CN113969370A - Bismuth-based liquid metal with melting point lower than 50 ℃ and preparation method thereof - Google Patents
Bismuth-based liquid metal with melting point lower than 50 ℃ and preparation method thereof Download PDFInfo
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- CN113969370A CN113969370A CN202111248138.XA CN202111248138A CN113969370A CN 113969370 A CN113969370 A CN 113969370A CN 202111248138 A CN202111248138 A CN 202111248138A CN 113969370 A CN113969370 A CN 113969370A
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- C22C30/04—Alloys containing less than 50% by weight of each constituent containing tin or lead
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Abstract
The invention discloses a bismuth-based liquid metal with a melting point lower than 50 ℃ and a preparation method thereof. Wherein the bismuth-based liquid metal comprises the following components in parts by mass: 35-40 parts of bismuth; 10-15 parts of tin; 15-21 parts of indium; 15-20 parts of lead; 5-10 parts of cadmium. The invention adjusts the proportion of alloy components in an alloying way to prepare the five-element bismuth-based liquid metal BiSnInPbCd with clear component proportion. The alloy is simply and uniformly melted by vacuum melting by using a tube sealing technology, the component proportion of the melted alloy can be ensured to be consistent with the initial addition proportion, the preparation method is simple and convenient, the good performance and high repeatability of the liquid metal can be ensured, and the melting point of the bismuth-based liquid metal provided by the invention is 46-47 ℃.
Description
Technical Field
The invention relates to the technical field of bismuth-based liquid metal, in particular to bismuth-based liquid metal with a melting point lower than 50 ℃ and a preparation method thereof.
Background
With the development of science and technology, liquid metal develops rapidly, especially in the aspect of electronic printing, high density heat dissipation, flexible antenna, liquid robot, etc., it has apparent advantage. And the bismuth (Bi) -based liquid metal is gradually appeared in the visual field of people as a novel multifunctional material, and has incomparable advantages in electric conduction and heat conduction and 3D printing application due to the consideration of the characteristics of the metal and the liquid and the higher melting point of the gallium. Bismuth-based liquid metals have a higher melting point and are solid at room temperature compared to gallium-based liquid metals, which makes them unique applications such as wearable electronics, flexible antennas, 3D printed metal materials. However, there are still some critical issues that restrict the development of bismuth-based liquid metals, such as melting point. At present, the melting point of bismuth-based liquid metal is not yet adaptable to various complex conditions, so that the development of bismuth-based liquid metal with lower melting point is an urgent requirement. The invention aims at reducing the melting point of the bismuth-based liquid metal, develops the alloy component with the melting point lower than 50 ℃, and further expands the service temperature range of the bismuth-based liquid metal.
Disclosure of Invention
Aiming at the technical problems, the invention provides the bismuth-based liquid metal with the melting point lower than 50 ℃ and the preparation method thereof, which obviously reduce the melting point of the bismuth-based liquid metal and improve the application range of the liquid metal in the field of medium temperature.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a bismuth-based liquid metal with a melting point lower than 50 ℃, which comprises the following components in parts by mass:
35-40 parts of bismuth; 10-15 parts of tin; 15-21 parts of indium; 15-20 parts of lead; 5-10 parts of cadmium.
In certain particular embodiments, the mass portion of bismuth may be 35 parts, 36 parts, 37 parts, 38 parts, 39 parts, 40 parts, or any portion therebetween.
In certain specific embodiments, the mass part of tin may be 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, or any parts therebetween.
In certain specific embodiments, the portion by mass of indium may be 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, 20 parts, 21 parts, or any portion therebetween.
In certain specific embodiments, the parts by mass of lead may be 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, 20 parts, or any parts therebetween.
In certain particular embodiments, the parts by mass of cadmium can be 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, or any parts therebetween.
As a preferred embodiment, the bismuth-based liquid metal consists of the following components in parts by mass:
38-40 parts of bismuth; 13-15 parts of tin; 19-21 parts of indium; 18-19% of lead; 7-10 parts of cadmium;
the melting point is 46-47 deg.C, such as 46.1 deg.C, 46.2 deg.C, 46.3 deg.C, 46.4 deg.C, 46.5 deg.C, 46.6 deg.C, 46.7 deg.C, 46.8 deg.C, 46.9 deg.C, 47 deg.C or any temperature in between.
