CN111254369A - Method for refining yttrium-containing zirconium-based amorphous alloy material - Google Patents
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- C22C45/00—Amorphous alloys
- C22C45/10—Amorphous alloys with molybdenum, tungsten, niobium, tantalum, titanium, or zirconium or Hf as the major constituent
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- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
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Abstract
The invention discloses a method for refining an yttrium-containing zirconium-based amorphous alloy material, which comprises the following specific steps of: (1) calculating and weighing various raw materials according to the component proportion of the target yttrium-containing zirconium-based amorphous alloy material; (2) sintering the aluminum-silicon spinel crucible covered with the yttrium oxide coating at 700-800 ℃ for 4-8 h; (3) sequentially adding various raw materials into the cleaned crucible; (4) firstly, vacuumizing a vacuum induction smelting furnace to enable the vacuum degree in the furnace to reach 0.01-0.05Pa, then filling argon with the volume percentage purity of 99.99% into the furnace to 0.01-0.03 MPa, and then supplying power to the vacuum induction smelting furnace; (5) heating a vacuum induction smelting furnace to 1000-1200 ℃ of furnace charge, and refining the raw materials, wherein the refining power is 90-120Kw, and the refining time is 2-20 min; (6) and after the refining is finished, carrying out charged pouring on the obtained yttrium-containing zirconium-based amorphous alloy material. The method improves the product quality of the yttrium-containing zirconium-based amorphous alloy material and reduces the production cost.
Description
Technical Field
The invention relates to a method for refining an yttrium-containing zirconium-based amorphous alloy material, belonging to the technical field of amorphous alloys.
Background
At present, the enthalpy value of formation of rare earth Y oxide is about 1903.6kJ/mol, the enthalpy value of formation of Zr oxide is about 1102.3kJ/mol, and Y is easier to combine with oxygen than Zr, so that rare earth Y can effectively absorb and eliminate oxygen in the experimental process and the master alloy matrix, and finally eliminate oxygen in the metal melt, but formed yttrium oxide scum is easy to be involved in the master alloy matrix, and inclusion particles are formed in an amorphous sample, thereby influencing the appearance and performance of the sample.
In addition, the smelting furnace adopted in the experiment is a vacuum induction smelting furnace, mainly because the furnace is simple in furnace material selection, does not need to be provided with electrodes, is high in production efficiency, simple to operate, large in electromagnetic stirring force, good in component consistency and the like, but the vacuum induction smelting furnace also has the following inherent defects: the slag in the furnace and the molten pool are mixed together, an oxide crucible is adopted to inevitably react with metal, and particularly, active metals such as zirconium, titanium and the like which are greatly utilized in amorphous alloy basically have no functions of desulfurization, dephosphorization and the like in an induction melting furnace.
Therefore, a set of refining process suitable for adding rare earth element yttrium to the zirconium-based amorphous alloy is particularly important for improving the product quality of the zirconium-based amorphous alloy.
Disclosure of Invention
Aiming at the existing technical problems, the invention provides a method for refining an yttrium-containing zirconium-based amorphous alloy material, so as to improve the product quality of the amorphous alloy and reduce the production cost.
In order to achieve the purpose, the invention provides a method for refining an yttrium-containing zirconium-based amorphous alloy material, which comprises the following specific steps:
(1) calculating and weighing various raw materials according to the component proportion of the target yttrium-containing zirconium-based amorphous alloy material;
(2) sintering the aluminum-silicon spinel crucible covered with the yttrium oxide coating at 700-800 ℃ for 4-8 h;
(3) cleaning the crucible, adding various raw materials into the crucible, and then putting the crucible into a vacuum induction melting furnace;
(4) firstly, vacuumizing a vacuum induction smelting furnace to ensure that the vacuum degree in the furnace reaches 0.01-0.05Pa, then filling argon with the volume percentage purity of 99.99% into the furnace to 0.01-0.03 MPa, and then transmitting power to the vacuum induction smelting furnace;
(5) heating a vacuum induction smelting furnace to 1000-1200 ℃ of furnace charge, and refining the raw materials, wherein the refining power is 90-120Kw, and the refining time is 2-20 min;
(6) and after the refining is finished, carrying out charged pouring on the obtained yttrium-containing zirconium-based amorphous alloy material.
