line on surface is cut residual lubricant medium process totally, from
And prevent owing to hard crisp layer exists the cracking possibility produced in the pressing process caused.The formula of described pickling is preferably nitre
Acid and Fluohydric acid., the concentration of described nitric acid is preferably 68wt%, and the concentration of described Fluohydric acid. is preferably 50wt%, described nitric acid and hydrogen
The volume ratio of fluoric acid is preferably 20:(2～3), the time of described pickling is preferably 2min～5min.
After being processed on hollow cast ingot surface, described hollow cast ingot is preheated by the present invention.Described preheat
The ORC being beneficial to tantalum alloy hollow cast ingot surface is combined with hollow cast ingot matrix surface.The present invention is preferably at box resistance
Stove or intermediate frequency furnace are preheated to 120 DEG C～180 DEG C.Described hollow cast ingot then will be at its surface-coated antioxidation after preheating
Coating, described ORC is preferably the suspension of waterglass, water and high temp glass powder, and thickness is preferably 2mm～3mm.Institute
State the strongest metal of ORC chemism this for tantalum carrying out protection is that tantalum material processes requisite operation,
Be prevented from tantalum alloy hollow cast ingot during following process with air contact, the surface quality making hollow cast ingot is preferable, and
And more it is prevented from the getter action that tantalio body causes in temperature rising；Described getter action is mainly the suction of oxygen, nitrogen
Suction and the suction of hydrogen, wherein the suction of oxygen will result in base material fragility strengthen, resistance of deformation increase, pressure processing mistake
The problem that journey is easy to crack, the intensity making tantalio material is increased by the suction of nitrogen, plasticity reduces deformation difficulty and increases, the suction of hydrogen
Enter will result in material embrittlement, pressing process cracking.The application is carried out after tantalum alloy ingot casting is carried out line cutting successively
Preheating and coat ORC is requisite step, and this is that after cutting due to line, preheating of employing is able to
Preferably coating surface ORC, should guarantee uniformly, be prone to be coated in coating hollow cast ingot surface, protect again
Material surface will be caused transition to aoxidize by card, it is therefore necessary to carries out the cooperation of preheating and ORC, ORC master
If in order to the heating of tantalum raw material is protected, being special a kind of guard method.
In order to make tantalum alloy hollow cast ingot have more excellent oxygen-proof property in the course of processing and have the effect of lubrication,
The present invention preferably uses thickness to be 0.3mm～0.5mm red copper foil parcel or the copper belt of 1.2～2.5mm on hollow cast ingot surface
Parcel, using thickness is that 0.8mm～1.2mm copper tube wraps up endoporus.At tantalum alloy hollow cast ingot surface and endoporus copper-clad paper tinsel, right
Material surfaces externally and internally has protective effect, improves surfaces externally and internally quality；Extrusion process has for extrusion die and pecker
Protective effect, prevents the mould damage that tack of materials and resistance of deformation cause；Also there is in extrusion process lubrication, reduce
Extrusion friction power and extruding force；Utilize red copper oxytropism and with the buffer action of outside air, it is to avoid tantalum alloy oxidation air-breathing,
The final surface quality ensureing tantalum alloy pipe.
According to the present invention, then heat after by the surface-coated ORC of tantalum alloy hollow cast ingot.Described add
Heat is to prepare to extrude, and makes ingot casting easily deform during extruding, and ensures the inside group of material after extruding
Knit and processing characteristics.The process of heating of the present invention particularly as follows:
Use intermediate frequency furnace that hollow cast ingot is heated to 750 DEG C～1350 DEG C, infrared thermometry or use box electricity
Hollow cast ingot is heated to 400 DEG C～600 DEG C by resistance stove, then be transferred in intermediate-frequency heating furnace to be heated to 750 DEG C～1350 DEG C or
Directly use chamber type electric resistance furnace that hollow cast ingot is heated to 400 DEG C～600 DEG C.
In order to make tantalum alloy hollow cast ingot size accurate, the present invention after heating, preferably, uses Forming Die
Tool steel 5CrNiMo carries out hot piercing, final forging temperature as list cone or the bipyramid drift of punching die, quenching hardness HRC50～55
≥600℃.After hot reaming, preferably, the outer surface of hollow cast ingot being carried out turning process, inner surface is carried out
The mechanical treatment that bore hole processes, to remove pollution layer and the defect of surfaces externally and internally, it is ensured that size is applicable to recipient requirement.In order to
Eliminate hollow cast ingot residual stress in the course of processing, and improve the purity of material, structure property and minimizing surface contamination,
Hollow cast ingot then carries out after described mechanical treatment vacuum heat, and the temperature of described vacuum heat is preferably tantalum alloy
The 30%～50% of fusing point, temperature retention time is 60～180min, vacuum≤1.6 × 10-3Pa.Tantalum for special composition composition closes
Gold, may still there will be the problem that material structure is the most poor after above-mentioned process, therefore to make material in processing procedure
Performance reach optimum state, then repeat to preheat-coat the operation of ORC-copper-clad paper tinsel-heating, above-mentioned operation
Identical with the parameter of manufacturing procedure first.
