CN103014386B - Preparation method of niobium-tungsten-molybdenum-zirconium alloy ingot - Google Patents

Preparation method of niobium-tungsten-molybdenum-zirconium alloy ingot Download PDF

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CN103014386B
CN103014386B CN201210528852.9A CN201210528852A CN103014386B CN 103014386 B CN103014386 B CN 103014386B CN 201210528852 A CN201210528852 A CN 201210528852A CN 103014386 B CN103014386 B CN 103014386B
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ingot casting
zirconium
pure zirconium
niobium
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CN103014386A (en
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武宇
赵鸿磊
王飞
郭海生
姚修楠
宜楠
文琳
张琨宇
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Xi'an noble rare metal materials Co.,Ltd.
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Xi'an Nuoboer Rare & Noble Metal Materials Co Ltd
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Abstract

The invention provides a preparation method of a niobium-tungsten-molybdenum-zirconium alloy ingot. The preparation method comprises the following steps: 1, tidily stacking a plurality of niobium-tungsten-molybdenum metal strips, laying a first pure zirconium in the middle of the stacked niobium-tungsten-molybdenum metal strips, and welding to form a smelting electrode; 2, performing twice vacuum electron beam smelting to the smelting electrode to obtain a semi-finished ingot; 3, cutting a second pure zirconium plate into a plurality of pure zirconium strips; 4, tightly attaching the pure zirconium strips to the outer surface of the semi-finished ingot to obtain a consumable electrode for electric arc smelting; and 5, performing twice vacuum consumable electric arc smelting to obtain the niobium-tungsten-molybdenum-zirconium alloy ingot. The niobium-tungsten-molybdenum-zirconium alloy ingot prepared according to the preparation method provided by the invention has favorable uniformity of components of organization, can keep low intensity without changing excellent room-temperature property and high-temperature property, and is significant to be used in spaceflight.

Description

A kind of preparation method of niobium tungsten zirconium alloy ingot casting
Technical field
The invention belongs to alloy preparing technical field, be specifically related to a kind of preparation method of niobium tungsten zirconium alloy ingot casting.
Background technology
Nb521 niobium tungstenalloy is the one of niobium tungsten zirconium alloy, is made up of matrix metal niobium and alloying element tungsten, molybdenum and zirconium; The nominal composition of Nb521 niobium tungstenalloy is Nb-5.0W-2.0Mo-1.0Zr, can long term operation below 1500 DEG C, there is good prospect of the application in space flight with rocket engine parts.Nb521 niobium tungstenalloy adopts electron beam furnace to carry out melting ingot casting conventionally, and the density of Nb521 niobium tungstenalloy is at 8.85g/cm 3～9.0g/cm 3between.In order to improve intensity; conventionally the carbon content of Nb521 niobium tungstenalloy ingot casting can be brought up to 0.05%～0.12%; this can generate again a large amount of carbide as ZrC, WC; the hardness of these carbide is all very high, can cause the bar of following process or sheet material to occur unexpected crackle, layering and peeling defect.Research shows, Nb521 niobium tungstenalloy, under the constant condition of tungsten, molybdenum content, only increases zirconium mass content to 1.7% left and right, just alloy density can be reduced to 8.75g/cm3 left and right, and can not fall low-alloyed room-temperature property and high-temperature behavior.Compared with using niobium hafnium alloy (NbHf10-1) with existing space flight of having shaped, zirconium mass content be 1.65%～1.75% niobium tungsten zirconium alloy can use temperature can improve 250 DEG C, hot strength 1600 DEG C time is two times of niobium hafnium alloy, and density has only increased less than 0.15g/cm than niobium hafnium alloy 3, the niobium tungsten zirconium alloy that therefore zirconium mass content is 1.65%～1.75% is significant for aerospace applications.
