CN104831093A - Zr-2.5Nb alloy casting ingot preparation method - Google Patents
Zr-2.5Nb alloy casting ingot preparation method Download PDFInfo
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Abstract
The present invention discloses a Zr-2.5Nb alloy casting ingot preparation method, which specifically comprises: welding an electrode block obtained by pressing Zr-Nb mixed powder and a sponge zirconium layered cloth into an electrode, and carrying out hollow consumable electrical arc smelting on the electrode three times to obtain the Zr-2.5Nb alloy casting ingot. According to the present invention, the Nb addition way is optimized and the single electrode-cloth mixed material is used so as to uniformly distribute Nb and Zr, the smelting process control is combined, and the three- consumable electrical arc smelting is used to obtain the Zr-2.5Nb alloy casting ingot with characteristics of low impurity content and uniform component. The method is suitable for industrial production.
Description
Technical field
The invention belongs to reasonable offer field, relate to a kind of preparation method of Zr-2.5Nb alloy cast ingot.
Background technology
Zirconium base alloy has low neutron-absorption cross-section, high-mechanical property, low irradiation creep performance and high corrosion resistance in reactor environment, is often used as setting-out to material.At present, water-cooled atomic power heap fuel coating material and pressure tube material mostly adopt Zr-2 and Zr-4 alloy.Zr-2.5Nb alloy is often used as setting-out to material and heavy water cooled reactor penstock etc.
Containing high-density, high-melting-point element nb in Zr-2.5Nb alloy, its fusing point is up to 2468 DEG C, and the fusing point of metallic Z r is only 1852 DEG C, and the two fusing point differs greatly, and in alloy melting process, is easy to form Nb niggerhead; Simultaneously because metal Nb density is 8.57g/cm
3, the density of metallic Z r is only 6.49g/cm
3, Nb element density is comparatively large, in alloy melting process, is easy to form gravity segregation.Therefore, adopt conventional vacuum consumable smelting technique cannot ensure Zr-2.5Nb alloy, and very easily form the metallurgical imperfection of Nb niggerhead.
Summary of the invention
The object of this invention is to provide a kind of preparation method of Zr-2.5Nb alloy cast ingot, solve the uneven of the Zr-2.5Nb alloying constituent that existing method prepares, easily produce the problem of segregation and niggerhead.
The technical solution adopted in the present invention is, a kind of preparation method of Zr-2.5Nb alloy cast ingot, specifically implements according to the following steps:
Step 1, prepare electrode block:
Nb powder and sponge zirconium powder Homogeneous phase mixing are made Zr-Nb powder mix, Zr-Nb powder mix and zirconium sponge is carried out layer-by-layer distribution, and bed of cloth is pressed into electrode block;
Step 2, prepare electrode:
With the electrode block that clamp step 1 prepares, be welded to connect and become electrode;
Step 3, melting:
Electrode step 2 obtained is inserted in vacuum consumable electrode arc furnace, and vacuum melting three times, namely obtains Zr-2.5Nb alloy cast ingot.
Feature of the present invention is also,
In step 1, the blending ratio of Nb powder and sponge zirconium powder is 1:1 in mass ratio.
In step 1, Nb Powder Particle Size is less than 200 orders, and zirconium sponge Powder Particle Size is less than 400 orders, and zirconium sponge granularity is at 2 ~ 8mm.
In step 1, electrode pressing pressure is 25 ~ 30MPa, dwell time 10 ~ 20s.
In step 2, electrode welding adopts water-cooled copper-base argon shield weldering.
In step 3, the parameter of three vacuum meltings is respectively:
Melting once: molten initial vacuum degree≤1.5Pa, leak rate≤0.8Pa/min, melting voltage 28 ~ 33V, melting electric current 6 ~ 9kA, stabilising arc current DC 4.0 ~ 8.0A, cooling time is greater than 2h;
Secondary smelting: molten initial vacuum degree≤1.5Pa, leak rate≤0.8Pa/min, melting voltage 30 ~ 34V, melting electric current 8 ~ 12kA, stabilising arc electric current exchanges 6.0 ~ 10.0A, and cooling time is greater than 3h;
Three meltings: molten initial vacuum degree≤1.0Pa, leak rate≤0.5Pa/min, melting voltage 30 ~ 33V, melting electric current 8 ~ 11kA, stabilising arc electric current exchanges 4.0 ~ 8.0A, and cooling time is greater than 4h.
In step 3, the crucible specification of melting once is Φ 280mm.
In step 3, the crucible specification of secondary smelting is Φ 360mm.
The crucible specification of three meltings in step 3 is Φ 440mm.
