CN119566326B - Liquid metal foam composite ink for 3D structure printing and preparation method and application thereof - Google Patents
Liquid metal foam composite ink for 3D structure printing and preparation method and application thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/22—Direct deposition of molten metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/08—Alloys with open or closed pores
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0042—Matrix based on low melting metals, Pb, Sn, In, Zn, Cd or alloys thereof
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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Abstract
本发明涉及液态金属功能复合材料技术领域，具体涉及一种用于3D立体结构打印的液态金属泡沫复合油墨及其制备方法和应用，所述方法包括如下步骤：（1）取适量液态金属与无机填料通过机械力混合，得到液态金属复合材料；（2）将步骤（1）得到的液态金属复合材料进行真空处理，得到液态金属泡沫复合油墨，所述制备方法无需水、膨胀物、发泡剂、骨架材料等添加物的添加，无需冷冻辅助，光固化、烧结、浇注在内的额外辅助成型技术所需的复杂的反应过程和设备，能够简单快速大量地制备低填料含量、高可注射性和高强度的新型液态金属泡沫复合油墨，可打印高精度且均匀的3D立体结构，可在生物医药、航空航天、电子和热界面等领域中应用。
The present invention relates to the technical field of liquid metal functional composite materials, and in particular to a liquid metal foam composite ink for 3D structure printing and a preparation method and application thereof. The method comprises the following steps: (1) taking an appropriate amount of liquid metal and an inorganic filler and mixing them by mechanical force to obtain a liquid metal composite material; (2) subjecting the liquid metal composite material obtained in step (1) to vacuum treatment to obtain a liquid metal foam composite ink. The preparation method does not require the addition of additives such as water, expanders, foaming agents, skeleton materials, etc., and does not require the complex reaction process and equipment required for additional auxiliary molding technologies such as freezing assistance, photocuring, sintering, and casting. It can simply, quickly, and in large quantities prepare a new type of liquid metal foam composite ink with low filler content, high injectability, and high strength, and can print high-precision and uniform 3D structures. It can be used in the fields of biomedicine, aerospace, electronics, and thermal interfaces.
Description
Technical Field
The invention relates to the technical field of liquid metal functional composite materials, in particular to liquid metal foam composite ink for 3D three-dimensional structure printing, and a preparation method and application thereof.
Background
Liquid Metal (LM) exhibits 3D printing potential in a number of applications, with its high thermal, electrical and flexible properties. However, at present, liquid metal is mainly applied to printing with 2D plane patterns, and compared with plane patterns, 3D three-dimensional printing can create complex geometric shapes, meet customization requirements and optimize material use, and the importance of the liquid metal in the fields of medical treatment, aerospace, electronics, construction and the like is increasingly prominent. However, successful printing of 3D nanostructures requires that the inks used possess the proper rheological properties, and therefore, processing modifications and rheology regulation of the inks are required.
Currently, the viscosity and mechanical properties of inks can be increased by the addition of fillers. For example, patent document CN116555654a discloses a liquid metal composite material with high printing accuracy and smoothness, which can be used for a new generation of flexible electronic 3D printing materials. Among other things, continuously increasing filler content can further increase ink strength, but can lead to print clogging and interruption. Another way is to prepare liquid metal foam by adding water, foaming agent, expansion material and template method, and use the action of oxide layer on the surface of bubbles to reduce the density of the material and improve the mechanical strength of the material. For example, patent document CN115341117B discloses a liquid metal foam, a liquid metal foam composite material and a method for preparing the same, wherein hydrogen generated by the reaction of liquid metal oxide and water causes the inside of liquid metal to generate a porous structure.
However, these additional additives can cause problems such as structural instability, corrosion, and residue. If the water-assisted self-foaming is continuously carried out after printing is finished, the size change and the instability of the printing structure are caused, the hardening can be caused for a long time to limit the flexibility of the printing structure, and the foaming agent can be easily corroded by liquid metal to form intermetallic compounds, so that the performance of the liquid metal foam is affected. Therefore, there is an urgent need to develop a novel liquid metal ink having a low filler content, high injectability, and high strength to meet the printing requirements of 3D stereoscopic structures.
Disclosure of Invention
Aiming at the problems existing in the application of liquid metal, the invention provides a preparation method of liquid metal foam with a printable 3D three-dimensional structure, which can create a three-dimensional printing structure with programmable porosity and adjustable strength through ink formulation and vacuum adjustment.