The invention also provides a preparation method of the bismuth-based liquid metal, which comprises the following steps:
(1) weighing raw materials of each component of the bismuth-based liquid metal according to a proportion;
(2) placing the raw materials of each component in the step (1) in an inert gas atmosphere, and sealing;
(3) heating until the raw materials of each component are melted to obtain a molten sample;
(4) and (4) uniformly dispersing the molten sample obtained after the treatment in the step (3) to obtain the bismuth-based liquid metal.
In certain embodiments, in step (1), the purity of the raw materials of each component is 99.99% and the surface oxide layer is polished with 800# sandpaper before weighing.
In certain specific embodiments, the inert gas atmosphere in step (2) is selected from inert gases such as nitrogen, carbon dioxide, helium, and the like.
In a preferable embodiment, in the step (2), the component materials are placed in a high-purity nitrogen atmosphere, and the cadmium raw material is placed at the bottommost part of the component materials, so that the volatilization of the cadmium can be avoided as much as possible.
In certain specific embodiments, in the step (2), the inert gas atmosphere may be established by pumping the inside of the reaction vessel to a vacuum degree of-0.01 to 0.1Pa, then filling the inert gas into the reaction vessel, and then performing gas washing, and repeating the steps three times. Preferably, the time for filling the inert gas is 5-10 seconds. The construction of the inert gas atmosphere can reduce the oxidation reaction in the sample melting process and ensure the consistency of the liquid metal components and the initial raw material proportion; in order to avoid the loss of the component content of the finally prepared liquid metal caused by the volatilization of the raw materials of each component in the reaction process, the tightness of the reaction vessel needs to be ensured, and in some specific embodiments, the necking part of the reaction vessel can be sintered after high-purity nitrogen is filled, so that the tube can be completely sealed, and the sealing is realized.
In a preferable embodiment, in the step (3), the heating temperature of the heating is 600 to 700 ℃.
Preferably, in the step (3), the time for melting the raw materials of each component is 5-10 minutes.
In a preferable embodiment, in the step (4), the uniform dispersion is ultrasonic oscillation dispersion.
Preferably, in the step (4), the temperature of the ultrasonic oscillation dispersion treatment is controlled to be 60-80 ℃, the ultrasonic frequency is controlled to be 40-60 KHz, and the ultrasonic power is 60-80W.
In the technical scheme of the invention, a tube sealing method filled with inert gas for protection is adopted. Pumping the reaction vessel to-0.01-0.1 Pa, filling high-purity nitrogen gas washing, pumping to-0.01-0.1 Pa again, repeatedly washing for 3 times, and finally filling high-purity nitrogen to ensure that the reaction vessel is in a high-purity nitrogen protection atmosphere. Thus, the oxidation of the alloy can be reduced in the process of melting, and the liquid metal component is ensured to be the same as the initial ratio.
The technical scheme has the following advantages or beneficial effects:
the invention provides a bismuth-based liquid metal with a melting point lower than 50 ℃ and a preparation method thereof. The invention discloses a method for preparing quinary BiSnInPbCd liquid metal with a melting point lower than 50 ℃ based on ternary eutectic BiSnIn (Bi: Sn: In: 53.8:19.2:27) with a melting point temperature of 80.18 ℃, which is discovered In the applicationQuaternary Bi prepared by adding 20 parts of Pb43Sn15.4In21.6Pb20The melting point temperature of the liquid metal is 57.60 ℃, four elements of Bi, Sn, In and Pb are analyzed, the enthalpy value of mixing between every two elements is found to be negative, the atomic acting force between various elements is weak, the solid solution phase is favorably formed, the intermediate compound with higher melting point is not favorably formed, and the feasibility of adding Sn, In, Pb and Cd to realize quinary alloying is proved. Therefore, the invention reduces the melting point temperature of the liquid metal by micro-adjusting the components and the proportion of the bismuth-based liquid metal in a micro-adding mode, has clear components and simple experiment, only needs simple vacuum melting to uniformly melt the bismuth-based liquid metal, and is an efficient melting point reduction mode capable of ensuring the good performance of the liquid metal.
