CN103834831A - Nanometer yttrium oxide dispersion-stiffened nickel base composite material in crystalline grain and preparation method thereof - Google Patents
Nanometer yttrium oxide dispersion-stiffened nickel base composite material in crystalline grain and preparation method thereof Download PDFInfo
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- CN103834831A CN103834831A CN201410087501.8A CN201410087501A CN103834831A CN 103834831 A CN103834831 A CN 103834831A CN 201410087501 A CN201410087501 A CN 201410087501A CN 103834831 A CN103834831 A CN 103834831A
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- yttrium oxide
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Abstract
The invention discloses a nanometer yttrium oxide dispersion-stiffened nickel base composite material in a crystalline grain and a preparation method thereof. The material is composed of a nickel matrix and a nanometer Y2O3 dispersed phase in a nickel matrix crystalline grain, wherein the molar content of Y2O3 is 0.25-4.7 mol%. The method comprises the following steps: mixing Ni or an Ni alloy with Y according to a molar ratio to the Y of 0.5-9.5 mol%, smelting, heating to 0-10 DEG C above the liquidus temperature thereof, oxidizing by using water vapor or CO2, and performing a reaction in-situ to generate Y2O3 particles. A nickel base high-temperature alloy material, which is subjected to dispersion stiffening in the crystalline grain of the matrix Ni, of nano Y2O3 can be obtained by means of the method.
Description
Technical field
The present invention relates to a kind of yttria dispersion strengthening nickel-base composite material technology of preparing, particularly a kind of in-situ oxidation is prepared the technology of preparing of yttrium oxide dispersion-strengthened nickel-base composite material in the crystal grain of matrix Ni.
Background technology
Nickel base superalloy, owing to having good high-temperature creep resistance, surface stability and anticorrosive oxidation susceptibility, has wide application space in high-temperature structural material field.Nickel base superalloy is combustion chamber and turbine component, energy source and power industry steam turbine and oil and natural gas industry wellhead component and the subsurface tool etc. with engine mainly for the preparation of aerospace.Because being usually used in preparation, nickel base superalloy uses in harsh Working environment, as bear the coefficient parts of high temperature, high speed and oxidation corrosion, and along with the development of Aeronautics and Astronautics, naval vessel gas engine and industrial ground combustion machine, the use temperature to material and high-temperature behavior require also day by day improving.In the preparation research of current nickel base superalloy, major objective is to improve the high-temperature behavior of material.The method that generally employing improves material alloysization and artificial introducing second-phase carries out disperse enhancing can effectively improve the intensity of material.In addition the temperature field formation directional solidificating alloy while, preparing alloy by control and single crystal alloy also can greatly improve the intensity of material.But the complex process of preparation directional freeze cylindrulite alloy and single crystal alloy is expensive.And the way that improves material alloys has not only improved the quality of material itself, also easily cause segregation.The powder metallurgy method of traditional introducing second phase particles dispersion-strengthened adopts powder metallurgical technique, by the oxide compound of high-melting-point, high thermal stability (as ThO
2, Y
2o
3deng) nano-scale particle disperse in nickel base superalloy matrix and the superalloy making, but be difficult to reach refinement and the homogenizing of particle by the method for direct interpolation nano level second-phase powder, and the disperse phase of adding is distributed in crystal boundary more.
It is that liquid phase in-situ reaction is prepared nanometer Y in crystal grain that the present invention adopts a kind of novel preparation method
2o
3dispersed particle-strengthened nickel-base composite material, can obtain Y in the crystal grain of matrix Ni by this method
2o
3grain refine, the nickel-base high-temperature matrix material being evenly distributed.
Summary of the invention
The object of this invention is to provide a kind of Y
2o
3grain refine and the novel nano yttrium oxide granular composite being evenly distributed.And the preparation method of this matrix material is provided, this preparation method's technique is simple, with low cost, has broad application prospects.
The present invention solves its technical problem and adopts following technical scheme:
In crystal grain provided by the invention, nano yttrium oxide disperse strengthens nickel-base composite material, and it is by Ni substrate and the nanometer Y in Ni substrate crystal grain
2o
3disperse phase composition, wherein Y
2o
3molar content be 0.25mol%-4.7mol%.
Described Y
2o
3the particle diameter of particle is 4～30nm.
