CN111551576A - Method for quantitatively evaluating influence of vacuum degree and oxidation products on performance of high-temperature alloy - Google Patents
Method for quantitatively evaluating influence of vacuum degree and oxidation products on performance of high-temperature alloy Download PDFInfo
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Abstract
The invention relates to a method for quantitatively evaluating the influence of vacuum degree and oxidation products on the performance of a high-temperature alloy, belonging to the field of high-temperature alloys; by controlling the graded vacuum degree and sequentially solidifying and aggregating the oxidation products during smelting and matching with a method for testing the comprehensive mechanical property of the corresponding state, the vacuum degree, the oxidation products and the influence of the oxidation products on the mechanical property of the nickel-based superalloy are quantitatively evaluated, meanwhile, the type and the content of the trace oxidation products in the alloy can be determined, a basis is provided for determining the tolerance of preparation process parameters, and technical support and guarantee are provided for preparing the high-purity superalloy, improving the qualification rate of nickel-based superalloy workpieces and reducing the cost. The invention solves the problem that the average gas content and the mechanical property can not be directly hooked due to the fact that the prior art only considers several factors of the vacuum degree, the average gas content (including the oxygen content) of a solidified sample and the mechanical property of the alloy.
Description
Technical Field
A method for quantitatively evaluating the influence of vacuum degree and oxidation products on the performance of high-temperature alloy belongs to the field of high-temperature alloy.
Background art:
the heart of the world where high temperature alloys are known as gas turbines has been the subject of attention from metallurgical workers. The preparation process of core hot-end parts such as powder high-temperature alloy turbine disks, single-crystal high-temperature alloy blades and the like of the current advanced gas turbine engines needs a key process of alloy remelting and pouring, and the remelting vacuum degree and the retention time are very important for the quality and the final service performance of the parts. In the process of development and production, corresponding processes need to be established for different parts, and the vacuum degree requirement during remelting is generally required to be provided in the process procedure. Vacuum system failure is sometimes encountered during the fabrication of the part due to incidental factors, resulting in a reduction in vacuum. Whether remelting normally occurs or the vacuum drops due to accidental factors, the alloy melt reacts with the environment at high temperature to inevitably form oxidation products, which have potential effects on the performance. Therefore, the effects of vacuum, gas content and oxidation products on the mechanical properties of the superalloy need to be quantitatively evaluated to aid in the determination of vacuum tolerance in the process.
In the prior art, the corresponding relation between the process and the alloy performance is evaluated by recording the smelting vacuum degree, measuring the average gas content (including oxygen content) of the solidified alloy and measuring the mechanical property. Practical results show that after the same alloy is smelted in a plurality of vacuum degrees with large difference, sometimes the average gas content (including oxygen content) of the alloy is not obviously different, but the mechanical property has large fluctuation, which causes difficulty in determining the relation between the process and the mechanical property and determining the tolerance of the process parameter.
By controlling the graded vacuum degree and the holding time during smelting, sequentially solidifying and aggregating the oxidation products and testing the comprehensive mechanical property of the corresponding state, the vacuum degree and the holding time, the oxidation products and the influence of the oxidation products on the mechanical property of the nickel-based superalloy are quantitatively evaluated, the type and the content of the oxidation products can be determined, a basis is provided for determining the tolerance of preparation process parameters, and technical support and guarantee are provided for preparing the high-purity superalloy, improving the qualification rate of the nickel-based superalloy parts and reducing the cost.
The invention content is as follows:
the invention relates to a method for quantitatively evaluating the influence of vacuum degree and oxidation products on the mechanical property of a high-temperature alloy, which aims to solve the problem that the influence of the vacuum degree and the mechanical property sensitivity of the oxidation products and the high-temperature alloy cannot be quantitatively measured in the past. By controlling the graded vacuum degree and sequentially solidifying and aggregating the oxidation products during smelting and matching with a method for testing the comprehensive mechanical property of the corresponding state, the vacuum degree, the oxidation products and the influence of the oxidation products on the mechanical property of the nickel-based superalloy are quantitatively evaluated, meanwhile, the type and the content of the oxidation products can be determined, a basis is provided for determining the tolerance of preparation process parameters, and technical support and guarantee are provided for preparing the high-purity superalloy, improving the qualification rate of the nickel-based superalloy parts and reducing the cost.
