CN111363987B - Amorphous alloy with ultrahigh initial crystallization temperature and preparation method thereof - Google Patents
Amorphous alloy with ultrahigh initial crystallization temperature and preparation method thereof Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C45/00—Amorphous alloys
- C22C45/003—Amorphous alloys with one or more of the noble metals as major constituent
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- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
- B22D11/0611—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by a single casting wheel, e.g. for casting amorphous metal strips or wires
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C33/00—Making ferrous alloys
- C22C33/003—Making ferrous alloys making amorphous alloys
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention relates to an amorphous alloy with ultrahigh initial crystallization temperature and a preparation method thereof, wherein the chemical formula of the alloy is WaTabRecOsdIreRufMogChBiThe content of each element in the formula is calculated by atomic percentage (at.%) as follows: a is 10-20, b is 10-20, c is 10-20, d is 10-20, e is 1-5, f is 1-5, g is 1-5, h is 5-20, i is 5-15, and a + b + c + d + e + f + g + h + i is 100. The amorphous alloy has the advantages of high controllability of the performance, simple preparation process, ultrahigh initial crystallization temperature, high room temperature and high temperature hardness, and has very important significance for breaking through the constraint that most of the existing amorphous alloys are only limited to be applied in the conventional environment due to the lower initial crystallization temperature and expanding the potential application of the amorphous alloy in more severe environments such as high temperature and the like.
Description
Technical Field
The invention relates to the technical field of amorphous alloy and preparation thereof, in particular to an amorphous alloy with ultrahigh initial crystallization temperature and a preparation method thereof.
Background
Amorphous alloys (also called metallic glass) are a class of alloys with short-range order and long-range disorder in atomic arrangement in the structure and uniform chemical components. The structure of the alloy does not have the defects of crystalline materials such as crystal boundary, tissue segregation, dislocation and the like, so that compared with the crystalline materials with the same components, the amorphous alloy has unique mechanical, physical and chemical properties and has very important potential application value in a plurality of fields such as aerospace, power electronics, oil gas exploration and exploitation and the like.
However, amorphous alloys, as a metastable material, transform into crystalline alloys when the temperature is raised to its initial crystallization temperature value (Tx), and accordingly lose their unique amorphous properties and fail. Therefore, the service temperature of the amorphous alloy must be lower than its Tx. However, Tx of most of the existing amorphous alloys does not exceed 550 ℃ (the relevant temperature value of the amorphous alloys in this specification is a value obtained when the temperature rise rate is 20 ℃/min without special description), which leads to that the application of the existing alloys is mainly in a normal temperature environment, and the application of the alloys in wider conditions such as high temperature is severely limited. In addition, the high and low mechanical properties such as hardness of the amorphous alloy are usually in positive correlation with the size of Tx, which means that the amorphous alloy with higher Tx often has excellent mechanical properties such as higher hardness. In addition, the Tx of most of the existing amorphous alloys is not more than 550 ℃, and people are difficult to perform systematic research on the main properties of the amorphous alloys such as hardness in a higher temperature range, so that the development of the amorphous alloys is further restricted.
Disclosure of Invention
The application provides an amorphous alloy with ultrahigh initial crystallization temperature and a preparation method thereof, which have very important significance for breaking through the constraint that most of the existing amorphous alloys are only limited to be applied in the conventional environment due to the lower initial crystallization temperature and expanding the potential application of the amorphous alloy in more severe environments such as high temperature and the like.
In order to achieve the purpose, the technical scheme of the invention is as follows:
an amorphous alloy with ultrahigh initial crystallization temperature and its chemical formula WaTabRecOsdIreRufMogChBiThe content of each element in the formula is calculated by atomic percentage (at.%) as follows: a is 10 to 20, b is 10 to 20, c is 10 to 20, d is 10 to 20, e is 1 to 5, f is 1 to 5, g is 1 to 5, h is 5 to 20, i is5 to 15, and a + b + c + d + e + f + g + h + i is 100.