But, after increasing zirconium to the mass content of zirconium be not less than 1.0% in Nb521 niobium tungstenalloy, adopt traditional electron beam melting mode will be due to the physical property feature such as solid solubility and the difference of zirconium and niobium density of zirconium in niobium, cause the segregation degree of zirconium in finished product alloy cast ingot to exceed 50%, thereby affect the consistence of material structure and performance.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, and a kind of preparation method of niobium tungsten zirconium alloy ingot casting is provided.The niobium tungsten zirconium alloy ingot casting that adopts the method to prepare has good structural constituent homogeneity, can keep niobium tungsten zirconium alloy to there is low density not changing under the room-temperature property of niobium tungsten zirconium alloy and the prerequisite of high-temperature behavior, significant for aerospace applications.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of niobium tungsten zirconium alloy ingot casting, it is characterized in that, and the method comprises the following steps:
Step 1, many length are to 300mm～1500mm, the niobium tungsten metal strip that width and thickness are 14mm～16mm neatly stacks, making the total length of the niobium tungsten metal strip after neatly stacking is 1200mm～1500mm, total width is 42mm～48mm, total thickness is 56mm～64mm, niobium tungsten metal strip after neatly stacking middle part level is laid the first pure zirconium plate again, then the niobium tungsten metal strip that is equipped with the first pure zirconium plate is placed in to argon arc welding case, niobium tungsten metal strip by the first pure zirconium plate and after neatly stacking carries out argon arc welding, obtains smelting electrode; The length of described the first pure zirconium plate and width all with neatly stack after niobium tungsten metal strip identical, the weight of described the first pure zirconium plate is 1.2%～1.25% of smelting electrode weight; In many described niobium tungsten metal strips, the quality percentage composition of tungsten is 4.7%～5.0%, and the quality percentage composition of molybdenum is 2.0%～2.3%, and surplus is niobium and inevitable impurity;
Step 2, smelting electrode described in step 1 is placed in to vacuum electron beam melting furnace, is not more than 2.0 × 10 in vacuum tightness -2under the condition of Pa, carry out twice vacuum electron beam melting, obtain work in-process ingot casting; The cross section of described work in-process ingot casting is that diameter is the circle of 85mm～105mm;
Step 3, the second pure zirconium plate that is 2.0mm by thickness are cut into many length and are 100mm, and width is the pure zirconium bar of 8mm～13mm, and the gross weight of many described pure zirconium bars is 0.5%～0.75% of the weight of work in-process ingot casting described in step 2;
Step 4, adopt iron wire many described pure zirconium bars in step 3 all to be adhere well to the outside surface of work in-process ingot casting, then the work in-process ingot casting that outside surface is pasted with to many pure zirconium bars is placed in argon arc welding case, many described pure zirconium bars are all carried out to argon arc welding with work in-process ingot casting, remove afterwards iron wire, obtain arc melting consumable electrode; Many described pure zirconium bars are all parallel with work in-process ingot casting along its length;
Step 5, arc melting described in step 4 is placed in to vacuum consumable arc-melting stove with consumable electrode carries out vacuum consumable arc-melting twice, obtain niobium tungsten zirconium alloy ingot casting; In described niobium tungsten zirconium alloy ingot casting, the quality percentage composition of zirconium is 1.65%～1.75%.
The preparation method of above-mentioned a kind of niobium tungsten zirconium alloy ingot casting, is characterized in that, in step 1, the density of many niobium tungsten metal strips is 7.9g/cm 3～8.4g/cm 3.
The preparation method of above-mentioned a kind of niobium tungsten zirconium alloy ingot casting, is characterized in that, in the ingot casting of work in-process described in step 2, the quality percentage composition of zirconium is 1.0%～1.15%, and the quality percentage composition of oxygen is not more than 0.01%.
The preparation method of above-mentioned a kind of niobium tungsten zirconium alloy ingot casting, is characterized in that, the integral multiple that the length value of the ingot casting of work in-process described in step 2 is 100, and the unit of described work in-process ingot casting length is mm.
The preparation method of above-mentioned a kind of niobium tungsten zirconium alloy ingot casting, it is characterized in that, the concrete system that in step 4, many described pure zirconium bars adhere well to work in-process ingot casting outside surface is: be first one group by every many described pure zirconium bars 3 and be divided into into n group, wherein n is that positive integer and n meet: 10≤n≤17; Then every group of pure zirconium bar all evenly laid at work in-process ingot casting outside surface, wherein first group of pure zirconium bar one end is concordant with work in-process ingot casting one end, 30 ° of second group of pure zirconium bar one end and relative first group of pure zirconium bar circumferential offset concordant with first group of pure zirconium bar the other end, 30 ° of the 3rd group of pure zirconium article one end and relative second group of pure zirconium article circumferential offset concordant with second group of pure zirconium article the other end, the rest may be inferred, until n organize pure zirconium article one end and (n-1) organize the pure zirconium article the other end concordant and relative (n-1) organize 30 ° of pure zirconium article circumferential offset; Keep second group of pure zirconium article consistent to the direction that n organizes pure zirconium article circumferential offset.
The preparation method of above-mentioned a kind of niobium tungsten zirconium alloy ingot casting, it is characterized in that, the detailed process of twice vacuum consumable arc-melting described in step 5 is: first described arc melting is not more than in vacuum tightness with consumable electrode under the condition of 1.0Pa and carries out vacuum consumable arc-melting for the first time, obtaining diameter is an ingot casting of 160mm; Then taking the head of a described ingot casting as the initiating terminal of vacuum consumable arc-melting for the second time, a described ingot casting is not more than in vacuum tightness under the condition of 1.0Pa and carries out vacuum consumable arc-melting for the second time, obtaining diameter is the niobium tungsten zirconium alloy ingot casting of 200mm.
