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Method for preparing calcium silicate/beta- tricalcium phosphate composite powder by two-step chemical precipitation method

A technology of tricalcium phosphate nanometer and composite powder, which is applied in the field of biomedical materials, can solve the problems of cumbersome washing, high temperature, complexity, etc., and achieves the effects of simple and easy preparation process, small grain size, and controllable composite ratio.

Inactive Publication Date: 2006-07-12
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method has the following disadvantages: due to the high temperature (1390-1500 ° C) and long time (more than 40 hours) in the sintering process of ceramics, the preparation process consumes a lot of energy and costs high
Although this method of mechanical ball milling and mixing is simple in process, its fatal disadvantages are: firstly, it is necessary to prepare different single ceramic powders, and the preparation process of each single ceramic powder requires complicated and cumbersome washing, filtering, and drying. , calcination and other processes; secondly, the application of mechanical ball milling mixing method must introduce ball milling media, the usual ball milling media is alumina or zirconia and other substances, so it is very easy to introduce impurities as ball milling media during the ball milling mixing process, and the field of biological materials The purity requirement of the material is very high, so the ball milling mixing process is a non-ideal technology for preparing biomaterials, and the compounding degree of the composite powder obtained by the ball milling method is usually not very uniform
Therefore, due to the uneven composite degree of the powder, poor sintering activity, and phase transition caused by high temperature during the sintering process, the mechanical strength of the prepared composite ceramics is not good, which affects a wider range of clinical applications, especially It is limited and other shortcomings in the occasions with high mechanical load requirements

Method used

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  • Method for preparing calcium silicate/beta- tricalcium phosphate composite powder by two-step chemical precipitation method
  • Method for preparing calcium silicate/beta- tricalcium phosphate composite powder by two-step chemical precipitation method
  • Method for preparing calcium silicate/beta- tricalcium phosphate composite powder by two-step chemical precipitation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take 40.72 grams of Ca(NO 3 ) 2 4H 2 O was dissolved in 1000 mL of deionized water and adjusted to pH = 11 with 1:1 ammonia water, and 49.00 g of Na 2 SiO 3 9H 2 Dissolve O in 1000 mL deionized water to obtain Na 2 SiO 3 aqueous solution. The above Ca(NO 3 ) 2 The solution was added dropwise to Na 2 SiO 3 In the solution, use 1:1 ammonia solution to keep the pH value of the reaction system at 11 during the addition process, continue stirring for 24 hours after addition, filter, wash with deionized water and absolute ethanol, filter dry, and dry at 80°C for 12 hours A dry powder is obtained, and the dry powder is calcined at 750° C. for 2 hours to obtain a white calcium silicate powder. Disperse the calcium silicate powder prepared above in 1000mL and dissolve 17.04 grams of (NH 4 ) 2 HPO 4 1000mL of pH 11.0 and 45.71 grams of Ca(NO 3 ) 2 4H 2 O aqueous solution was added dropwise to the above-mentioned suspension, and the pH value of the reaction system...

Embodiment 2

[0024] Take 49.60 grams of Ca(NO 3 ) 2 4H 2 O was dissolved in 1500 mL of deionized water, and adjusted to pH = 10.5 with aqueous sodium hydroxide solution, and 59.39 g of Na 2 SiO 3 9H 2 Dissolve O in 1000 mL deionized water to obtain Na 2 SiO 3 aqueous solution. The above Ca(NO 3 ) 2 solution added to Na 2 SiO 3 In the solution, use sodium hydroxide aqueous solution to keep the pH value of the reaction system at 10.5 during the addition process, continue to stir for 24 hours after addition, filter, wash with deionized water and absolute ethanol, filter dry, and dry at 80°C for 12 hours to obtain a dry powder body, the dry powder was calcined at 700°C for 2 hours to obtain white calcium silicate powder. The calcium silicate powder that above-mentioned preparation obtains is dispersed in 1000mL and is dissolved with 48.44 grams (NH 4 ) 2 HPO 4 1000mL of pH 10.5 and 129.93 grams of Ca(NO 3 ) 2 4H 2 O aqueous solution was added dropwise to the above suspension. ...

Embodiment 3

[0026] Take 86.80 grams of Ca(NO 3 ) 2 4H 2 O was dissolved in 1000 mL deionized water, and adjusted to pH = 11 with 1:1 ammonia water, and 103.94 g of Na 2 SiO 3 9H 2 Dissolve O in 1000 mL deionized water to obtain Na 2 SiO 3 aqueous solution. The above Ca(NO 3 ) 2 The solution was added dropwise to Na 2 SiO 3 In the solution, use 1:1 ammonia solution to keep the pH value of the reaction system at 11 during the addition process, continue stirring for 24 hours after addition, filter, wash with deionized water and absolute ethanol, filter dry, and dry at 80°C for 12 hours A dry powder is obtained, and the dry powder is calcined at 750° C. for 2 hours to obtain a white calcium silicate powder. The calcium silicate powder prepared above was strongly dispersed in 1000mL dissolved with 15.57 grams of (NH 4 ) 2 HPO 4 1000mL of pH 11.0 and 41.76 grams of Ca(NO 3 ) 2 4H 2 O aqueous solution was added dropwise to the above-mentioned suspension, and the pH value of the ...

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Abstract

The invention relates to a method for preparing calcium silicate / beta- tricalcium phosphate nanometer complex powder in the field of biology medical material. It is characterized in that it adopts soluble silicate, calcium nitrate, diammonium phosphate and ammonia and so on as raw material. It uses the soluble silicate and calcium nitrate as raw material to prepare calcium silicate nanometer fiber powder by chemical precipitation, it distracts the calcium silicate nanometer fiber powder into the water solution of diammonium phosphate and adjusts the PH value to obtain the stain remover, it then drops the silicate nanometer fiber powder into the stain remover to do the second chemical precipitation to generate the tricalcium phosphate precipitation, then it washes and burns at 780-1000 deg. to obtain the calcium silicate / beta- tricalcium phosphate nanometer complex powder.

Description

technical field [0001] The invention relates to a method for preparing calcium silicate / beta-tricalcium phosphate nanocomposite powder by a two-step chemical precipitation method, which belongs to the field of biomedical materials. Background technique [0002] Inorganic biomedical hard tissue repair and replacement materials mainly include calcium-phosphorus-based biomaterials and calcium-silicon-based biomaterials. Among them, the research on calcium-phosphorus-based biomaterials has a long history. Past studies have found that hydroxyapatite has good bioactivity among calcium-phosphorus-based materials, but poor biodegradability, while β-tricalcium phosphate biomaterials have good biodegradability but low bioactivity. In recent years, calcium-silicon-based biomaterials such as bioactive glass and calcium silicate have attracted more and more attention due to their excellent bioactivity and degradability. In addition to the composition of the material, the structure of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/626C04B35/22C04B35/447
Inventor 常江林开利
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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