The purpose of the invention is realized by the following technical scheme:
the method for quantitatively evaluating the influence of the vacuum degree and the oxidation product on the performance of the high-temperature alloy is characterized by comprising the following steps of: preparing high-temperature alloy samples solidified under different vacuum conditions by controlling the graded vacuum degree and the holding time during smelting, measuring the mechanical properties of the samples under different vacuum conditions, remelting the high-temperature alloy samples under different vacuum conditions again under high vacuum, adopting sequential solidification to aggregate oxidation products, identifying the types of the oxidation products, determining the forms, components and contents of the oxidation products under different vacuum conditions, and determining and evaluating the quantitative relation of the vacuum degree and the influences of the forms, types and contents of the oxidation products on the performance of the high-temperature alloy.
The grading vacuum degree refers to different vacuum degree grades of high, medium and low, the highest vacuum degree is the ultimate vacuum degree of the equipment, and the lowest vacuum degree can reach the atmospheric environment.
The high-temperature alloy sample is obtained by remelting a cut high-temperature alloy master alloy ingot in a vacuum induction melting furnace, and placing the melt into a furnace 10 after melting and cleaning-2Pa-103Respectively cooling and solidifying under the conditions of different vacuum degrees of Pa and 1-100min of holding time.
The high-temperature alloy master alloy ingot is prepared by vacuum induction melting.
The sequentially solidified and aggregated oxidation product is prepared by remelting and solidifying high-temperature alloy samples under different vacuum conditions at 10 DEG C- 3Pa-10-4Remelting again in a Pa high vacuum environment, and sequentially cooling to realize sequential solidification processes of solid, solid-liquid and liquid from bottom to top respectively, so that oxidation products with relatively low density in the alloy float upwards and gather in a last solidification region on the upper surface in the sequential solidification process.
The identification of the oxidation product species is carried out by using synchrotron radiation X-ray diffraction identification.
The shape, the components and the content of the oxidation product under different vacuum conditions are determined by a scanning electron microscope and an energy spectrum, and the content of the oxidation product is determined by adopting quantitative metallographic phase.
The quantitative relationship is at 10-2Pa-103Pa vacuum degree, 1-100min holding time, ppm gas content and oxidation product content, and quantitative corresponding relation of high temperature alloy performance under corresponding conditions.
Before remelting again, the high-temperature alloy samples under different vacuum conditions need to be processed into gas test samples and mechanical property test bars, and gas content and mechanical property tests are respectively carried out.
The gas content test comprises oxygen, nitrogen and hydrogen, and the measurement of mechanical properties comprises tensile property, impact property, fatigue property, endurance property and performance of high-temperature alloy service requirement examination.
The technical scheme of the invention has the advantages that:
the invention prepares the high-temperature alloy samples solidified under different vacuum conditions by controlling the graded vacuum degree during smelting, and measures the mechanical properties of the samples under different vacuum conditions. Remelting high-temperature alloy samples under different vacuum conditions again under high vacuum, adopting sequential solidification to aggregate oxidation products, identifying the types of the oxidation products and determining the content of the oxidation products under different vacuum conditions. And determining and evaluating the quantitative relation of the influence of the vacuum degree, the form, the type and the content of the oxidation product on the mechanical property of the high-temperature alloy.
Firstly, controlling the graded vacuum degree during smelting, approaching to actual production, and efficiently obtaining different vacuum conditions; secondly, the oxidation product is aggregated by adopting a high-vacuum remelting sequential solidification method, so that the problems that the content of the oxidation product is extremely low and the oxidation product is too dispersed to be found and quantitatively analyzed in the prior art are solved; thirdly, quantitative analysis of oxidation products is introduced, so that the defect that the hook cannot be formed only through the average gas content and the mechanical property of the alloy in the prior art is overcome; fourthly, accurately quantifying the oxidation product by adopting a mode of combining synchrotron radiation X-rays and quantitative metallographic phase or extraction separation; fifth, the presence of oxygen (in the combined state and in the free state) can be quantitatively determined; sixthly, four key factors of vacuum degree, gas content, oxidation products and high-temperature alloy mechanical property are comprehensively considered, and a basis is provided for formulating the process parameter tolerance.
The invention solves the problem that the average gas content and the mechanical property can not be hooked due to the fact that only several factors of the vacuum degree, the average gas content (including the oxygen content) of a solidified sample and the mechanical property of the alloy are considered in the prior art.
