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Method for preparing calcium phosphate series bioceramic nano-powder

A bio-ceramic and nano-powder technology is applied in the preparation of calcium phosphate-based bio-ceramic nano-powder and the field of calcium phosphate-based bio-ceramic nano-powder, which can solve the problems of unsatisfactory powder particle size and achieve the effect of high purity

Inactive Publication Date: 2004-12-29
SOUTHEAST UNIV
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Problems solved by technology

Chinese patent ZL02138721.4 "synthesis of hydroxyapatite powder by self-combustion method" discloses a kind of (NH 4 ) 2 HPO 4 and Ca(NO 3 ) 2 4H 2 O is the self-combustion method of preparing hydroxyapatite powder as raw material. The calcination temperature is 750°C. The primary average particle size of the prepared hydroxyapatite powder is 85nm, and the secondary average particle size is 494.6nm. The particle size of the powder is still not ideal

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  • Method for preparing calcium phosphate series bioceramic nano-powder
  • Method for preparing calcium phosphate series bioceramic nano-powder

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[0009] The preparation method of the present invention is: according to the Ca / P molar ratio is 1.5-1.67 and takes the calculated amount of calcium nitrate Ca (NO 3 ) 2 4H 2 O and trimethyl phosphate (CH 3 O) 3 PO, dissolved in distilled water and alcohol respectively; then add citric acid C 6 h 8 o 7 After fully dissolving, mix the calcium nitrate aqueous solution and the trimethyl phosphate alcohol solution, adjust the pH of the mixture to 3-11 with ammonia water, and age at room temperature for 12-48 hours; then dry at 80-190°C for 2-10 hours to generate xerogels; and finally calcined at 500-600°C for 1-3 hours to obtain the required nano powder.

[0010] By controlling the Ca / P atomic ratio between 1.5 and 1.67, calcium phosphate-based bioceramic nanopowders, such as hydroxyapatite Ca 10 (PO 4 ) 6 (OH) 6 , Ca / P=1.67; β-tricalcium phosphate β-Ca 3 (PO 4 ) 2 , Ca / P=1.5; or a biphasic bioceramic composed of hydroxyapatite and β-tricalcium phosphate. In biphasic ...

Embodiment 1

[0013] Weigh the calculated amount of calcium nitrate 19.706g (0.0835mol) and trimethyl phosphate 7.05g (0.05mol) according to the Ca / P molar ratio of 1.67, dissolve them with 80ml of distilled water and 30ml of alcohol respectively, and then add them to the calcium nitrate aqueous solution After fully dissolving 16.032g of citric acid in an equimolar amount with calcium ions, mix calcium nitrate aqueous solution and trimethyl phosphate alcohol solution, adjust the pH of the mixture to 7.5 with ammonia water, age at room temperature for 48 hours, and then at 190°C Drying at low temperature for 2 hours to form a xerogel, and finally calcining at 600°C for 1 hour to obtain the desired hydroxyapatite nanopowder. like figure 1 As shown in (a), X-ray diffraction XRD phase composition analysis shows that the main crystal phase of the prepared product is hydroxyapatite. figure 2 It is a transmission electron microscope TEM photograph of the hydroxyapatite nanopowder. It can be seen...

Embodiment 2

[0015] Weigh 17.7g (0.075mol) of calcium nitrate and 7.05g (0.05mol) of trimethyl phosphate according to the Ca / P molar ratio of 1.5, dissolve them in 80ml of distilled water and 30ml of alcohol, and then add them to the calcium nitrate aqueous solution. After fully dissolving 14.4g of citric acid with an equimolar amount of calcium ions, mix calcium nitrate aqueous solution and trimethyl phosphate alcohol solution, adjust the pH of the mixture to 11 with ammonia water, age at room temperature for 48 hours, and then dry at low temperature for 3 hours to form a xerogel, and finally calcined at 600°C for 2 hours to obtain the desired β-tricalcium phosphate nanopowder. like figure 1 As shown in (b), X-ray diffraction XRD phase composition analysis shows that the main crystal phase of the prepared product is β-tricalcium phosphate.

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Abstract

The present invention is the preparation process of serial calcium phosphate bioceramic powder, including hydroxyapetite, beta-tricalcium phophate and biphase hydroxyapetite / beta-tricalcium phophate ceramic. The preparation process includes: weighing calcium nitrate and trimethyl phosphate in the molar Ca / P ratio of 1.5-1.67 and dissolving in distilled water and alcohol separately; adding citric acid in the equal molar amount of calcium ion to calcium nitrate aqua and dissolving fully; mixing the calcium nitrate aqua and trimethyl phosphate alcohol solution, regulating the pH value of the mixed solution with ammonia water to 3-11 and ageing at room temperature for 12-48 hr; drying at 80-190 deg.c for 2-10 hr to produce dry gel; and calcining at 500-600 deg.c for 1-3 hr to obtain required nano powder.

Description

technical field [0001] The invention relates to a method for preparing calcium phosphate-based bioceramic nanopowder, more precisely, a method that can prepare hydroxyapatite HA, β-tricalcium phosphate β-TCP and HA / β-TCP dual-phase ceramics in The invention discloses a new method for calcium phosphate-based bioceramic nanopowder, belonging to the technical field of nanobiological ceramics synthesis. Background technique [0002] The main inorganic substances of human hard tissues are calcium phosphate-based bioceramics such as hydroxyapatite and β-calcium phosphate. Therefore, from the perspective of biocompatibility and bioactivity, artificially synthesized hydroxyapatite, β-calcium phosphate and The dual-phase bioceramic material composed of them is currently an ideal human hard tissue replacement material. It should be pointed out that the calcium phosphate ceramics in bone tissue are mainly deposited in the collagen matrix in the form of nano p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/447C04B35/622
Inventor 储成林林萍华董寅生浦跃朴郭大勇闵建华刘斌郭超
Owner SOUTHEAST UNIV
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