Further, the aluminum-silicon spinel crucible is mainly made of alumina and silica according to the weight ratio of 78% and 22%.
Furthermore, the preparation process of the yttrium oxide coating is as follows: firstly, mixing yttrium oxide and ethanol according to a volume ratio of 5: 1, mixing and stirring uniformly to obtain slurry; then uniformly coating the slurry on the inner wall of the crucible, and standing for 1 h; then the crucible is put into a muffle furnace to be sintered for 10 to 12 hours at high temperature (1200-.
In the technical scheme, the crucible is an aluminum-silicon spinel crucible covered with an yttrium oxide coating, the service life of the crucible can be effectively prolonged, and the production cost is reduced for the following specific reasons: in the process of selecting the ceramic crucible, the stability of the crucible is as follows from the view point of reacting with the amorphous alloy: the yttrium oxide crucible, the calcium oxide crucible, the zirconium oxide crucible and the aluminum oxide crucible are all adopted, and the volume of the yttrium oxide crucible is small at present, so the calcium oxide crucible is preferably selected; however, in the actual use process, for example, a silicon oxide, magnesium oxide and barium zirconate crucible is added for trial use, and the problem that the crucible with good stability has poor service life is found; for example, the most stable calcium oxide crucible is not suitable for being used in the humid environment of south China because the calcium oxide crucible needs to be used in a non-water environment or is pulverized, and even the calcium oxide crucible used in the month of February and February is subjected to natural pulverization and collapse after being unsealed; for example, the barium zirconate crucible is cracked after about 10 furnaces are used, so that the problem of steel leakage is caused, the cost of the crucible is high, and each kilogram of the crucible is about 20 yuan, so that the crucible is not suitable for smelting zirconium alloy; finally, the aluminum-silicon spinel crucible with the weight ratio of the aluminum oxide to the silicon oxide being 78% and 22% respectively is adopted, and the independently developed yttrium oxide coating technology is combined, so that the service life of the aluminum-silicon spinel crucible can reach 50-60 furnaces, the use cost is reduced to 0.78 yuan/Kg, and the comprehensive performance is very excellent.
Furthermore, the aluminum oxide sheet is embedded into the opening of the crucible to serve as a slag blocking plate, the slag blocking plate is 5-10mm away from the bottom of the crucible opening groove, the size is 60mm x 40mm x 15mm, larger floating objects can be isolated in advance, and certain slag blocking and purifying effects are achieved on molten soup.
Furthermore, the upper end of the pouring material flow passage is provided with a filtering device which mainly comprises a filtering pouring cup and ZrO2And a ceramic filter disk of ZrO2The ceramic filter plate is embedded into the filtering sprue cup, so that the double-filtering effect is achieved, the molten soup can be adsorbed and filtered, and the quality of the yttrium-zirconium-based amorphous alloy material is improved.
Preferably, the refining power of the vacuum induction melting furnace is 120Kw, and the refining time is 3 min.
Preferably, the refining power of the vacuum induction melting furnace is 120Kw, and the refining time is 9 min.
The refining parameters of the vacuum induction smelting furnace can effectively prevent yttrium oxide particles from agglomerating and improve the forming capacity of the zirconium-based amorphous alloy.
In summary, the method of the present invention has the following technical advantages:
1. the aluminum-silicon spinel crucible covered with the yttrium oxide coating is adopted, so that the service life of the crucible is prolonged, and the production cost is reduced;
2. the slag baffle and the filtering device are additionally arranged, so that the content of oxygen and scum in the yttrium-zirconium-based amorphous alloy cast ingot is reduced, and the surface quality of the yttrium-zirconium-based amorphous alloy die casting is improved;
3. the refining parameters of the vacuum induction smelting furnace are selected, so that the quality of the yttrium-containing zirconium-based amorphous alloy product is improved.