Detailed Description
The technical solution of the present invention will be further described with reference to the following examples:
the method for quantitatively evaluating the influence of the vacuum degree and the oxidation product on the mechanical property of the high-temperature alloy solves the problem that the average gas content and the mechanical property cannot be hooked due to the fact that only the vacuum degree, the average gas content (including the oxygen content) of a solidified sample and the multiple factors of the mechanical property of the alloy are considered in the prior art, quantitative parameters of the oxidation product are introduced through remelting and sequential solidification in high vacuum, quantitative evaluation of five key factors of the vacuum degree, the holding time, the gas content, the oxidation product and the mechanical property of the high-temperature alloy is achieved, and basis is provided for determining the tolerance of preparation process parameters.
The method for quantitatively evaluating the influence of the vacuum degree and the oxidation products on the mechanical property of the high-temperature alloy comprises the following specific steps:
step one, preparing a high-temperature alloy master alloy ingot by adopting vacuum induction melting, and cutting the high-temperature alloy master alloy ingot into required weight;
remelting the master alloy ingot, placing the melt under different vacuum conditions after clearing, and respectively cooling and solidifying to obtain high-temperature alloy samples under different vacuum conditions; the different vacuum conditions were obtained by the time to shut down the vacuum pump after purging.
Thirdly, sampling the remelted and solidified high-temperature alloy samples under different vacuum conditions to test the gas content and the mechanical property; the gas content is measured by oxygen, nitrogen and hydrogen, and the mechanical properties are measured by tensile property, impact property, fatigue property and endurance property
And the performance of the service requirement evaluation of the high-temperature alloy.
Step four, polishing and cleaning the surfaces of the remelting and solidifying high-temperature alloy samples under different vacuum conditions, remelting again and sequentially solidifying under a high-vacuum environment, and aggregating oxidation products;
identifying the type of the oxidation product after the high vacuum sequential solidification and aggregation, and determining the form and the content of the oxidation product; the identification of the types of the oxidation products adopts synchrotron radiation X-ray diffraction, the morphological analysis of the oxidation products adopts a scanning electron microscope, and the quantity of the oxidation products adopts quantitative metallographic phase or extraction separation analysis.
And step six, establishing a quantitative corresponding relation among the vacuum degree, the gas content, the oxidation product amount and the mechanical property of the high-temperature alloy, and providing a basis for the tolerance selection of the process parameters.
Example 1
The technical scheme adopted by the invention comprises the following specific steps:
(1) preparing a high-temperature alloy master alloy ingot by adopting vacuum induction melting, wherein the alloy comprises 50kg of Ni-34% of Cr-5% of W-3% of Mo-1% of Nb-1% of Ti-1% of Al-0.5% of C;
(2) remelting the cut master alloy ingot in a vacuum induction furnace, and placing the alloy melt under normal vacuum condition after melting and cleaning<10-1Pa, keeping for 20min, cooling and solidifying the alloy to room temperature after casting to obtain a high-temperature alloy sample under the normal remelting vacuum condition;
(3) respectively cutting a gas test sample and a standard mechanical property test for the remelted and solidified high-temperature alloy sampleAnd testing the gas content and the mechanical property by using a rod. The oxygen content in the gas content is 12ppm, the nitrogen content is 27ppm, the room-temperature tensile strength of the alloy is 785.5MPa, the elongation is 19.2 percent, and the room-temperature impact toughness is 45.7J/cm2The lasting life at 800 ℃/206MPa is 46.6 h;
(4) polishing the surface of the remelted and solidified high-temperature alloy sample, cleaning the surface by using acetone, and cleaning the surface at 10 DEG C-3Remelting again in a Pa high-vacuum environment, and sequentially cooling from bottom to top to realize the sequential solidification process of solid, solid-liquid two-phase and liquid, so that trace (ppm) level oxidation products with relatively low density in the alloy float upwards and gather in a final solidification area on the upper surface in the sequential solidification process;
(5) method for identifying that oxidation product after high vacuum sequential solidification and aggregation is mainly Al by adopting scanning electron microscope/energy spectrum and synchrotron radiation X-ray diffraction2O3And Cr2O3The content of oxidation products is measured to be 0.76mm by adopting a quantitative metallographic method2/kg；
(6) Build up of vacuum degree (<10-1Pa) and holding time (20min), gas content (12ppm of O and 27ppm of N), oxidation product content (0.76 mm)2/kg) and high-temperature alloy mechanical property (tensile strength at room temperature of 785.5MPa, elongation of 19.2%, impact toughness at room temperature of 45.7J/cm2, and endurance life at 800 ℃/206MPa of 46.6 h).