Further, it has a chemical formula of W13Ta19Re17Os19Ir4Ru4Mo4C12B8。
Further, it has a chemical formula of W16Ta16Re19Os16Ir3Ru2Mo3C13B12。
Further, it has a chemical formula of W19Ta17Re19Os19Ir2Ru2Mo2C10B10。
A preparation method of an amorphous alloy with ultrahigh initial crystallization temperature comprises the following steps:
step one, batching: according to WaTabRecOsdIreRufMogChBiWeighing pure raw materials according to the chemical formula;
step two, smelting WaTabRecOsdIreRufMogChBiMother alloy ingot: putting the raw materials weighed in the step one into a vacuum arc melting furnace, and adjusting the vacuum degree in the furnace to be less than or equal to 5 multiplied by 10－3Pa, smelting at 3000-4000 ℃ for 1-5 min, smelting for 1-5 times under the smelting condition to uniformly smelt the raw materials, cooling along with the furnace, and taking out a master alloy ingot;
step three: preparation of WaTabRecOsdIreRufMogChBiAmorphous alloy: firstly, completely melting the master alloy ingot prepared in the step two by using an induction furnace in a rapid solidification device, and then carrying out W casting by using a melt rotary quenching method or a copper mold casting methodaTabRecOsdIreRufMogChBiThe melt is rapidly cooled and solidified to obtain WaTabRecOsdIreRufMogChBiIs not in a state of being polymerizedAnd (4) gold material.
The invention has the beneficial effects that:
1. the invention relates to an amorphous alloy with ultrahigh initial crystallization temperature, and the initial crystallization temperature value (T) thereofx) Can reach 950-1070 ℃, which is higher than the T of most existing amorphous alloysxAbove about 400 ℃; meanwhile, part of the alloy also has obvious glass transition temperature (T)g) And can reach 880-920 ℃, which is higher than that of the existing most amorphous alloys by more than 350 ℃; the amorphous alloy has high thermal stability, can obviously improve the use temperature of the amorphous alloy, and is beneficial to the use of the amorphous alloy at high temperature.
2. The ultra-high initial crystallization temperature amorphous alloy has high room temperature Vickers microhardness (H)v) (ii) a At room temperature HvThe content of the amorphous alloy is 17-25 GPa, and the value is higher than that of H of most of conventional amorphous alloysvThe thickness is about 1 time higher, and part of the thickness exceeds that of ceramic materials such as corundum and the like, and the amorphous alloy can be used as a room-temperature superhard wear-resistant coating material to further expand the application field of amorphous alloys.
3. The invention relates to an amorphous alloy with ultrahigh initial crystallization temperature, which has high-temperature Hv(ii) a The alloy still has Vickers microhardness of about 10GPa at the temperature of about 700 ℃, and the common amorphous alloy such as zirconium-based alloy can be failed at the temperature because of crystallization and even melting; can effectively ensure the performance stability of the amorphous alloy under severe conditions such as high temperature and the like, and is expected to break through the constraint that most of the existing amorphous alloys are only limited to be applied to the conventional environment due to the lower initial crystallization temperature.
4. The ultrahigh initial crystallization temperature amorphous alloy has 9 constituent elements, is favorable for regulating and controlling the initial crystallization temperature, the glass transition temperature, the hardness and other properties of the alloy in a wider component range, is favorable for obtaining the ultrahigh initial crystallization temperature amorphous alloy with different performance characteristics, and further better meets the requirements of practical application.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of an as-cast sample of the amorphous alloy composition of three examples of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following examples, it being understood that the described examples are only a part of the examples of the present invention, and not all examples. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides an amorphous alloy with ultrahigh initial crystallization temperature, which has a chemical formula of WaTabRecOsdIreRufMogChBiThe content of each element in the formula is calculated by atomic percentage (at.%) as follows: a is 10-20, b is 10-20, c is 10-20, d is 10-20, e is 1-5, f is 1-5, g is 1-5, h is 5-20, i is 5-15, and a + b + c + d + e + f + g + h + i is 100.
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention include, but are not limited to, the scope shown in the following examples.
