Preparation method of beta-tricalcium phosphate nanometer coating

A technology of tricalcium phosphate nanometer and tricalcium phosphate, which is applied in the direction of coating, electrolytic coating, electrophoretic plating, etc., can solve the problems of high equipment price, high requirements for preparation environment conditions, and complicated operation, so as to enhance the binding force and avoid Phase change and embrittlement, energy saving effect

Active Publication Date: 2017-04-26
SOUTH CHINA UNIV OF TECH
4 Cites 3 Cited by

AI-Extracted Technical Summary

Problems solved by technology

[0004] Common methods for preparing β-TCP coatings include plasma spraying, physical and chemical vapor deposition, electrophoretic deposition, powder metallurgy, etc. However, methods such as plasma spraying, ...
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Abstract

The invention discloses a preparation method of a beta-tricalcium phosphate nanometer coating. The preparation method comprises the following steps: (1) adding dispersant in a calcium source solution, uniformly stirring, adding a phosphorus source solution dropwise, and continuously stirring, ageing, filtering, washing, freezing, drying and calcining the mixture to obtain a beta-tricalcium phosphate powder; (2) adding the prepared beta-tricalcium phosphate powder in ethanol, carrying out ball milling and standing to prepare a stable beta-tricalcium phosphate suspension; and (3) taking a gold sheet as a working electrode, a platinum electrode as a counter electrode and the beta-tricalcium phosphate suspension as an electrolyte, applying direct current between the electrodes, and carrying out electrophoretic deposition on the surface of the gold sheet to obtain the beta-tricalcium phosphate nanometer coating. According to the preparation method, phase change and embrittlement caused in the high temperature process are prevented, the binding force of substrate metal and the beta-tricalcium phosphate nanometer coating is strengthened, the energy is saved, and the roughness of the beta-tricalcium phosphate nanometer coating can be controlled by controlling the electric field intensity and the time of electrophoretic deposition.

Application Domain

Electrophoretic coatings

Technology Topic

Electrophoretic depositionChemistry +14

Image

  • Preparation method of beta-tricalcium phosphate nanometer coating
  • Preparation method of beta-tricalcium phosphate nanometer coating
  • Preparation method of beta-tricalcium phosphate nanometer coating

Examples

  • Experimental program(3)

Example Embodiment

[0044] Example 1
[0045] The preparation of the β-TCP nanocoating of this embodiment includes the following steps:
[0046] (1) With 0.45mol/L Ca(NO 3 ) 2 ·4H 2 O solution is calcium source, 0.5mol/L (NH 4 ) 2 HPO 4 The solution is phosphorus source, adjust the amount of calcium source and phosphorus source to control the molar ratio of Ca/P to 1.5; add dispersant polyethylene glycol to calcium source and stir evenly; use ammonia water to adjust the pH of phosphorus source solution to 9.0; The phosphorus source solution was added dropwise to the calcium source solution under the condition of stirring at 400 r/min. During the dropping process, the pH of the reaction solution system was kept at 7.0. Washed with deionized water until the pH of the supernatant was 7.0, freeze-dried, and calcined at 800 °C for 3 h to obtain β-TCP powder;
[0047] figure 1 It is the XRD pattern of the synthesized β-TCP powder. It can be seen from the figure that the synthesized powder is a pure-phase β-TCP powder without other impurity phases; figure 2 The SEM image of the synthesized β-TCP powder shows that the synthesized β-TCP powder is spherical nanoparticles of different sizes.
[0048] (2) Weighing the prepared β-TCP powder, adding it into ethanol to prepare a 1wt% suspension, ball milling at a speed of 774r/min for 12h, and standing for 6h to obtain a stable suspension;
[0049] (3) Using the gold piece as the working electrode and the platinum electrode as the counter electrode, apply a direct current of 25V/cm between the electrodes for 1min, 5min and 10min respectively, take out the gold piece, and ultrasonically treat it in absolute ethanol (28kHz, 100W). ) for 1 min, the particles with weak surface binding were washed off, and the β-TCP nanocoating samples 11, 12 and 13 were obtained on the surface of the gold sheet.
[0050] The roughness of the β-TCP nanocoating samples 11, 12 and 13 prepared in this example is shown in Table 1.
[0051] Table 1 Roughness of β-TCP nanocoating samples 11, 12 and 13
[0052] sample Roughness (nm) 11 0.87 12 2.05 13 2.46
[0053] image 3 The AFM topography of the surface of the gold sheet used in this example shows that the roughness is 0.46 nm, and the surface is relatively flat.
[0054] Figure 4 to Figure 6 AFM topography of samples 11-13 of β-TCP nanocoatings deposited by electrophoresis for 1min, 5min, and 10min under the electric field strength of 25V/cm, respectively.
[0055] From Table 1 and Figure 2 to Figure 6 It can be seen that the size of the gold flake β-TCP powder deposited by electrophoresis on the surface of the gold flake increases with the increase of electrophoretic deposition time. When the electrophoretic deposition time is 5 min, the particle size deposited on the surface of the gold flake is moderate and the coverage is relatively uniform; The deposition amount of β-TCP on the sheet surface increased with the increase of the electrophoretic deposition time, and the roughness of the β-TCP nanocoating became larger with the increase of the electrophoretic deposition time; the time increased from 1 min to 5 min, the roughness and deposition amount The increase is obvious, while the increase of deposition amount and roughness is smaller with the increase of electrophoresis time from 5 min to 10 min.