The preparation method of above-mentioned a kind of niobium tungsten zirconium alloy ingot casting, is characterized in that, in the tungsten of niobium described in step 5 zirconium alloy ingot casting, the quality percentage composition of oxygen is not more than 0.02%.
The present invention compared with prior art has the following advantages:
1, the invention provides a kind of method of preparing niobium tungsten zirconium alloy ingot casting, the melting technology that the present invention adopts vacuum electron beam melting and vacuum arc melting to combine is prepared niobium tungsten zirconium alloy ingot casting; The alloy cast ingot that adopts the present invention to prepare has good structural constituent homogeneity, can pass through sheet material, bar or the tubing of the method manufacture high-temperature uses such as follow-up extruding, forging, rolling.
2, adopt the niobium tungsten zirconium alloy ingot casting prepared of the present invention under the constant condition of tungsten, molybdenum content, only the quality percentage composition of zirconium is increased to 1.65%～1.75%, can under the prerequisite that does not change good room-temperature property and high-temperature behavior, keep niobium tungsten zirconium alloy to there is low density, significant for aerospace applications.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Brief description of the drawings
Fig. 1 is the diagrammatic cross-section that the present invention is equipped with the niobium tungsten metal strip after neatly stacking of the first pure zirconium plate.
Fig. 2 is that the present invention adopts iron wire many pure zirconium bars to be attached to the one-piece construction schematic diagram of work in-process ingot casting outside surface.
Fig. 3 is the A-A cutaway view Amplified image of Fig. 2.
Fig. 4 is the B-B cutaway view Amplified image of Fig. 2.
Description of reference numerals:
1-niobium tungsten metal strip; The pure zirconium plate of 2-first; 3-work in-process ingot casting;
The pure zirconium bar of 4-; 5-iron wire.
Embodiment
Embodiment 1
The preparation method of the niobium tungsten zirconium alloy ingot casting of the present embodiment comprises the following steps:
Step 1,48 width and thickness are to 14mm, length is that the niobium tungsten metal strip 1 of 300mm neatly stacks, making the length of the niobium tungsten metal strip after neatly stacking is 1200mm, width is 42mm, thickness is 56mm, niobium tungsten metal strip after neatly stacking middle part level is laid the first pure zirconium plate 2 again, then the niobium tungsten metal strip that is equipped with the first pure zirconium plate 2 is placed in to argon arc welding case, niobium tungsten metal strip by the first pure zirconium plate 2 and after neatly stacking carries out argon arc welding, obtains the smelting electrode that weight is 22.6Kg; The length of described the first pure zirconium plate 2 and width all with neatly stack after niobium tungsten metal strip identical, the weight of described the first pure zirconium plate 2 is 1.25% of smelting electrode weight; After described niobium tungsten metal strip 1 mixes compacting by niobium powder, tungsten powder and molybdenum powder, sintering obtains; In described niobium tungsten metal strip 1, the quality percentage composition of tungsten is 4.7%, and the quality percentage composition of molybdenum is 2.3%, and surplus is niobium and inevitable impurity, and the density of described niobium tungsten metal strip 1 is 7.9g/cm 3;
Step 2, smelting electrode described in step 1 being placed in to vacuum electron beam melting furnace, is 1.1 × 10 in vacuum tightness -2under the condition of Pa, carry out twice vacuum electron beam melting, obtaining diameter is 85mm, the cylindrical semi-finished product ingot casting 3 that length is 1100mm, and in described work in-process ingot casting 3, the quality percentage composition of zirconium is 1.15%, the mass content of oxygen is 60ppm;
Step 3, the second pure zirconium plate is cut into 33 length is 100mm, width is 8mm, and the gross weight that thickness is 4,33 described pure zirconium bars 4 of pure zirconium bar of 2.0mm is 0.6% of 3 weight of work in-process ingot casting described in step 2; The length of 33 pure zirconium bars 4 and be all not more than ± 0.2mm of the error of width after cutting;
