CN114058887B - Preparation method of thorium-containing iridium alloy - Google Patents
Preparation method of thorium-containing iridium alloy Download PDFInfo
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- CN114058887B CN114058887B CN202111373867.8A CN202111373867A CN114058887B CN 114058887 B CN114058887 B CN 114058887B CN 202111373867 A CN202111373867 A CN 202111373867A CN 114058887 B CN114058887 B CN 114058887B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/04—Alloys based on a platinum group metal
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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Abstract
The invention discloses a preparation method of thorium-containing iridium alloy, which comprises the following steps: (1) high-purity iridium powder is adopted as a raw material and is pressed on a cold isostatic press to obtainObtaining a pressed iridium block; (2) sequentially putting the iridium blocks into a hydrogen pre-sintering furnace and a vacuum high-temperature sintering furnace for sintering to obtain sintered iridium blocks; (3) transferring the iridium block obtained by sintering to an electric arc melting furnace to be melted with tungsten-thorium alloy to obtain thorium-containing iridium alloy; (4) and cleaning the iridium alloy ingot, transferring the iridium alloy ingot to an electron beam furnace for smelting, and pouring to obtain the thorium-doped iridium tungsten alloy ingot. According to the invention, tungsten and thorium doped elements are introduced through the tungsten-thorium electrode in the electric arc melting process, so that the preparation process of the conventional thorium-containing iridium alloy can be simplified, and the uniformity of the doped elements can be ensured to the greatest extent. By adjusting the content of thorium in the tungsten-thorium electrode, the regulation and control of the content of thorium in the iridium alloy can be realized. Meanwhile, the prepared alloy has the characteristics of small grain size and excellent performance, and meets the requirements of 238 The need for cladding material for Pu isotope power supplies.
Description
Technical Field
The invention belongs to the technical field of isotope heat source, power supply and noble metal manufacturing, and particularly relates to a preparation method of thorium-containing iridium alloy.
Background
The melting point of the iridium is 2450 ℃, the use temperature can reach 2200 ℃, the iridium does not have obvious oxidation phenomenon under the atmospheric environment below 1000 ℃, has better high-temperature endurance strength and creep strength, and still has good mechanical property at about 1600 ℃, so the iridium is ideal 238 Pu isotope power supply cladding material. However, pure iridium has poor processability and is brittle under high temperature conditions, and needs to be improved by alloying with other elements. In the United states of America 238 The main preparation process of the iridium alloy used in the Pu isotope power supply comprises the following steps: firstly adding tungsten element into iridium raw material and adopting electron beamSmelting to prepare iridium-tungsten alloy, adding thorium and aluminum elements to perform electric arc smelting, and finally performing electron beam smelting and electric arc smelting to obtain the iridium-tungsten alloy. The preparation process is complex, and the uniformity control difficulty of the trace elements added in the smelting process is high. Therefore, the preparation process of the tungsten-thorium alloy is improved, and the thorium-containing iridium alloy with uniform components and excellent performance is obtained for China 238 The development of Pu isotope power supplies is of great significance.
Disclosure of Invention
The invention aims to provide a preparation method of thorium-containing iridium alloy.
The technical scheme of the invention is as follows:
a preparation method of thorium-containing iridium alloy is characterized by comprising the following steps:
tungsten-thorium alloy is used as an electrode, the tungsten-thorium alloy and an iridium block which is pressed and sintered are smelted for multiple times in a vacuum electric arc furnace, and impurities are removed by electron beam smelting, so that the thorium-containing uniform iridium alloy can be obtained. The method comprises the following specific steps:
(1) pressing high-purity iridium powder serving as a raw material on a cold isostatic press to obtain a pressed iridium block;
(2) sequentially putting the iridium blocks into a hydrogen pre-sintering furnace and a vacuum high-temperature sintering furnace for sintering to obtain sintered iridium blocks; (ii) a
(3) Transferring the iridium block obtained by sintering into an electric arc melting furnace to be melted with tungsten-thorium alloy to obtain thorium-containing iridium alloy;
(4) cleaning the iridium alloy, transferring the iridium alloy to an electron beam melting furnace for melting, and casting to obtain the thorium-doped iridium alloy cast ingot.
