CN111346572B - Method for controlling shape of solidified liquid drop and application - Google Patents
Method for controlling shape of solidified liquid drop and application Download PDFInfo
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- CN111346572B CN111346572B CN202010193017.9A CN202010193017A CN111346572B CN 111346572 B CN111346572 B CN 111346572B CN 202010193017 A CN202010193017 A CN 202010193017A CN 111346572 B CN111346572 B CN 111346572B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/30—Auxiliary operations or equipment
- B29C64/307—Handling of material to be used in additive manufacturing
- B29C64/314—Preparation
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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
- B33Y10/00—Processes of additive manufacturing
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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
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K2101/00—Articles made by soldering, welding or cutting
- B23K2101/36—Electric or electronic devices
- B23K2101/42—Printed circuits
Abstract
According to the method for controlling the shape of the solidified liquid drop and the application thereof, the method for controlling the shape of the solidified liquid drop comprises the steps of preparing a suspension containing nano-particles; dripping the suspension on the surface of the supercooling bottom plate to obtain liquid drops on the surface of the bottom plate; the liquid drops are subjected to solidification nucleation on the supercooling bottom plate, the solidification nucleation occurs on a solid-liquid contact surface, and then a solidification interface is gradually pushed upwards; the nano particles are gathered at the front of a solidification interface to form a dense particle accumulation layer; and (3) propelling a particle accumulation layer at the three-phase boundary position, so that the free energy gradient initiates a compensation flow which flows from the center to the periphery in parallel to the solidification interface, the liquid is continuously transported to the surface of the liquid drop from the inside of the liquid drop, and the shape of the solidified liquid drop is finally obtained. The method has simple process, and the shape of the liquid drop can be controlled only by adding corresponding micro-nano particles; the performance of the device is not influenced, the application range is wide, and the larger the scale span is.
Description
Technical Field
The invention belongs to the technical field of liquid drop solidification, and particularly relates to a method for controlling the shape of a solidified liquid drop and application thereof.
Background
Neglecting the influence of gravity, the shape of the liquid drop under the action of surface tension is a ball or a spherical cut, and the shape of the liquid drop after solidification can not be obviously changed. Some reported special cases, such as density change before and after solidification (water freezing), and further such as droplet solidification in shear flow, have slight changes in droplet shape, but still do not change the basic fact that the droplet solidified in the shape of a sphere or spherical cut.
In some industrial applications, the nearly spherical liquid drops can reduce the space matching degree of devices, for example, the spherical cutting soldering tin in a micro circuit board increases the height of a welding point position, and the integral further miniaturization of a microelectronic system is limited; for example, in three-dimensional printing, the porosity of a device is high due to accumulation of spherical liquid drops, the mechanical strength and the air tightness of a material are seriously influenced, and an effective technology for solving the problem is not provided at present.
Disclosure of Invention
In order to solve the above problems, an object of the present invention is to provide a method for controlling the shape of solidified droplets and an application thereof.
The present invention provides a method for controlling the shape of coagulated droplets, characterized by comprising preparing a suspension containing nanoparticles; dripping the suspension on the surface of the supercooling bottom plate to obtain liquid drops on the surface of the bottom plate; the liquid drops are subjected to solidification nucleation on the supercooling bottom plate, the solidification nucleation occurs on a solid-liquid contact surface, and then a solidification interface is gradually pushed upwards; the nano particles are gathered at the front of a solidification interface to form a dense particle accumulation layer; and (3) propelling a particle accumulation layer at the three-phase boundary position, so that the free energy gradient initiates a compensation flow which flows from the center to the periphery in parallel to the solidification interface, the liquid is continuously transported to the surface of the liquid drop from the inside of the liquid drop, and the shape of the solidified liquid drop is finally obtained.
The method for controlling the shape of the solidified liquid drop provided by the invention can also have the following characteristics: wherein, the matrix medium is degassed, added with a surfactant, mixed with the nano-particles, and subjected to electromagnetic stirring and ultrasonic oscillation to obtain a stable dispersion system.
In addition, the method for controlling the shape of the coagulated droplet provided by the present invention may further include: wherein the particle size of the nanoparticles is less than three orders of magnitude the droplet size.
In addition, the method for controlling the shape of the solidified droplet provided by the present invention may further have the following features: wherein, the method for preparing the suspension comprises the following steps: putting 100ml of deionized water into a beaker, heating the deionized water to 90 ℃, and then putting the heated deionized water into a vacuum vessel for natural cooling and degassing; adding 0.1g of sodium dodecyl sulfate into the cooled deionized water, and electromagnetically stirring until the sodium dodecyl sulfate is completely dissolved to obtain a sodium dodecyl sulfate solution; adding 3.6g of titanium dioxide nano particles into a sodium dodecyl sulfate solution, and stirring for more than 2 hours through electromagnetism to obtain the stable water-based titanium dioxide nano fluid.