The invention has the beneficial effects as follows, by optimizing the addition manner of Nb element, adopt single-piece electrode interspersion material, Nb, Zr element is uniformly distributed, in conjunction with the process control of melting, adopt the mode of three consumable arc-meltings, obtain that foreign matter content is low, the Zr-2.5Nb titan alloy casting ingot of uniform composition, be applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 be the embodiment of the present invention prepare Zr-2.5Nb alloy cast ingot head, middle part and afterbody Nb element genesis analysis figure.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
The invention provides a kind of preparation method of Zr-2.5Nb alloy cast ingot, specifically implement according to the following steps:
Step 1, prepare electrode block:
By Nb powder and sponge zirconium powder in mass ratio 1:1 Homogeneous phase mixing make Zr-Nb powder mix, Zr-Nb powder mix and zirconium sponge are carried out layer-by-layer distribution, and with large hydraulic press, bed of cloth is pressed into electrode block, pressing pressure is 25 ~ 30MPa, dwell time 10 ~ 20s.
Wherein Nb Powder Particle Size is less than 200 orders, and zirconium sponge Powder Particle Size is less than 400 orders, and zirconium sponge granularity is at 2 ~ 8mm.
Layer-by-layer distribution zirconium sponge and Zr-Nb powder mix is divided into some parts respectively, then one deck sponge zirconium powder, and one deck Zr-Nb powder mix, carries out cloth successively.In the present invention, zirconium sponge equivalent is divided into 4 parts, Zr-Nb powder mix equivalent is divided into three parts, then one deck zirconium sponge, one deck Zr-Nb powder mix carries out cloth.The number of plies of layer-by-layer distribution can be adjusted as required in actual production.
Step 2, prepare electrode:
With the electrode block that clamp step 1 prepares, adopting water-cooled copper-base argon shield weldering to be welded to connect by electrode block becomes electrode.
Solder joint requires that electrode electrode used therein number of blocks is determined according to crucible length for silver gray or faint yellow.
Step 3, melting:
Electrode step 2 obtained is inserted in vacuum consumable electrode arc furnace, and vacuum melting three times, namely obtains Zr-2.5Nb alloy cast ingot.
In order to obtain the ingot casting of interior tissue and uniform composition, after molten bath is formed, need control melting electric current, voltage and stabilising arc parameter, to guarantee the stability of fusion process, the design parameter of three vacuum meltings controls as follows:
Melting once: crucible specification Φ 280mm, molten initial vacuum degree≤1.5Pa, leak rate≤0.8Pa/min, melting voltage 28 ~ 33V, melting electric current 6 ~ 9kA, stabilising arc current DC 4.0 ~ 8.0A, cooling time is greater than 2h;
Secondary smelting: crucible specification Φ 360mm, molten initial vacuum degree≤1.5Pa, leak rate≤0.8Pa/min, melting voltage 30 ~ 34V, melting electric current 8 ~ 12kA, stabilising arc electric current exchanges 6.0 ~ 10.0A, and cooling time is greater than 3h;
Three meltings: crucible specification Φ 440mm, molten initial vacuum degree≤1.0Pa, leak rate≤0.5Pa/min, melting voltage 30 ~ 33V, melting electric current 8 ~ 11kA, stabilising arc electric current exchanges 4.0 ~ 8.0A, and cooling time is greater than 4h.
The present invention, by selecting higher-grade 2 ~ 8mm small-particle zirconium sponge, strictly controls the impurity content in starting material; Select high-quality Nb powder (granularity is less than 200 orders) and sponge zirconium powder (granularity is less than 400 orders), preparation Zr-Nb powder mix, ensure that mixing of powder mix, and can obtain closely knit electrode block after compacting; Single-piece electrode interspersion material will be adopted before electrode compacting, electrode block cloth can be made more even; Adopt vacuum consumable electrode arc furnace to carry out three meltings, fusion process strictly controls vacuum tightness, leak rate, smelting parameter etc., makes that the horizontal and vertical homogeneity of whole ingot casting composition is all improved, foreign matter content reduces.
Embodiment 1
By 120 object Nb powder and 200 order sponge zirconium powders in mass ratio 1:1 Homogeneous phase mixing make Zr-Nb powder mix, Zr-Nb powder mix and 2 ~ 4mm zirconium sponge are carried out layer-by-layer distribution, by large hydraulic press pressure, bed of cloth is pressed into electrode block, pressing pressure is 30MPa, dwell time 10s.Use clamp electrode block, adopt water-cooled copper-base argon shield weldering that electrode block is welded into electrode.
