CN110672611B - A method for identifying delta phase hydrides and FCC-Zr precipitates in zirconium alloys - Google Patents
A method for identifying delta phase hydrides and FCC-Zr precipitates in zirconium alloys Download PDFInfo
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- 150000004678 hydrides Chemical class 0.000 title claims abstract description 40
- 229910001093 Zr alloy Inorganic materials 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000002244 precipitate Substances 0.000 title abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000010453 quartz Substances 0.000 claims abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000008859 change Effects 0.000 claims abstract description 6
- 229910052786 argon Inorganic materials 0.000 claims abstract description 5
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 238000001556 precipitation Methods 0.000 claims abstract 9
- 230000005540 biological transmission Effects 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 abstract description 10
- 238000011160 research Methods 0.000 abstract description 5
- 238000012360 testing method Methods 0.000 abstract description 4
- 229910045601 alloy Inorganic materials 0.000 description 11
- 239000000956 alloy Substances 0.000 description 11
- 239000011159 matrix material Substances 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 5
- 229910052726 zirconium Inorganic materials 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000009461 vacuum packaging Methods 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000010587 phase diagram Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011824 nuclear material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000012858 packaging process Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000001226 reprecipitation Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
本发明提供一种鉴别锆合金中δ相氢化物和FCC‑Zr析出相的方法，具体步骤为：对锆合金样品中需要鉴别是FCC‑Zr相或者δ相氢化物的析出相进行观察分析，记录并标记其准确位置；将上述中锆合金样品采用石英管真空封装，并充以惰性气体氩气保护；将封装后的锆合金样品置于箱式电阻炉中，将炉温保持在500～600℃静置1～10小时后空冷；待锆合金样品冷却后破碎石英管，取出锆合金样品，然后对于锆合金相同位置进行观察分析，如果析出相消失或尺寸明显减小，则为δ相氢化物，若析出相仍然存在或析出相尺寸基本无变化，则为FCC‑Zr析出相。本发明通过简单的热处理可实现对锆合金中复杂的析出相的结构鉴别，便于试验中操作，简单实用，成本低廉，对于锆合金的研究具有重要意义。
The invention provides a method for identifying δ-phase hydrides and FCC-Zr precipitation phases in zirconium alloys. The specific steps are as follows: observing and analyzing the precipitation phases that need to be identified as FCC-Zr phases or δ-phase hydrides in a zirconium alloy sample, Record and mark its exact position; the above-mentioned medium zirconium alloy samples are vacuum-sealed in a quartz tube and filled with inert gas argon for protection; the packaged zirconium alloy samples are placed in a box-type resistance furnace, and the furnace temperature is kept at 500~ After standing at 600℃ for 1-10 hours, air cooling; after the zirconium alloy sample is cooled, break the quartz tube, take out the zirconium alloy sample, and then observe and analyze the same position of the zirconium alloy. If the precipitate phase disappears or the size is significantly reduced, it is the delta phase Hydride, if the precipitate still exists or the size of the precipitate does not change substantially, it is the FCC-Zr precipitate. The invention can realize the structure identification of the complex precipitation phase in the zirconium alloy through simple heat treatment, is convenient for operation in the test, is simple and practical, and has low cost, and is of great significance to the research of the zirconium alloy.
Description
Technical Field
The invention belongs to the field of zirconium alloy, and particularly provides a method for identifying delta-phase hydride and FCC-Zr precipitated phase in zirconium alloy.
Background
The zircaloy has a low thermal neutron absorption cross section, good corrosion resistance and moderate mechanical properties, and is widely applied to core structural materials (such as fuel cladding, pressure pipe, support, orifice pipe and the like) of nuclear reactors. The zirconium alloy service environment is high-temperature high-pressure water and steam at the temperature of 300-400 ℃, oxygen in the water reacts with the zirconium matrix to form zirconium oxide, hydrogen atoms are released, and the hydrogen atoms are fused into the zirconium matrix. When the concentration of hydrogen exceeds the solubility limit of the matrix zirconium, hydrides may precipitate in the matrix of zirconium and zirconium alloys. The hydride is a typical brittle phase, the presence of the hydride can deteriorate the strength and toughness of the material, and the hydride can also generate certain growth stress due to volume expansion during the formation process. The presence of hydrides can lead to failure of the reactor structure, which can ultimately affect the quality and safety of the reactor operation. Based on the specificity of the materials for nuclear reactors, the formation mechanism, morphology, distribution and control manner of hydrides in zirconium alloys have been receiving attention from researchers of nuclear materials.