Drawings
FIG. 1 shows a bismuth-based liquid metal (Bi) in example 143Sn15.4In21.6Pb20)93Cd7DSC test result chart of (1);
FIG. 2 shows a bismuth-based liquid metal (Bi) in example 243Sn15.4In21.6Pb20)90Cd10DSC test result chart of (1);
FIG. 3 shows the bismuth-based liquid metal Bi of comparative example 153.8Sn19.2In27DSC test result chart of (1);
FIG. 4 shows the bismuth-based liquid metal Bi of comparative example 243Sn15.4In21.6Pb20DSC test result chart of (1).
Detailed Description
The following examples are only a part of the present invention, and not all of them. Thus, the detailed description of the embodiments of the present invention provided below is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the invention without making creative efforts, belong to the protection scope of the invention.
The method for preparing liquid metal in the following examples and comparative examples comprises the following steps:
(1) weighing a proper pure metal sample, wherein the purity of the selected pure metal sample is 99.99%, then polishing a surface oxidation layer by using 800# abrasive paper, filling the sample into a sample bag filled with absolute ethyl alcohol, and putting the sample bag into a Jie' e JP-010S ultrasonic cleaning machine for cleaning. And drying the cleaned sample, and then putting the sample into a reaction vessel in the order of cadmium, zinc, bismuth, lead and indium.
(2) Filling high-purity nitrogen into a reaction vessel (a quartz test tube with the inner diameter of 9mm, the outer diameter of 12mm and the height of 29 cm), and applying a tube sealing machine (Partulab MRVS-1002; purchased from Bailibo science and technology (China) and subjected to vacuum pumping and tube sealing treatment. The specific operation is as follows: and (3) placing the test tube filled with the sample into a tube sealing machine, opening a mechanical pump, then opening a vacuum pump, opening an air suction valve, pumping the vacuum degree in the test tube to-0.01-0.1 Pa, closing the air suction valve, opening a high-purity nitrogen side air inlet valve, closing the air inlet valve after 5-10 s, and pumping the vacuum degree to-0.01-0.1 Pa again. Repeatedly washing gas for at least 3 times, and filling high-purity nitrogen after the washing gas is finished to construct a protective atmosphere; and then sintering and sealing the test tube port by using a hydrogen flame gun to complete the tube sealing process.
(3) And heating the reaction vessel to 600-700 ℃, and keeping the temperature for 5-10 minutes until the pure metal sample is melted to obtain a liquid metal melt sample.
(4) And carrying out ultrasonic oscillation dispersion treatment on the liquid metal molten sample, wherein the temperature of the ultrasonic dispersion treatment is controlled to be 60-80 ℃, the ultrasonic frequency is controlled to be 40-60 KHz, the ultrasonic power is 60-80W, and the ultrasonic dispersion treatment time is controlled to be 30 minutes to obtain uniform liquid metal.
In the following examples, the melting point of bismuth-based liquid metals was tested as follows: the bismuth-based liquid metal belongs to a solid state at normal temperature, and an alloy in the middle of a test tube is selected for a DSC experiment. Approximately 10mg of the sample was cut into an aluminum platen and compacted with a platen machine. The DSC initial temperature is set to be 30 ℃, the end point temperature is set to be 60 ℃, and the heating rate is 5 k/min. The onset temperature after the measurement was taken as the melting point of the alloy.
Example 1
In this example, the liquid metal is (Bi)43Sn15.4In21.6Pb20)93Cd7(the mass portion is 40.0 portions of bismuth, 20.1 portions of indium, 18.6 portions of lead, 14.3 portions of tin and 7 portions of cadmium), the preparation method comprises the following steps:
(1) weighing a pure metal sample with the total mass of about 5g, polishing a surface oxidation layer by using 800# abrasive paper, filling the pure metal sample into a sample bag filled with absolute ethyl alcohol, and putting the sample bag into an ultrasonic cleaning machine for cleaning. And drying the cleaned sample, and then putting the sample into a reaction vessel in the order of cadmium, zinc, bismuth, lead and indium.