Step 4, adopt iron wire 5 33 described pure zirconium bars 4 in step 3 all to be adhere well to the outside surface of work in-process ingot casting 3, then the work in-process ingot casting 3 that outside surface is pasted with to 33 pure zirconium bars 4 is placed in argon arc welding case, argon arc welding is all carried out to work in-process ingot casting 3 in 33 described pure zirconium bar 4 one end, remove afterwards iron wire 5, obtain arc melting consumable electrode; 33 described pure zirconium bars 3 are all parallel along its length with work in-process ingot casting 3; The concrete system that 33 described pure zirconium bars 4 adhere well to work in-process ingot casting 3 outside surfaces is: be first one group by every 33 described pure zirconium bars 43 and be divided into into 11 groups; Then every group of pure zirconium bar 4 all evenly laid at the outside surface of work in-process ingot casting 3, wherein first group of pure zirconium bar 4 one end is concordant with work in-process ingot casting 3 one end, 30 ° of second group of pure zirconium bar 4 one end and relative first group of pure zirconium bar 4 circumferential offset concordant with first group of pure zirconium bar 4 the other end, 30 ° of the 3rd group of pure zirconium article 4 one end and relative second group of pure zirconium article 4 circumferential offset concordant with second group of pure zirconium article 4 the other ends, the rest may be inferred, until the 11st group of pure zirconium article 4 one end are concordant with the 10th group of pure zirconium article 4 the other end and 30 ° of relative the 10th group of pure zirconium article 4 circumferential offset; Keep the direction of second group of pure zirconium article 4 to the 11st groups of pure zirconium article 4 circumferential offset consistent;
Step 5, arc melting described in step 4 is placed in to vacuum consumable arc-melting stove with consumable electrode, first under the condition that is 0.47Pa with consumable electrode in vacuum tightness by described arc melting, carry out vacuum consumable arc-melting for the first time, obtaining diameter is an ingot casting of 160mm; Then taking the head of a described ingot casting as the initiating terminal of vacuum consumable arc-melting for the second time, under the condition that is 0.47Pa, carry out vacuum consumable arc-melting for the second time by a described ingot casting in vacuum tightness, obtaining diameter is the niobium tungsten zirconium alloy ingot casting of 200mm.
The niobium tungsten zirconium alloy ingot casting composition analysis data of the present embodiment are in table 1.
The niobium tungsten zirconium alloy ingot casting composition analysis data of table 1 embodiment of the present invention 1
Figure BDA00002556304400061
As shown in Table 1, in the niobium tungsten zirconium alloy ingot casting of the present embodiment, the quality percentage composition of tungsten is 5.12%～5.13%, the quality percentage composition of molybdenum is 1.97%～2.04%, the quality percentage composition of zirconium is 1.65%～1.67%, the quality percentage composition of oxygen is 0.012%～0.016%, illustrates that the niobium tungsten zirconium alloy ingot casting of the present embodiment has good structural constituent homogeneity.
Embodiment 2
The preparation method of the niobium tungsten zirconium alloy ingot casting of the present embodiment comprises the following steps:
Step 1,24 width and thickness are to 15mm, length is that the niobium tungsten metal strip 1 of 600mm neatly stacks, making the length of the niobium tungsten metal strip after neatly stacking is 1200mm, width is 45mm, thickness is 60mm, niobium tungsten metal strip after neatly stacking middle part level is laid the first pure zirconium plate 2 again, then the niobium tungsten metal strip that is equipped with the first pure zirconium plate 2 is placed in to argon arc welding case, niobium tungsten metal strip by the first pure zirconium plate 2 and after neatly stacking carries out argon arc welding, obtains the smelting electrode that weight is 27.2Kg; The length of described the first pure zirconium plate 2 and width all with neatly stack after niobium tungsten metal strip identical, the weight of described the first pure zirconium plate 2 is 1.2% of smelting electrode weight; After described niobium tungsten metal strip 1 mixes compacting by niobium powder, tungsten powder and molybdenum powder, sintering obtains; In described niobium tungsten metal strip 1, the quality percentage composition of tungsten is 5.0%, and the quality percentage composition of molybdenum is 2.0%, and surplus is niobium and inevitable impurity, and the density of described niobium tungsten metal strip 1 is 8.3g/cm 3;
Step 2, smelting electrode described in step 1 is placed in to vacuum electron beam melting furnace is 0.8 × 10 in vacuum tightness -2under the condition of Pa, carry out twice vacuum electron beam melting, obtaining diameter is 95mm, the cylindrical semi-finished product ingot casting 3 that length is 1000mm, and in described work in-process ingot casting 3, the quality percentage composition of zirconium is 1.0%, the mass content of oxygen is 50ppm;
Step 3, the second pure zirconium plate is cut into 30 length is 100mm, width is 11.3mm, and the gross weight that thickness is 4,30 described pure zirconium bars 4 of pure zirconium bar of 2.0mm is 0.7% of 3 weight of work in-process ingot casting described in step 2; The length of 30 pure zirconium bars 4 and be all not more than ± 0.2mm of the error of width after cutting;
