Preparation method of Bi-In-Sn liquid metal dispersed particles
Bi-In-Sn liquid metal dispersion particles were prepared by heating and melting and high-speed stirring, which solved the problems of low preparation efficiency, high cost and difficulty in large-scale production in the existing technology. It achieved low-cost, high-efficiency preparation and particle size control, and is suitable for the field of orthopedic medicine.
Patent Information
- Application Number
- CN202511701410.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-19
- Publication Date
- 2026-02-24
AI Technical Summary
Existing Bi-In-Sn alloy particle preparation technologies are inefficient, costly, and difficult to scale up, failing to meet the actual needs of fields such as orthopedics.
Bi-In-Sn liquid metal dispersion particles were prepared using heating equipment and a high-speed stirrer. The particle size was formed and controlled by heating and melting, adding PVA solution, high-speed stirring, rinsing and drying.
This technology enables low-cost, high-efficiency, and large-scale preparation of Bi-In-Sn particles, adapting to different remediation needs, reducing equipment and raw material costs, and ensuring particle quality and biocompatibility.
Smart Images
Figure CN121551610A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of liquid metal technology, and in particular to a method for preparing Bi-In-Sn liquid metal dispersion particles. Background Technology
[0002] Bi-In-Sn alloys have shown significant application potential in the field of orthopedic medicine due to their unique low-temperature solid-liquid phase transformation characteristics. Their low-temperature melting and room-temperature solidification characteristics can meet the needs of minimally invasive operations in bone repair surgery areas. Therefore, compared with bulk Bi-In-Sn alloys, micron-sized Bi-In-Sn particles that meet the area limitations of the surgical area are better able to meet the practical application needs in clinical and experimental settings, and have become one of the key material forms of interest in this field.
[0003] However, current technical solutions for preparing Bi-In-Sn alloy particles have significant limitations: existing methods generally rely on ultrasonic crushers equipped with a constant-temperature module as the core equipment. This technical approach has three major problems: first, the preparation efficiency is low, the single preparation cycle is long, and it is difficult to quickly respond to the immediate demand for particles in experiments or production; second, the actual output is limited, the processing capacity of ultrasonic crushers is small, and it is impossible to achieve large-scale batch preparation; third, the initial investment cost is high, the equipment purchase and maintenance costs of dedicated constant-temperature ultrasonic crushers are high, which increases the economic threshold for the implementation of the technology.
[0004] The shortcomings of the existing technologies mentioned above make it difficult to simultaneously achieve low cost, high efficiency, and large-scale production of Bi-In-Sn particles, thus hindering their further application in fields such as orthopedics. Therefore, there is an urgent need for a method for preparing Bi-In-Sn particles that requires low equipment, is easy to operate, has controllable costs, and can achieve batch production, in order to address the pain points of the existing technologies. Summary of the Invention
[0005] The purpose of this invention is to provide a method for preparing Bi-In-Sn liquid metal dispersion particles to solve the above-mentioned problems.
[0006] This invention provides a method for preparing Bi-In-Sn liquid metal dispersion particles, comprising the following steps: S1: Place a large piece of Bi-In-Sn alloy in a heating device and heat it until the Bi-In-Sn alloy is completely melted; S2: Add PVA solution to the molten Bi-In-Sn alloy obtained in step S1. The amount of PVA solution added is sufficient to cover the liquid Bi-In-Sn alloy. Then continue heating until the Bi-In-Sn alloy is completely melted again. S3: Stir the mixture of the completely melted liquid Bi-In-Sn alloy and PVA solution from step S2 at high speed until obvious liquid Bi-In-Sn alloy particles are formed. S4: After the liquid Bi-In-Sn alloy particles obtained in step S3 have solidified naturally, the particles are rinsed multiple times with deionized water to remove residual PVA from the particle surface. S5: Dry the particles after rinsing in step S4 to obtain Bi-In-Sn particles.