After tantalum alloy hollow cast ingot is heated, carried out the operation extruded, make material at three-dimensional compressive stress
Effect under radially, axial and circumferential generation homogeneous deformation.The extrusion equipment used in extrusion process according to the present invention can
Thinking the oil pressure forward extrusion equipment such as 1650T, 3150T, 3500T, 5500T, extrusion ratio is preferably >=4.After hollow cast ingot is heated
Extrude again, beneficially material deform upon so as to get tantalum alloy pipe uniform small grains.
In order to ensure material surface quality, and the crackling avoiding hollow cast ingot to produce in extrusion process causes follow-up
The cracking of material in the course of processing, preferably, the tantalum alloy pipe after extruding has been carried out pickling by the present invention.Described acid
The solution washed is nitric acid and Fluohydric acid., and the concentration of described nitric acid is preferably 68wt%, and the concentration of described Fluohydric acid. is preferably 50wt%,
Described nitric acid is preferably 20:(2～3 with the volume ratio of Fluohydric acid .), the time of described pickling is preferably 2min～5min.
According to the present invention, after described tantalum alloy pipe carries out pickling, the material after pickling is carried out vacuum heat.Institute
Stating vacuum heat is under fine vacuum negative pressure and high temperature, utilizes the oxide on tantalum alloy pipe surface and other impurity internal
Vapour pressure is different, makes peroxide breaks down and volatilization further, thus it is dirty to improve the purity of material, structure property and minimizing surface
Dye.The temperature of described vacuum heat is preferably the 30%～50% of tantalum alloy fusing point, temperature retention time be preferably 60min～
180min, vacuum is preferably≤1.6 × 10-3Pa, more preferably 1.5 × 10-3Pa～1.0 × 10-3Pa。
It, after tantalum alloy pipe is carried out vacuum heat, is rolled by the present invention.Described rolling be multiple roll, three
Roller and annular distance type two rolling system, present invention preferably employs annular distance type cold rolling, and this rolling technique is relative to three rollers and multiroll rolling skill
Art can be greatly improved passes working modulus, shortens the production cycle of tubing, improves structure property and reduces wall thickness deviation.Road
Secondary working modulus is preferably 10%～80%, and angle of revolution is preferably 17 °～57 °, and feed is preferably 0～10mm electrodeless adjustable, returns
Transfer into the double feeding of single rotary feeding system, dual AC power or dual AC power list can be used to be sent into.
In order to eliminate the residual stress in the operation of rolling and processing hardening, and material is made to have preferable surface quality,
Preferably, the present invention has carried out the operation of vacuum heat after rolling.The temperature of described vacuum heat is preferred
For the 30%～50% of tantalum alloy fusing point, temperature retention time is preferably 60min～180min, vacuum≤1.6 × 10-3Pa。
Tantalum alloy pipe through rolling is preferably employed kerosene soak or ultrasonic waves for cleaning, make the surface of material after cleaning
Presenting metal true qualities gloss, surfaces externally and internally is without the external contaminant such as greasy dirt, impurity.Carried out vacuum heat subsequently.
According to the present invention, the tantalum alloy pipe through vacuum heat is preferably carried out surface oxidation treatment, described surface
Oxidation processes produces surface compact high price oxide-film, thus avoids base material to cause surface damage and raising to draw in the case of frictional force
Frictional force during stretching.The heating-up temperature of described surface oxidation treatment is preferably 180 DEG C～700 DEG C, at described surface oxidation
The time of reason is preferably 2min～70min.Described surface oxidation treatment preferably employs box or well formula resistance furnace, in atmospheric environment
Under carry out.Tantalum alloy pipe through surface oxidation treatment is preferably carried out pickling, to remove surface impurity.Described pickling molten
Liquid is preferably nitric acid and Fluohydric acid., and described nitric acid is preferably 20:(2～3 with the volume ratio of Fluohydric acid .), the concentration of described nitric acid is
68wt%, the concentration of described Fluohydric acid. is 50wt%.Pipe through overpickling has preferably been carried out calcination.Described calcination can be by relatively
Thin diameter surfaces externally and internally, the especially external contaminant of inner surface residual decompose under middle temperature XHV condition of negative pressure and wave
Send out, thus improve the clean-up performance of tubing.Described calcination is preferably carried out in vacuum annealing furnace, and vacuum is preferably≤1.6 × 10- 3Pa, temperature is preferably 450 DEG C～550 DEG C, and the time is preferably 20min～60min.