Step 4, adopt iron wire 5 30 described pure zirconium bars 4 in step 3 all to be adhere well to the outside surface of work in-process ingot casting 3, then the work in-process ingot casting 3 that outside surface is pasted with to 30 pure zirconium bars 4 is placed in argon arc welding case, argon arc welding is all carried out to work in-process ingot casting 3 in 30 described pure zirconium bar 4 one end, remove afterwards iron wire 5, obtain arc melting consumable electrode, 30 described pure zirconium bars 3 are all parallel along its length with work in-process ingot casting 3, the concrete system that 30 described pure zirconium bars 4 adhere well to work in-process ingot casting 3 outside surfaces is: be first one group by every 30 described pure zirconium bars 43 and be divided into into 10 groups, then every group of pure zirconium bar 4 all evenly laid at the outside surface of work in-process ingot casting 3, wherein first group of pure zirconium bar 4 one end is concordant with work in-process ingot casting 3 one end, 30 ° of second group of pure zirconium bar 4 one end and relative first group of pure zirconium bar 4 circumferential offset concordant with first group of pure zirconium bar 4 the other end, 30 ° of the 3rd group of pure zirconium article 4 one end and relative second group of pure zirconium article 4 circumferential offset concordant with second group of pure zirconium article 4 the other ends, the rest may be inferred, until the 10th group of pure zirconium article 4 one end are concordant with the 9th group of pure zirconium article 4 the other end and 30 ° of relative the 9th group of pure zirconium article 4 circumferential offset, keep the direction of second group of pure zirconium article 4 to the 10th groups of pure zirconium article 4 circumferential offset consistent,
Step 5, arc melting described in step 4 is placed in to vacuum consumable arc-melting stove with consumable electrode, first under the condition that is 0.53Pa with consumable electrode in vacuum tightness by described arc melting, carry out vacuum consumable arc-melting for the first time, obtaining diameter is an ingot casting of 160mm; Then taking the head of a described ingot casting as the initiating terminal of vacuum consumable arc-melting for the second time, under the condition that is 0.53Pa, carry out vacuum consumable arc-melting for the second time by a described ingot casting in vacuum tightness, obtaining diameter is the niobium tungsten zirconium alloy ingot casting of 200mm.
The niobium tungsten zirconium alloy ingot casting composition analysis data of the present embodiment are in table 2.
The niobium tungsten zirconium alloy ingot casting composition analysis data of table 2 embodiment of the present invention 2
As shown in Table 2, in the niobium tungsten zirconium alloy ingot casting of the present embodiment, the quality percentage composition of tungsten is 4.98%～5.20%, the quality percentage composition of molybdenum is 2.06%～2.10%, the quality percentage composition of zirconium is 1.68%～1.74%, the quality percentage composition of oxygen is 0.010%～0.012%, illustrates that the niobium tungsten zirconium alloy ingot casting of the present embodiment has good structural constituent homogeneity.
Embodiment 3
The preparation method of the niobium tungsten zirconium alloy ingot casting of the present embodiment comprises the following steps:
Step 1,12 width and thickness are to 16mm, the niobium tungsten metal strip 1 that length is 1200mm neatly stacks, making the length of the niobium tungsten metal strip after neatly stacking is 1200mm, width is 48mm, thickness is 64mm, niobium tungsten metal strip after neatly stacking middle part level is laid the first pure zirconium plate 2 again, then the niobium tungsten metal strip that is equipped with the first pure zirconium plate 2 is placed in to argon arc welding case, niobium tungsten metal strip by the first pure zirconium plate 2 and after neatly stacking carries out argon arc welding, obtains the smelting electrode that weight is 29.9Kg; The length of described the first pure zirconium plate 2 and width all with neatly stack after niobium tungsten metal strip identical, the weight of described the first pure zirconium plate 2 is 1.25% of smelting electrode weight; After described niobium tungsten metal strip 1 mixes compacting by niobium powder, tungsten powder and molybdenum powder, sintering obtains; In described niobium tungsten metal strip 1, the quality percentage composition of tungsten is 4.8%, and the quality percentage composition of molybdenum is 2.2%, and surplus is niobium and inevitable impurity, and the density of described niobium tungsten metal strip 1 is 8.0Kg/cm 3;