Inserted by electrode in vacuum consumable electrode arc furnace, vacuum melting obtains Zr-2.5Nb alloy cast ingot three times, and concrete technology parameter is:
Melting once: crucible specification Φ 280mm, molten initial vacuum degree 1.5Pa, leak rate 0.8Pa/min, melting voltage 28V, melting electric current 6kA, stabilising arc current DC 4.0A, cooling time 2.5h;
Secondary smelting: crucible specification Φ 360mm, molten initial vacuum degree 1.5Pa, leak rate 0.8Pa/min, melting voltage 30V, melting electric current 8kA, stabilising arc electric current exchanges 6.0A, cooling time 3.2h;
Three meltings: crucible specification Φ 440mm, molten initial vacuum degree 1.0Pa, leak rate 0.5Pa/min, melting voltage 30V, melting electric current 8kA, stabilising arc electric current exchanges 4.0A, cooling time 4.3h.
Embodiment 2
By 140 object Nb powder and 270 order sponge zirconium powders in mass ratio 1:1 Homogeneous phase mixing make Zr-Nb powder mix, Zr-Nb powder mix and 4 ~ 6mm zirconium sponge are carried out layer-by-layer distribution, by large hydraulic press pressure, bed of cloth is made electrode block, pressing pressure is 27MPa, dwell time 15s.Use clamp electrode block, adopt water-cooled copper-base argon shield weldering that electrode block is welded into electrode.
Inserted by electrode in vacuum consumable electrode arc furnace, vacuum melting obtains Zr-2.5Nb alloy cast ingot three times, and concrete technology parameter is:
Melting once: crucible specification Φ 280mm, molten initial vacuum degree 1.3Pa, leak rate 0.5Pa/min, melting voltage 30V, melting electric current 8kA, stabilising arc current DC 6.0A, cooling time 3h;
Secondary smelting: crucible specification Φ 360mm, molten initial vacuum degree 1.2Pa, leak rate 0.7Pa/min, melting voltage 32V, melting electric current 10kA, stabilising arc electric current exchanges 8.0A, cooling time 3.5h;
Three meltings: crucible specification Φ 440mm, molten initial vacuum degree 0.8Pa, leak rate 0.3Pa/min, melting voltage 31V, melting electric current 10kA, stabilising arc electric current exchanges 6.0A, cooling time 5h.
Embodiment 3
By 170 object Nb powder and 325 order sponge zirconium powders in mass ratio 1:1 Homogeneous phase mixing make Zr-Nb powder mix, Zr-Nb powder mix and 6 ~ 8mm zirconium sponge are carried out layer-by-layer distribution, by large hydraulic press pressure, bed of cloth is made electrode block, pressing pressure is 25MPa, dwell time 20s.Use clamp electrode block, adopt water-cooled copper-base argon shield weldering that electrode block is welded into electrode.
Inserted by electrode in vacuum consumable electrode arc furnace, vacuum melting obtains Zr-2.5Nb alloy cast ingot three times, and concrete technology parameter is:
Melting once: crucible specification Φ 280mm, molten initial vacuum degree 1.0Pa, leak rate 0.7Pa/min, melting voltage 33V, melting electric current 9kA, stabilising arc current DC 8.0A, cooling time 2.8h;
Secondary smelting: crucible specification Φ 360mm, molten initial vacuum degree 1.0Pa, leak rate 0.5Pa/min, melting voltage 34V, melting electric current 12kA, stabilising arc electric current exchanges 10.0A, cooling time 4h;
Three meltings: crucible specification Φ 440mm, molten initial vacuum degree 0.6Pa, leak rate 0.4Pa/min, melting voltage 33V, melting electric current 11kA, stabilising arc electric current exchanges 8.0A, cooling time 4.8h.
Fig. 1 is Zr-2.5Nb alloy cast ingot head, middle part and afterbody Nb element genesis analysis figure, to the 3 batches of specifications prepared in embodiment be the Zr-2.5Nb alloy cast ingot of Φ 440mm longitudinal head, in, 3, tail and cross section 5 sampling, chemical composition detection is carried out to its principal element and impurity element, each elemental composition in each position of data presentation ingot casting be evenly distributed and batch between stability better; To ingot casting head, in, tail bit section carry out X-ray transmission, result display do not find any component segregation and metallurgical imperfection.
Claims (9)
1. a preparation method for Zr-2.5Nb alloy cast ingot, is characterized in that, specifically implements according to the following steps:
Step 1, prepare electrode block:
Nb powder and sponge zirconium powder Homogeneous phase mixing are made Zr-Nb powder mix, Zr-Nb powder mix and zirconium sponge is carried out layer-by-layer distribution, and bed of cloth is pressed into electrode block;
Step 2, prepare electrode:
Electrode is welded to connect into the electrode block that clamp step 1 prepares;
Step 3, melting:
Electrode step 2 obtained is inserted in vacuum consumable electrode arc furnace, and vacuum melting three times, namely obtains Zr-2.5Nb alloy cast ingot.