The FCC-Zr precipitated phase of face-centered cubic structure is a new precipitated phase discovered by related researchers in recent years in zirconium alloys of HCP structural phase, and research on its formation mechanism and alloy properties is still at the beginning. However, the morphology, lattice constant and orientation relationship of the FCC-Zr precipitated phase and the HCP-Zr matrix are similar to those of a hydride (delta phase hydride), and since the electron microscope technology cannot analyze the distribution characteristics of hydrogen elements, the two precipitated phases cannot be identified by either the scanning electron microscope or the transmission electron microscope technology, which brings great inconvenience to the development of related scientific research. Therefore, it is important to invent a practical method for identifying the delta phase hydride and the FCC phase in the zirconium alloy.
Disclosure of Invention
The invention aims to provide a method for accurately and quickly distinguishing a delta-phase hydride and an FCC-Zr precipitated phase. The invention provides a method for identifying delta-phase hydride and FCC-Zr precipitated phase with face-centered cubic structure in zirconium alloy, which comprises the following steps:
the method comprises the following steps: observing and analyzing the needle-like phase needing to be identified as FCC-Zr phase or delta phase hydride by adopting a metallographic microscope (OM), or a Scanning Electron Microscope (SEM) or a Transmission Electron Microscope (TEM), and recording and marking the accurate position of the needle-like phase; wherein, a metallographic microscope (OM), a Scanning Electron Microscope (SEM) or a Transmission Electron Microscope (TEM) is adjusted according to the size of the precipitated phases, and the precipitated phases with different sizes need to adopt different instruments.
Step two: vacuum packaging the zirconium alloy sample in the step one by using a quartz tube, and filling inert gas argon for protection; in the packaging process, the surface of the sample is ensured not to be polluted, and the purpose of filling the inert gas argon is to prevent the sample from generating oxidation pollution in the subsequent treatment and influencing the test;
step three: carefully placing the packaged sample in a box-type resistance furnace, keeping the furnace temperature at 500-600 ℃, standing for 1-10 hours, and then air-cooling; in the process, the surface of the sample must be ensured not to be polluted; the cooling speed is high, and a non-furnace cooling mode is adopted for cooling, so that hydrogen formed by decomposition is prevented from forming hydride again, and the analysis result is influenced;
step four: and (3) crushing the quartz tube after the sample is cooled, taking out the sample, and observing and analyzing the same position of the sample by using a metallographic microscope, a scanning electron microscope or a transmission electron microscope which is consistent with the step one, wherein if the precipitated phase disappears (or the size is obviously reduced), the precipitated phase is delta-phase hydride, and if the precipitated phase still exists (or the size of the precipitated phase is basically unchanged), the precipitated phase is FCC-Zr.
The invention provides a method for identifying delta-phase hydride and FCC-Zr precipitated phase of zirconium alloy, which is based on the difference pair of thermal stability of two precipitated phasesWhich are differentiated. The hydrogen atoms in the hydride occupy interstitial sites in the crystal lattice of the zirconium matrix and are therefore also referred to as interstitial hydrides. Therefore, the arrangement of atoms in the crystal lattice of the zirconium alloy matrix does not change too much due to the presence of hydrogen, but the distance between adjacent atoms is slightly increased. The formation of this type of hydride is related to the nature of the metal, the temperature and the hydrogen partial pressure, since the hydrogen atoms occupy interstitial sites of the matrix lattice. And their own properties are very similar to those of the parent metal and have very strong reducibility. The stability of such hydrides is particularly poor. Referring to the Zr-H binary phase diagram of FIG. 1, it can be seen from FIG. 1 that when the sample is heat treated at a specific temperature (550 ℃ C. -600 ℃ C.), delta → alpha + H occurs2↑，αH→α+H2↑，βH→α+β+H2@ etc., during which the alloy releases hydrogen gas. When the temperature is kept between 500 ℃ and 600 ℃, the hydride is decomposed to form hydrogen and is diffused to the surface of the sample. And for the FCC-Zr precipitated phase, the research shows that the thermal stability of the FCC-Zr precipitated phase is between that of HCP-Zr and BCC-Zr phases, and the FCC-Zr precipitated phase can exist stably when being kept at the temperature of 500-600 ℃. When the sample is cooled after the temperature is maintained, the hydrogen formed by decomposition is difficult to form hydride again because the cooling speed is high. Thus, it can be judged whether the needle phase is a delta phase hydride or an FCC-Zr phase based on the change of the needle phase before and after the treatment. After the heat preservation at 500-600 ℃, the hydride can be decomposed by rapid cooling, and the FCC-Zr phase can still exist stably, thereby achieving the purpose of identifying two precipitated phases.
In the method, if the heat treatment temperature is high or the sample size is small, the heat preservation time can be correspondingly reduced; on the contrary, when the heat treatment temperature is low, the heat preservation time can be correspondingly prolonged so as to ensure that hydrides in the alloy completely disappear; in the method, in order to protect the surface of the sample from pollution, vacuum packaging must be ensured so as to achieve the aim of quasi-in-situ observation; in the method of the present invention, the cooling rate must be fast to prevent re-precipitation of the hydride during the cooling process.