Step 2, smelting electrode described in step 1 is placed in to vacuum electron beam melting furnace is 2.0 × 10 in vacuum tightness -2under the condition of Pa, carry out twice vacuum electron beam melting, obtaining diameter is 105mm, the cylindrical semi-finished product ingot casting 3 that length is 1700mm, and in described work in-process ingot casting 3, the quality percentage composition of zirconium is 1.15%, the mass content of oxygen is 80ppm;
Step 3, the second pure zirconium plate is cut into 51 length is 100mm, width is 9.8mm, and the gross weight that thickness is 4,51 described pure zirconium bars 4 of pure zirconium bar of 2.0mm is 0.5% of 3 weight of work in-process ingot casting described in step 2; The length of 51 pure zirconium bars 4 and be all not more than ± 0.2mm of the error of width after cutting;
Step 4, adopt iron wire 5 51 described pure zirconium bars 4 in step 3 all to be adhere well to the outside surface of work in-process ingot casting 3, then the work in-process ingot casting 3 that outside surface is pasted with to 51 pure zirconium bars 4 is placed in argon arc welding case, argon arc welding is all carried out to work in-process ingot casting 3 in 51 described pure zirconium bar 4 one end, remove afterwards iron wire 5, obtain arc melting consumable electrode; 51 described pure zirconium bars 3 are all parallel along its length with work in-process ingot casting 3; The concrete system that 51 described pure zirconium bars 4 adhere well to work in-process ingot casting 3 outside surfaces is: be first one group by every 51 described pure zirconium bars 43 and be divided into into 17 groups; Then every group of pure zirconium bar 4 all evenly laid at the outside surface of work in-process ingot casting 3, wherein first group of pure zirconium bar 4 one end is concordant with work in-process ingot casting 3 one end, 30 ° of second group of pure zirconium bar 4 one end and relative first group of pure zirconium bar 4 circumferential offset concordant with first group of pure zirconium bar 4 the other end, 30 ° of the 3rd group of pure zirconium article 4 one end and relative second group of pure zirconium article 4 circumferential offset concordant with second group of pure zirconium article 4 the other ends, the rest may be inferred, until the 17th group of pure zirconium article 4 one end are concordant with the 16th group of pure zirconium article 4 the other end and 30 ° of relative the 16th group of pure zirconium article 4 circumferential offset; Keep the direction of second group of pure zirconium article 4 to the 17th groups of pure zirconium article 4 circumferential offset consistent;
Step 5, arc melting described in step 4 is placed in to vacuum consumable arc-melting stove with consumable electrode, first under the condition that is 0.33Pa with consumable electrode in vacuum tightness by described arc melting, carry out vacuum consumable arc-melting for the first time, obtaining diameter is an ingot casting of 160mm; Then taking the head of a described ingot casting as the initiating terminal of vacuum consumable arc-melting for the second time, under the condition that is 0.33Pa, carry out vacuum consumable arc-melting for the second time by a described ingot casting in vacuum tightness, obtaining diameter is the niobium tungsten zirconium alloy ingot casting of 200mm.
The niobium tungsten zirconium alloy ingot casting composition analysis data of the present embodiment are in table 3.
The niobium tungsten zirconium alloy ingot casting composition analysis data of table 3 embodiment of the present invention 3
Figure BDA00002556304400101
As shown in Table 3, in the niobium tungsten zirconium alloy ingot casting of the present embodiment, the quality percentage composition of tungsten is 4.98%～5.03%, the quality percentage composition of molybdenum is 1.95%～1.98%, the quality percentage composition of zirconium is 1.65%～1.68%, the quality percentage composition of oxygen is 0.014%～0.017%, illustrates that the niobium tungsten zirconium alloy ingot casting of the present embodiment has good structural constituent homogeneity.
Embodiment 4
The preparation method of the niobium tungsten zirconium alloy ingot casting of the present embodiment comprises the following steps:
Step 1,12 width and thickness are to 14mm, the niobium tungsten metal strip 1 that length is 1500mm neatly stacks, making the length of the niobium tungsten metal strip after neatly stacking is 1500mm, width is 42mm, thickness is 56mm, niobium tungsten metal strip after neatly stacking middle part level is laid the first pure zirconium plate 2 again, then the niobium tungsten metal strip that is equipped with the first pure zirconium plate 2 is placed in to argon arc welding case, niobium tungsten metal strip by the first pure zirconium plate 2 and after neatly stacking carries out argon arc welding, obtains the smelting electrode that weight is 30Kg; The length of described the first pure zirconium plate 2 and width all with neatly stack after niobium tungsten metal strip identical, the weight of described the first pure zirconium plate 2 is 1.22% of smelting electrode weight; After described niobium tungsten metal strip 1 mixes compacting by niobium powder, tungsten powder and molybdenum powder, sintering obtains; In described niobium tungsten metal strip 1, the quality percentage composition of tungsten is 4.8%, and the quality percentage composition of molybdenum is 2.3%, and surplus is niobium and inevitable impurity, and the density of described niobium tungsten metal strip 1 is 8.4g/cm 3;