2. the preparation method of a kind of Zr-2.5Nb alloy cast ingot according to claim 1, is characterized in that, in described step 1, the blending ratio of Nb powder and sponge zirconium powder is 1:1 in mass ratio.
3. the preparation method of a kind of Zr-2.5Nb alloy cast ingot according to claim 1, it is characterized in that, in described step 1, Nb Powder Particle Size is less than 200 orders, and zirconium sponge Powder Particle Size is less than 400 orders, and zirconium sponge granularity is at 2 ~ 8mm.
4. the preparation method of a kind of Zr-2.5Nb alloy cast ingot according to claim 1, is characterized in that, in described step 1, electrode pressing pressure is 25 ~ 30MPa, dwell time 10 ~ 20s.
5. the preparation method of a kind of Zr-2.5Nb alloy cast ingot according to claim 1, is characterized in that, in described step 2, electrode welding adopts water-cooled copper-base argon shield weldering.
6. the preparation method of a kind of Zr-2.5Nb alloy cast ingot according to claim 1, it is characterized in that, in described step 3, the parameter of three vacuum meltings is respectively:
Melting once: molten initial vacuum degree≤1.5Pa, leak rate≤0.8Pa/min, melting voltage 28 ~ 33V, melting electric current 6 ~ 9kA, stabilising arc current DC 4.0 ~ 8.0A, cooling time is greater than 2h;
Secondary smelting: molten initial vacuum degree≤1.5Pa, leak rate≤0.8Pa/min, melting voltage 30 ~ 34V, melting electric current 8 ~ 12kA, stabilising arc electric current exchanges 6.0 ~ 10.0A, and cooling time is greater than 3h;
Three meltings: molten initial vacuum degree≤1.0Pa, leak rate≤0.5Pa/min, melting voltage 30 ~ 33V, melting electric current 8 ~ 11kA, stabilising arc electric current exchanges 4.0 ~ 8.0A, and cooling time is greater than 4h.
7. the preparation method of a kind of Zr-2.5Nb alloy cast ingot according to claim 6, is characterized in that, in described step 3, the crucible specification of melting once is Φ 280mm.
8. the preparation method of a kind of Zr-2.5Nb alloy cast ingot according to claim 6, is characterized in that, in described step 3, the crucible specification of secondary smelting is Φ 360mm.
9. the preparation method of a kind of Zr-2.5Nb alloy cast ingot according to claim 6, is characterized in that, the crucible specification of three meltings in described step 3 is Φ 440mm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105950912A (en) * | 2016-06-30 | 2016-09-21 | 西部超导材料科技股份有限公司 | Preparation method for medical Zr-2.5 Nb alloy ingot |
| CN112501448A (en) * | 2020-11-11 | 2021-03-16 | 湖南金天钛业科技有限公司 | Method for smelting alloy in vacuum consumable mode |
| RU2800271C1 (en) * | 2022-03-04 | 2023-07-19 | Акционерное общество "Чепецкий механический завод" | Method for manufacturing ingots of zirconium alloys |
| WO2023167611A1 (en) * | 2022-03-04 | 2023-09-07 | Акционерное общество "Чепецкий механический завод" | Method for producing ingots of zirconium alloys based on magnesiothermic sponge |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102051493A (en) * | 2011-01-26 | 2011-05-11 | 西北有色金属研究院 | Preparation method of multielement titanium alloy |
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- 2015-04-14 CN CN201510176470.8A patent/CN104831093A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051493A (en) * | 2011-01-26 | 2011-05-11 | 西北有色金属研究院 | Preparation method of multielement titanium alloy |
Non-Patent Citations (1)
| Title |
|---|
| 张孝全等: "Zr-2.5Nb合金的研究及重水堆压力管的试制", 《稀有金属合金加工》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105950912A (en) * | 2016-06-30 | 2016-09-21 | 西部超导材料科技股份有限公司 | Preparation method for medical Zr-2.5 Nb alloy ingot |
| CN112501448A (en) * | 2020-11-11 | 2021-03-16 | 湖南金天钛业科技有限公司 | Method for smelting alloy in vacuum consumable mode |
| CN112501448B (en) * | 2020-11-11 | 2022-05-03 | 湖南金天钛业科技有限公司 | Method for smelting alloy in vacuum consumable mode |
| RU2800271C1 (en) * | 2022-03-04 | 2023-07-19 | Акционерное общество "Чепецкий механический завод" | Method for manufacturing ingots of zirconium alloys |
| WO2023167611A1 (en) * | 2022-03-04 | 2023-09-07 | Акционерное общество "Чепецкий механический завод" | Method for producing ingots of zirconium alloys based on magnesiothermic sponge |
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Application publication date: 20150812 |