Method for preparing hydroxyapatite-based composite bioceramic material through in-situ reaction

A technology of composite bioceramics and hydroxyapatite, which is applied in the field of biomedical biomaterial preparation, can solve the problems of large fluctuation range of mechanical properties of composite materials, high cost of carbon nanotube preparation, failure to prevent interstitial fluid penetration, etc., and achieve improved interphase Bonding strength, shortened production cycle, good wetting effect

Active Publication Date: 2015-10-21
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the addition of carbon nanotubes greatly increases the preparation cost, and the mechanical properties of the composite material fluctuate widely.
The experiment also found that when the mass content of carbon nanotubes exceeds 25%, due to the low density of carbon nanotubes, the positions of the matrix and the reinforcement phase are exchanged, and it is difficult to synthesize the required materials at a temperature of about 1300 ° C.
In addition, a large number of studies have shown that coating a layer of hydroxyapatite on the surface of titanium alloys, magnesium alloys and other metals can obtain biomaterials with better mechanical properties, but the obtained coating has more pores, which cannot prevent tissue fluid from penetrating, and the interface is easy to corrode. Cause the coating to fall off in the later stage and the dissolution of harmful ions, causing great harm to the patient's body

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) According to Ca / P=1.67, the Ca(NO 3 ) 2 solution, (NH 4 ) 2 HPO 4 Solution, account for 20wt% of composite powder to prepare Al(NO 3 ) 3 9H 2 O solution.

[0024] (2) press Ca / F=5:1 to step (1) in (NH 4 ) 2 HPO 4 Add NH 4 F and stir to mix evenly;

[0025] (3) Add the mixed solution in step (2) dropwise to Ca(NO 3 ) 2 In the solution, add 2.5wt% polyethylene glycol 1500 as dispersant, and adopt 70 ℃ of water baths to heat and keep stirring, adopt ammonia water to adjust PH=10 value in the reaction process, after dropping, continue to add Al(NO 3 ) 3 9H 2 The O solution was added dropwise to the above mixed solution, and after the dropwise addition, the stirring was continued for 30 minutes, sealed and left standing for 24 hours;

[0026] (4) Remove the supernatant from the solution obtained in step (3) and sonicate for 20 minutes, then filter, wash, dry, and grind to obtain a composite powder precursor;

[0027] (5) Calcining the powder obtained in ...

Embodiment 2

[0032] Add NH 4 F makes Ca / F=10:1, and adds 5wt% polyethylene glycol 1500, Al(NO 3 ) 3 9H 2 The amount of O is calculated as alumina accounts for 30wt% of the composite powder. The precursor is calcined at 1000°C for 1 hour to obtain fluorine-substituted hydroxyapatite and alumina nanocomposite powder, which is then sintered at 1300°C. The flexural strength of the prepared composite material is 193.3MPa, and the fracture toughness is 3.8MPa m 1 / 2 , Vickers hardness is 543HV1 / 10; Other conditions are the same as embodiment one.

Embodiment 3

[0034] Al(NO 3 ) 3 9H 2 The amount of O is calculated based on alumina accounting for 30wt% of the composite powder, Al(NO 3 ) 3 9H 2Continue to stir for 30 minutes after the O solution is added dropwise, remove the supernatant after standing still for 48 hours, and then sonicate for 40 minutes. The precursor is calcined at 1100°C for 1 hour to obtain fluorine-substituted hydroxyapatite and alumina nanocomposite powder, and sintered at 1300°C . The flexural strength of the prepared composite material is 187.2MPa, and the fracture toughness is 3.2MPa m 1 / 2 , Vickers hardness is 538HV1 / 10; Other conditions are the same as embodiment one.

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Abstract

The invention belongs to the technical field of biomedical biomaterial preparation, and relates to a method for preparing a hydroxyapatite-based composite bioceramic material through an in-situ reaction. According to the method, calcium nitrate tetrahydrate (Ca(NO3)2.4H2O), diammonium hydrogen phosphate ((NH4)2HPO4), aluminum nitrate nonahydrate (Al(NO3)3.9H2O) and ammonium fluoride (NH4F) serve as raw materials, a chemical precipitation method is adopted to prepare fluorine-doped hydroxyapatite and aluminium oxide nanometer composite powder, and then hydroxyapatite-based composite bioceramic is prepared through hot-pressed sintering. The in-situ method is adopted to synthesize the hydroxyapatite and aluminium oxide nanometer composite powder, and uniform distribution of aluminum oxide in a hydroxyapatite matrix is improved; the prepared hydroxyapatite-based composite bioceramic has high biocompatibility and mechanical properties and can be used in the field of repairing or replacing bone tissue of a human body.

Description

technical field [0001] The invention belongs to the technical field of biomedical biomaterial preparation, and relates to a method for preparing hydroxyapatite-based composite bioceramic materials by in-situ reaction. Background technique [0002] Due to their good physical, chemical and biological compatibility, biomedical inorganic materials have achieved a lot of research results in just a decade. However, due to its high brittleness, easy to break, and a great difference in the structure of human hard tissues, so far there is still no material that can fully meet the physiological function requirements of the human body. Hydroxyapatite (Hydroxyapatite, HA or HAP) is an inorganic component of bone tissue, with good biocompatibility and bioactivity, and is widely used in bone tissue repair and replacement, stomatology and other fields. However, its poor mechanical properties limit its application in load-bearing materials. Although SiC whiskers can be used to toughen hyd...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/447A61L27/12A61K6/033A61K6/838
Inventor 张希华张聪毅袁建军孙凯窦金河
Owner SHANDONG UNIV
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