Example 2
The technical scheme adopted by the invention comprises the following specific steps:
(1) preparing a high-temperature alloy master alloy ingot by adopting vacuum induction melting, wherein the alloy comprises the components of Ni-34% of Cr-5% of W-3% of Mo-1% of Nb-1% of Ti-1% of Al-0.5% of C, and taking 100 kg;
(2) remelting the cut master alloy ingot in a vacuum induction furnace, placing the alloy melt in a vacuum degree of 100Pa after melting and cleaning, keeping for 1min, cooling and solidifying to room temperature after alloy casting, and obtaining a high-temperature alloy sample under a remelting vacuum condition of 100Pa/1 min;
(3) and respectively cutting a gas test sample and a standard mechanical property test bar from the remelted and solidified high-temperature alloy sample, and testing the gas content and the mechanical property. In gas contentThe oxygen content is 15ppm, the nitrogen content is 21.5ppm, and the room temperature impact toughness of the alloy is 25.5J/cm2The lasting life at 800 ℃/206MPa is 41.5 h;
(4) polishing the surface of the remelted and solidified high-temperature alloy sample, cleaning the surface by using acetone, and cleaning the surface at 10 DEG C-3Remelting again in a Pa high-vacuum environment, and sequentially cooling from bottom to top to realize the sequential solidification process of solid, solid-liquid two-phase and liquid, so that trace (ppm) level oxidation products with relatively low density in the alloy float upwards and gather in a final solidification area on the upper surface in the sequential solidification process;
(5) method for identifying that oxidation product after high vacuum sequential solidification and aggregation is mainly Al by adopting scanning electron microscope/energy spectrum and synchrotron radiation X-ray diffraction2O3And Cr2O3The content of oxidation products is measured to be 8.22mm by adopting a quantitative metallographic method2/kg；
(6) Vacuum (100Pa) and holding time (1min) were established, gas content (15ppm of O and 21.5ppm of N), oxidation product content (8.22 mm)2Kg) and mechanical properties of the superalloy (room temperature impact toughness of the alloy 25.5J/cm)2800 ℃/206MPa of lasting life is 41.5 h).
Example 3
The technical scheme adopted by the invention comprises the following specific steps:
(1) preparing a high-temperature alloy master alloy ingot by adopting vacuum induction melting, wherein the alloy comprises 50kg of Ni-34% of Cr-5% of W-3% of Mo-1% of Nb-1% of Ti-1% of Al-0.5% of C;
(2) remelting the cut master alloy ingot in a vacuum induction furnace, placing the alloy melt under the vacuum condition of 100-110Pa after melting and cleaning, keeping for 10min, cooling and solidifying the alloy after casting to room temperature to obtain a high-temperature alloy sample under the normal remelting vacuum condition;
(3) and respectively cutting a gas test sample and a standard mechanical property test bar from the remelted and solidified high-temperature alloy sample, and testing the gas content and the mechanical property. The oxygen content in the gas content is 14.5ppm, the nitrogen content is 22.5ppm, the room-temperature tensile strength of the alloy is 798MPa, the elongation is 6.4 percent, and the room-temperature impact toughness is 27.8J/cm2，800℃/20The 6MPa durable life is 42.5 h;
(4) polishing the surface of the remelted and solidified high-temperature alloy sample, cleaning the surface by using acetone, and cleaning the surface at 10 DEG C-3Remelting again in a Pa high-vacuum environment, and sequentially cooling from bottom to top to realize the sequential solidification process of solid, solid-liquid two-phase and liquid, so that trace (ppm) level oxidation products with relatively low density in the alloy float upwards and gather in a final solidification area on the upper surface in the sequential solidification process;
(5) method for identifying that oxidation product after high vacuum sequential solidification and aggregation is mainly Al by adopting scanning electron microscope/energy spectrum and synchrotron radiation X-ray diffraction2O3And Cr2O3And composite oxides of Cr, Ni, Al, Ti, Si, Ca and rare earth, and the content of oxidation products is 59.1mm measured by a quantitative metallographic method2/kg；
(6) Establishing a vacuum (100-2Kg) and mechanical properties of the high-temperature alloy (room-temperature tensile strength of 798MPa, elongation of 6.4%, room-temperature impact toughness of 27.8J/cm2The 800 ℃/206MPa durable life is 42.5h) is determined according to the quantitative corresponding relation of five key factors.