In crystal grain provided by the invention, the preparation method of nano yttrium oxide disperse enhancing nickel-base composite material is: be 0.5mol%～9.5mol% mix after melting with Y by the mol ratio of Y by Ni or Ni alloy, be heated to above 0～10 ℃ of its liquidus temperature, adopt water vapour or CO
2be oxidized, reaction in－situ generates Y
2o
3particle.
In aforesaid method, described Y
2o
3the mol ratio of particle in Ni substrate crystal grain can be 0.25mol%-4.7mol%.
In aforesaid method, described Y
2o
3the particle diameter of particle can be 4～30nm.
In aforesaid method, use atmosphere furnace or vacuum oven that the sample after melting is heated to above 0～10 ℃ of its liquidus temperature.
In aforesaid method, can adopt water vapour or CO
2the time being oxidized is 1～120min.
The present invention has following major advantage compared with existing yttrium oxide disperse enhancing nickel-base composite material:
1. in preparation technology, the yttrium atom in employing nickel yttrium liquation, at liquid phase in-situ oxidation, utilizes liquation solidify growing up of inhibited oxidation yttrium particle and prevent its segregation.In position in oxidation reaction process, along with Y atom in-situ oxidation generates Y
2o
3particle, Y
2o
3regional area will poor Y near particle, and topical solutions is because the minimizing of Y will be separated out solid phase Ni under liquidus temperature.Y
2o
3particle can play the effect that promotes liquation forming core with the form of nucleating agent, and the Ni solidifying is at Y
2o
3particle can hinder again Y around
2o
3growing up of particle, thus the nano yttrium oxide particle that disperse distributes on the tiny Ni substrate of crystal grain, generated.
2. structurally, possess yttrium oxide and nickel and have the feature of coherence relation.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Fig. 2 mixes rear melting by Ni and Y according to the ratio of the mol ratio of Y 0.5%, then sample is heated to 1427 ℃ of liquidus temperatures in atmosphere furnace, under water vapour atmosphere, be oxidized 1min after the microstructure of nano yttrium oxide disperse reinforced composite in gained crystal grain.
Fig. 3 mixes rear melting by Ni and Y according to the ratio of the mol ratio of Y 0.5%, then sample is heated to 1427 ℃ of liquidus temperatures in atmosphere furnace, under water vapour atmosphere, be oxidized 1min after the electron-diffraction diagram material phase analysis of nano yttrium oxide disperse reinforced composite in gained crystal grain.
Fig. 4 mixes rear melting by Ni and Y according to the ratio of the mol ratio of Y 0.5%, then sample is heated to more than liquidus temperature 1 ℃ (1428 ℃) in atmosphere furnace, under water vapour atmosphere, be oxidized 1min after the microstructure of nano yttrium oxide disperse reinforced composite in gained crystal grain.
Fig. 5 mixes rear melting by Ni and Y according to the ratio of the mol ratio of Y 0.5%, then sample is heated to more than liquidus temperature 5 ℃ (1432 ℃) in atmosphere furnace, under water vapour atmosphere, be oxidized 1min after the microstructure of nano yttrium oxide disperse reinforced composite in gained crystal grain.
Fig. 6 mixes rear melting by Ni and Y according to the ratio of the mol ratio of Y 0.5%, then sample is heated to more than liquidus temperature 10 ℃ (1437 ℃) in atmosphere furnace, under water vapour atmosphere, be oxidized 1min after the microstructure of nano yttrium oxide disperse reinforced composite in gained crystal grain.
Fig. 7 mixes rear melting by Ni and Y according to the ratio of the mol ratio of Y 0.5%, then sample is heated to 1427 ℃ of liquidus temperatures in atmosphere furnace, under water vapour atmosphere, be oxidized 60min after the microstructure of nano yttrium oxide disperse reinforced composite in gained crystal grain.
Fig. 8 mixes rear melting by Ni and Y according to the ratio of the mol ratio of Y 0.5%, then sample is heated to 1427 ℃ of liquidus temperatures in atmosphere furnace, under water vapour atmosphere, be oxidized 120min after the microstructure of gained nano yttrium oxide disperse reinforced composite.
Fig. 9 mixes rear melting by Ni and Y according to the ratio of the mol ratio of Y 3%, then in atmosphere furnace, sample is heated to more than liquidus temperature 10 ℃ (1409 ℃), at CO
2under atmosphere, be oxidized the microstructure of gained nano yttrium oxide disperse reinforced composite after 1min.
