CN111139388A - Low-alloy-element-reinforced high-temperature oxidation-resistant self-passivated tungsten alloy and preparation method thereof - Google Patents
Low-alloy-element-reinforced high-temperature oxidation-resistant self-passivated tungsten alloy and preparation method thereof Download PDFInfo
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- 229910001080 W alloy Inorganic materials 0.000 title claims abstract description 47
- 230000003647 oxidation Effects 0.000 title claims abstract description 31
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000000956 alloy Substances 0.000 claims abstract description 43
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 42
- 230000035939 shock Effects 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 40
- 238000000498 ball milling Methods 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 29
- 238000005245 sintering Methods 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 10
- 238000005204 segregation Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 7
- 230000001276 controlling effect Effects 0.000 claims description 6
- 238000000280 densification Methods 0.000 claims description 5
- 239000011159 matrix material Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 230000003213 activating effect Effects 0.000 claims description 4
- 238000005551 mechanical alloying Methods 0.000 claims description 4
- 238000002161 passivation Methods 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000011863 silicon-based powder Substances 0.000 claims description 3
- 230000004584 weight gain Effects 0.000 claims description 3
- 235000019786 weight gain Nutrition 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 101100478277 Homo sapiens SPTA1 gene Proteins 0.000 claims 2
- 102100037608 Spectrin alpha chain, erythrocytic 1 Human genes 0.000 claims 2
- 238000005728 strengthening Methods 0.000 abstract 1
- 238000005275 alloying Methods 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000006104 solid solution Substances 0.000 description 2
- 235000013619 trace mineral Nutrition 0.000 description 2
- 239000011573 trace mineral Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 229910019580 Cr Zr Inorganic materials 0.000 description 1
- 229910019817 Cr—Zr Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 229910004339 Ti-Si Inorganic materials 0.000 description 1
- 229910010978 Ti—Si Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 229910002070 thin film alloy Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
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Abstract
The invention discloses a self-passivating tungsten alloy (SPTA) with low alloy element strengthening high-temperature oxidation resistance and a preparation method thereof. Thermal shock oxidation experiments show that the introduction of low alloy elements can obviously enhance the high-temperature oxidation resistance of the SPTA.
Description
Technical Field
The invention belongs to the field of refractory tungsten (W) alloy applied under extreme conditions (high temperature and oxidation), and particularly relates to a low-alloy-element self-passivating tungsten alloy with strengthened high-temperature oxidation resistance and a preparation method thereof.
Background
Tungsten (W) has the advantages of high melting point (about 3410 ℃), high thermal conductivity, low thermal expansion coefficient, good high-temperature mechanical property and the like, and has wide application prospect in extreme environments. However, W is very easily oxidized under a high-temperature oxidizing atmosphere, thereby affecting its use at high temperatures. Such as: after the first wall W material for the future nuclear fusion device is subjected to neutron irradiation, the first wall W material has certain radioactivity; if oxidation, volatilization occurs, there is a risk of nuclear radioactivity leakage. Therefore, it is necessary to develop a W alloy material having good oxidation resistance. Self-passivating tungsten alloys (SPTA) are used to ensure continued use by the addition of alloying elements that preferentially form a dense protective scale on their surface, which prevents oxidation of W.
At present, the SPTA with better oxidation resistance is obtained mainly by optimizing components and regulating and controlling a microstructure. For example, when the composition of W-Cr-Zr thin film alloy is optimized, the W alloy has an optimal Zr/Cr ratio (5-10%) when the Cr content is sufficient. Generally, the content of Cr in SPTA is about 10-14 wt.%, and the solid solution temperature is above 1400 ℃. In the aspect of microstructure regulation, the nano W alloy can be prepared by adopting a low-temperature and high-pressure sintering technology, and the corresponding sintering temperature is lower than 1200 ℃. However, when the W alloy is sintered at a temperature lower than the solid solution temperature, Cr element is inevitably segregated, which is disadvantageous in improving the high-temperature oxidation resistance thereof. The Field Assisted Sintering (FAST) technology utilizes a current field of pulse direct current and a stress field of axial external load to sinter sintered powder, and can realize rapid densification of refractory metal materials at low temperature. Therefore, the invention optimizes the composition of the SPTA by adding low alloy elements, and then carries out densification by FAST to prepare the SPTA with high-density, fine-grain and little segregation/homogeneous structure, so as to have good high-temperature oxidation resistance.
Disclosure of Invention
The invention aims to provide a low-alloy-element-reinforced high-temperature-oxidation-resistance self-passivated tungsten alloy (SPTA) and a preparation method thereof.