Finally by carrying out vacuum heat through tantalum alloy pipes of calcination or other processing of process, eliminate in the course of processing
Residualinternal stress.The temperature of described vacuum heat is preferably the 30%～50% of tantalum alloy fusing point, and temperature retention time is preferably
60min～180min, vacuum≤1.6 × 10-3Pa。
From the foregoing, during tantalum alloy control is standby, first tantalum alloy ingot casting carries out line cutting and draws hole, line cuts
Technology can improve the inner surface quality of tantalum alloy hollow cast ingot after processing, coaxiality of inner hole, reduction wall thickness deviation and improve material
The comprehensive utilization ratio of material；The hollow cast ingot obtained is preheated, it is ensured that ORC is uniformly coated with on hollow cast ingot surface
Apply；Then at hollow cast ingot surface-coated ORC, effectively prevent tantalum alloy hollow cast ingot in the course of processing with sky
Gas contacts, and improves the surface quality of pipe；Then again carry out heating and squeezing by the hollow cast ingot of coating ORC
Pressure, tantalum alloy hollow cast ingot deform upon so as to get tantalum alloy pipe uniform small grains；Then by through crimp
Pipe carries out vacuum heat, and this heat treatment mode can improve the purity of pipe, structure property, and reduces surface contamination；Will
Pipe after vacuum heat rolls, it is ensured that the size of rolling pipe and surfaces externally and internally quality, and makes pipe deform
Uniformly, finally carry out vacuum heat, effectively eliminated the residual stress in material processing and recrystallized structure,
The tantalum alloy pipe mechanical property making preparation eventually is preferable.
In order to make tantalum alloy pipe have preferable surface quality and combination property, the present invention increases the most after rolling
Material surface carried out oxidation processes and calcination.The present invention, during preparing tantalum alloy, has carried out line cutting-add successively
The manufacturing procedure of heat-coating ORC-heating-extruding-vacuum heat-rolling-vacuum heat, makes tantalum alloy ingot casting
Uniformly, and it is the most contaminated to avoid material in the course of processing in deformation, makes the surface quality of material of preparation preferably and mechanical property
Can be higher.
In order to be further appreciated by the present invention, the preparation method of the tantalum alloy pipe provided the present invention below in conjunction with embodiment is entered
Row describes in detail, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
1) tantalum alloy ingot casting is through three electronic torch meltings, a diameter of 153mm of ingot casting, and the composition of ingot casting is as shown in table 1:
Table 1 tantalum alloy ingot casting constituent content information table
2) using spark puncher and wire cutting machine that tantalum alloy ingot casting carries out line cutting and draw hole, obtaining internal diameter is 60mm's
Tantalum alloy hollow cast ingot；
3) step 2) the tantalum alloy hollow cast ingot that obtains is preheated to 180 DEG C, then at tantalum alloy pipe in chamber type electric resistance furnace
Base surfaces externally and internally coating ORC；
4) tantalum alloy pipe Frequency Induction Heating step 3) obtained is to 1200～1350 DEG C, at 1650T oil pressure forward
Extruding in extrusion equipment, the extruding of tantalum alloy pipe is to a diameter of 95mm, and internal diameter is 60mm；Then by the tantalum alloy after extruding
Pipe carries out pickling in the nitric acid mixed solution with Fluohydric acid., and the concentration of nitric acid is 68wt%, and the concentration of Fluohydric acid. is 50wt%,
Nitric acid is 20:(2～3 with the volume ratio of Fluohydric acid .)；
5) tantalum alloy pipe step 4) obtained carries out vacuum heat, and the temperature of heat treatment is 1450 DEG C, and the time is
90min；Use 3T Single arm that tantalum alloy pipe carries out straightening, the straight degree of visual inspection；Tantalum alloy pipe through straightening is entered
Driving cylindrical and bore hole, remove the defect of surfaces externally and internally；
6) the tantalum alloy pipe using annular distance type cold-rolling mill to obtain step 5) rolls, and after rolling, the external diameter of pipe is
82mm, wall thickness is 13.0mm, a diameter of 58.5mm～56mm of plug in the operation of rolling；Again roll, the tantalum alloy pipe after rolling
The external diameter of base is 67mm, and external diameter is 8.5mm, a diameter of 52.5mm～50mm of plug in the operation of rolling；Again roll, after rolling
The external diameter of tantalum alloy pipe be 54.0mm, wall thickness is 4.5mm, a diameter of 52.5mm～50mm of plug in the operation of rolling；
7) tantalum alloy pipe step 6) obtained carries out pickling in the mixed solution of nitric acid and Fluohydric acid., nitric acid dense
Degree is 68wt%, and the concentration of Fluohydric acid. is 50wt%, and nitric acid is 20:(2～3 with the volume ratio of Fluohydric acid .)；