Figure 10 mixes rear melting by Ni and Y according to the ratio of the mol ratio of Y 3%, then sample is heated to more than liquidus temperature 10 ℃ (1409 ℃) in atmosphere furnace, under water vapour atmosphere, be oxidized 1min after the microstructure of gained nano yttrium oxide disperse reinforced composite.
Embodiment
The invention discloses a kind of nano yttrium oxide nickel-base composite material that disperse strengthens in the crystal grain of matrix Ni and preparation method thereof.This material is by Ni substrate and the nanometer Y in Ni substrate crystal grain
2o
3disperse phase composition, wherein Y
2o
3mol ratio in Ni substrate crystal grain is 0.25mol%-4.7mol%, and the particle diameter of particle is 4～30nm.Its preparation method is: Ni or Ni alloy are mixed to rear melting with Y by a mole 0.5-9.4mol% of Y; Then sample is heated to more than liquidus temperature 0～10 ℃ of melting in atmosphere furnace, and passes into water vapor or CO
2by the yttrium in-situ oxidation in nickel yttrium liquation, pass into water vapour or CO
2time is 1～120min, prepares the disperse of intracrystalline nano yttrium oxide and strengthens nickel-base composite material.Specific embodiment is as follows:
In order to understand better the present invention, below in conjunction with embodiment and accompanying drawing, the invention will be further described, but content of the present invention is not only confined to the following examples.
Embodiment 1: Ni and Y are mixed to rear melting according to the ratio of the mol ratio of Y 0.5%, then sample is heated to 1427 ℃ of liquidus temperatures in atmosphere furnace, and pass into water vapor by the yttrium in-situ oxidation in nickel yttrium liquation, passing into the water vapour time is 1min, prepares nano yttrium oxide disperse in crystal grain and strengthens nickel-base composite material.As shown in Figure 2, as shown in Figure 3, in-situ oxidation reaction forms Y at intracrystalline to material phase analysis to its microstructure
2o
3particle, its particle diameter is 4-6nm.
Embodiment 2: the Heating temperature in embodiment 1 is become to liquidus temperature above 1 ℃ (1428 ℃), prepare nano yttrium oxide disperse in crystal grain and strengthen nickel-base composite material.Its microstructure as shown in Figure 4, forms Y at intracrystalline
2o
3particle, its particle diameter is 7-9nm.
Embodiment 3: the Heating temperature in embodiment 1 is become to liquidus temperature above 5 ℃ (1432 ℃), prepare nano yttrium oxide disperse in crystal grain and strengthen nickel-base composite material.Its microstructure as shown in Figure 5.Form Y at intracrystalline
2o
3particle, its particle diameter is 8-10nm.
Embodiment 4: the Heating temperature in embodiment 1 is become to liquidus temperature above 10 ℃ (1437 ℃), prepare nano yttrium oxide disperse in crystal grain and strengthen nickel-base composite material.Its microstructure as shown in Figure 6.In-situ oxidation reaction forms Y at intracrystalline
2o
3particle, its particle diameter is 9-11nm.
Embodiment 5: the water vapour time that passes in embodiment 1 is become to 60min, prepare nano yttrium oxide disperse in crystal grain and strengthen nickel-base composite material.Its microstructure as shown in Figure 7.Form Y at intracrystalline
2o
3particle, its particle diameter is 8-10nm.
Embodiment 6: the water vapour time that passes in embodiment 1 is become to 120min, prepare nano yttrium oxide disperse in crystal grain and strengthen nickel-base composite material.Its microstructure as shown in Figure 8, forms Y at intracrystalline
2o
3particle, its particle diameter is 8-10nm.
Embodiment 7: Ni and Y are mixed to rear melting according to the mol ratio of Y 3%, then in atmosphere furnace, sample is heated to more than liquidus temperature 10 ℃ (1409 ℃), and passes into CO
2by the yttrium in-situ oxidation in nickel yttrium liquation, pass into CO
2time is 1min, prepares nano yttrium oxide disperse in crystal grain and strengthens nickel-base composite material.Its microstructure as shown in Figure 9 in-situ oxidation reaction forms Y at intracrystalline
2o
3particle, its particle diameter is 8-10nm.
Embodiment 8: Ni and Y are mixed to rear melting according to the mol ratio of Y 3%, then sample is heated to more than liquidus temperature 10 ℃ (1409 ℃) in atmosphere furnace, and pass into water vapour by the yttrium in-situ oxidation in nickel yttrium liquation, passing into the water vapour time is 1min, prepares nano yttrium oxide disperse in crystal grain and strengthens nickel-base composite material.Its microstructure as shown in figure 10.In-situ oxidation reaction forms Y at intracrystalline
2o
3particle, its particle diameter is 8-10nm.