Example Embodiment

[0056] Example 2
[0057] The preparation of the β-TCP nanocoating of this embodiment includes the following steps:
[0058] (1) With 0.45mol/L Ca(NO 3 ) 2 ·4H 2 O solution is calcium source, 0.5mol/L (NH 4 ) 2 HPO 4 The solution is phosphorus source, adjust the dosage of calcium source and phosphorus source to control the molar ratio of Ca/P to 1.5; add dispersant polyethylene glycol into calcium source and stir evenly; adjust the pH of phosphorus source solution with ammonia water to 9.0; The solution was added dropwise to the calcium source solution under the stirring condition of 400r/min. During the dropwise addition, the pH of the reaction solution system was kept at 7.0. After the dropwise addition, the stirring was continued for 10h, aged for 2d, filtered, and deionized water was used. Washed until the pH of the supernatant was 7.0, freeze-dried, and calcined at 800 °C for 3 h to obtain β-TCP powder;
[0059] (2) Weighing the prepared β-TCP powder, adding it into ethanol to prepare a 1wt% suspension, ball milling at a speed of 774r/min for 12h, and standing for 6h to obtain a stable suspension;
[0060] (3) Using the gold piece as the working electrode and the platinum electrode as the counter electrode, apply a 100V/cm DC current between the electrodes for 1min and 5min, and then take out the gold piece, ultrasonically treat it in absolute ethanol (28kHz, 100W) for 1min, and wash off the surface. The loosely bound particles were used to obtain β-TCP nanocoating samples 21 and 22 on the surface of gold flakes.
[0061] The roughness of the β-TCP nanocoating prepared in this example is shown in Table 2.
[0062] Table 2 Roughness of β-TCP nanocoating samples 21 and 22
[0063] sample Roughness (nm) 21 1.90 22 2.51
[0064] Figure 7 and Figure 8 AFM topography of β-TCP nanocoating samples 21 and 22 prepared by electrophoretic deposition under the electric field strength of 100 V/cm for 1 min and 5 min, respectively; it can be seen from the figure that with the increase of electrophoretic deposition time, the deposition amount increases, and the roughness of the β-TCP nanocoating samples increases with the electrophoretic deposition time.
[0065] From Table 2 and Figure 7 , Figure 8 It can be seen that, compared with the sample 11 in Example 1, the deposition amount and roughness of the sample 21 increased significantly; and compared with the sample 12, the increase in the deposition amount and the roughness of the sample 22 became smaller. It can be seen that in the case of electrophoretic deposition for 1 min, as the electric field intensity increases from 25V/cm to 100V/cm, the deposition amount and roughness increase significantly. When the time increased to 5 min, the increase of deposition amount and roughness became smaller with the increase of voltage.
[0066] Compared with Example 1, after the time was increased from 1 min to 5 min, the increase in deposition amount and roughness was smaller.

Example Embodiment

[0067] Example 3
[0068] The β-TCP nanocoating obtained by electrophoretic deposition under the electric field strength of 25V/cm for 5min was used in QCM-D technology to study the adsorption behavior of bovine serum albumin (BSA) on it, including the following steps:
[0069] (1) The preparation of β-TCP nanocoating is the same as in Example 1, and the electrophoretic deposition time is 5min;
[0070] (2) The adsorption behavior of bovine serum albumin (BSA) on the β-TCP nanocoating was studied by QCM-D technology, and BSA was dissolved in PBS buffer solution to prepare a 1 mg/ml bovine serum albumin solution. The PBS buffer solution was introduced first, and the BSA solution was introduced after the baseline equilibrium was stable, and the adsorption was observed until the adsorption reached equilibrium.
[0071] Figure 9 and Figure 10 are the frequency Δf and dissipation value ΔD of BSA adsorbed on β-TCP nanocoatings with time, respectively. It can be seen from the figure that the β-TCP nanocoating prepared under this condition can obtain clear frequency Δf and dissipation value. Value ΔD change graph, and the protein is stably bound to the surface of the gold sheet during the protein adsorption process. Therefore, the β-TCP nanocoatings prepared under this condition can be used to study the dynamic adsorption process of proteins by QCM-D technology.
[0072] It can be seen from the figure that after BSA is introduced, the Δf value decreases rapidly, accompanied by a rapid increase in the ΔD value, and the equilibrium is quickly reached. This indicates that during the adsorption process, BSA will rapidly and massively spread on the surface of the coating, occupying the adsorption sites, and then the amount of adsorption is basically unchanged and the conformation of BSA does not rearrange.

PUM

PropertyMeasurementUnit
Roughness0.46nm

Description & Claims & Application Information

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