The invention relates to a low-alloy-element reinforced high-temperature oxidation resistance self-passivated tungsten alloy SPTA, which comprises the following components:
the content of the passivating element is more than or equal to 10 wt% and less than or equal to 13 wt%, the content of the activating element is more than 0 wt% and less than or equal to 1 wt%, the content of the low alloy element is more than 0 wt% and less than or equal to 0.5 wt%, and the balance is W.
The passivation element is Cr; the activating elements are Y and Zr; the low alloy element is Ti and/or Si, preferably Ti and Si.
It is to be noted that the contents of the low alloying elements in the above ratios are defined for Ti and Si, respectively, not for the total content of the low alloying elements. That is, in the self-passivating tungsten alloy SPTA of the present invention, 0 wt.% < Ti < 0.5 wt.%, 0 wt.% < Si < 0.5 wt.%. No matter the low alloy element is independent Ti or Si, or Ti and Si, the proportioning requirements are met.
According to the number of element types in the W alloy, the W alloy is named according to the following scheme:
the W-Cr-Y-Zr-Ti alloy is named ZW5 ("Z" and "W" denote "self-passivating" and "tungsten alloy", respectively; 5 denotes the number of species of elements in the W alloy).
The W-Cr-Y-Zr-Ti-Si alloy is named ZW6 ("Z" and "W" denote "self-passivating" and "tungsten alloy", respectively; 6 denotes the number of species of elements in the W matrix).
The low-alloy element reinforced high-temperature oxidation resistance SPTA has the characteristics of high compactness, fine grains and a small amount of segregation/homogeneous structure, the relative density of the SPTA is more than 98%, and the grain size of the SPTA is about 200 nm.
The SPTA with low alloy element and strengthened high-temperature oxidation resistance is subjected to thermal shock high-temperature oxidation resistance test at 1000 ℃ in air atmosphere, and the quality change of the SPTA during oxidation is analyzedBehavior, optimization of the W alloy composition. The alloy is obtained by optimizing the components, when trace elements Ti and Si are simultaneously added into the W alloy, the obtained ZW6 alloy block has the optimal high-temperature oxidation resistance, and the oxidation weight gain is less than 5mg/cm after the alloy block is oxidized for 165h2。
In the low-alloy-element-reinforced high-temperature oxidation-resistant self-passivated tungsten alloy, the mass fractions of Ti and Si are less than 0.5 wt.%, the relative density of the W alloy is more than 98.5%, and a matrix is a fine-grained SPTA block with little segregation and even a homogeneous structure.
The invention relates to a preparation method of a low-alloy-element-reinforced high-temperature oxidation-resistant self-passivated tungsten alloy SPTA, which is characterized in that low alloy elements are uniformly dispersed in a W-Cr matrix by adopting a mechanical alloying technology, then FAST is adopted to densify powder, and technological parameters in a sintering process are controlled to obtain high-density and fine-grain SPTA with different components. The method specifically comprises the following steps:
step 1: mixing W powder, Cr powder, Y powder, Zr powder, Ti powder, Si powder and the like with the purity of 99.5% according to a certain component ratio, putting 110g of the mixture into a hard alloy ball milling tank with hard alloy balls for mechanical ball milling, and regulating and controlling ball milling time, ball milling rotation speed, ball-to-material ratio, ball milling atmosphere and the like to obtain homogeneous W alloy powder;
step 2: the obtained homogeneous W alloy powder is densified by FAST, and the SPTA block body with high densification, fine grains and a small amount of segregation/homogeneous structure is prepared by controlling the technological parameters such as sintering temperature, pressure, heating rate, isothermal time and the like in the sintering process.
In order to avoid oxidation of the powder during ball milling, preparation in the early stage of powder ball milling was carried out in an Ar atmosphere glove box.
In order to obtain homogeneous W alloy powder, the mechanical alloying technological parameter regulation and control range is as follows: the ball milling time is 2-80 h, the ball milling rotation speed is 300-600 rad/min, the ball-material ratio is 5: 1-15: 1, and the ball milling atmosphere is Ar.
In order to optimize the W alloy microstructure, the FAST process parameter control range is as follows: the sintering temperature is 1000-1400 ℃, the pressure is 50-100 MPa, the heating rate is 50-300 ℃/min, and the heat preservation time is 0-5 min.
The SPTA of the invention adopts W as a matrix, ensures that a sufficient amount of passivation element Cr forms an oxide skin on the surface of W, and then adds trace elements Y, Zr, Ti, Si and the like, wherein the Y element can improve the strength of the oxide skin on the surface; zr is used for slowing down the diffusion of Cr cation; the low alloy elements (Ti and Si) are added to optimize the SPTA components, and the FAST low-temperature rapid densification technology is combined, so that the SPTA block with a high-density, fine-grain and small-amount segregation/homogeneous structure is obtained, and the high-temperature oxidation resistance of the SPTA block is effectively and lowly enhanced.