In the invention, the liquid metal composite material is a liquid metal composite material obtained by adding inorganic filler into liquid metal.
In the invention, the liquid metal foam composite ink is obtained by vacuum processing of a liquid metal composite material.
The preparation process of the liquid metal composite material and the liquid metal foam composite ink does not need to use templates or other materials (such as water, expansion particles, foaming agents, templates, organic hollow framework materials and the like), and the preparation process, equipment and operation are simple. The invention discloses a liquid metal foam composite ink manufactured by vacuum processing, in particular to a porous structure with adjustable porosity, which is produced in a liquid metal composite material by taking micro bubbles generated in the preparation process of liquid metal and inorganic filler as a nucleating agent through an ink formula and a vacuum regulation mode.
The invention is realized by the following technical proposal
The preparation method of the liquid metal foam composite ink for 3D three-dimensional structure printing is characterized by comprising the following steps of:
(1) Mixing inorganic filler with volume fraction of 1.25-vol-15: 15 vol% with liquid metal by mechanical force to obtain a liquid metal composite material, wherein the liquid metal is one of gallium metal, gallium-indium alloy and gallium-indium-tin alloy or a mixture of the liquid metals, and the inorganic filler is at least one of zinc oxide, tungsten oxide and gallium oxide or a grading mixture of the zinc oxide, tungsten oxide and gallium oxide;
(2) And (3) carrying out vacuum treatment on the liquid metal composite material obtained in the step (1) to obtain the liquid metal foam composite ink, wherein the preparation process of the liquid metal foam composite ink does not comprise the use of water, expansion particles, foaming agent, template agent and organic hollow framework material.
Wherein the particle size of the inorganic filler in the step (1) is 10 nanometers-20 micrometers;
further, the mechanical force in step (1) is provided by ball milling, grinding or sanding.
Further, the grinding time in the step (1) is 10-60 min, the rotating speed is 10-130 rpm, and the purpose is to uniformly mix the liquid metal and the filler into paste.
Further, the vacuum treatment mode in the step (2) is at least one of a vacuum pump, a vacuum box, a vacuum mixer and a vacuum freeze dryer.
Further, in the step (2), the vacuum degree is 10-100 kPa, and the time is 10-300s.
In another aspect, the invention provides a liquid metal foam composite ink for 3D three-dimensional structure printing, which is prepared by the preparation method, wherein the liquid metal foam ink does not comprise water, expansion particles, a foaming agent, a template agent and an organic hollow framework material.
Further, when the liquid metal foam composite ink is used for 3D printing, no additional auxiliary forming technology is needed, and the additional auxiliary forming technology comprises freezing auxiliary, photo-curing, sintering and pouring.
Further, the porosity and strength of the liquid metal foam composite ink are controlled according to the ink formula and vacuum regulation, and the liquid metal foam composite ink presents a porous structure with multiple bubbles inside.
On the other hand, the invention provides application of the liquid metal foam composite ink in the fields of biomedicine, aerospace, electronic and thermal interfaces and the like.
The invention also provides application of the liquid metal foam composite ink in the fields of biomedicine, aerospace, electronic and thermal interfaces and the like.
The principle of the invention is that (1) in the step (1), mechanical force mixing can lead liquid metal and inorganic filler to form lattice permeation and coordination, so that the liquid metal is changed into a non-flowing fluid state of paste from Newtonian fluid, and finally the liquid metal composite material is obtained, and the porosity and strength of the liquid metal foam composite ink obtained in the step (2) can be controlled according to the ink formula and vacuum regulation and control, and the porous structure of internal multiple bubbles is presented. Compared with the method using additives such as water, expanded particles, foaming agent, template agent, organic hollow framework material additive and the like, the method can introduce air by utilizing the mechanochemical action in the preparation process of the liquid metal composite ink, so as to generate micro bubbles, and the micro bubbles are used as a vacuum foaming nucleating agent to prepare the liquid metal foam composite ink. In the structure of bubbles in the liquid metal foam composite ink, the surface gallium oxide provides additional strength and support for the whole ink, and lays a foundation for printing of a 3D three-dimensional structure, so that the liquid metal foam composite ink does not need to comprise additional auxiliary forming technologies of freezing auxiliary, photo-curing, sintering and pouring when being used for 3D printing.