Drawings
FIG. 1 is a graph of a ground sample made in examples A-F of the present invention;
FIG. 2 is a graph showing the analysis of inclusions in cast ingot samples produced by examples A to F of the present invention;
FIG. 3 is a structural view of an aluminum silicon spinel crucible embedded slag trap of the present invention;
FIG. 4 is a top view of the structure of the aluminum silicon spinel crucible embedded slag trap of the present invention;
FIG. 5 is a cross-sectional view taken along line C-C of FIG. 4 in accordance with the present invention;
FIG. 6 is an enlarged view taken at point I of FIG. 5 in accordance with the present invention;
FIG. 7 is an enlarged view taken at point II of FIG. 4 in accordance with the present invention;
FIG. 8 is a statistical chart of oxygen content and loss in ingot samples made before and after the addition of the slag trap of the present invention;
FIG. 9 is a block diagram of a filter assembly according to the present invention;
FIG. 10 is a cross-sectional view of a filter assembly of the present invention;
FIG. 11 is a SEM comparison of an ingot sample before and after filtration using a filtration apparatus of the present invention;
FIG. 12 is a comparison of the macro topography of ingot samples with and without ceramic filter membranes according to the present invention;
in the figure: 1. crucible, 2 slag trap, 3 filtering pouring cup, 4, ZrO2A ceramic filter cup.
Detailed Description
The present invention will be further described with reference to the following examples.
First, the method of the present invention optimizes the refining parameters. When in implementation, the specific steps for refining the yttrium-containing zirconium-based amorphous alloy material are as follows:
(1) calculating and weighing various required raw materials according to the component proportion of the target yttrium-containing zirconium-based amorphous alloy material.
(2) Sintering the crucible at 700-800 ℃ for 4-8 h.
(3) The crucible is cleaned, various raw materials are added into the crucible, and then the crucible is placed into a vacuum induction melting furnace.
(4) The experiment adopts a vacuum induction smelting furnace, the vacuum induction smelting furnace is firstly vacuumized to ensure that the vacuum degree in the furnace reaches 0.01-0.05Pa, then argon with the purity of 99.99 percent in volume percentage is filled into the furnace to 0.01-0.03 MPa, and then the vacuum induction smelting furnace is powered on.
(5) Heating a vacuum induction smelting furnace to 1000-1200 ℃ of furnace charge, and refining the raw materials, wherein the refining power is 90-120Kw, and the refining time is 2-20 min.
The corresponding refining experimental parameters of the embodiments A to F are shown in the table 1, wherein in the embodiment A, B, C, the refining powers of the vacuum induction melting furnaces are the same and are all 90Kw, and the refining time is sequentially prolonged and is respectively 3min, 9min and 15 min; in example D, E, F, the refining powers of the vacuum induction melting furnaces were all 120Kw and all 90Kw, and the refining times were sequentially extended for 3, 9, and 15min, respectively.
TABLE 1
| Experiment number | Refining power/Kw | Refining time (min) |
| A | 90 | 3 |
| B | 90 | 9 |
| C | 90 | 15 |
| D | 120 | 3 |
| E | 120 | 9 |
| F | 120 | 15 |
(6) And carrying out charged pouring after refining. Sampling and die-casting the yttrium-containing zirconium-based amorphous alloy materials prepared in the embodiments A to F on a die-casting machine to obtain the following sizes: 110mm ﹡ 10mm ﹡ 2 mm. The sample was then sampled transversely, mounted, and ground, and the ground sample was prepared for subsequent evaluation as shown in FIG. 1.
The oxygen content and the damage rate of the yttrium-containing zirconium-based amorphous alloy samples obtained in examples a to F were measured, and the results of the measurement are shown in table 2, which enables evaluation of the effect of the improvement of the process of the present invention.
TABLE 2
| Experiment number | O content (ppm) | Rate of loss |
| A | 78.8 | 3.3％ |
| B | 163.2 | 3.8％ |
| C | 127 | 6.2％ |
| D | 152.2 | 3.3％ |
| E | 96.5 | 4.3％ |
| F | 96.1 | 5.2％ |
And the number and the size of the inclusion particles in the grinding sample are observed under a scanning electron microscope and are comprehensively evaluated to obtain more comprehensive evaluation data. As shown in FIG. 2, the analysis of inclusions in the samples obtained in examples A to F is shown from left to right and from top to bottom, and the results are analyzed to obtain comprehensive data as shown in Table 3.