8) tantalum alloy pipe step 7) obtained is at 1450 DEG C, and 60min carries out vacuum annealing, and then manual tantalum of repairing closes
The surfaces externally and internally of gold pipe, removes surface defect, checks surfaces externally and internally defect and mechanically or manually repairs；
9) tantalum alloy pipe step 8) obtained rolls, and the pipe external diameter after rolling is 52.0mm, and wall thickness is
3mm, a diameter of 44mm of plug used；Again being rolled by the pipe obtained, being rolled into external diameter is 50.0mm, and wall thickness is
The pipe of 3.5mm, a diameter of 43mm of plug this time used in the operation of rolling；The pipe obtained is rolled again, rolls
Making external diameter is 48.0mm, and wall thickness is the pipe of 3mm, a diameter of 42mm of plug this time used in the operation of rolling；To obtain
Pipe again roll, being rolled into external diameter is 46.0mm, and wall thickness is the pipe of 2.5mm, this time used in operation of rolling
A diameter of 41mm of plug；Again being rolled by the pipe obtained, being rolled into external diameter is 44.0mm, and wall thickness is the pipe of 1.75mm
Base, a diameter of 40.5mm of plug this time used in the operation of rolling；The pipe obtained is repaiied material, inspection；Pipe is rolled again
System, a diameter of 40.0 ± 0.1mm of plug used, obtaining external diameter is 43.0 ± 0.15mm, and wall thickness is the pipe of 1.5 ± 0.15mm
Base；
10) tantalum alloy pipe step 9) obtained carries out pickling in the nitric acid mixed solution with Fluohydric acid., nitric acid
Concentration is 68wt%, and the concentration of Fluohydric acid. is 50wt%, and nitric acid is 20:(2～3 with the volume ratio of Fluohydric acid .)；
11) tantalum alloy pipe step 10) obtained is at 1450 DEG C, and 60min carries out vacuum annealing, obtains tantalum alloy pipe.
The tantalum alloy pipe obtained is carried out flaring test: intercept the pipeline section of 2 times of diameters, use the enlarging cone of 60 ° of cone angles to be expanded extremely by internal diameter
The 20% of diameter, surface is visible by naked eyes crackle；Or internal diameter is expanded to the 18% of diameter, surface by the enlarging cone using 45 ° of cone angles
It is visible by naked eyes crackle；
12) the tantalum alloy pipe obtained being carried out room temperature tensile test, test result is as shown in table 2:
The room temperature tensile properties tables of data of the tantalum alloy pipe of table 2 embodiment 1 preparation
13) tantalum alloy pipe step 11) obtained carries out air pressure detection: use air pressure testing machine, in sealing in keeping pipe
Portion's pressure is 0.707Mpa, keeps 10 seconds ne-leakage phenomenons.
Embodiment 2
1) tantalum alloy ingot casting is through three electronic torch meltings, a diameter of 153mm of ingot casting, and the composition of ingot casting is as shown in table 3:
Table 3 tantalum alloy ingot casting constituent content information table (wt%)
2) using spark puncher and wire cutting machine that tantalum alloy ingot casting carries out line cutting and draw hole, obtaining internal diameter is 45mm's
Tantalum alloy hollow cast ingot；
3) step 2) the tantalum alloy hollow cast ingot that obtains is preheated to 180 DEG C in chamber type electric resistance furnace, then empty at tantalum alloy
Heart ingot casting surfaces externally and internally coating ORC；
4) tantalum alloy hollow cast ingot Frequency Induction Heating step 3) obtained is to 850 DEG C, at a diameter of 155mm oil pressure just
Extruding in extrusion equipment, the extruding of tantalum alloy pipe is to a diameter of 95mm, and internal diameter is 45mm；Then the tantalum after extruding is closed
Gold pipe carries out pickling in the nitric acid mixed solution with Fluohydric acid., and the concentration of nitric acid is 68wt%, and the concentration of Fluohydric acid. is
50wt%, nitric acid is 20:(2～3 with the volume ratio of Fluohydric acid .)；
5) tantalum alloy pipe step 4) obtained carries out vacuum heat, and the temperature of heat treatment is 1300 DEG C, and the time is
90min；Use 3T Single arm that tantalum alloy pipe carries out straightening, the straight degree of visual inspection；Tantalum alloy pipe through straightening is entered
Driving cylindrical and bore hole, remove the defect of surfaces externally and internally；
6) the tantalum alloy pipe using annular distance type cold-rolling mill to obtain step 5) rolls, and after rolling, the external diameter of pipe is
82mm, internal diameter is 20mm, a diameter of 44.5mm～42mm of plug in the operation of rolling；Again roll, the tantalum alloy pipe after rolling
External diameter be 67mm, internal diameter is 14.5mm, a diameter of 40.5mm～38mm of plug in the operation of rolling；Again roll, after rolling
The external diameter of tantalum alloy pipe be 54.0mm, internal diameter is 10mm, a diameter of 36.5mm～34mm of plug in the operation of rolling；
7) tantalum alloy pipe step 6) obtained carries out carrying out pickling, nitric acid in the nitric acid mixed solution with Fluohydric acid.