Step 2, smelting electrode described in step 1 is placed in to vacuum electron beam melting furnace is 1.0 × 10 in vacuum tightness -2under the condition of Pa, carry out twice vacuum electron beam melting, obtaining diameter is 100mm, the cylindrical semi-finished product ingot casting 3 that length is 1500mm, and in described work in-process ingot casting 3, the quality percentage composition of zirconium is 1.15%, the quality percentage composition of oxygen is 0.01%;
Step 3, the second pure zirconium plate is cut into 45 length is 100mm, width is 13mm, and the gross weight that thickness is 4,45 described pure zirconium bars 4 of pure zirconium bar of 2.0mm is 0.75% of 3 weight of work in-process ingot casting described in step 2; The length of 45 pure zirconium bars 4 and be all not more than ± 0.2mm of the error of width after cutting;
Step 4, adopt iron wire 5 45 described pure zirconium bars 4 in step 3 all to be adhere well to the outside surface of work in-process ingot casting 3, then the work in-process ingot casting 3 that outside surface is pasted with to 45 pure zirconium bars 4 is placed in argon arc welding case, argon arc welding is all carried out to work in-process ingot casting 3 in 45 described pure zirconium bar 4 one end, remove afterwards iron wire 5, obtain arc melting consumable electrode; 45 described pure zirconium bars 3 are all parallel along its length with work in-process ingot casting 3; The concrete system that 45 described pure zirconium bars 4 adhere well to work in-process ingot casting 3 outside surfaces is: be first one group by every 45 described pure zirconium bars 43 and be divided into into 15 groups; Then every group of pure zirconium bar 4 all evenly laid at the outside surface of work in-process ingot casting 3, wherein first group of pure zirconium bar 4 one end is concordant with work in-process ingot casting 3 one end, 30 ° of second group of pure zirconium bar 4 one end and relative first group of pure zirconium bar 4 circumferential offset concordant with first group of pure zirconium bar 4 the other end, 30 ° of the 3rd group of pure zirconium article 4 one end and relative second group of pure zirconium article 4 circumferential offset concordant with second group of pure zirconium article 4 the other ends, the rest may be inferred, until the 15th group of pure zirconium article 4 one end are concordant with the 14th group of pure zirconium article 4 the other end and 30 ° of relative the 14th group of pure zirconium article 4 circumferential offset; Keep the direction of second group of pure zirconium article 4 to the 15th groups of pure zirconium article 4 circumferential offset consistent;
Step 5, arc melting described in step 4 is placed in to vacuum consumable arc-melting stove with consumable electrode, first under the condition that is 1.0Pa with consumable electrode in vacuum tightness by described arc melting, carry out vacuum consumable arc-melting for the first time, obtaining diameter is an ingot casting of 160mm; Then taking the head of a described ingot casting as the initiating terminal of vacuum consumable arc-melting for the second time, under the condition that is 1.0Pa, carry out vacuum consumable arc-melting for the second time by a described ingot casting in vacuum tightness, obtaining diameter is the niobium tungsten zirconium alloy ingot casting of 200mm.
The niobium tungsten zirconium alloy ingot casting composition analysis data of the present embodiment are in table 4.
The niobium tungsten zirconium alloy ingot casting composition analysis data of table 4 embodiment of the present invention 4
As shown in Table 4, in the niobium tungsten zirconium alloy ingot casting of the present embodiment, the quality percentage composition of tungsten is 5.12%～5.14%, the quality percentage composition of molybdenum is 1.95%～2.02%, the quality percentage composition of zirconium is 1.70%～1.75%, the quality percentage composition of oxygen is 0.015%～0.02%, illustrates that the niobium tungsten zirconium alloy ingot casting of the present embodiment has good structural constituent homogeneity.
The above, be only preferred embodiment of the present invention, not the present invention imposed any restrictions.Every any simple modification of above embodiment being done according to invention technical spirit, change and equivalence change, and all still belong in the protection domain of technical solution of the present invention.