TABLE 3
| Experiment number | A | B | C | D | E | F |
| Amount of yttrium oxide | 15 | 5 | 10 | 0 | 4 | 2 |
| Average size (μm) | 4.31 | 4.298 | 5.978 | 0 | 2.055 | 5.72 |
It can be seen that the results of the three groups of example A, B, C are inferior to those of the three groups of example C, D, E in comparison of the two dimensions, and the difference between the two groups is the selection of refining power, the reaction of the molten pool is severe when 120Kw refining is adopted, the temperature is higher, yttrium oxide particles are correspondingly dispersed to be finer and even to be the size which can not be captured by SEM, but the service life of the crucible is reduced when the process is also adopted, and the mode is more seriously eroded when the temperature is too high during furnace pouring. Transverse comparative analysis of the results in three groups, example A, B, C and example C, D, E, except that there was some error in the observation (the result was 0) in the group of example D, led to the following conclusion: when the refining process is increased to 12 minutes, the particle size increases again because a portion of the oxide particles re-agglomerate and an excessively long time increases the amount of dross formed in the crucible.
Comprehensively considering, according to the two sets of parameters of the embodiment D, E, namely the refining power of the vacuum induction melting furnace is 120Kw and the refining time is 3min, or the refining power of the vacuum induction melting furnace is 120Kw and the refining time is 9min, the invention can make outstanding improvement effect on the yttrium oxide particles.
Secondly, the method optimizes the crucible and the slag discharge technology. In the implementation, the invention adopts aluminum-silicon spinel crucibles with the weight ratios of aluminum oxide to silicon oxide of 78% and 22%, respectively, and combines with the independently developed yttrium oxide coating technology, namely, yttrium oxide and ethanol are mixed according to the volume ratio of 5: 1, uniformly mixing to form slurry, uniformly coating the slurry on the inner wall of an aluminum-silicon spinel crucible, standing for one hour, sintering the crucible in a muffle furnace at high temperature (1200-1400 ℃) for 10-12 hours, and cooling along with the furnace. Tests prove that the service life of the aluminum-silicon spinel crucible covered with the yttrium oxide coating can reach 50-60 furnaces, and meanwhile, the use cost of the whole refining process is reduced to 0.78 yuan/Kg, so that the aluminum-silicon spinel crucible covered with the yttrium oxide coating has very excellent comprehensive performance.
In addition, the invention reforms the crucible mouth of the yttrium oxide coated aluminum-silicon spinel crucible, as shown in fig. 3-7, an aluminum oxide sheet is embedded in the mouth part of the crucible 1 to be used as a slag baffle plate 2, the placing position of the slag baffle plate 2 is 5-10mm away from the bottom of the mouth groove of the crucible 1, the size is 60mm x 40mm x 15mm, larger floating objects can be isolated in advance, and the molten soup has certain slag baffle and purification effects.
As shown in fig. 8, after the slag trap 2 is added to the crucible opening of the aluminum-silicon spinel crucible, the average oxygen content index of the yttrium-containing zirconium-based amorphous alloy material ingot is 371; when the slag blocking plate is not added, the average oxygen content index of the yttrium-containing zirconium-based amorphous alloy material ingot is 472. From the data, the addition of the slag trap 2 can effectively reduce the oxygen content of the yttrium-zirconium-based amorphous alloy material ingot, and certainly, the slag trap 2 can prevent a part of molten liquid from entering the ingot casting mold, so that the yield of the yttrium-zirconium-based amorphous alloy material is influenced, and the influence is only about 1.4%.
Furthermore, the method optimizes the measures such as filtration and the like which are beneficial to the purification of the amorphous alloy. As shown in FIGS. 9-10, the present invention incorporates a filtering means at the upper end of the sprue channel consisting essentially of a filtering tundish 3 and ZrO2 Ceramic filter cup 4 and ZrO2The ceramic filter plate cup 4 is embedded into the filtering sprue cup 3, so that a double-filtering effect is achieved, the molten soup can be adsorbed and filtered, and the quality of the yttrium-zirconium-based amorphous alloy material is improved.