Example 1:
an amorphous alloy with ultrahigh initial crystallization temperature, specifically W13Ta19Re17Os19Ir4Ru4Mo4C12B8The amorphous alloy is prepared by the following method:
the method comprises the following steps: ingredients
Pure W, pure Ta, pure Re, pure Os, pure Ir, pure Ru, pure Mo, pure C and pure B with the required purity of more than 99 wt.% are calculated and weighed according to the components;
step two: smelting master alloy ingot
Putting the raw materials weighed in the step one into a vacuum arc melting furnace, and adjusting the vacuum degree in the furnace to be 1 multiplied by 10－3Pa, the smelting temperature is 3300-3600 ℃, the smelting time is 2min, the raw materials are smelted uniformly by 3 times under the smelting condition, and the mother alloy ingot is taken out after the raw materials are cooled along with the furnace;
step three: preparation of amorphous alloy
Firstly, preparing the W prepared in the second step13Ta19Re17Os19Ir4Ru4Mo4C12B8Putting the alloy ingot into an induction furnace of a rapid solidification device to completely melt the alloy ingot, and then obtaining W with the thickness of about 30 mu m by a melt spinning method13Ta19Re17Os19Ir4Ru4Mo4C12B8An alloy strip sample; the corresponding preparation parameter is that the vacuum degree is 1 multiplied by 10-2Pa, induction current of 24-27A and spray casting pressure of 0.06 MPa.
W from example 113Ta19Re17Os19Ir4Ru4Mo4C12B8The cast alloy sample is tested and analyzed by XRD (as shown in figure 1), DSC and mechanical experiment, and the following results are obtained: the structure is in a single amorphous state (as shown in figure 1), the glass transition temperature is 887 ℃, the initial crystallization temperature is 968 ℃, the Vickers hardness at room temperature is about 19GPa, and the Vickers hardness at the temperature of about 700 ℃ is still as high as about 9.5 GPa.
Example 2:
an amorphous alloy with ultrahigh initial crystallization temperature, specifically W16Ta16Re19Os16Ir3Ru2Mo3C13B12The amorphous alloy is prepared by the following method:
the method comprises the following steps: ingredients
Pure W, pure Ta, pure Re, pure Os, pure Ir, pure Ru, pure Mo, pure C and pure B with the required purity of more than 99 wt.% are calculated and weighed according to the components;
step two: smelting master alloy ingot
Putting the raw materials weighed in the step one into a vacuum arc melting furnace, and adjusting the vacuum degree in the furnace to be 1 multiplied by 10－3Pa, the smelting temperature is 3400-3700 ℃, the smelting time is 2min, the raw materials are evenly smelted by 3 times under the smelting condition, and the master alloy ingot is taken out after the raw materials are cooled along with the furnace;
step three: preparation of bulk amorphous alloys
Firstly, preparing the W prepared in the second step16Ta16Re19Os16Ir3Ru2Mo3C13B12Putting the alloy ingot into an induction furnace of a rapid solidification device to completely melt the alloy ingot, and then obtaining W with the thickness of about 30 mu m by a melt spinning method16Ta16Re19Os16Ir3Ru2Mo3C13B12Alloy bar samples; the corresponding preparation parameter is that the vacuum degree is 1 multiplied by 10-2Pa, induction current 25-27A and spray casting pressure 0.06 MPa.
W from example 216Ta16Re19Os16Ir3Ru2Mo3C13B12The cast alloy sample is tested and analyzed by XRD (as shown in figure 1), DSC and mechanical experiment, and the following results are obtained: the structure of the material is in a single amorphous state (as shown in figure 1), the glass transition temperature is 902 ℃, the initial crystallization temperature is 993 ℃, the Vickers apparent hardness at room temperature is about 21.2GPa, and the Vickers apparent hardness at the temperature of about 700 ℃ is still as high as about 9.7 GPa.
Example 2 was chosen as the best embodiment of the invention.
