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Preparation method of nanocrystalline metal microspheres for 3D printing

A technology of metal microspheres and 3D printing, which is applied in the direction of nanotechnology, metal processing equipment, nanotechnology, etc. for materials and surface science, and can solve the problem of obvious microspheres, as small as a dozen microns, as large as hundreds of microns, and microspheres. Inhomogeneous particle size distribution, particle size difference, internal active flow loss and other problems, to achieve the effect of good particle size consistency, improved effect, and improved performance

Pending Publication Date: 2022-06-24
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Various traditional methods of preparing metal microspheres, such as spray drying, suspension polymerization, ion cross-linking and emulsion evaporation, have disadvantages such as unstable external force, uneven shear force when different phases are mixed, and loss of internal active fluid.
The particle size distribution of the microspheres obtained by the above preparation method is uneven, and the difference in particle size is obvious, ranging from as small as a dozen microns to as large as hundreds of microns

Method used

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  • Preparation method of nanocrystalline metal microspheres for 3D printing

Examples

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preparation example Construction

[0037] The preparation method specifically comprises the following steps:

[0038] S1) Use metal nitrate as raw material to configure an unstable precursor solution;

[0039] S2) The unstable precursor solution obtained in S1) is used as the dispersed phase, and the silicone oil is used as the continuous phase, and microfluidic technology is used to process to obtain microsphere droplets with a diameter of 40-300 μm;

[0040] S3) placing the S2) microsphere droplets in silicone oil, and irradiating the microsphere droplets in the silicone oil with ultraviolet rays to stimulate the curing of the photocuring agent in the microsphere droplets to form a gel microsphere body;

[0041] S4) Perform impurity removal on the gel microsphere green body obtained in S3), and then perform calcination reduction after drying, to obtain nanocrystalline metal microspheres for 3D printing.

[0042] The specific steps of the S1) are:

[0043] S1.1) Weigh an appropriate amount of metal nitrate p...

Embodiment 1

[0061] S1) Weigh 10g of copper nitrate into a beaker, measure 90mL of deionized water with a measuring cylinder and pour it into the beaker, stir with a glass rod for two minutes to obtain a copper nitrate solution, cool the prepared copper nitrate solution to 0~5℃, This solution is denoted as A solution.

[0062] Prepare a mixed solution of hexamethylenetetramine with a molar concentration of 2 mol / L and urea with a molar concentration of 2 mol / L. The mixed volume ratio is hexamethylenetetramine: urea=1:3, and 3wt.% photosensitizer is added. Resin and photoinitiator (1:1), the solution was cooled to 0-5°C, and this solution was recorded as solution B.

[0063] S2) Mix A solution and B solution to obtain a precursor solution. The volume ratio of solution A and solution B mixed is 3:2.

[0064] S3) The prepared precursor solution is used as the dispersed phase, and the silicone oil is used as the continuous phase; the continuous phase flow rate is set to 3 mL / min, and the con...

Embodiment 2

[0070] S1) Weigh 10g of nickel nitrate into a beaker, pour 90mL of deionized water measured in a measuring cylinder into the beaker, stir with a glass rod for two minutes to obtain a copper nitrate solution, and cool the prepared nickel nitrate solution to 0~5 ℃, this solution is recorded as A solution.

[0071] Prepare a mixed solution of hexamethylenetetramine with a molar concentration of 2 mol / L and urea with a molar concentration of 2 mol / L, the mixed volume ratio is hexamethylenetetramine: urea=1:3, add 3wt.% photosensitizer Resin and photoinitiator (1:1), the solution is cooled to 0~5℃, this solution is recorded as B solution.

[0072] S2) Mix A solution and B solution to obtain a precursor solution. The volume ratio of solution A and solution B mixed is about 3:2.

[0073] S3) Take the prepared precursor solution as the dispersed phase and silicone oil as the continuous phase, set the flow rate of the continuous phase to 2.5mL / min and the flow rate of the dispersed p...

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Abstract

The invention belongs to the technical field of powder metallurgy, and particularly relates to a preparation method of nanocrystalline metal microspheres for 3D printing. The method comprises the following steps: rapidly mixing stable solutions into an unstable precursor solution at room temperature by adopting an internal gel method, rapidly dispersing the precursor solution into liquid drops by utilizing a micro-fluidic technology to obtain gel microspheres, and washing, drying and reducing to obtain the spherical metal microspheres. The droplet microfluidic technology is relatively simple to operate, the prepared microspheres are uniform in particle size and good in monodispersity, and the particle size deviation can be stably controlled below 5%; moreover, the reagent consumption is low, the safety coefficient is high, the internal composition content can be controlled, and a more ordered internal structure is realized. The metal microspheres prepared through the method are good in uniformity and sphericity degree and are in the micron scale level, and the crystal grains forming microsphere particles are smaller than or equal to 100 nm. According to the invention, a microfluidic technology and a 3D printing technology are combined to prepare the nanocrystalline metal microspheres with high purity and good sphericity.

Description

technical field [0001] The invention belongs to the technical field of powder metallurgy, and particularly relates to a preparation method of nanocrystalline metal microspheres for 3D printing. Background technique [0002] Metal powder material is the raw material for metal 3D printing, and the basic properties of its powder have a great relationship with the quality of the final molded product. The requirements of metal 3D printing for powder are mainly in the aspects of chemical composition, particle shape, particle size and particle size distribution, fluidity, and recyclability. The fluidity of the powder directly affects the uniformity of powder spreading or the stability of powder feeding. If the powder fluidity is too poor, it is easy to cause uneven thickness of the powder layer and uneven metal melting in the scanning area, resulting in uneven internal structure of the product and affecting the forming quality. The powder with high fluidity is easy to fluidize, d...

Claims

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Application Information

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IPC IPC(8): B22F9/22B22F1/054B22F10/28C01G3/02C01G49/06C01G53/04B33Y10/00B33Y70/00B82Y30/00B82Y40/00
CPCB22F9/22B22F10/28C01G3/02C01G53/04C01G49/06B33Y10/00B33Y70/00B82Y30/00B82Y40/00C01P2004/32Y02P10/25
Inventor 陈鹏起方青青程继贵台运霄杨建许荡魏邦争
Owner HEFEI UNIV OF TECH
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