The invention has the beneficial effects that the liquid metal foam composite ink and the preparation method thereof are provided, the preparation method does not need the addition of additives such as water, expansion matters, foaming agents, framework materials and the like, does not need the complicated reaction process and equipment required by additional auxiliary forming technologies such as freezing auxiliary, photo-curing, sintering and pouring, and can simply and rapidly prepare a large amount of liquid metal foam composite ink. The novel liquid metal ink with low filler content, high injectability and high strength is obtained, and the high-strength ink obtained by rheological control can print a high-precision and uniform 3D three-dimensional structure. Can be applied in the fields of biological medicine, aerospace, electronic and thermal interfaces and the like.
Drawings
The accompanying drawings, which are included to provide a further understanding of embodiments of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the principles of the application. In the drawings:
FIG. 1 is a flow chart of the preparation of a liquid metal foam composite ink. Adding inorganic filler into liquid metal to form a liquid metal composite material, and further carrying out vacuum processing to prepare liquid metal foam composite ink;
FIG. 2 is an image of the appearance and volume change of the liquid metal composite with vacuum processed liquid metal foam composite ink of different filler volume fractions shown in comparative example 1 and example 2;
FIG. 3 is an SEM image of a liquid metal foam composite ink of example 2 with different filler volume fractions;
FIG. 4 is SEM images of liquid metal foam composite ink obtained at various vacuum times in example 3;
FIG. 5 is a graph showing viscosity measurements for liquid metal foam composite inks of example 2 with different filler volume fractions;
FIG. 6 is a comparison of viscosity test of liquid metal composites with different filler volume fractions as shown in comparative example 1 and example 2 to liquid metal foam composite ink after vacuum processing;
FIG. 7 is a graph showing the storage modulus and loss modulus test values for liquid metal foam composite inks of example 2 with different filler volume fractions;
FIG. 8 is a comparison of viscosity test of liquid metal composites with different filler volume fractions as shown in comparative example 1 and example 2 to liquid metal foam composite ink after vacuum processing;
Fig. 9 is a printed single line structure of comparative example 2 and a change after one day of standing;
fig. 10 is a 3D stereoscopic image of a liquid metal foam print.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clear and clear, the details of the implementation of the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
It should be noted that, in embodiments of the present invention, all such expressions as "first" and "second" are used only to distinguish between two entities or parameters that are the same name but different. Thus, the use of "first" and "second" is merely descriptive convenience and should not be construed as limiting the embodiments of the invention, which will not be described in any way in the following embodiments.
It should be understood that the exemplary embodiments described herein are merely illustrative examples of the present invention. Although several embodiments are described in detail herein, various modifications and alterations are fully feasible to those skilled in the art without materially departing from the inventive subject matter. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Comparative example 1
1.818G of 20 nm tungsten oxide and 127.19 g gallium indium tin liquid metal were placed in an agate automated mortar and ground under air for 20: 20 min to give a paste-like LM-WO 3 (1.25 vol%) composite.
3.635G of 20 nm tungsten oxide and 125.38 g gallium indium tin liquid metal were placed in an agate automated mortar and ground under air for 20: 20 min to give a paste-like LM-WO 3 (2.5 vol%) composite.
7.27G of 20 nm tungsten oxide and 122.36 g gallium indium tin liquid metal were placed in an agate automated mortar and ground under air for 20: 20 min to give a paste-like LM-WO 3 (5 vol%) composite.
10.255 G of 20 nm tungsten oxide and 119.14 g gallium indium tin liquid metal were placed in an agate automated mortar and ground 20 min in an air environment to give a paste-like LM-WO 3 (7.5 vol%) composite.
14.54G of 20 nm tungsten oxide and 115.92 g gallium indium tin liquid metal were placed in an agate automated mortar and ground under air for 20: 20 min to give a paste-like LM-WO 3 (10 vol%) composite.
18.175G of 20 nm tungsten oxide and 112.7 g gallium indium tin liquid metal were placed in an agate automated mortar and ground 20 min in an air environment to give a paste-like LM-WO 3 (10 vol%) composite.
They were further subjected to rheological testing.