(2) Inert gas is filled into a reaction vessel (a quartz test tube with the inner diameter of 9mm, the outer diameter of 12mm and the height of 29 cm), and a tube sealing machine is used for vacuumizing and tube sealing treatment, wherein the vacuum degree is 0.01 Pa. Repeatedly washing gas for at least 3 times, and filling high-purity nitrogen after the washing gas is finished to construct a protective atmosphere; and then sintering and sealing the test tube port by using a hydrogen flame gun to complete the tube sealing process.
(3) And heating the reaction vessel to 700 ℃, and keeping the temperature for 5-10 minutes until the pure metal sample is melted to obtain a molten sample.
(4) And (3) carrying out ultrasonic oscillation dispersion treatment on the liquid metal molten sample, controlling the temperature of the ultrasonic dispersion treatment at 80 ℃, controlling the ultrasonic frequency at 40KHz, controlling the ultrasonic power at 80W, and controlling the ultrasonic dispersion treatment time at 30 minutes to obtain uniform liquid metal.
(5) The melting point was determined to be 46.30 deg.C by TA-DSC250 test (see FIG. 1)
Example 2
In this example, the liquid metal is (Bi)43Sn15.4In21.6Pb20)90Cd10(the mass portion is 38.7 portions of bismuth, 19.4 portions of indium, 18 portions of lead, 13.9 portions of tin and 10 portions of cadmium), the preparation method comprises the following steps:
(1) weighing a pure metal sample with the total mass of about 5g, polishing a surface oxidation layer by using 800# abrasive paper, filling the sample into a sample bag filled with absolute ethyl alcohol, and putting the sample bag into an ultrasonic cleaning machine for cleaning. And drying the cleaned sample, and then putting the sample into a reaction vessel in the order of cadmium, zinc, bismuth, lead and indium.
(2) Inert gas is filled into a reaction vessel (a quartz test tube with the inner diameter of 9mm, the outer diameter of 12mm and the height of 29 cm), and a tube sealing machine is used for vacuumizing and tube sealing treatment, wherein the vacuum degree is 0.01 Pa. Repeatedly washing gas for at least 3 times, and filling high-purity nitrogen after the washing gas is finished to construct a protective atmosphere; and then sintering and sealing the test tube port by using a hydrogen flame gun to complete the tube sealing process.
(3) And heating the reaction vessel to 700 ℃, and keeping the temperature for 5-10 minutes until the pure metal sample is melted to obtain a molten sample.
(4) And (3) carrying out ultrasonic oscillation dispersion treatment on the liquid metal sample, controlling the temperature of the ultrasonic dispersion treatment at 80 ℃, controlling the ultrasonic frequency at 40KHz, controlling the ultrasonic power at 80W, and controlling the ultrasonic dispersion treatment time at 30 minutes to obtain completely uniform liquid metal.
(5) The melting point was determined to be 46.45 ℃ by TA-DSC250 test (see FIG. 2).
Comparative example 1
The liquid metal in this comparative example is Bi53.8Sn19.2In27The system comprises the following components in parts by weight: 53.8 parts of bismuth, 19.2 parts of tin and 27 parts of indium, and the preparation method is the same as that in example 1. The melting point temperature was 80.18 ℃ as measured by TA-DSC250 (see FIG. 3)
Comparative example 2
The liquid metal in this comparative example is Bi43Sn15.4In21.6Pb20The system comprises the following components in parts by weight: 43 parts of bismuth, 15.4 parts of tin, 21.6 parts of indium and 20 parts of lead, and the preparation method is the same as that in example 1. The melting point temperature, as measured by TA-DSC250 (see FIG. 4), was 57.60 ℃.
The liquid metal system and melting point in the above examples and comparative examples are shown in Table 1.
TABLE 1
| System of | TA-DSC melting Point (. degree. C.) | |
| Example 1 | (Bi43Sn15.4In21.6Pb20)93Cd7 | 46.30℃ |
| Example 2 | (Bi43Sn15.4In21.6Pb20)90Cd10 | 46.45℃ |
| Comparative example 1 | Bi53.8Sn19.2In27 | 80.18℃ |
| Comparative example 2 | Bi43Sn15.4In21.6Pb20 | 57.60℃ |
As can be seen from Table 1, the melting point temperature of the five-component system provided by the invention has a tendency of being obviously reduced compared with the melting point of the quaternary liquid metal; the tube sealing method can ensure that the loss of each component in the reaction process is reduced as much as possible and the consistency of each component before and after the reaction is kept.