Wherein, the content of thorium in the tungsten-thorium alloy electrode is 1-4%.
Wherein, the working parameters of the electric arc melting furnace are as follows: current 400A, vacuum degree less than 1.9X 10 -2 Pa。
Wherein the frequency of arc melting is more than 4.
Wherein, the parameters of the electron beam melting furnace are as follows: the beam current is 188mA, the vacuum degree is less than 8.4 multiplied by 10 < -4 > Pa, and the smelting times are more than 2 times;
wherein the purity of the iridium powder raw material is more than 99.9 percent; the pressing force of the cold isostatic press is 80MPa to 100MPa, and each pressed iridium block weighs 30g to 50 g.
Wherein the working parameters of the hydrogen pre-sintering furnace are as follows: the sintering temperature is 1000 ℃, the sintering time is 1-2 h, and the sintering atmosphere is hydrogen.
Wherein the working parameters of the vacuum high-temperature sintering furnace are as follows: the sintering temperature is 1500 ℃, the sintering time is 4-6 h, and the vacuum degree is less than 1.0 multiplied by 10 -2 Pa。
Wherein, the iridium alloy ingot is cleaned by aqua regia, and the cleaning time is more than 5 min.
The preparation method has the advantages that:
the method adopts tungsten-thorium alloy as an electrode, the tungsten-thorium alloy is smelted with a pressed and sintered iridium block in an electric arc furnace, and impurities are removed by electron beam smelting, so that the thorium-containing uniform iridium alloy can be obtained. Tungsten and thorium doped elements are introduced simultaneously through a tungsten-thorium electrode in the electric arc melting process, the existing preparation process of the thorium-containing iridium alloy can be simplified, and the uniformity of the doped elements can be ensured to the maximum extent through repeated electric arc melting. By adjusting the content of thorium in the tungsten-thorium electrode, the regulation and control of the content of thorium in the iridium alloy can be realized. In addition, compared with a powder metallurgy method, the method does not need ball milling, and reduces the loss in the ball milling process; compared with pure electric arc melting, the method further removes volatile impurities through electron beam melting, can eliminate dendrite segregation and internal stress, improves the plasticity of the iridium alloy, and has better performance.
Detailed Description
Example 1
The iridium alloy of the embodiment comprises the following components in percentage by mass: w3400ppm, Th 68ppm, the balance Ir and unavoidable impurities.
The preparation of the iridium alloy of the embodiment comprises the following steps:
step (1), weighing 35g of iridium powder with the purity of 99.95%, transferring the iridium powder to a mold, and pressing the iridium powder in a cold isostatic press with the pressing force of 80 MPa;
and (2) transferring the pressed iridium block into a hydrogen furnace for presintering, wherein the working parameters are as follows: the sintering temperature is 1000 ℃, the sintering time is 1h, and the sintering atmosphere is hydrogen:
sinteringTransferring the iridium block to a vacuum high-temperature sintering furnace for sintering, wherein the working parameters are as follows: the sintering temperature is 1500 ℃, the sintering time is 4 hours, and the vacuum degree is less than 1.0 multiplied by 10 -2 Pa。
Step (3), transferring the iridium block into a vacuum arc melting furnace, adding 120mg of tungsten-thorium alloy electrode with Th content of 2 wt%, setting current 400A, and keeping vacuum degree less than 1.9 multiplied by 10 -2 Smelting for 6 times;
step (4), soaking the iridium alloy ingot obtained by smelting in aqua regia for 10min, cleaning and drying;
transferring the iridium alloy ingot into an electron beam smelting furnace, setting an electron beam current of 188mA, and keeping the vacuum degree to be less than 8.4 multiplied by 10 - 4 Pa, smelting for 3 times;
pouring into thorium-doped iridium tungsten alloy cast ingots by adopting a water-cooling copper mold.