[0007] Preferably, in the above-mentioned method for preparing Bi-In-Sn liquid metal dispersed particles, the heating equipment in steps S1 and S2 is a water bath, an oil bath, or an electric heating mantle, and the heating temperature of the heating equipment is based on the ability to make the Bi-In-Sn alloy reach a completely melted state.
[0008] Preferably, in the above-mentioned method for preparing Bi-In-Sn liquid metal dispersion particles, the high-speed stirring time in step S3 is ≤10 minutes to avoid PVA molecules in the mixed system from bonding and solidifying with each other.
[0009] Preferably, in the above-mentioned method for preparing Bi-In-Sn liquid metal dispersed particles, the stirring speed in step S3 is negatively correlated with the particle size of the low-temperature Bi-In-Sn particles obtained in step S5: when the stirring speed is 1000 rpm, the particle size of the low-temperature Bi-In-Sn particles is 400-500 μm; when the stirring speed is 1500 rpm, the particle size of the low-temperature Bi-In-Sn particles is 200-300 μm; and when the stirring speed is 2000 rpm, the particle size of the low-temperature Bi-In-Sn particles is 40-100 μm.
[0010] Preferably, in the above-mentioned method for preparing Bi-In-Sn liquid metal dispersion particles, the drying process in step S5 is freeze-drying or natural drying.
[0011] Preferably, in the above-mentioned method for preparing Bi-In-Sn liquid metal dispersed particles, the polar hydroxyl groups in the PVA solution in step S2 form hydrogen bonds with the oxide layer on the surface of the liquid Bi-In-Sn alloy particles formed in step S3. The hydrogen bonds and van der Waals forces work together to assist in the dispersion of the liquid Bi-In-Sn alloy particles.
[0012] Therefore, the present invention employs the above-described method for preparing Bi-In-Sn liquid metal dispersion particles, which has the following beneficial effects: (1) It does not rely on a dedicated constant-temperature ultrasonic breaker. The core equipment consists only of a conventional heating device and a high-speed stirrer. The heating device has wide adaptability and can be selected from common laboratory / industrial settings such as water bath, oil bath, or electric heating mantle, as long as it can meet the melting temperature of Bi-In-Sn alloy. This design completely avoids the dependence of existing technologies on expensive dedicated equipment, significantly reduces equipment procurement and maintenance costs, and simplifies equipment operation procedures.
[0013] (2) By optimizing the process sequence and parameters, the preparation cycle is greatly shortened and the preparation efficiency is high. The high-speed stirring time is less than 10 minutes to prepare particles of 40-500μm, which can effectively avoid the mutual bonding and solidification of PVA molecules, while ensuring that the liquid Bi-In-Sn alloy is fully dispersed into particles. Combined with the process design of one-time heating and melting and batch dispersion, compared with the small-capacity batch processing mode of the existing ultrasonic crusher, it can achieve large-scale preparation in a short time, significantly improve the output per unit time, and meet the large-scale demand of Bi-In-Sn particles for experiments or production.
[0014] (3) The raw material cost is low. The PVA solution used in the process is inexpensive and used in small quantities, so there is no need for expensive consumables. The equipment cost is low. The purchase cost of conventional heating and stirring equipment is much lower than that of a dedicated constant temperature ultrasonic crusher, and the energy consumption is also lower. The overall process has no high-cost links, and the preparation cost can be controlled at a low level while ensuring the quality of the particles.
[0015] (4) The particle size can be directionally controlled by adjusting the high-speed stirring speed, such as 1000rpm corresponding to 400-500μm, 1500rpm corresponding to 200-300μm, and 2000rpm corresponding to 40-100μm, which can adapt to the particle size requirements of different surgical areas and different repair needs in fields such as bone medicine; the residual PVA on the particle surface can be completely removed by rinsing with deionized water multiple times, so as to avoid impurities affecting the biocompatibility or physical properties of the particles.