The above description is only for the preferred embodiment of the present invention and is not intended to limit the scope of the present invention, and all equivalent modifications made by the contents of the present specification and the drawings, or applied directly or indirectly to other related technical fields, are included in the scope of the present invention.
Claims (8)
1. A bismuth-based liquid metal having a melting point of less than 50 ℃ is characterized by consisting of the following components in parts by mass:
35-40 parts of bismuth; 10-15 parts of tin; 15-21 parts of indium; 15-20 parts of lead; 5-10 parts of cadmium.
2. The bismuth-based liquid metal of claim 1, wherein the liquid metal consists of, in parts by mass:
38-40 parts of bismuth; 13-15 parts of tin; 19-21 parts of indium; 18-19% of lead; 7-10 parts of cadmium.
3. The bismuth-based liquid metal according to claim 2, wherein the bismuth-based liquid metal has a melting point of 46 to 47 ℃.
4. The method for producing a bismuth-based liquid metal according to any one of claims 1 to 3, characterized by comprising the steps of:
(1) weighing raw materials of each component of the bismuth-based liquid metal according to a proportion;
(2) placing the raw materials of each component in the step (1) in an inert gas atmosphere, and sealing;
(3) heating until the raw materials of each component are melted to obtain a molten sample;
(4) and (4) uniformly dispersing the molten sample obtained in the step (3) to obtain the bismuth-based liquid metal.
5. The production method according to claim 4, wherein in the step (2), the respective component materials are placed in a high-purity nitrogen atmosphere, and the cadmium raw material is placed at the lowermost part of the respective component materials.
6. The method according to claim 4, wherein the heating temperature in the step (3) is 600 to 700 ℃.
7. The method according to claim 4, wherein in the step (4), the uniform dispersion is ultrasonic oscillation dispersion.
8. The preparation method according to claim 7, wherein in the step (4), the temperature of the ultrasonic oscillation dispersion is controlled to be 60-80 ℃, the ultrasonic frequency is controlled to be 40-60 KHz, and the ultrasonic power is 60-80W.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114959357A (en) * | 2022-05-25 | 2022-08-30 | 长沙有色冶金设计研究院有限公司 | Bismuth-base alloy and energy-storage heat exchange method |
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|---|---|---|---|---|
| SU464643A1 (en) * | 1973-07-02 | 1975-03-25 | Предприятие П/Я Г-4149 | Fusible alloy |
| US4623514A (en) * | 1985-05-31 | 1986-11-18 | The United States Of America As Represented By The Secretary Of The Navy | Liquid metal brush material for electrical machinery systems |
| JP2001195963A (en) * | 2000-01-11 | 2001-07-19 | Uchihashi Estec Co Ltd | Alloy temperature fuse |
| US20170151598A1 (en) * | 2014-05-29 | 2017-06-01 | Agency For Science, Technology And Research | Imprinting Metallic Substrates at Hot Working Temperatures |
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2021
- 2021-10-26 CN CN202111248138.XA patent/CN113969370A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU464643A1 (en) * | 1973-07-02 | 1975-03-25 | Предприятие П/Я Г-4149 | Fusible alloy |
| US4623514A (en) * | 1985-05-31 | 1986-11-18 | The United States Of America As Represented By The Secretary Of The Navy | Liquid metal brush material for electrical machinery systems |
| JP2001195963A (en) * | 2000-01-11 | 2001-07-19 | Uchihashi Estec Co Ltd | Alloy temperature fuse |
| US20170151598A1 (en) * | 2014-05-29 | 2017-06-01 | Agency For Science, Technology And Research | Imprinting Metallic Substrates at Hot Working Temperatures |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114959357A (en) * | 2022-05-25 | 2022-08-30 | 长沙有色冶金设计研究院有限公司 | Bismuth-base alloy and energy-storage heat exchange method |
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