Example 3:
an amorphous alloy with ultrahigh initial crystallization temperature, specifically W19Ta17Re19Os19Ir2Ru2Mo2C10B10The amorphous alloy is prepared by the following method:
the method comprises the following steps: ingredients
Pure W, pure Ta, pure Re, pure Os, pure Ir, pure Ru, pure Mo, pure C and pure B with the required purity of more than 99 wt.% are calculated and weighed according to the components;
step two: smelting master alloy ingot
Putting the raw materials weighed in the step one into a vacuum arc melting furnace, and adjusting the vacuum degree in the furnace to be 1 multiplied by 10－3Pa, the smelting temperature is 3500-3800 ℃, the smelting time is 2min, the raw materials are evenly smelted by 3 times under the smelting condition, and the mother alloy ingot is taken out after the raw materials are cooled along with the furnace;
step three: preparation of amorphous alloy
Firstly, preparing the W prepared in the second step19Ta17Re19Os19Ir2Ru2Mo2C10B10Putting the alloy ingot into an induction furnace of a rapid solidification device to completely melt the alloy ingot, and then obtaining W with the thickness of about 30 mu m by a melt spinning method19Ta17Re19Os19Ir2Ru2Mo2C10B10An alloy strip sample; the corresponding preparation parameter is that the vacuum degree is 1 multiplied by 10-2Pa, induction current 25-28A and spray casting pressure 0.06 MPa.
W from example 119Ta17Re19Os19Ir2Ru2Mo2C10B10The cast alloy sample is tested and analyzed by XRD (as shown in figure 1), DSC and mechanical experiment, and the following results are obtained: the structure is in a single amorphous state (as shown in figure 1), the initial crystallization temperature is 1030 ℃, the Vickers apparent hardness at room temperature is about 22.8GPa, and the hardness is still as high as about 10.1GPa at a temperature of about 700 ℃.
The present invention has been described in terms of specific examples, which are provided to aid understanding of the invention and are not intended to be limiting. Any partial modification or replacement within the technical scope of the present disclosure by a person skilled in the art should be included in the scope of the present disclosure.
Claims (5)
1. An amorphous alloy with ultrahigh initial crystallization temperature, which is characterized in that the chemical formula is WaTabRecOsdIreRufMogChBiThe content of each element in the formula is calculated by atomic percentage (at.%) as follows: a is 10-20, b is 10-20, c is 10-20, d is 10-20, e is 1-5, f is 1-5, g is 1-5, h is 5-20, i is 5-15, and a + b + c + d + e + f + g + h + i is 100.
2. The ultra-high initial crystallization temperature amorphous alloy according to claim 1, whereinCharacterized in that: having a chemical formula of W13Ta19Re17Os19Ir4Ru4Mo4C12B8。
3. The ultra-high initial crystallization temperature amorphous alloy according to claim 1, wherein: having a chemical formula of W16Ta16Re19Os16Ir3Ru2Mo3C13B12。
4. The ultra-high initial crystallization temperature amorphous alloy according to claim 1, wherein: having a chemical formula of W19Ta17Re19Os19Ir2Ru2Mo2C10B10。
5. The method for preparing the ultra-high initial crystallization temperature amorphous alloy according to claim 1, comprising the steps of:
step one, batching: according to WaTabRecOsdIreRufMogChBiWeighing pure raw materials according to the chemical formula;
step two, smelting WaTabRecOsdIreRufMogChBiMother alloy ingot: putting the raw materials weighed in the step one into a vacuum arc melting furnace, and adjusting the vacuum degree in the furnace to be less than or equal to 5 multiplied by 10－3Pa, smelting at 3000-4000 ℃ for 1-5 min, smelting for 1-5 times under the smelting condition to uniformly smelt the raw materials, cooling along with the furnace, and taking out a master alloy ingot;
step three: preparation of WaTabRecOsdIreRufMogChBiAmorphous alloy: firstly, completely melting the master alloy ingot prepared in the step two by using an induction furnace in a rapid solidification device, and then carrying out W casting by using a melt rotary quenching method or a copper mold casting methodaTabRecOsdIreRufMogChBiThe melt is rapidly cooled and solidified to obtain WaTabRecOsdIreRufMogChBiAnd (3) amorphous alloy materials.
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