In addition, the method for controlling the shape of the solidified droplet provided by the present invention may further have the following features: and dripping the suspension liquid onto the surface of the supercooling bottom plate by using an injector, wherein the distance between the lower end of the injector and the surface of the supercooling bottom plate is 5-20 mm.
In addition, the method for controlling the shape of the solidified droplet provided by the present invention may further have the following features: wherein the volume of the liquid drop is 5-10 mul.
In addition, the method for controlling the shape of the coagulated droplet provided by the present invention may further include: wherein, the bottom plate adopts heat conduction material, and its initial temperature sets up 8-12 ℃ below the freezing point of matrix medium equilibrium state.
In addition, the method for controlling the shape of the coagulated droplet provided by the present invention may further include: the liquid drops are solidified in a closed bin, protective gas, polymer or liquid metal matrix are arranged in the closed bin, and the protective gas adopts inert gas.
Use of any of the above methods of controlling the shape of a solidified droplet in a soldering process.
Use of a method of controlling the shape of a solidified droplet as described in any one of the above in three-dimensional printing.
Action and effects of the invention
According to the method for controlling the shape of the solidified liquid drop and the application thereof, the scheme provided by the invention has the following advantages:
(1) the process is simple, and the shape of the liquid drop can be controlled only by adding corresponding micro-nano particles;
(2) the performance of the device is not influenced, the micro-nano particles are transferred to the top end of the liquid drop after the liquid drop is solidified, and the whole liquid drop is still a pure matrix medium;
(3) the method is suitable for a wide range of matrix media, water, organic solvents, polymers, liquid metal and the like;
(4) the larger the scale span, the droplet radius can be from centimeter to submicron.
Drawings
FIG. 1 is a schematic side view of a droplet containing micro-nano particles in an embodiment before solidification nucleation;
FIG. 2 is a schematic diagram of solidification nucleation of a droplet containing micro-nano particles in an embodiment;
FIG. 3 is a schematic top view of a droplet marked with a compensating stream in an embodiment;
FIG. 4 is a schematic view showing a solidification shape of a droplet in the example;
FIG. 5 is a photo of the liquid drop with the micro-nano particles added in the embodiment before solidification; and
fig. 6 is a photo of the solidified liquid drop added with micro-nano particles in the embodiment.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the following embodiments are combined with the accompanying drawings to specifically describe the method for controlling the shape of the solidified liquid drop and the application thereof.
Examples
During the solidification of the continuous medium, the micro-or nano-particles suspended inside can be removed from the solidified phase (ice) by hindering the molecular lattice matching of the continuous medium (water), i.e. the solidification segregation behavior of the particles. At higher particle concentrations, the removed particles may accumulate at the solidification interface front, forming a dense layer of particle packing. Near the three-phase boundary (water/ice/air), the particle packing layer is pushed forward to generate a large amount of free interfaces (particles/air), and the total free energy of the system is increased. The continuous medium is replenished from the interior of the drop to the triple junction driven by the free energy gradient, and this compensating flow parallel to the solidification interface causes the solidified shape of the drop to change. The invention utilizes the principle of liquid drop shape change, and controls the shape of the solidified liquid drop by adding micro-nano particles into a continuous medium.
A method of controlling a shape of a coagulated droplet of the present embodiment includes:
and preparing a stable suspension of the micro-nano particles.
And (3) degassing the matrix medium by using ultrasound/heating/vacuum, adding a surfactant, mixing with the weighed micro-nano particles, and obtaining a stable dispersion system by electromagnetic stirring and ultrasonic oscillation.
The particle size of the micro-nano particles is selected according to a standard, the smaller the particle size is, the better the particle size is, and the particle size in practical application needs to be at least three orders of magnitude smaller than the size of the liquid drops so as to ensure the uniformity of a mixed system. If the diameter of the liquid drop is 2mm, the diameter of the corresponding particle is below 2 μm.
The type and concentration criteria of the surfactant will depend on the material of the matrix medium and the particles. For example, in the case of the combination of water-based metal particles, the surfactant is cetyl trimethylammonium bromide or sodium lauryl sulfate, and the concentration of the surfactant is below the critical micelle concentration (critical micelle concentration).
Preparing the water-based titanium dioxide nanofluid. 100ml of deionized water is put into a beaker, heated to 90 ℃ and then put into a vacuum dish for natural cooling and degassing. 0.1g of sodium lauryl sulfate was added to the cooled deionized water and stirred magnetically until completely dissolved. 3.6g of titanium dioxide nanoparticles (5nm, anatase) were added to the sodium dodecyl sulfate solution and stirred electromagnetically for more than 2 hours to give a stable water-based titanium dioxide nanofluid with a volume concentration of about 1%.