Claims (6)

1. a preparation method for niobium tungsten zirconium alloy ingot casting, is characterized in that, the method comprises the following steps:
Step 1, many length are to 300mm～1500mm, the niobium tungsten metal strip (1) that width and thickness are 14mm～16mm neatly stacks, making the total length of the niobium tungsten metal strip after neatly stacking is 1200mm～1500mm, total width is 42mm～48mm, total thickness is 56mm～64mm, niobium tungsten metal strip after neatly stacking middle part level is laid the first pure zirconium plate (2) again, then the niobium tungsten metal strip being equipped with after neatly the stacking of the first pure zirconium plate (2) is placed in to argon arc welding case, niobium tungsten metal strip by the first pure zirconium plate (2) and after neatly stacking carries out argon arc welding, obtain smelting electrode, the length of described the first pure zirconium plate (2) and width all with neatly stack after niobium tungsten metal strip identical, the weight of described the first pure zirconium plate (2) is 1.2%～1.25% of smelting electrode weight, in many described niobium tungsten metal strips (1), the quality percentage composition of tungsten is 4.7%～5.0%, and the quality percentage composition of molybdenum is 2.0%～2.3%, and surplus is niobium and inevitable impurity,
Step 2, smelting electrode described in step 1 is placed in to vacuum electron beam melting furnace, is not more than 2.0 × 10 in vacuum tightness -2under the condition of Pa, carry out twice vacuum electron beam melting, obtain work in-process ingot casting (3); The cross section of described work in-process ingot casting (3) is that diameter is the circle of 85mm～105mm;
Step 3, the second pure zirconium plate that is 2.0mm by thickness are cut into many length and are 100mm, width is the pure zirconium bar (4) of 8mm～13mm, and the gross weight of many described pure zirconium bars (4) is 0.5%～0.75% of work in-process ingot casting described in step 2 (3) weight;
Step 4, employing iron wire (5) all adhere well to many described pure zirconium bars (4) in step 3 the outside surface of work in-process ingot casting (3), then the work in-process ingot casting (3) that outside surface is pasted with to many pure zirconium bars (4) is placed in argon arc welding case, many described pure zirconium bars (4) are all carried out to argon arc welding with work in-process ingot casting (3), remove afterwards iron wire (5), obtain arc melting consumable electrode; Many described pure zirconium bars (4) are all parallel with work in-process ingot casting (3) along its length;
Step 5, arc melting described in step 4 is placed in to vacuum consumable arc-melting stove with consumable electrode carries out vacuum consumable arc-melting twice, obtain niobium tungsten zirconium alloy ingot casting; In described niobium tungsten zirconium alloy ingot casting, the quality percentage composition of zirconium is 1.65%～1.75%;
In step 4, many described pure zirconium bars (4) adhere well to the concrete system of work in-process ingot casting (3) outside surface and are: be first one group by every many described pure zirconium bars (4) 3 and be divided into into n group, wherein n is that positive integer and n meet: 10≤n≤17, then every group of pure zirconium bar (4) all evenly laid at work in-process ingot casting (3) outside surface, wherein first group of pure zirconium bar (4) one end is concordant with work in-process ingot casting (3) one end, 30 ° of second group of pure zirconium bar (4) one end and relative first group of pure zirconium bar (4) circumferential offset concordant with first group of pure zirconium bar (4) the other end, 30 ° of the 3rd group of pure zirconium article (4) one end and relative second group of pure zirconium article (4) circumferential offset concordant with second group of pure zirconium article (4) the other end, the rest may be inferred, until n organize pure zirconium article (4) one end and (n-1) organize pure zirconium article (4) the other end concordant and relative (n-1) organize 30 ° of pure zirconium article (4) circumferential offset, keep second group of pure zirconium article (4) consistent to the direction that n organizes pure zirconium article (4) circumferential offset.
2. the preparation method of a kind of niobium tungsten zirconium alloy ingot casting according to claim 1, is characterized in that, in step 1, the density of many niobium tungsten metal strips (1) is 7.9g/cm 3～8.4g/cm 3.
3. the preparation method of a kind of niobium tungsten zirconium alloy ingot casting according to claim 1, it is characterized in that, in the ingot casting of work in-process described in step 2 (3), the quality percentage composition of zirconium is 1.0%～1.15%, and the quality percentage composition of oxygen is not more than 0.01%.
4. the preparation method of a kind of niobium tungsten zirconium alloy ingot casting according to claim 1, it is characterized in that, the integral multiple that the length value of the ingot casting of work in-process described in step 2 (3) is 100, the unit of described work in-process ingot casting (3) length is mm.
5. the preparation method of a kind of niobium tungsten zirconium alloy ingot casting according to claim 1, it is characterized in that, in step 5, the detailed process of twice vacuum consumable arc-melting is: first described arc melting is not more than in vacuum tightness with consumable electrode under the condition of 1.0Pa and carries out vacuum consumable arc-melting for the first time, obtaining diameter is an ingot casting of 160mm; Then using the head of a described ingot casting as the initiating terminal of vacuum consumable arc-melting for the second time, a described ingot casting is not more than in vacuum tightness under the condition of 1.0Pa and carries out vacuum consumable arc-melting for the second time, obtaining diameter is the niobium tungsten zirconium alloy ingot casting of 200mm.
6. the preparation method of a kind of niobium tungsten zirconium alloy ingot casting according to claim 1, is characterized in that, in the tungsten of niobium described in step 5 zirconium alloy ingot casting, the quality percentage composition of oxygen is not more than 0.02%.
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