Concentration be 68wt%, the concentration of Fluohydric acid. is 50wt%, and the volume ratio of nitric acid and Fluohydric acid. is 20:(2～3)；
8) tantalum alloy pipe step 7) obtained is at 1350 DEG C, and 60min carries out vacuum annealing, and then manual tantalum of repairing closes
The surfaces externally and internally of gold pipe, removes surface defect, checks surfaces externally and internally defect and mechanically or manually repairs；
9) tantalum alloy pipe step 8) obtained rolls, and the pipe external diameter after rolling is 42.0mm, and internal diameter is
6mm, a diameter of the 32.5 of plug used～30mm；Again being rolled by the pipe obtained, being rolled into external diameter is 33.0mm,
Internal diameter is the pipe of 4mm, a diameter of 27mm～25mm of plug this time used in the operation of rolling；The pipe obtained is entered again
Row rolling, being rolled into external diameter is 24.0mm, and internal diameter is the pipe of 3mm, plug this time used in operation of rolling a diameter of
20mm～18mm；
10) tantalum alloy pipe step 9) obtained carries out carrying out pickling, nitre in the nitric acid mixed solution with Fluohydric acid.
The concentration of acid is 68wt%, and the concentration of Fluohydric acid. is 50wt%, and nitric acid is 20:(2～3 with the volume ratio of Fluohydric acid .)；
11) tantalum alloy pipe step 10) obtained is at 1350 DEG C, and 60min carries out vacuum annealing；Check the tantalum after annealing
The surfaces externally and internally defect of alloy pipe stock is also mechanically or manually repaired；
12) tantalum alloy pipe step 11) obtained rolls, and the pipe external diameter after rolling is 15.6mm, and internal diameter is
1.8mm, a diameter of 10.4mm of plug used；Again being rolled by the pipe obtained, being rolled into external diameter is 11.4mm, interior
Footpath is the pipe of 1.1mm, a diameter of 9.4mm of plug this time used in the operation of rolling；The pipe obtained is rolled again
System, being rolled into external diameter is 10.4mm, and internal diameter is the pipe of 1.0mm, plug this time used in operation of rolling a diameter of
8.5mm；Again being rolled by the pipe obtained, being rolled into external diameter is 9.4mm, and internal diameter is the pipe of 0.9mm, and this rolled
A diameter of 7.6mm of plug used in journey；Again being rolled by the pipe obtained, being rolled into external diameter is 8.5mm, and internal diameter is
The pipe of 0.8mm, a diameter of 7.0mm of plug this time used in the operation of rolling；The pipe obtained is rolled again, rolls
Making external diameter is 7.7mm, and internal diameter is the pipe of 0.7mm, a diameter of 6.5mm of plug this time used in the operation of rolling；
13) will be according to step 10) and 11 by step 12)) pickling and annealing after again roll, being rolled into external diameter is
7.0mm, internal diameter is the pipe of 0.7mm, a diameter of 6.0mm of plug this time used in the operation of rolling；By the pipe that obtains again
Secondary rolling, being rolled into external diameter is 6.4mm, and internal diameter is the pipe of 0.5mm, the diameter of plug this time used in operation of rolling
For 5.5mm；Again being rolled by the pipe obtained, being rolled into external diameter is 5.64mm, and internal diameter is the pipe of 0.32mm, and this rolls
A diameter of 5.5mm of the plug used in the process of system；Again being rolled by the pipe obtained, being rolled into external diameter is 5.0mm, interior
Footpath is the pipe of 0.25mm, a diameter of 4.5mm of plug this time used in the operation of rolling；The pipe obtained is rolled again
System, being rolled into external diameter is 4.42mm, and internal diameter is the pipe of 0.17mm, plug this time used in operation of rolling a diameter of
4.0mm；
14) tantalum alloy pipe step 13) obtained carries out washing oil removing successively, surfaces externally and internally processes, dish is round and end socket
After carry out calcination in a vacuum furnace, the temperature of calcination is 500 DEG C, and the time is 20min；
15), after tantalum alloy pipe step 14) obtained is rinsed, soaks and checks, finally stretch, in drawing process
Size be followed successively by Finally obtaining external diameter is 1.0mm, and internal diameter is the tantalum alloy pipe of 0.55mm.
Tantalum alloy pipe embodiment 2 prepared carries out flaring test: intercept the pipeline section of 2 times of diameters, uses the expansion of 60 ° of cone angles
Internal diameter is expanded to the 20% of diameter by prostomum, and tantalum alloy tube-surface is visible by naked eyes crackle；The tantalum alloy pipe of preparation is carried out air pressure inspection
Surveying: use air pressure testing machine, sealing internal pressure in keeping pipe is 0.707Mpa, keeps 10 seconds ne-leakage phenomenons.
The tantalum alloy pipe of preparation is carried out room temperature tensile test, and test result is as shown in table 4:
The room temperature tensile properties tables of data of the tantalum alloy pipe of table 4 embodiment 2 preparation
Embodiment 3
1) tantalum alloy ingot casting is through three electronic torch meltings, a diameter of 153mm of ingot casting, and the composition of ingot casting is as shown in table 5:
The elemental composition table of table 5 tantalum alloy ingot casting
Other operating procedure is same as in Example 1, prepares tantalum alloy pipe.