For some combinations of matrix media and particulate materials, the mixing fluid is stable and no surfactant needs to be added. The method is suitable for various matrix media, including water, organic solvents, polymers, liquid metal and the like.
The bottom plate is a smooth heat conducting material, and the initial temperature reference value is 8-12 ℃ lower than the equilibrium freezing point of the matrix medium, in the embodiment, 10 ℃ lower than the equilibrium freezing point of the matrix medium. The initial temperature of the soleplate 30 is set to-10 ℃ for the water-based medium, and heterogeneous nucleation is ensured to occur at a solid-liquid contact point.
Setting environmental factors: the liquid drops are solidified on a supercooling bottom plate in the closed bin.
The protective gas in the closed bin is selected according to the base medium material. Such as water-based media, can be filled with dry air, nitrogen, and the like. For polymer and liquid metal substrates, inert gas is selected to prevent chemical reaction between the substrate medium and ambient gas during solidification.
The bottom plate 30 is a heat conductive material, and the initial contact angle of the liquid drop can be adjusted by adjusting the wettability of the surface of the bottom plate, wherein the initial temperature reference value is 8-12 ℃ lower than the equilibrium freezing point of the matrix medium, and in the embodiment, the initial temperature reference value is 10 ℃ lower than the equilibrium freezing point of the matrix medium. If the initial temperature of the bottom plate is set to be-10 ℃ for the water-based medium, heterogeneous nucleation is guaranteed to occur at a solid-liquid contact point.
In the examples, the sealed chamber was filled with nitrogen gas, and the chamber was at room temperature and one standard atmosphere. The bottom plate was a clean, smooth silicon wafer with a temperature of about-10 c.
Because the pressure in the bin has slight influence on the liquid drop solidification phenomenon, the pressure in the bin can be vacuum, negative pressure, normal pressure or high pressure. From the economic point of view, normal pressure is preferably selected. The temperature in the compartment may be selected to be greater than or equal to the temperature of the floor.
The temperature control of the soleplate 30 can be controlled by liquid gas (liquid nitrogen), dry ice and other refrigerants besides using thermoelectric cooling fins.
For matrix media with melting point higher than room temperature, such as polymers and liquid metals, the actual temperature of the supercooling bottom plate can be set to room temperature or heated.
As shown in fig. 1, a 1ml syringe is used to drop the nanofluid on the surface of the supercooling bottom plate 30, so as to obtain a droplet 20 on the surface of the bottom plate, wherein the droplet 20 contains a plurality of micro-nano particles 10.
In the embodiment, the distance from the lower end of the injector to the surface of the bottom plate 30, namely the drop height, is 5-20 mm, and needs to be larger than the diameter of the liquid drop 20. The droplets 20 impact the floor surface at a low velocity and the subsequent deployment and retraction process is negligible.
The volume of the single liquid drop 20 can be adjusted according to the surface tension, viscosity and injector pipe diameter of the mixed liquid, the radius of the liquid drop 20 can be from centimeter to submicron, the volume of the liquid drop 20 is about 5-10 μ l, and in the embodiment, the volume of the liquid drop 20 is about 7 μ l.
For matrix media with melting point above room temperature, the injector should be insulated to protect the latter from heat prior to dripping, ensuring that the droplets 20 do not solidify before they touch the floor.
The mechanism for introducing the droplets 20 can be selected by placing the droplets 20 on the substrate 30 first and then gradually reducing the temperature of the substrate, or by suddenly placing the substrate 30 carrying the droplets in a supercooled environment, in addition to dropping to the supercooled substrate.
The droplets 20 undergo nucleation of solidification on the surface of the undercooling bottom plate 30, which occurs at the solid/liquid interface, followed by gradual upward displacement of the solidification interface.
When the concentration of the micro-nano particles 10 is high, the removed micro-nano particles 10 can be gathered at the solidification interface front to form a dense particle accumulation layer, as shown in fig. 2, a plurality of micro-nano particles 10 are gathered in front of the solidification front due to segregation to form a layer of densely arranged particle bands 11.
Near the three-phase boundary (water/ice/air), the propulsion of the micro-nano particles 10 accumulation layer can generate a large amount of free interfaces (particles/air), and the total free energy of the system is improved. Driven by the free energy gradient, the continuous medium is supplemented to the three-phase intersection from the interior of the liquid drop, and the compensation flow parallel to the solidification interface causes the shape of the solidified liquid drop to change.
Due to the particle packing layer propulsion at the three-phase (liquid/solid/air) interface, the free energy gradient induces a compensating flow L parallel to the solidification interface, as shown in fig. 3, flowing from the center to the periphery, which continuously transports the liquid from the interior of the droplet to the surface of the droplet and finally to the solidified shape 40 of the droplet as shown in fig. 4.
Fig. 5 is a photograph of the droplet added with the micro-nano particles before solidification, and the shape of the droplet is hemispherical.