Drawings
FIG. 1 is a microstructure view of a ZW4 alloy block. As can be seen from FIG. 1, a large number of dark gray precipitated phases are present in the structure of the ZW4 alloy, and the spectral results show that this region is a Cr-rich phase.
FIG. 2 is a microstructure view of a ZW5 alloy block. From fig. 2, it can be seen that the size and number of segregation phases are significantly reduced after a small amount of Ti element is added to the ZW5 alloy.
FIG. 3 is a microstructure view of a ZW6 alloy block. From fig. 3, it can be seen that, after adding small amounts of Ti and Si elements to the ZW6 alloy, only a small amount of segregation phase exists in the W alloy; as can be seen from FIG. 3, the grain size of the W alloy is about 200 nm.
FIG. 4 is a mass change curve of the W alloy oxidized for 165 hours at 1000 ℃ in an air atmosphere. It was found that the W alloy with addition of minute amounts of Ti and Si showed the least mass change.
Detailed Description
Example 1:
under Ar protective atmosphere, 96.36g of W powder with the purity of 99.5 percent, 12.54g of Cr powder, 0.66g of Y powder and 0.44g of Zr powder are weighed in sequence, and are put into a WC ball milling tank with the volume of 250ml together with WC balls according to the ball-to-material ratio of 5:1, and then ball milling is carried out on a planetary ball mill by a ball milling process with the ball milling speed of 250rad/min and the ball milling time of 80h, so as to obtain homogeneous alloy powder. Then, the alloy powder was loaded in a graphite mold and densified by the FAST technique. The sintering process comprises the following steps: the heating rate is about 146 ℃/min, the sintering temperature is 1150 ℃, the pressure is 90MPa, and the temperature is not preserved.
FIG. 1 is a structural diagram of ZW4 alloy obtained under the process conditions. It was found that a large amount of dark gray precipitated phases were present in the structure of the W alloy. The relative density was higher than 98.5% as measured by archimedes drainage method.
Example 2:
under Ar protective atmosphere, 96.14g of W powder with the purity of 99.5 percent, 12.54g of Cr powder, 0.66g of Y powder, 0.44g of Zr powder and 0.22g of Ti powder are weighed in sequence, and are put into a WC ball-milling tank with 250ml together with WC balls according to the ball-to-material ratio of 5:1, and then ball-milling is carried out on a planetary ball mill by a ball-milling process with the ball-milling rotating speed of 250rad/min and the ball-milling time of 80h, so as to obtain homogeneous alloy powder. Then, the alloy powder was loaded in a graphite mold and densified by the FAST technique. The sintering process comprises the following steps: the heating rate is about 146 ℃/min, the sintering temperature is 1150 ℃, the pressure is 90MPa, and the temperature is not preserved.
FIG. 2 is a structural diagram of ZW5 alloy obtained under the process conditions. It was found that the size and number of segregation phases decreased significantly with the addition of a small amount of Ti element to the ZW4 alloy. The relative density was higher than 98.5% as measured by archimedes drainage method.
Example 3:
under Ar protective atmosphere, 96.09g of W powder with the purity of 99.5 percent, 12.54g of Cr powder, 0.66g of Y powder, 0.44g of Zr powder, 0.22g of Ti powder and 0.055g of Si powder are weighed in sequence, and are put into a WC ball milling tank with 250ml together with WC balls according to the ball-to-material ratio of 5:1, and then ball milling is carried out on a planetary ball mill by a ball milling process with the ball milling speed of 250rad/min and the ball milling time of 80 hours to obtain homogeneous alloy powder. Then, the alloy powder was loaded in a graphite mold and densified by the FAST technique. The sintering process comprises the following steps: the heating rate is about 146 ℃/min, the sintering temperature is 1150 ℃, the pressure is 90MPa, and the temperature is not preserved.
FIG. 3 is a structural diagram of ZW6 alloy obtained under the process conditions. It can be found that only a small amount of segregation phase exists in the W alloy after a small amount of Ti and Si elements are simultaneously added in the ZW6 alloy; as can be seen from FIG. 3, the grain size of the W alloy is about 200 nm. The relative density was higher than 98.5% as measured by archimedes drainage method.