Tantalum alloy pipe embodiment 3 prepared carries out flaring test: intercept the pipeline section of 2 times of diameters, uses the expansion of 60 ° of cone angles
Internal diameter is expanded to the 20% of diameter by prostomum, and tantalum alloy tube-surface is visible by naked eyes crackle；The tantalum alloy pipe of preparation is carried out air pressure inspection
Surveying: use air pressure testing machine, sealing internal pressure in keeping pipe is 0.707Mpa, keeps 10 seconds ne-leakage phenomenons.
The tantalum alloy pipe of preparation is carried out room temperature tensile test, and test result is as shown in table 6:
The room temperature tensile properties tables of data of the tantalum alloy pipe of table 6 embodiment 3 preparation
Embodiment 4
1) tantalum alloy ingot casting is through three electronic torch meltings, a diameter of 153mm of ingot casting, and the composition of ingot casting is as shown in table 7:
The elemental composition table of table 7 tantalum alloy ingot casting
Other operating procedure is same as in Example 2, prepares tantalum alloy pipe.
Tantalum alloy pipe embodiment 4 prepared carries out flaring test: intercept the pipeline section of 2 times of diameters, uses the expansion of 60 ° of cone angles
Internal diameter is expanded to the 20% of diameter by prostomum, and tantalum alloy tube-surface is visible by naked eyes crackle；The tantalum alloy pipe of preparation is carried out air pressure inspection
Surveying: use air pressure testing machine, sealing internal pressure in keeping pipe is 0.707Mpa, keeps 10 seconds ne-leakage phenomenons.
The tantalum alloy pipe of preparation is carried out room temperature tensile test, and test result is as shown in table 8:
The room temperature tensile properties tables of data of the tantalum alloy pipe of table 8 embodiment 4 preparation
Embodiment 5
1) by tantalum alloy ingot casting through three electronic torch meltings, a diameter of 153mm of ingot casting, the composition of ingot casting such as table 9 institute
Show:
The elemental composition table of table 9 tantalum alloy ingot casting
Other operating procedure is same as in Example 1, prepares tantalum alloy pipe.
Tantalum alloy pipe embodiment 5 prepared carries out flaring test: use the enlarging cone of 45 ° of cone angles to expand internal diameter to diameter
18% surface, tantalum alloy pipe is visible by naked eyes crackle.The tantalum alloy pipe of preparation is carried out air pressure detection: use air pressure testing machine,
Sealing internal pressure in keeping pipe is 0.707Mpa, keeps 10 seconds ne-leakage phenomenons.
The tantalum alloy pipe obtained is carried out room temperature tensile test, and test result is as shown in table 10:
The room temperature tensile properties tables of data of the tantalum alloy pipe of table 10 embodiment 5 preparation
Embodiment 6
1) by tantalum alloy ingot casting through three electronic torch meltings, a diameter of 153mm of ingot casting, the composition of ingot casting such as table 11 institute
Show:
The elemental composition table of table 11 tantalum alloy ingot casting
Other operating procedure is same as in Example 1, prepares tantalum alloy pipe.
Tantalum alloy pipe embodiment 6 prepared carries out flaring test: use the enlarging cone of 45 ° of cone angles to expand internal diameter to diameter
18%, tantalum alloy tube-surface is visible by naked eyes crackle；The tantalum alloy pipe of preparation is carried out air pressure detection: use air pressure testing machine,
Sealing internal pressure in keeping pipe is 0.707Mpa, keeps 10 seconds ne-leakage phenomenons.
The tantalum alloy pipe obtained is carried out room temperature tensile test, and test result is as shown in table 12:
The room temperature tensile properties tables of data of the tantalum alloy pipe of table 12 embodiment 6 preparation
Embodiment 7
1) by tantalum alloy ingot casting through three electronic torch meltings, a diameter of 153mm of ingot casting, the composition of ingot casting such as table 13 institute
Show:
The elemental composition table of table 13 tantalum alloy ingot casting
Other operating procedure is same as in Example 1, prepares tantalum alloy pipe.
Tantalum alloy pipe embodiment 7 prepared carries out flaring test: intercept the pipeline section of 2 times of diameters, uses the expansion of 60 ° of cone angles
Internal diameter is expanded to the 20% of diameter by prostomum, and tantalum alloy tube-surface is visible by naked eyes crackle；The tantalum alloy pipe of preparation is carried out air pressure inspection
Surveying: use air pressure testing machine, sealing internal pressure in keeping pipe is 0.707Mpa, keeps 10 seconds ne-leakage phenomenons.