The method for identifying the delta phase hydride and the FCC-Zr precipitated phase in the zirconium alloy, which is provided by the invention, has the advantages that: the structure identification of complex precipitated phases in the zirconium alloy can be realized only through simple heat treatment, the operation in the test is convenient, the method is simple and practical, the cost is low, and the method has important significance for the research of the zirconium alloy.
Drawings
FIG. 1 is a Zr-H binary phase diagram.
FIG. 2 shows the morphology of an acicular precipitated phase OM in the Zr-4 alloy before heat treatment.
FIG. 3 shows the morphology of acicular precipitated phase OM in the heat-treated Zr-4 alloy.
FIG. 4 is an SEM morphology of an acicular precipitated phase in a Zr-4 alloy before heat treatment.
FIG. 5 is an SEM morphology of acicular precipitated phase in heat treated Zr-4 alloy.
FIG. 6 is TEM morphology of needle-like precipitated phase in pure Zr before heat treatment.
FIG. 7 is TEM morphology of needle-like precipitated phase in pure Zr after heat treatment.
Detailed Description
Example 1
In the embodiment, in order to identify whether the acicular precipitated phase in a zirconium alloy sample belongs to delta-phase hydride or FCC-Zr phase, the method for identifying the delta-phase hydride and the FCC-Zr precipitated phase in the zirconium alloy is adopted, and the types of the acicular precipitated phase in the Zr-4 alloy are identified by virtue of a metallographic microscope (OM), a Scanning Electron Microscope (SEM) and a Transmission Electron Microscope (TEM) respectively, and the method comprises the following specific steps:
observing and analyzing a needle-shaped precipitated phase (known as FCC-Zr phase or delta phase hydride) needing to be identified in a Zr-4 alloy sample by adopting a metallographic microscope, a scanning electron microscope and a transmission electron microscope, and recording the position (the OM and SEM observed samples are the same sample, and the specific position of the needle-shaped precipitated phase needing to be identified is marked by microhardness indentation), wherein the morphology of the needle-shaped precipitated phase OM of the Zr-4 alloy sample is shown in figure 2, the morphology of the corresponding needle-shaped phase SEM under different magnifications is shown in figure 3, and the morphology of the individual needle-shaped phase TEM is shown in figure 4;
respectively carrying out vacuum packaging on the block-shaped test sample and the transmission sample by using a quartz tube, introducing inert gas argon for protection, and carrying out air cooling after heat preservation for 6 hours in a box-type furnace resistance furnace at the furnace temperature of 600 ℃ (the whole process ensures that the surface of the sample is free from pollution);
and taking out the sample after cooling, and observing and analyzing the structure or the needle-like phase at the same position under a metallographic microscope, a scanning electron microscope and a transmission electron microscope respectively, wherein the metallographic microstructure and the scanning electron microscopic appearance of the sample after heat treatment are respectively shown in fig. 5 and 6. It can be seen that the amount of needle-like phases in the heat-treated sample did not change significantly; it is shown that the needle phase in the Zr-4 alloy should not be a hydride, and the dimensions before and after heat treatment are not significantly reduced for the needle phase at the same position, confirming that it should be an FCC-Zr phase; also, the morphology and size of the same needle-like phase in TEM did not change significantly (as shown in FIG. 7), indicating that the needle-like precipitated phase is FCC-Zr phase.
The invention is not the best known technology.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
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| CN109060857A (en) * | 2018-05-23 | 2018-12-21 | 中国科学院金属研究所 | A kind of zircaloy the second phase corrosive agent and caustic solution |
| CN109459455A (en) * | 2019-01-11 | 2019-03-12 | 中国科学院金属研究所 | A kind of electrochemical etching method for observing zircaloy nano-second-phase |
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| CN109060857A (en) * | 2018-05-23 | 2018-12-21 | 中国科学院金属研究所 | A kind of zircaloy the second phase corrosive agent and caustic solution |
| CN109459455A (en) * | 2019-01-11 | 2019-03-12 | 中国科学院金属研究所 | A kind of electrochemical etching method for observing zircaloy nano-second-phase |
Non-Patent Citations (3)
| Title |
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| In situ TEM observation of FCC Ti formation at elevated temperatures;Qian Yu 等;《Scripta Materialia》;20170704;第140卷;第9-12页 * |
| 含Ge Zircaloy-4合金晶体学;刘承泽;《万方数据知识服务平台》;20190823;第1-131页 * |
| 氢化-脱氢法制备锆粉工艺研究;张恒 等;《稀有金属》;20110530;第35卷(第3期);第417-421页 * |
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