It can be seen from the results of examples 1, 2 and 3 that the gas content of the superalloy does not increase significantly (only by 17-25%) when the vacuum degree is reduced and the retention time of the lower vacuum degree is prolonged, but the amount of generated oxidation products is increased significantly (by 1-2 orders of magnitude), the strength index of the corresponding mechanical properties is not significantly affected (room temperature tensile strength and endurance life), and the plasticity index (elongation and impact toughness) is significantly reduced by 40-67%. The method realizes the quantitative relation evaluation of five key factors of the vacuum degree, the retention time, the gas content, the oxidation product content and the mechanical property of the high-temperature alloy, and provides a basis for determining the tolerance of the alloy preparation process parameters.
Claims (10)
1. The method for quantitatively evaluating the influence of the vacuum degree and the oxidation product on the performance of the high-temperature alloy is characterized by comprising the following steps of: preparing high-temperature alloy samples solidified under different vacuum conditions by controlling the graded vacuum degree and the holding time during smelting, measuring the gas content and the mechanical property of the samples under different vacuum conditions, remelting the high-temperature alloy samples under different vacuum conditions again under high vacuum, adopting sequential solidification to aggregate oxidation products, identifying the types of the oxidation products, determining the forms, the components and the content of the oxidation products under different vacuum conditions, determining the existence form of oxygen, and determining and evaluating the quantitative relation of the influence of the vacuum degree, the gas content, the forms, the types and the content of the oxidation products on the performance of the high-temperature alloy.
2. The method for quantitatively evaluating the influence of the vacuum degree and the oxidation products on the mechanical property of the high-temperature alloy as claimed in claim 1, wherein the method comprises the following steps: the grading vacuum degree refers to different vacuum degree grades of high, medium and low, the highest vacuum degree is the ultimate vacuum degree of the equipment, and the lowest vacuum degree can reach the atmospheric environment.
3. The method for quantitatively evaluating the influence of the vacuum degree and the oxidation products on the mechanical property of the high-temperature alloy as claimed in claim 1, wherein the method comprises the following steps: the high-temperature alloy sample is obtained by remelting a cut high-temperature alloy master alloy ingot in a vacuum induction melting furnace, and placing the melt into a furnace 10 after melting and cleaning-2Pa-103Respectively cooling and solidifying under the conditions of different vacuum degrees of Pa and 1-100min of holding time.
4. The method for quantitatively evaluating the influence of the vacuum degree and the oxidation products on the mechanical property of the high-temperature alloy as claimed in claim 3, wherein the method comprises the following steps: the high-temperature alloy master alloy ingot is prepared by vacuum induction melting.
5. The method for quantitatively evaluating the influence of the vacuum degree and the oxidation products on the mechanical property of the high-temperature alloy according to claim 1, wherein the method comprises the following steps: the sequentially solidified and aggregated oxidation product is prepared by remelting and solidifying high-temperature alloy samples under different vacuum conditions at 10 DEG C-3Pa-10-4Remelting again in a Pa high vacuum environment, and sequentially cooling to realize sequential solidification process from bottom to top of solid, solid-liquid and liquid respectively, so as to obtain trace (ppm) level in alloyThe oxidation products float and gather in the last solidification area of the upper surface in the sequential solidification process.
6. The method for quantitatively evaluating the influence of the vacuum degree and the oxidation products on the mechanical property of the high-temperature alloy according to claim 1, wherein the method comprises the following steps: the identification of the oxidation product species is carried out by using synchrotron radiation X-ray diffraction identification.
7. The method for quantitatively evaluating the influence of the vacuum degree and the oxidation products on the mechanical property of the high-temperature alloy according to claim 1, wherein the method comprises the following steps: the shape, the components and the content of the oxidation product under different vacuum conditions are determined by a scanning electron microscope and an energy spectrum, and the content of the oxidation product is determined by adopting a quantitative metallographic phase or an extraction separation method.
8. The method for quantitatively evaluating the influence of the vacuum degree and the oxidation products on the mechanical property of the high-temperature alloy according to claim 1, wherein the method comprises the following steps: the quantitative relationship is at 10-2Pa～103Pa vacuum degree, 1-100min holding time, ppm gas content, oxidation product amount and corresponding quantitative corresponding relation of high temperature alloy performance.