The tantalum alloy pipe obtained is carried out room temperature tensile test, and test result is as shown in table 14:
The room temperature tensile properties tables of data of the tantalum alloy pipe of table 14 embodiment 7 preparation
Embodiment 8
1) by tantalum alloy ingot casting through three electronic torch meltings, a diameter of 153mm of ingot casting, the composition of ingot casting such as table 15 institute
Show:
The elemental composition table of table 15 tantalum alloy ingot casting
Other operating procedure is same as in Example 1, prepares tantalum alloy pipe.
Tantalum alloy pipe embodiment 8 prepared carries out flaring test: intercept the pipeline section of 2 times of diameters, uses the expansion of 60 ° of cone angles
Internal diameter is expanded to the 20% of diameter by prostomum, and surface is visible by naked eyes crackle；The tantalum alloy pipe of preparation is carried out air pressure detection: use
Air pressure testing machine, sealing internal pressure in keeping pipe is 0.707Mpa, keeps 10 seconds ne-leakage phenomenons.
The tantalum alloy pipe obtained is carried out room temperature tensile test, and test result is as shown in table 16:
The room temperature tensile properties tables of data of the tantalum alloy pipe of table 16 embodiment 8 preparation
Embodiment 9
1) by tantalum alloy ingot casting through three electronic torch meltings, a diameter of 153mm of ingot casting, the composition of ingot casting such as table 17 institute
Show:
The elemental composition table of table 17 tantalum alloy ingot casting
Other operating procedure is same as in Example 1, prepares tantalum alloy pipe.
Tantalum alloy pipe embodiment 9 prepared carries out flaring test: intercept the pipeline section of 2 times of diameters, uses the expansion of 60 ° of cone angles
Internal diameter is expanded to the 20% of diameter by prostomum, and tantalum alloy tube-surface is visible by naked eyes crackle；The tantalum alloy pipe of preparation is carried out air pressure inspection
Surveying: use air pressure testing machine, sealing internal pressure in keeping pipe is 0.707Mpa, keeps 10 seconds ne-leakage phenomenons.
The tantalum alloy pipe obtained is carried out room temperature tensile test, and test result is as shown in table 18:
The room temperature tensile properties tables of data of the tantalum alloy pipe of table 18 embodiment 9 preparation
Embodiment 10
1) by tantalum alloy ingot casting through three electronic torch meltings, a diameter of 153mm of ingot casting, the composition of ingot casting such as table 19 institute
Show:
The elemental composition table of table 19 tantalum alloy ingot casting
Other operating procedure is same as in Example 1, prepares tantalum alloy pipe.
Tantalum alloy pipe embodiment 10 prepared carries out flaring test: intercept the pipeline section of 2 times of diameters, uses 60 ° of cone angles
Internal diameter is expanded to the 20% of diameter by enlarging cone, and surface is visible by naked eyes crackle；The tantalum alloy pipe of preparation is carried out air pressure detection: adopt
With air pressure testing machine, sealing internal pressure in keeping pipe is 0.707Mpa, keeps 10 seconds ne-leakage phenomenons.
The tantalum alloy pipe obtained is carried out room temperature tensile test, and test result is as shown in table 20:
The room temperature tensile properties tables of data of the tantalum alloy pipe of table 20 embodiment 10 preparation
The explanation of above example is only intended to help to understand method and the core concept thereof of the present invention.It is right to it should be pointed out that,
For those skilled in the art, under the premise without departing from the principles of the invention, it is also possible to the present invention is carried out
Some improvement and modification, these improve and modify in the protection domain also falling into the claims in the present invention.
Described above to the disclosed embodiments, makes professional and technical personnel in the field be capable of or uses the present invention.
Multiple amendment to these embodiments will be apparent from for those skilled in the art, as defined herein
General Principle can realize without departing from the spirit or scope of the present invention in other embodiments.Therefore, the present invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and principles disclosed herein and features of novelty phase one
The widest scope caused.
Claims (6)
1. the preparation method of tantalum alloy pipe, comprises the following steps:
A) tantalum alloy ingot casting is carried out line cutting and draws hole, obtain hollow cast ingot, then carry out surface process；
B) being preheated by the hollow cast ingot that step a) obtains, the hollow cast ingot surface-coated antioxidation after preheating is coated with
Layer；
C) hollow cast ingot that step b) obtains is heated again, the hollow cast ingot after heating again is extruded；
D) pipe that step c) obtains is carried out vacuum heat, the pipe after vacuum heat is rolled；
E) pipe that step d) obtains is carried out vacuum heat, obtain tantalum alloy pipe；Described tantalum alloy ingot casting includes
Zr, 0.5wt% of W, 0.7wt%～1.2wt% of Nb, 1.8wt%～17.5wt% of 1.5wt%～45wt%～
C, 0.015wt%～0.025wt% of Rb, 0.015wt%～0.025wt% of Hf, 0.7wt%～3.5wt% of 3.0wt%
N Yu 0.015wt%～0.025wt% Y at least one, and the Ta of surplus.