[0016] The technical solution of the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. Attached Figure Description
[0017] Figure 1 This is a process flow diagram for preparing Bi-In-Sn particles according to the present invention; Figure 2 Optical images of the Bi-In-Sn particles of the present invention, wherein: a) shows Bi-In-Sn particles dispersed in a PVA solution; b) shows Bi-In-Sn particles of different sizes obtained at different stirring speeds; Figure 3Optical images of Bi-In-Sn particles of different sizes according to the present invention, wherein a) is an optical image of 400-500μm particles with a stirring speed of 1000rpm; b) is an optical image of 200-300μm particles with a stirring speed of 1500rpm; and c) is an optical image of 40-100μm particles with a stirring speed of 2000rpm. Detailed Implementation
[0018] To better understand the above technical solutions, a detailed description of the solutions will be provided below in conjunction with the accompanying drawings and specific embodiments. Obviously, the described embodiments are merely some, not all, of the embodiments of the present invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.
[0019] The terminology used in the embodiments of this invention is for the purpose of describing particular embodiments only and is not intended to limit the invention. The singular forms “a,” “the,” and “the” as used in the embodiments of this invention and the appended claims are also intended to include the plural forms, and “multiple” generally includes at least two unless the context clearly indicates otherwise.
[0020] It should also be noted that the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that an article or device that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such an article or device. Without further limitation, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the article or device that includes said element.
[0021] This invention provides a method for preparing Bi-In-Sn liquid metal dispersion particles, comprising the following steps: S1: Place a large piece of Bi-In-Sn alloy in a heating device and heat it until the Bi-In-Sn alloy is completely melted; S2: Add PVA solution to the molten Bi-In-Sn alloy obtained in step S1. The amount of PVA solution added is sufficient to cover the liquid Bi-In-Sn alloy. Then continue heating until the Bi-In-Sn alloy is completely melted again. S3: Stir the mixture of the completely melted liquid Bi-In-Sn alloy and PVA solution from step S2 at high speed until obvious liquid Bi-In-Sn alloy particles are formed. S4: After the liquid Bi-In-Sn alloy particles obtained in step S3 have solidified naturally, the particles are rinsed multiple times with deionized water to remove residual PVA from the particle surface. S5: Dry the particles after rinsing in step S4 to obtain Bi-In-Sn particles.
[0022] To further optimize the above technical solution, the heating equipment in steps S1 and S2 is a water bath, an oil bath, or an electric heating mantle, and the heating temperature of the heating equipment is based on the ability to make the Bi-In-Sn alloy reach a completely molten state.
[0023] To further optimize the above technical solution, the high-speed stirring time in step S3 is ≤10 minutes to avoid PVA molecules in the mixed system from bonding and solidifying.
[0024] To further optimize the above technical solution, the stirring speed in step S3 is negatively correlated with the particle size of the low-temperature Bi-In-Sn particles obtained in step S5: when the stirring speed is 1000 rpm, the particle size of the low-temperature Bi-In-Sn particles is 400-500 μm; when the stirring speed is 1500 rpm, the particle size of the low-temperature Bi-In-Sn particles is 200-300 μm; and when the stirring speed is 2000 rpm, the particle size of the low-temperature Bi-In-Sn particles is 40-100 μm.
[0025] To further optimize the above technical solution, the drying process in step S5 is freeze drying or natural drying.
[0026] To further optimize the above technical solution, the polar hydroxyl groups in the PVA solution in step S2 form hydrogen bonds with the oxide layer on the surface of the liquid Bi-In-Sn alloy particles formed in step S3. The hydrogen bonds and van der Waals forces work together to assist in the dispersion of the liquid Bi-In-Sn alloy particles.
[0027] To provide a clearer and more detailed description of the preparation method of Bi-In-Sn liquid metal dispersion particles provided by the embodiments of the present invention, the following description will be based on specific embodiments.