9. The method for quantitatively evaluating the influence of the vacuum degree and the oxidation products on the mechanical property of the high-temperature alloy according to claim 1, wherein the method comprises the following steps: before remelting again, the high-temperature alloy samples under different vacuum conditions need to be processed into gas test samples and mechanical property test bars, and gas content and mechanical property tests are respectively carried out.
10. The method for quantitatively evaluating the influence of the vacuum degree and the oxidation products on the mechanical property of the high-temperature alloy according to claim 9, wherein the method comprises the following steps: the gas content test comprises oxygen, nitrogen and hydrogen, and the measurement of mechanical properties comprises tensile property, impact property, fatigue property, endurance property and performance of high-temperature alloy service requirement examination.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010386895.2A CN111551576B (en) | 2020-05-09 | 2020-05-09 | Method for quantitatively evaluating influence of vacuum degree and oxidation products on high-temperature alloy performance |
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| CN111551576A true CN111551576A (en) | 2020-08-18 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112553679A (en) * | 2020-11-03 | 2021-03-26 | 中国航发北京航空材料研究院 | Monomer separation method for harmful phase of isothermal forging die material for turbine disc |
| CN112986522A (en) * | 2021-02-05 | 2021-06-18 | 中国航发北京航空材料研究院 | High-efficiency determination method for oxygen existence form of high-temperature alloy powder |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07239327A (en) * | 1994-02-28 | 1995-09-12 | Nippon Steel Corp | Evaluation of cleanliness of metal |
| JPH10318947A (en) * | 1997-05-16 | 1998-12-04 | Nippon Steel Corp | Method for analyzing non-metal inclusion in metal |
| CN103123329A (en) * | 2012-12-31 | 2013-05-29 | 上海大学 | Rapid detection method and rapid detection device of non-metallic inclusions in metal |
| CN105738656A (en) * | 2014-12-12 | 2016-07-06 | 宝山钢铁股份有限公司 | Experiment method for realizing in-situ observation on inclusion in bearing steel liquid |
| CN107607567A (en) * | 2017-09-28 | 2018-01-19 | 华南理工大学 | The quantitatively characterizing method of non-metallic inclusion in a kind of Ni-base Superalloy Powder |
-
2020
- 2020-05-09 CN CN202010386895.2A patent/CN111551576B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07239327A (en) * | 1994-02-28 | 1995-09-12 | Nippon Steel Corp | Evaluation of cleanliness of metal |
| JPH10318947A (en) * | 1997-05-16 | 1998-12-04 | Nippon Steel Corp | Method for analyzing non-metal inclusion in metal |
| CN103123329A (en) * | 2012-12-31 | 2013-05-29 | 上海大学 | Rapid detection method and rapid detection device of non-metallic inclusions in metal |
| CN105738656A (en) * | 2014-12-12 | 2016-07-06 | 宝山钢铁股份有限公司 | Experiment method for realizing in-situ observation on inclusion in bearing steel liquid |
| CN107607567A (en) * | 2017-09-28 | 2018-01-19 | 华南理工大学 | The quantitatively characterizing method of non-metallic inclusion in a kind of Ni-base Superalloy Powder |
Non-Patent Citations (5)
| Title |
|---|
| 刘继雄等: "两种精炼工艺对管线钢中非金属夹杂物的影响", 《物理测试》 * |
| 孟宇等: "真空熔炼精炼真空度对K465合金氧化夹杂的影响", 《第十四届国际真空科学与工程应用学术会议论文（摘要）集》 * |
| 常全举: "真空感应冶炼高纯钢氮氧含量控制研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
| 耿鑫等: "真空感应炉坩埚材质对Cr12钢纯净度的影响", 《材料与冶金学报》 * |
| 董世通: "真空感应炉冶炼Cr12钢工艺研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112553679A (en) * | 2020-11-03 | 2021-03-26 | 中国航发北京航空材料研究院 | Monomer separation method for harmful phase of isothermal forging die material for turbine disc |
| CN112553679B (en) * | 2020-11-03 | 2024-02-09 | 中国航发北京航空材料研究院 | Method for separating harmful phase monomer from isothermal forging die material for turbine disk |
| CN112986522A (en) * | 2021-02-05 | 2021-06-18 | 中国航发北京航空材料研究院 | High-efficiency determination method for oxygen existence form of high-temperature alloy powder |
| CN112986522B (en) * | 2021-02-05 | 2024-01-12 | 中国航发北京航空材料研究院 | High-efficiency determination method for oxygen existence form of superalloy powder |
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