Comparative example 2
7.27G of 20 nm tungsten oxide and 122.36 g gallium indium tin liquid metal were placed in an agate automated mortar and ground under air for 20: 20min to give a paste-like LM-WO 3 (5 vol%) composite. Subsequently 6.48g of water was added and grinding was continued for 5min to give H 20-LM-WO3 (5 vol%) foam composite. This was loaded into a 10ml syringe, programmed with a direct write 3D printer and printed using a 0.7mm nozzle.
The precision of the printing ink is 0.7 mm, after one day of placement, the precision is reduced to 1 mm, and the uneven phenomenon appears on the surface of the printing ink.
Example 1
1.4 G zinc oxide and 127.19 g gallium indium tin liquid metal are placed in an agate automatic mortar, and ground 40 and min under an air environment to obtain a pasty liquid metal composite material. Then placing the mixture into a vacuum box, and vacuumizing for 300s at 10 kPa, so as to obtain the liquid metal-zinc oxide foam composite ink.
Example 2
The 6 liquid metal composite materials in the comparative example 1 are respectively placed into a vacuum box, and vacuumized for 60 seconds under the condition of 100kPa, so that the porous liquid metal-tungsten oxide foam composite ink can be prepared. This was loaded into a 10ml syringe, programmed with a direct write 3D printer and printed using a nozzle of 0.7 mm.
The precision of the printing ink is about 0.7 mm, the precision is kept unchanged after being placed for one day, the precision is 0.7 mm, and the surface of the printing ink is smooth.
They were further imaged and their viscosity and modulus values were measured with a rotarheometer. The tendency of the total bubble volume to increase and then decrease with increasing filler content was measured for the liquid metal-tungsten oxide foam composite ink. The viscosity and the modulus of the liquid metal foam composite ink are greatly improved compared with those of the liquid metal composite material.
Example 3
The LM-WO 3 (5 vol%) composite material obtained in example 2 was separated into five equal parts and placed in a vacuum box, and vacuum was applied to the parts under 100kPa for 0s, 10s, 60 s, 90 s and 120 s respectively to obtain liquid metal-tungsten oxide foam composite ink with different vacuum times.
Further taking scanning electron microscope images of them, it was observed that under a vacuum condition of 100kp, the cavitation volume increased first and then decreased as the vacuum time increased.
Fig. 1 shows a flow chart for the preparation of a liquid metal foam composite ink. The pure liquid metal presents a low-viscosity fluid shape, spontaneously contracts to form spherical liquid drops due to the action of high surface tension, forms a uniform pasty liquid metal composite material after adding inorganic filler, and further carries out vacuum processing to form the porous liquid metal foam composite ink with volume expansion.
Fig. 2 shows the appearance and volume change images of the liquid metal composite with the vacuum processed liquid metal foam composite ink of different filler volume fractions shown in comparative example 1 and example 2. From the figure it can be seen that the liquid metal composite has a significant increase in volume after undergoing vacuum processing and that as the filler volume fraction increases, the total bubble volume undergoes a tendency to increase and then decrease. Wherein the total volume of the liquid metal foam composite ink can be up to 2.5 times of the total volume of the liquid metal composite material.
Fig. 3 shows SEM images of liquid metal foam composite inks of different filler volume fractions in example 2. As can be seen from the figure, increasing the filler content results in an increase in the number of bubbles. The filler particles may act as nucleation sites to assist in the precipitation of gas from the liquid metal matrix to form bubbles. Higher filler content provides more nucleation sites, thereby increasing the total number of bubbles.
An increase in filler content also results in a decrease in bubble size. This is because more filler particles means that bubble nucleation sites are more dispersed, and the available volume near each nucleation site is smaller, thereby limiting the growth space of individual bubbles.
Fig. 4 shows SEM images of liquid metal foam composite ink obtained at different vacuum times in example 3. It can be seen from the figure that under a vacuum condition of 100kp, the cavitation volume increases and then decreases as the vacuum time increases. In a short time, the original micro-bubbles are gradually expanded at a nucleation point under a low pressure state, and the total volume of foam air holes is increased. However, when the vacuum time is too long to exceed 60 seconds, the continued low pressure causes the cells to coalesce and collapse into a layered structure after the vacuum is withdrawn, and the total volume of foam cells decreases.