Embodiment 9: Ni-13mol%Cu alloy and Y are mixed to rear melting according to the mol ratio of Y 9.5%, then sample is heated to 1310 ℃ of liquidus temperatures in atmosphere furnace, and pass into water vapor by the yttrium in-situ oxidation in nickel yttrium liquation, passing into the water vapour time is 1min, prepare nano yttrium oxide disperse and strengthen nickel-base composite material, in-situ oxidation reaction forms Y at intracrystalline
2o
3particle, its particle diameter is 20-30nm.
Claims (7)
1. in crystal grain, nano yttrium oxide disperse strengthens a nickel-base composite material, it is characterized in that by Ni substrate and the nanometer Y in Ni substrate crystal grain
2o
3disperse phase composition, wherein Y
2o
3molar content be 0.25mol%-4.7mol%.
2. in crystal grain according to claim 1, nano yttrium oxide disperse strengthens nickel-base composite material, it is characterized in that described Y
2o
3the particle diameter of particle is 4～30nm.
3. the preparation method of nano yttrium oxide disperse enhancing nickel-base composite material in a crystal grain, it is characterized in that the method is: be 0.5mol%～9.5mol% mix after melting with Y by the mol ratio of Y by Ni or Ni alloy, be heated to above 0～10 ℃ of its liquidus temperature, adopt water vapour or CO
2be oxidized, reaction in－situ generates Y
2o
3particle.
4. preparation method according to claim 3, is characterized in that described Y
2o
3the mol ratio of particle in Ni substrate crystal grain is 0.25mol%-4.7mol%.
5. preparation method according to claim 3, is characterized in that described Y
2o
3the particle diameter of particle is 4～30nm.
6. preparation method according to claim 3, is characterized in that using atmosphere furnace or vacuum oven that the sample after melting is heated to above 0～10 ℃ of its liquidus temperature.
7. preparation method according to claim 3, is characterized in that adopting water vapour or CO
2the time being oxidized is 1～120min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110527856A (en) * | 2019-09-20 | 2019-12-03 | 无锡市东杨新材料股份有限公司 | A kind of preparation method of great surface quality, high-intensity nickel alloy band |
| CN113061781A (en) * | 2021-03-16 | 2021-07-02 | 中国科学院上海应用物理研究所 | Nickel-based composite material and molten salt reactor core structural member |
Citations (2)
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|---|---|---|---|---|
| CN102251131A (en) * | 2011-06-30 | 2011-11-23 | 北京科技大学 | Method for preparing injection-molding nickel-base ODS (oxide dispersion strengthened) alloy |
| CN102660696A (en) * | 2012-05-14 | 2012-09-12 | 南昌大学 | Dispersion strengthening copper-based composite material and preparation method thereof |
-
2014
- 2014-03-11 CN CN201410087501.8A patent/CN103834831B/en not_active Expired - Fee Related
Patent Citations (2)
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| CN102251131A (en) * | 2011-06-30 | 2011-11-23 | 北京科技大学 | Method for preparing injection-molding nickel-base ODS (oxide dispersion strengthened) alloy |
| CN102660696A (en) * | 2012-05-14 | 2012-09-12 | 南昌大学 | Dispersion strengthening copper-based composite material and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| JIN-JU PARK ET AL: "Synthesis of Ni-Y2O3 nanocomposite powders by a very high speed planetary milling process: Microstructural development and refinement behavior", 《POWDER TECHNOLOGY》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110527856A (en) * | 2019-09-20 | 2019-12-03 | 无锡市东杨新材料股份有限公司 | A kind of preparation method of great surface quality, high-intensity nickel alloy band |
| CN110527856B (en) * | 2019-09-20 | 2021-04-30 | 无锡市东杨新材料股份有限公司 | Preparation method of high-surface-quality and high-strength nickel alloy strip |
| CN113061781A (en) * | 2021-03-16 | 2021-07-02 | 中国科学院上海应用物理研究所 | Nickel-based composite material and molten salt reactor core structural member |
| CN113061781B (en) * | 2021-03-16 | 2022-02-22 | 中国科学院上海应用物理研究所 | Nickel-based composite material and molten salt reactor core structural member |
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| CN103834831B (en) | 2016-03-30 |
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