As shown in fig. 11, as can be seen from SEM images of the internal surface topography of the ingot sample before and after the addition of the filtering device, the filtering device is added in the present invention, so that the oxide particles inside the ingot sample are significantly reduced. Furthermore, as shown in FIG. 12, from the macro morphology of the ingot sample, ZrO was not added to the right2The surface of a casting filtered by the ceramic filter plate cup 4 has a large block surface-level burning loss phenomenon, and ZrO is added on the left side2The surface quality of the casting filtered by the ceramic filter plate cup 4 is obviously improved. Therefore, the filtering device can effectively improve the surface quality of the zirconium-based amorphous alloy die casting.
The foregoing describes some of the many possible embodiments of the invention in order to provide a basic understanding of the invention and is not intended to identify key or critical elements of the invention or to delineate the scope of the invention. It is easily understood that according to the technical solution of the present invention, other implementations that can be substituted with each other can be suggested by those skilled in the art without changing the spirit of the present invention. Therefore, the above-mentioned embodiments and the accompanying drawings are only exemplary illustrations of the technical solutions of the present invention, and should not be construed as all of the present invention or as limitations or limitations on the technical solutions of the present invention.
Claims (7)
1. A method for refining an yttrium-containing zirconium-based amorphous alloy material is characterized by comprising the following specific steps:
(1) calculating and weighing various raw materials according to the component proportion of the target yttrium-containing zirconium-based amorphous alloy material;
(2) sintering the aluminum-silicon spinel crucible covered with the yttrium oxide coating at 700-800 ℃ for 4-8 h;
(3) cleaning the crucible, adding various raw materials into the crucible, and then putting the crucible into a vacuum induction melting furnace;
(4) firstly, vacuumizing a vacuum induction smelting furnace to enable the vacuum degree in the furnace to reach 0.01-0.05Pa, then filling argon with the volume percentage purity of 99.99% into the furnace to 0.01-0.03 MPa, and then supplying power to the vacuum induction smelting furnace;
(5) heating a vacuum induction smelting furnace to the temperature of furnace charge of 1000-1200 ℃, and refining the raw materials, wherein the refining power is 90-120Kw, and the refining time is 2-20 min;
(6) and after the refining is finished, carrying out charged pouring on the obtained yttrium-containing zirconium-based amorphous alloy material.
2. A method for refining an amorphous alloy material containing yttrium and zirconium according to claim 1, wherein said aluminum-silicon spinel crucible is made mainly of alumina and silica in the weight ratio of 78% and 22%.
3. A method for refining an yttrium-containing zirconium-based amorphous alloy material according to claim 1 or 2, wherein the yttrium oxide coating is prepared by the following steps: firstly, mixing yttrium oxide and ethanol according to a volume ratio of 5: 1, mixing and stirring uniformly to obtain slurry; then uniformly coating the slurry on the inner wall of the crucible, and standing for 1 h; then the crucible is put into a muffle furnace to be sintered for 10 to 12 hours at the temperature of 1200-1400 ℃, and then is cooled along with the furnace.
4. A method for refining an yttrium-containing zirconium-based amorphous alloy material according to claim 1 or 2, wherein the crucible mouth is embedded with alumina flakes as a slag trap, and the slag trap is 5-10mm away from the bottom of the crucible mouth groove.
5. A method for refining an amorphous alloy material containing yttrium and zirconium according to claim 1 or 2, wherein a filter consisting essentially of a filter cup and ZrO is installed at the upper end of the flow channel2And a ceramic filter disk of ZrO2The ceramic filter disc is embedded inside the filter pouring cup.
6. The method for refining an yttrium-zirconium-based amorphous alloy material according to claim 1, wherein the refining power of the vacuum induction melting furnace is 120Kw, and the refining time is 3 min. .
7. The method for refining an yttrium-zirconium-based amorphous alloy material according to claim 1, wherein the refining power of the vacuum induction melting furnace is 120Kw, and the refining time is 9 min.
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| CN115231916B (en) * | 2022-07-13 | 2023-08-15 | 西安西工大思强科技股份有限公司 | Magnesia-alumina spinel forming crucible and manufacturing method thereof |
| CN115403392A (en) * | 2022-08-24 | 2022-11-29 | 广东省科学院资源利用与稀土开发研究所 | Crucible base body for smelting titanium-based gold storage alloy and preparation method and application thereof |
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