Preparation method of hydroxyl apatite and application of hydroxyl apatite in 3D printing moulding

A technology of hydroxyapatite and 3D printing, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of undiscovered hydroxyapatite material research, and achieve low cost, simple process flow, and chemical reaction easy effect

Active Publication Date: 2017-11-17
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Beyond that, no specific research has been found on hydroxyapatite materials suitable for 3D printing

Method used

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  • Preparation method of hydroxyl apatite and application of hydroxyl apatite in 3D printing moulding
  • Preparation method of hydroxyl apatite and application of hydroxyl apatite in 3D printing moulding
  • Preparation method of hydroxyl apatite and application of hydroxyl apatite in 3D printing moulding

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1, a preparation and molding process of hydroxyapatite powder that can be used for 3D printing:

[0043]1), at room temperature, weigh 49.11g (0.334mol) of calcium chloride dihydrate and 14.19g (0.1mol) of phosphorus pentoxide, respectively dissolve them in 200ml of deionized water and 200ml of absolute ethanol, and stir for 2 hours respectively;

[0044] 2), take 50ml of calcium chloride aqueous solution in step 1) and stir in a beaker, and take 50ml of phosphorus pentoxide alcohol solution with a syringe, slowly drop into the beaker (dropping time is 2 minutes), and stir at room temperature for 2h;

[0045] 3) Place the mixed solution obtained in step 2) in a 60°C oven for aging for 48 hours;

[0046] In the above aging process, the mixed solution is placed in an open container, and the opening of the container is sealed with a plastic wrap, and some small holes are set on the plastic wrap to facilitate the discharge of volatile gas; after the aging is comp...

Embodiment 2

[0063] Example 2, a preparation and molding process of hydroxyapatite powder that can be used for 3D printing

[0064] Change the heat treatment temperature in Step 5) of Example 1 from 800°C to 600°C, and the rest are the same as in Example 1. The prepared main crystal phase is still hydroxyapatite with a high degree of crystallinity. The observation results under the transmission electron microscope are as follows: image 3 As shown, granular nano-hydroxyapatite grains were obtained, and the grain diameter was about 20 nm.

[0065] Comparative Example 2-1. The heat treatment temperature in Example 2 was changed from 600°C to 500°C, and the rest were the same as in Example 2.

[0066] Comparative Example 2-2, the heat treatment temperature in Example 2 was changed from 600°C to 700°C, and the rest were the same as in Example 2.

[0067] By X-ray diffraction, the law of the phase change with the heat treatment temperature was analyzed, and the results were as follows: Fig...

Embodiment 3

[0071] Example 3, a preparation and molding process of hydroxyapatite powder that can be used for 3D printing

[0072] The total mass of hydroxyapatite fine powder added in Step 7 of Example 1 was changed from 7.5 g to 8 g, and the rest were the same as in Example 1.

[0073] The compressive strength of the final printed hydroxyapatite 3D model was measured to be 7.53MPa. It can be seen that with the increase of the mass ratio of powder in the slurry, the strength of the printed product is slightly improved. This is a consequence of the decrease in porosity in the model as the solids content increases.

[0074] Comparative Example 3-1. The total mass of hydroxyapatite fine powder added in Example 3 was changed from 8g to 6g, and the rest were the same as in Example 3. Due to the low solid content, the viscosity of the slurry is not enough to achieve molding during the printing process.

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Abstract

The invention discloses a preparation method of hydroxyl apatite. The preparation method is a sol-gel method and comprises the following steps: individually dissolving a calcium source and a phosphorus source into different solvents, mixing two solvents, aging obtained mixed solution at a temperature of 40 to 60 DEG C, drying obtained gel in a baking oven with a temperature of 80 to 100 DEG C, and subjecting obtained dry gel to a heat treatment (600 to 800 DEG C) so as to obtain block shaped hydroxyl apatite. The invention also provides an application of hydroxyl apatite in 3D printing moulding. The application comprises the following steps: ball-grinding hydroxyl apatite, sieving, adding a PVA solution with a mass concentration of 3 to 10%, blending to obtain slurry; carrying out layer casting and moulding by a ceramic 3D printer; placing obtained model in a sintering furnace; carrying out a heat treatment for 4.5 to 5.5 hours at a temperature of 500 to 800 DEG C, and finally cooling the product in the furnace.

Description

technical field [0001] The present invention relates to a preparation method of hydroxyapatite powder material and its 3D printing molding process, in particular to a sol-gel preparation of hydroxyapatite and extrusion of a hydroxyapatite slurry 3D printing technology of accumulation forming. Background technique [0002] Hydroxyapatite (HA for short), its chemical formula is written as Ca 10 (PO 4 ) 6 (OH) 2 . HA is the main inorganic component of human and animal bones, accounting for about 60% of human bones. It is a needle-like crystal with a length of 20-40nm and a thickness of 1.5-3.0nm, and collagen fibers are regularly arranged around it. The structure of dentary bone is also similar to natural bone, but the content of HA in dentary bone is as high as 97%. Hydroxyapatite is a biocompatible therapeutic material that can be used in the medical field due to its non-toxic, non-irritating, non-sensitizing, non-mutagenic and carcinogenic properties. At present, the ...

Claims

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Application Information

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IPC IPC(8): C04B35/624C04B35/447C01B25/32B33Y70/00
CPCB33Y70/00C01B25/32C01P2002/72C01P2004/03C01P2004/04C04B35/447C04B35/624C04B2235/96
Inventor 郭兴忠陆子介黄凯越王奇玄尹朋岸杨辉
Owner ZHEJIANG UNIV
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