The present invention is not limited to the above-described embodiments, and those skilled in the art will be able to make various modifications without creative efforts from the above-described conception, and fall within the scope of the present invention.
Claims (9)
1. A preparation method of thorium-containing iridium alloy is characterized by comprising the following steps:
the method comprises the following specific steps:
(1) pressing high-purity iridium powder serving as a raw material on a cold isostatic press to obtain a pressed iridium block;
(2) sequentially putting the iridium blocks into a hydrogen pre-sintering furnace and a vacuum high-temperature sintering furnace for sintering to obtain sintered iridium blocks;
(3) transferring the iridium block obtained by sintering into an electric arc melting furnace to be repeatedly melted with tungsten-thorium alloy to obtain thorium-containing iridium alloy;
(4) cleaning the thorium-containing iridium alloy, transferring the thorium-containing iridium alloy to an electron beam furnace for smelting, and pouring to obtain a thorium-doped iridium tungsten alloy cast ingot.
2. The method for preparing the thorium-containing iridium alloy according to claim 1, wherein the content of thorium in the tungsten-thorium alloy electrode is 1-4%.
3. The method for preparing the thorium-iridium alloy in claim 1, wherein the operating parameters of an electric arc smelting furnace are as follows: the current is 400A, and the vacuum degree is less than 1.9 multiplied by 10-2 Pa.
4. The method for preparing the thoriated iridium alloy according to claim 1, wherein the number of times of arc melting is more than 4.
5. The method for preparing the thoriated iridium alloy according to claim 1, wherein the parameters of an electron beam melting furnace are as follows: the beam current is 188mA, the vacuum degree is less than 8.4 multiplied by 10 < -4 > Pa, and the smelting times are more than 2 times.
6. The preparation method of the thorium-containing iridium alloy according to claim 1, wherein in the step (1), the purity of the iridium powder raw material is more than 99.9%; the pressing force of the cold isostatic press is 80MPa to 100MPa, and each pressed iridium block weighs 30g to 50 g.
7. The method for preparing the thorium-containing iridium alloy as claimed in claim 1, wherein in the step (2), the operating parameters of the hydrogen pre-sintering furnace are as follows: the sintering temperature is 1000 ℃, the sintering time is 1-2 h, and the sintering atmosphere is hydrogen.
8. The preparation method of the thorium-containing iridium alloy according to claim 1, wherein in the step (2), the working parameters of the vacuum high-temperature sintering furnace are as follows: the sintering temperature is 1500 ℃, the sintering time is 4-6 h, and the vacuum degree is less than 1.0 multiplied by 10 < -2 > Pa.
9. The method for preparing the thorium-containing iridium alloy according to claim 1, wherein in the step (4), aqua regia is adopted for cleaning the iridium alloy ingot, and the cleaning time is more than 5 min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4253872A (en) * | 1977-02-16 | 1981-03-03 | The United States Of America As Represented By The United States Department Of Energy | Thorium doped iridium alloy for radioisotope heat sources |
| CN101831568A (en) * | 2010-05-21 | 2010-09-15 | 西北有色金属研究院 | Method for preparing superhigh temperature resistant iridium alloy by using powder metallurgy method |
| CN102168200B (en) * | 2011-03-29 | 2012-07-11 | 西北有色金属研究院 | Preparation method of the high-density iridium alloy billet |
| CN110079719B (en) * | 2019-06-13 | 2020-04-17 | 西北有色金属研究院 | Method for increasing hafnium content in tantalum-tungsten alloy |
| CN111961897B (en) * | 2020-09-14 | 2022-03-29 | 大连理工大学 | Method for preparing high-purity nickel-based high-temperature alloy by vacuum induction melting-casting-electron beam refining process |
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