Preparation method the most according to claim 1, it is characterised in that preheat described in step b) at chamber type electric resistance furnace or
Carrying out in intermediate frequency furnace, pre-warmed temperature is 120 DEG C～180 DEG C.
Preparation method the most according to claim 1, it is characterised in that again heat at intermediate frequency furnace described in step c)
In carry out, the temperature of described heating is 750 DEG C～1350 DEG C.
Preparation method the most according to claim 1, it is characterised in that the temperature of vacuum heat described in step d) is tantalum
The 30%～50% of alloy melting point, the time is 60～180min, vacuum≤1.6 × 10-3Pa。
Preparation method the most according to claim 1, it is characterised in that also include after rolling described in step d): will roll
Pipe after system uses chamber type electric resistance furnace or well formula resistance furnace to carry out surface oxidation treatment, the heating temperature of described surface oxidation treatment
Degree is 180～700 DEG C, and the time is 2min～70min.
Preparation method the most according to claim 1, it is characterised in that pipe also includes after carrying out surface oxidation treatment:
Using vacuum annealing furnace that the pipe of surface oxidation treatment is carried out calcination, the temperature of described calcination is 450 DEG C～550 DEG C,
Time is 20min～60min.
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| CN104492849B (en) * | 2014-11-29 | 2016-03-23 | 西安诺博尔稀贵金属材料有限公司 | A kind of preparation method of used by nuclear reactor hafnium square rod |
| CN104550312A (en) * | 2014-12-10 | 2015-04-29 | 宁夏东方钽业股份有限公司 | Processing method of large seamless tantalum or tantalum alloy pipe |
| CN104550280A (en) * | 2014-12-22 | 2015-04-29 | 宁夏东方钽业股份有限公司 | Method for continuously producing tantalum or tantalum alloy large-size wire rod |
| CN107584251B (en) * | 2017-09-08 | 2019-04-16 | 西北有色金属研究院 | A kind of manufacturing process of tantalum alloy shaped piece |
| CN109652692B (en) * | 2018-12-05 | 2020-05-26 | 湖北第二师范学院 | Hydrogen-embrittlement-resistant tantalum alloy for biomedical implantation, and production method, application and material thereof |
| CN109675956A (en) * | 2018-12-28 | 2019-04-26 | 宁夏东方钽业股份有限公司 | A kind of preparation method of small dimension Niobium Superconducting stick |
| CN111530962B (en) * | 2020-05-14 | 2021-08-24 | 成都先进金属材料产业技术研究院有限公司 | Production method for small-caliber thick-wall titanium alloy seamless pipe |
| CN111570390A (en) * | 2020-05-19 | 2020-08-25 | 宁波江丰电子材料股份有限公司 | Treatment method of tantalum part in glow discharge mass spectrometer |
| CN111744984A (en) * | 2020-06-18 | 2020-10-09 | 宁夏东方钽业股份有限公司 | Preparation method of tantalum alloy and niobium alloy tube blank |
| CN112359256A (en) * | 2020-08-18 | 2021-02-12 | 长沙南方钽铌有限责任公司 | Tantalum alloy, tantalum alloy seamless tube preparation method and tantalum alloy seamless tube |
| CN112359257A (en) * | 2020-08-18 | 2021-02-12 | 长沙南方钽铌有限责任公司 | Tantalum alloy, tantalum alloy seamless tube preparation method and tantalum alloy seamless tube |
| CN112342446A (en) * | 2020-08-18 | 2021-02-09 | 长沙南方钽铌有限责任公司 | Tantalum alloy, tantalum alloy seamless tube preparation method and tantalum alloy seamless tube |
| CN112322951B (en) * | 2020-08-18 | 2022-11-29 | 长沙南方钽铌有限责任公司 | Tantalum alloy seamless tube and preparation method thereof |
| CN114102160B (en) * | 2021-11-29 | 2023-10-31 | 中国兵器工业第五九研究所 | High-performance high-efficiency preparation method of tantalum alloy hyperboloid space structural member |
| CN115522089B (en) * | 2022-10-10 | 2023-06-23 | 南京理工大学 | Method for preparing tantalum material through deformation |
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| GB1022486A (en) * | 1963-07-11 | 1966-03-16 | Imp Metal Ind Kynoch Ltd | Tantalum alloys |
| US3390983A (en) * | 1964-04-20 | 1968-07-02 | Westinghouse Electric Corp | Tantalum base alloys |
| US3791821A (en) * | 1968-10-30 | 1974-02-12 | Westinghouse Electric Corp | Tantalum base alloys |
| CN1560300A (en) * | 2004-03-09 | 2005-01-05 | 株洲硬质合金集团有限公司 | Preparation method of Taw Yalloy bar |
| CN102909237B (en) * | 2012-11-22 | 2015-09-09 | 宁夏东方钽业股份有限公司 | A kind of preparation method of TA18 thick-wall tube |
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