Fig. 5 shows the viscosity test values for the liquid metal foam composite ink of example 2 for different filler volume fractions. As can be seen from the figure, the viscosity value of the liquid metal foam composite ink gradually increases as the volume fraction of the filler increases.
Fig. 6 shows the viscosity test comparison of the liquid metal composites of different filler volume fractions shown in comparative example 1 and example 2 with the liquid metal foam composite ink after vacuum processing. From the comparison value, the viscosity of the liquid metal foam is obviously improved compared with that of the liquid metal ink before vacuum, the micro-pores play a key role in the liquid metal foam, and the larger the total volume of the bubbles is, the more obvious the rheological behavior of the liquid metal is influenced. The rheological behavior at 5% liquid metal filler volume fraction is close to the viscosity value of 10% liquid metal ink filler volume fraction prior to vacuum. The volume fraction of filler required to reach high viscosity is significantly reduced.
Fig. 7 shows the storage modulus and loss modulus test values for the liquid metal foam composite ink of example 2 for different filler volume fractions. As can be seen from the figure, the storage modulus and loss modulus values of the liquid metal foam composite ink gradually increase as the volume fraction of filler increases.
Fig. 8 shows the storage modulus and loss modulus value test versus values for the liquid metal composites of different filler volume fractions shown in comparative example 1 and example 2 versus the liquid metal foam composite ink after vacuum processing. From the comparison it can be seen that the modulus of the liquid metal foam is significantly improved compared to the liquid metal ink before vacuum.
Fig. 9 shows the printed single line structure of comparative example 2 and the variation after one day of placement. The upper graph shows images before and after the foam composite material of H 20-LM-WO3 (5 vol%) with water as an additive is placed, the precision of printing ink is 0.7 and mm, after the printing ink is placed for one day, the precision is reduced to 1 mm, and the uneven phenomenon occurs on the surface of the printing ink. The lower graph shows images before and after the vacuum foaming LM-WO 3 (5 vol%) foam composite material is placed, the precision of printing ink is about 0.7 mm, the precision is kept unchanged after being placed for one day, the precision is 0.7 mm, and the surface of the printing ink is smooth.
Fig. 10 shows a liquid metal foam printing 3D stereoscopic image with a printing accuracy of 180 μm. The high strength, high viscosity and high modulus of the liquid metal foam are exhibited, and the purpose of self-supporting three-dimensional molding can be achieved without any auxiliary molding means (such as refrigeration assistance, photo-curing, sintering, casting and the like) in the printing process, so that a printing finished product with a 3D three-dimensional structure is constructed. The printing path is further designed, so that the method can be applied to manufacturing complex structures in the fields of biological medicine, aerospace, electronic and thermal interfaces and the like.
The physical and chemical property detection of the liquid metal foam composite ink comprises the following steps:
rheology of the ink the rheological properties of the ink were evaluated using an MCR302 rheometer (Anton Paar, austria).
The measurement uses a plate-to-plate geometry with a diameter of 8mm and a gap of 1 mm, maintaining a constant temperature of 25 ℃.
Microstructure characterization liquid metal foam composite ink was frozen and truncated with liquid nitrogen, and then scanned with a scanning electron microscope (SEM,
Hitachi S-4800) characterizes the cross-sectional morphology of the ink.
In summary, if the highest porosity liquid metal foam composite is desired, a moderate filler volume fraction (about 5%) can be selected, a small particle size (20 nm), and a moderate vacuum time (60 s). The higher porosity can increase the content of the gallium oxide layer spontaneously produced on the surface of the air bubble, and the effect of the oxide layer on the surface of the air bubble is utilized to reduce the density of the material and improve the mechanical strength of the material. The preparation process of the invention does not need to use templates or other materials (such as water, expanded particles, foaming agents, templates, organic hollow framework materials and the like), and has simple preparation process, equipment and operation. Adverse effects of additives on ink printing, such as continuous water-assisted self-foaming after printing, resulting in dimensional changes and instabilities of the printed structure and hardening over time, are avoided, limiting the flexibility.
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the invention, and is not meant to limit the scope of the invention, but to limit the invention to the particular embodiments, and any modifications, equivalents, improvements, etc. that fall within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (8)
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| CN119189294B (en) * | 2024-11-22 | 2025-03-21 | 西安交通大学 | Method and device for forming multi-bubble fusion foaming structure based on direct bubble writing |
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