Fig. 6 is a photograph of the solidified droplet added with micro-nano particles, wherein the droplet is in a spherical table shape, and it can be seen that the top of the droplet is changed from a spherical shape to a plane, thereby reducing the height of the droplet.
The micro-nano particles 10 are transferred to the top end of the liquid drop after the liquid drop is solidified, and the whole liquid drop is still a pure matrix medium.
In the method for controlling the shape of the solidified liquid drop by adding the micro-nano particles, the top shape of the liquid drop is changed, so that the height of the liquid drop is reduced. The technology of the embodiment is applied to the soldering process, and is beneficial to further miniaturization of the whole microelectronic system.
The technology of the embodiment is applied to three-dimensional printing, and can overcome the defects that the porosity of a device is very high due to accumulation of spherical liquid drops, and the mechanical strength and the air tightness of the material are seriously influenced.
Effects and effects of the embodiments
The method and application for controlling the shape of the solidified liquid drop according to the embodiment have the following advantages:
the process is simple, and the shape of the liquid drop can be controlled only by adding corresponding micro-nano particles;
furthermore, the performance of the device is not influenced, and the micro-nano particles are transferred after the liquid drops are solidified
Further, the whole liquid drop is still a pure matrix medium to the top end of the liquid drop;
furthermore, the method is suitable for a wide range of matrix media, water, organic solvents, polymers, liquid metal and the like;
further, the larger the scale span, the droplet radius can be from centimeter to submicron;
furthermore, the method is applied to a soldering process, and is beneficial to further miniaturization of the whole microelectronic system;
further, in the application of three-dimensional printing, the defects that the porosity of a device is high due to accumulation of spherical liquid drops, and the mechanical strength and the air tightness of the material are seriously influenced can be overcome.
The above embodiments are preferred examples of the present invention, and are not intended to limit the scope of the present invention.
Claims (7)
1. A method of controlling the shape of a solidified droplet, comprising:
preparing a suspension containing nanoparticles;
dripping the suspension on the surface of the supercooling bottom plate to obtain liquid drops on the surface of the bottom plate;
the liquid drops are subjected to solidification nucleation on the supercooling bottom plate, the solidification nucleation occurs on a solid-liquid contact surface, and then a solidification interface is gradually pushed upwards;
the nano particles are gathered at the front of a solidification interface to form a dense particle accumulation layer;
the particle accumulation layer at the three-phase boundary position is advanced, so that the free energy gradient initiates a compensating flow which flows from the center to the periphery in parallel with the solidification interface, the liquid is continuously transported to the surface of the liquid drop from the inside of the liquid drop, the top of the liquid drop is changed from a spherical shape to a plane, and the shape of the solidified liquid drop is finally obtained and is in a spherical frustum shape,
wherein the method for preparing the suspension comprises the following steps:
placing 100mL of deionized water into a beaker, heating the deionized water to 90 ℃, and then placing the heated deionized water into a vacuum vessel for natural cooling and degassing;
adding 0.1g of sodium dodecyl sulfate into the cooled deionized water, and electromagnetically stirring until the sodium dodecyl sulfate is completely dissolved to obtain a sodium dodecyl sulfate solution;
adding 3.6g of titanium dioxide nano particles into a sodium dodecyl sulfate solution, electromagnetically stirring for more than 2 hours to obtain stable water-based titanium dioxide nano fluid,
the bottom plate is made of heat conducting material, the initial temperature is set to be 8-12 ℃ lower than the freezing point of the matrix medium in an equilibrium state,
the liquid drops are solidified in a closed bin, and protective gas is arranged in the closed bin.
2. The method of controlling a frozen droplet shape of claim 1, wherein:
wherein, the matrix medium is degassed, added with a surfactant, mixed with the nano-particles, and subjected to electromagnetic stirring and ultrasonic oscillation to obtain a stable dispersion system.
3. A method of controlling a frozen droplet shape as claimed in claim 1, wherein:
wherein the nanoparticle has a particle size that is less than three orders of magnitude smaller than the droplet size.
4. The method of controlling a frozen droplet shape of claim 1, wherein:
the suspension is dripped to the surface of the supercooling bottom plate by using an injector, and the distance from the lower end of the injector to the surface of the bottom plate is 5-20 mm.
5. The method of controlling a frozen droplet shape of claim 1, wherein:
wherein the volume of the liquid drop is 5-10 mu L.
6. Use of a method of controlling the shape of a solidified droplet according to any one of claims 1-5 in a soldering process.
7. Use of a method of controlling the shape of a coagulated droplet according to any one of claims 1 to 5 in three-dimensional printing.
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| CA2691531A1 (en) * | 2007-06-22 | 2008-12-31 | Board Of Regents,The University Of Texas System | Formation of stable submicron peptide or protein particles by thin film freezing |
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