Example 4:
and (3) carrying out high-temperature oxidation resistance test on the self-passivation W alloy of three systems obtained by sintering the discharge plasma at the temperature of 1000 ℃ in an air atmosphere. The oxidation weight gain of the W alloy was found to be significantly reduced after low alloying elements of Ti or/and Si, with the best oxidation resistance of the ZW6 alloy. The addition of low alloy elements Ti and Si can improve the structural uniformity of the W alloy and improve the oxidation resistance of the W alloy.
Claims (8)
1. A low-alloy-element reinforced high-temperature oxidation-resistant self-passivated tungsten alloy is characterized by comprising the following components:
the content of the passivating element is more than or equal to 10 wt% and less than or equal to 13 wt%, the content of the activating element is more than 0 wt% and less than or equal to 1 wt%, the content of the low alloy element is more than 0 wt% and less than or equal to 0.5 wt%, and the balance is W.
The passivation element is Cr; the activating elements are Y and Zr; the low alloy element is Ti and/or Si.
2. The self-passivating tungsten alloy of claim 1, wherein:
the low alloy elements are Ti and Si.
3. The self-passivating tungsten alloy of claim 1 or 2, wherein:
the relative density of the self-passivated tungsten alloy is more than 98%, and the grain size is about 200 nm.
4. The nano-W alloy of claim 1 or 2, wherein:
after the W alloy is oxidized for 160 hours under the air atmosphere and multiple thermal shock at the temperature of 1000 ℃, the oxidation weight gain of the W alloy is less than 5mg/cm2。
5. A method for preparing the low-alloy-element reinforced high-temperature oxidation-resistant self-passivated tungsten alloy according to claim 1 or 2, which is characterized by comprising the following steps:
the method comprises the steps of uniformly dispersing low alloy elements in a W-Cr matrix by adopting a mechanical alloying technology, then densifying powder by adopting FAST, and controlling process parameters in a sintering process to obtain high-density and fine-grain SPTA with different components.
6. The method according to claim 5, characterized by comprising the steps of:
step 1: mixing W powder, Cr powder, Y powder, Zr powder, Ti powder, Si powder and the like with the purity of 99.5% according to a certain component ratio, putting 110g of the mixture into a hard alloy ball milling tank with hard alloy balls for mechanical ball milling, and regulating and controlling ball milling time, ball milling rotation speed, ball-to-material ratio, ball milling atmosphere and the like to obtain homogeneous W alloy powder;
step 2: the obtained homogeneous W alloy powder is densified by FAST, and the SPTA block body with high densification, fine grains and a small amount of segregation/homogeneous structure is prepared by controlling the technological parameters such as sintering temperature, pressure, heating rate, isothermal time and the like in the sintering process.
7. The method of claim 5, wherein:
the mechanical alloying process parameter regulation and control range is as follows: the ball milling time is 2-80 h, the ball milling rotation speed is 300-600 rad/min, the ball-material ratio is 5: 1-15: 1, and the ball milling atmosphere is Ar.
8. The method of claim 5, wherein:
the FAST process parameter regulation range is as follows: the sintering temperature is 1000-1400 ℃, the pressure is 50-100 MPa, the heating rate is 50-300 ℃/min, and the heat preservation time is 0-5 min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108515174A (en) * | 2018-04-27 | 2018-09-11 | 合肥工业大学 | A kind of resistance to high temperature oxidation W-Cr-Ti composite material and preparation methods |
| CN108866498A (en) * | 2018-08-10 | 2018-11-23 | 合肥工业大学 | A kind of W self-passivation alloy and preparation method thereof with long-time high temperature oxidation resistance |
| CN109943743A (en) * | 2019-04-28 | 2019-06-28 | 合肥工业大学 | A kind of high-densit, fine brilliant, homogeneous texture self-passivation tungsten alloy preparation method |
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- 2020-03-09 CN CN202010156402.6A patent/CN111139388A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108515174A (en) * | 2018-04-27 | 2018-09-11 | 合肥工业大学 | A kind of resistance to high temperature oxidation W-Cr-Ti composite material and preparation methods |
| CN108866498A (en) * | 2018-08-10 | 2018-11-23 | 合肥工业大学 | A kind of W self-passivation alloy and preparation method thereof with long-time high temperature oxidation resistance |
| CN109943743A (en) * | 2019-04-28 | 2019-06-28 | 合肥工业大学 | A kind of high-densit, fine brilliant, homogeneous texture self-passivation tungsten alloy preparation method |
Non-Patent Citations (2)
| Title |
|---|
| ELISA SAL等: "High temperature microstructural stability of self-passivating W-Cr-Y alloys for blanket first wall application", 《FUSION ENGINEERING AND DESIGN》 * |
| 谭晓月等: "自钝化钨合金在未来核聚变装置中的潜在应用与研究现状", 《材料热处理学报》 * |
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