Calcium phosphate biological ceramic with superfine uniform crystal grains and preparation method of calcium phosphate biological ceramic

A technology of bioceramics and uniform grains, which can be used in drug delivery, tissue regeneration, and pharmaceutical formulations. It can solve the problems of poor mechanical properties of calcium phosphate bioceramics, and achieve excellent mechanical properties, optimized mechanical properties, and scientific design.

Active Publication Date: 2022-03-11
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] One of the purposes of the present invention is to provide a method for preparing calcium phosphate bioceramics with ultrafine uniform grains, so as to solve the problem of poor mechanical properties of calcium phosphate bioceramics in the prior art

Method used

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  • Calcium phosphate biological ceramic with superfine uniform crystal grains and preparation method of calcium phosphate biological ceramic
  • Calcium phosphate biological ceramic with superfine uniform crystal grains and preparation method of calcium phosphate biological ceramic
  • Calcium phosphate biological ceramic with superfine uniform crystal grains and preparation method of calcium phosphate biological ceramic

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Embodiment 1

[0043] This embodiment discloses the preparation method of the calcium phosphate bioceramics of ultrafine uniform grains of the present invention, specifically:

[0044] (1) Weigh 6g of primary hydroxyapatite powder (HA), and pre-sinter it at a low temperature at 600°C for 4 hours to obtain the pre-sintered powder and the microscopic morphology of the primary hydroxyapatite powder as attached figure 1 As shown in A.

[0045] (2) The calcined powder is subjected to wet ball milling, the medium is absolute ethanol, the volume is 50mL, the ball milling speed is 450rpm, and the ball milling time is 14h; the slurry after ball milling is centrifuged at 5000rpm for 5min, and then the centrifuged The supernatant was centrifuged for a second time at 10,000rpm for 5 minutes, and the supernatant obtained from the second centrifugation was centrifuged at 12,000rpm for 5 minutes, and the precipitate was collected, dried, ground and sieved to obtain phosphoric acid with small grain size an...

Embodiment 2

[0052] In this embodiment, whether low-temperature pre-sintering and the temperature of low-temperature pre-sintering are investigated: when low-temperature pre-sintering is not used, compared with Example 1, there is no step (1), and the rest of the conditions are the same; different pre-sintering temperatures are used , the pre-sintering temperature is as shown in the table below, and all the other conditions are the same as in Example 1.

[0053] Table 1 Pre-sintering temperature investigation results table

[0054]

[0055] It can be seen from the above table that when the pre-sintering temperature is 600-900°C, the obtained calcium phosphate bioceramic has a small average grain size, narrow distribution, good compressive strength, and good compressive strength.

[0056] The micro-morphology of the calcium phosphate powder prepared at the pre-sintering temperature of 700 °C is shown in the attached figure 1 As shown in C, compared with the unoptimized calcium phosphate...

Embodiment 3

[0060] This embodiment investigates whether to quench and different quenching methods: when not quenching, in the two-step sintering, after the second step of sintering and heat preservation, cool with the furnace, and the rest of the conditions are the same as in Example 1; when using different quenching methods , concrete quenching conditions are as shown in the table below, and all the other conditions are with embodiment 1:

[0061] Table 2 Quenching method investigation results table

[0062]

[0063]

[0064] It can be seen from the above table that the quenching method of the present invention is better than quenching and cooling in stages, and is better than cooling with furnace without quenching.

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Abstract

The invention discloses a calcium phosphate biological ceramic with ultrafine uniform crystal grains and a preparation method thereof, belongs to the technical field of biomedical materials, and solves the problem of poor mechanical properties of the calcium phosphate biological ceramic in the prior art. The preparation method of the calcium phosphate biological ceramic with the superfine uniform crystal grains comprises the following steps: pre-sintering initial calcium phosphate powder at low temperature to form a primary crystal phase; carrying out wet ball-milling treatment on the presintered calcium phosphate powder, carrying out gradient centrifugation on the ball-milled slurry, and separating to obtain calcium phosphate powder with small grain size and narrow distribution; preparing a ceramic green body from calcium phosphate powder obtained after ball milling and centrifugation; performing two-step sintering on the ceramic green body, and immediately performing quenching and rapid cooling treatment after the second-step sintering heat preservation is finished, so as to obtain the calcium phosphate biological ceramic. The calcium phosphate ceramic prepared by the method disclosed by the invention is uniform in grain size, not only has excellent mechanical properties, but also has relatively good biological activity, and meets the requirements of clinical bearing bone defect repair.

Description

technical field [0001] The invention belongs to the technical field of biomedical materials, and in particular relates to a calcium phosphate bioceramic with ultrafine uniform grains and a preparation method thereof. Background technique [0002] Calcium phosphate bioceramics have been applied in the field of bone repair due to their good biocompatibility, osteoinductivity and osteogenic activity, but they cannot be used in the field of load-bearing bone repair due to their natural brittleness and low fracture toughness. [0003] The prior art discloses that the mechanical properties of calcium phosphate ceramics can be significantly improved by refining the grain size of calcium phosphate ceramics. For example, the literature (Applied Mechanics and Materials, 2011, 83: 237-243) points out that with the increase of the grain size of calcium phosphate ceramics, If it is large, its Vickers hardness and fracture toughness will decrease. It is an effective method to improve the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/447C04B35/622A61L27/12
CPCC04B35/447C04B35/622A61L27/12C04B2235/602C04B2235/6567C04B2235/661C04B2235/785C04B2235/96A61L2430/02A61L2400/12
Inventor 李向锋李琪鹏马子涵朱向东曹全乐王烨敬杨天廖桐霄谭文暄张兴栋
Owner SICHUAN UNIV
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