[0028] Example 1 like Figure 1-2 As shown, step 1: melting of Bi-In-Sn alloy. Take one piece of Bi-In-Sn alloy and place it in a 250mL beaker. Put the beaker into a constant temperature water bath and set the water bath temperature to 80℃. After heating for 3 minutes, the alloy is observed to melt.
[0029] Step 2: Add PVA solution and remelt. Slowly pour 150 mL of 2 wt% PVA solution into the beaker containing the liquid Bi-In-Sn alloy. The solution volume should be enough to completely cover the surface of the liquid metal by 2 cm to avoid metal exposure and oxidation. Maintain the water bath temperature at 80℃ and continue heating for 2 minutes to remelt the Bi-In-Sn alloy.
[0030] Step 3: High-speed stirring and dispersion. Insert the stirring paddle of the stirrer into the mixing system, set the stirring speed to 1000 rpm, and start stirring. During the stirring process, it is observed that the liquid Bi-In-Sn alloy gradually disperses into spherical particles in the PVA solution. Because the polar hydroxyl groups of PVA molecules form hydrogen bonds with the oxide layer on the surface of the metal particles, the van der Waals forces work together to inhibit particle agglomeration. At this time, a large number of uniform liquid metal particles are suspended in the mixing system.
[0031] Step 4: Solidification and rinsing. Remove the beaker from the water bath and slowly rinse the particles with deionized water until the pH of the rinse solution is consistent with that of the deionized water, confirming that there is no PVA residue on the particle surface.
[0032] Step 5: Freeze-drying. Transfer the rinsed Bi-In-Sn particles to the sample tray of the freeze dryer, spread them out, set the cold trap temperature to -50℃, and dry for 4 hours to obtain loose Bi-In-Sn particles without clumping.
[0033] The obtained Bi-In-Sn particles are as follows Figure 3 As shown in (a), the Bi-In-Sn particles are regular spherical with uniform particle size distribution, ranging from 400 to 500 μm, as observed by an optical microscope.
[0034] Example 2 Except for step 3, where the high-speed stirring speed is set to 1500 rpm, the other steps are exactly the same as in Example 1.
[0035] The obtained Bi-In-Sn particles are as follows Figure 3 As shown in (b), the particles remain spherical under an optical microscope, exhibiting good dispersibility and no obvious agglomeration; the particle size range is 200-300 μm.
[0036] Example 3 Except for step 3, where the high-speed stirring speed is set to 2000 rpm, the other steps are exactly the same as in Example 1.
[0037] The obtained Bi-In-Sn particles are as follows Figure 3 As shown in (c), under an optical microscope, the particles are small spherical and show no signs of breakage; the particle size ranges from 40 to 100 μm.
[0038] Examples 1-3 successfully prepared Bi-In-Sn particles with the target particle size, ranging from 40 to 500 μm, with high particle purity and good dispersibility. The preparation process showed significant advantages in terms of equipment cost, preparation efficiency, yield, and particle uniformity, fully achieving the goals of low cost, high efficiency, large scale, and controllability. The heating equipment and drying method had no special dependence on the equipment.
[0039] Therefore, this invention employs the aforementioned method for preparing Bi-In-Sn liquid metal dispersed particles, eliminating the need for a dedicated isothermal ultrasonic disruptor. The core equipment consists only of a conventional heating device and a high-speed stirrer. Furthermore, the heating equipment is highly adaptable, utilizing common laboratory / industrial equipment such as water baths, oil baths, or electric heating mantles, as long as they meet the melting temperature requirements of the Bi-In-Sn alloy. This design completely avoids the reliance on expensive specialized equipment found in existing technologies, significantly reducing equipment procurement and maintenance costs while simplifying operation. By optimizing the process sequence and parameters, the preparation cycle is greatly shortened, resulting in high efficiency. High-speed stirring within 10 minutes can prepare particles of 40-500 μm, effectively preventing PVA molecules from bonding and solidifying, while ensuring the liquid Bi-In-Sn alloy is fully dispersed into particles. Combined with a single-stage heating and melting process and batch dispersion design, compared to the small-capacity, multi-stage processing mode of existing ultrasonic disruptors, this method enables large-scale preparation in a short time, significantly increasing yield per unit time and meeting the large-scale requirements of experimental or production applications for Bi-In-Sn particles.
[0040] The raw material cost is low, as the PVA solution used in the process is inexpensive and used in small quantities, eliminating the need for expensive consumables. Equipment costs are also low, with the purchase cost of conventional heating and stirring equipment being far lower than that of a dedicated constant-temperature ultrasonic disruptor, and energy consumption is also lower. The overall process has no high-cost components, allowing for low-cost preparation while ensuring particle quality. Particle size can be directionally controlled by adjusting the high-speed stirring speed; for example, 1000 rpm corresponds to 400-500 μm, 1500 rpm to 200-300 μm, and 2000 rpm to 40-100 μm, adapting to the particle size requirements of different surgical areas and repair needs in fields such as orthopedics. Multiple rinses with deionized water thoroughly remove residual PVA from the particle surface, preventing impurities from affecting the particle's biocompatibility or physical properties.
[0041] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit them. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can still be made to the technical solutions of the present invention, and these modifications or equivalent substitutions cannot cause the modified technical solutions to deviate from the spirit and scope of the technical solutions of the present invention.
Claims
1. A method for preparing Bi-In-Sn liquid metal dispersion particles, characterized in that, Includes the following steps: S1: Place a large piece of Bi-In-Sn alloy in a heating device and heat it until the Bi-In-Sn alloy is completely melted; S2: Add PVA solution to the molten Bi-In-Sn alloy obtained in step S1. The amount of PVA solution added is sufficient to cover the liquid Bi-In-Sn alloy. Then continue heating until the Bi-In-Sn alloy is completely melted again. S3: Stir the mixture of the completely melted liquid Bi-In-Sn alloy and PVA solution from step S2 at high speed until obvious liquid Bi-In-Sn alloy particles are formed. S4: After the liquid Bi-In-Sn alloy particles obtained in step S3 have solidified naturally, the particles are rinsed multiple times with deionized water to remove residual PVA from the particle surface. S5: Dry the particles after rinsing in step S4 to obtain Bi-In-Sn particles.
2. The method for preparing Bi-In-Sn liquid metal dispersion particles according to claim 1, characterized in that, The heating equipment mentioned in steps S1 and S2 is a water bath, an oil bath, or an electric heating mantle. The heating temperature of the heating equipment is based on the requirement that the Bi-In-Sn alloy can reach a completely melted state.
3. The method for preparing Bi-In-Sn liquid metal dispersion particles according to claim 1, characterized in that, The high-speed stirring time in step S3 shall be ≤10 minutes to avoid PVA molecules in the mixed system from bonding and solidifying together.
4. The method for preparing Bi-In-Sn liquid metal dispersion particles according to claim 1, characterized in that, The stirring speed in step S3 is negatively correlated with the particle size of the low-temperature Bi-In-Sn particles obtained in step S5: when the stirring speed is 1000 rpm, the particle size of the low-temperature Bi-In-Sn particles is 400-500 μm; when the stirring speed is 1500 rpm, the particle size of the low-temperature Bi-In-Sn particles is 200-300 μm; and when the stirring speed is 2000 rpm, the particle size of the low-temperature Bi-In-Sn particles is 40-100 μm.
5. The method for preparing Bi-In-Sn liquid metal dispersion particles according to claim 1, characterized in that, The drying process described in step S5 is freeze drying or natural drying.
6. The method for preparing Bi-In-Sn liquid metal dispersion particles according to claim 1, characterized in that, In step S2, the polar hydroxyl groups in the PVA solution form hydrogen bonds with the oxide layer on the surface of the liquid Bi-In-Sn alloy particles formed in step S3. The hydrogen bonds and van der Waals forces work together to assist in the dispersion of the liquid Bi-In-Sn alloy particles.