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

A technology of tricalcium phosphate and composite powder, which is applied in the field of biomedical materials, can solve the problems of cumbersome washing, complexity, and long time, and achieve the effect of simple and easy preparation process, controllable composite ratio, and uniform composite degree

Inactive Publication Date: 2007-10-24
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
This method for preparing powder also has the following disadvantages: first, before preparing the composite powder, it is necessary to prepare a well-dispersed β-tricalcium phosphate powder, otherwise it will cause uneven mixing of the prepared composite powder, And affect the mechanical strength of the ceramic sintered body; second, the preparation of β-tricalcium phosphate powder also needs to go through processes such as precipitation, aging, multiple times of full washing, filtration, and drying, and then in the suspension of β-tricalcium phosphate powder After the calcium silicate powder is precipitated in the liquid, the same process of precipitation, aging, multiple times of full washing, filtration, and drying must be carried out again; third, due to the precipitation in the suspension of β-tricalcium phosphate powder Calcium silicate powder is generated and compounded with the β-tricalcium phosphate powder in the suspension at the same time. Due to the conventional stirring process conditions, the two components of β-tricalcium phosphate and calcium silicate will not be uniform. The shortcomings of composites, which further affect the mechanical strength of ceramic sintered bodies; Fourth, when preparing composite ceramics, sintering is carried out at 1300-1400 ° C, which is much higher than the sintering temperature of calcium silicate and β-tricalcium phosphate , and inevitably lead to the transformation of all the phases of the β-tricalcium phosphate component into the α-tricalcium phosphate phase. As already described above, the rapid degradation rate of α-tricalcium phosphate also limits the use of this type of material in Clinical application; Fifth, due to the uneven composite degree of the powder, poor sintering activity, phase transition caused by high temperature during sintering, etc., the mechanical strength of the prepared composite ceramics is not good, which affects more Wide range of clinical applications, especially limited in occasions with high mechanical load requirements
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 requirements of the material are very high, so the ball milling mixing process is a non-ideal technology for preparing biological materials

Method used

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

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Experimental program
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Effect test

Embodiment 1

[0031] Take 216.05 grams of Ca(NO 3 ) 2 4H 2 O was dissolved in deionized water to prepare a 0.5mol / L aqueous solution, and adjusted to pH=11 with 1:1 ammonia water, and 122.50 grams of Na 2 SiO 3 9H 2 O and 42.60 g of (NH 4 ) 2 HPO 4 Dissolve in deionized water to prepare a 0.5 mol / L aqueous solution, and adjust pH=11. The above Ca(NO 3 ) 2 solution added to Na 2 SiO 3 and (NH 4 ) 2 HPO 4 In the mixed solution, the pH value of the reaction system was maintained at 11 with 1:1 ammonia solution during the feeding process, and the stirring was continued for 24 hours after the addition, filtered and washed to obtain a wet powder, and the wet powder was dried at 80°C for 12 hours to obtain The dry powder is calcined at 800°C for 2 hours to obtain a uniform composite calcium silicate / β-tricalcium phosphate composite powder with a mass percentage of 50:50. The morphology of the prepared composite powder is shown in Figure 2A, and the size is about 80-100 nanometers; t...

Embodiment 2

[0033] The raw materials used are as described above.

[0034] Take 216.05 grams of Ca(NO 3 ) 2 4H 2 O was dissolved in deionized water to prepare a 2.0mol / L aqueous solution, and adjusted to pH=11 with 1:1 ammonia water, and 122.50 grams of Na 2 SiO 3 9H 2 O and 42.60 g of (NH 4 ) 2 HPO 4 Dissolve in deionized water to prepare a 2.0 mol / L aqueous solution, and adjust the pH to 11 with 1:1 ammonia water. The above Ca(NO 3 ) 2 solution added to Na 2 SiO 3 and (NH 4 ) 2 HPO 4 In the mixed solution, the pH value of the reaction system was maintained at 11 with a 1:1 ammonia solution during the feeding process, and the stirring was continued for 36 hours after the addition, filtered and washed to obtain a wet powder, and the wet powder was dried at 80°C for 12 hours to obtain The dry powder is calcined at 1000° C. for 2 hours to obtain a uniform composite calcium silicate / β-tricalcium phosphate composite powder with a mass percentage of 50:50. The morphology of the...

Embodiment 3

[0036] The raw materials used are as described above.

[0037] Take 226.04 grams of Ca(NO 3 ) 2 4H 2 O is dissolved in deionized water and prepared as a 0.5mol / L aqueous solution, and adjusted to pH=11 with aqueous sodium hydroxide solution, and 24.50 grams of Na 2 SiO 3 9H 2 O and 76.68 g of (NH 4 ) 2 HPO 4 Dissolve in deionized water to prepare a 0.5 mol / L aqueous solution, and adjust to pH=11 with aqueous sodium hydroxide solution. The above Ca(NO 3 ) 2 solution added to Na 2 SiO 3 and (NH 4 ) 2 HPO 4 In the mixed solution, the pH of the reaction system was maintained at 11 with sodium hydroxide aqueous solution during the feeding process, and the stirring was continued for 12 hours after the addition, filtered and washed to obtain a wet powder, and the wet powder was dried at 80°C for 12 hours to obtain a dry powder. The dry powder was calcined at 800° C. for 1 hour to obtain a uniform composite calcium silicate / β-tricalcium phosphate composite powder with a...

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Abstract

The invention relates to a method of preparing composite powder of calcium metasilicate / beta-tricalcium phosphate by in-situ chemical precipitation, belonging to biomedical material field; which is characterized by: take calcium nitrate, mammonium phosphate dibasic and sodium silicate as raw material; prepare settled miscible liquids of mammonium phosphate dibasic and sodium silicate, calcium nitrate liquids, adjust the pH to 10-12; add the calcium nitrate liquids drop by drop into the miscible liquids of mammonium phosphate dibasic and sodium silicate to occur in-situ chemical precipitation, settle metasilicate and beta-tricalcium phosphate through one-step chemical reaction at the same time to accomplish the even composition of said two component and produce composite powder of calcium metasilicate / beta-tricalcium phosphate. The crystal size of composite powder of calcium metasilicate / beta-tricalcium phosphate produced in said invention could be controlled between 50 nanometers and 2 micrometres following the preparing technique; said invention is characterized by: preparing technique is easy to accomplish and convenient to spread with less preparing operating steps and lower cost, etc.

Description

technical field [0001] The invention relates to a method for preparing calcium silicate / β-tricalcium phosphate composite powder by an in-situ chemical precipitation method, and 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, calcium-phosphorus-based biomaterials have a long history. Previous studies have found that hydroxyapatite in calcium-phosphorus-based materials has better bioactivity but poor degradability, while β-tricalcium phosphate biomaterials have better degradability but low bioactivity. In recent years, calcium-silicon-based biomaterials such as bioactive glass and calcium silicate materials have attracted more and more attention due to their excellent bioactivity and degradability. In addition to the composition of the material, the structure of the material, the...

Claims

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Application Information

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Patent Type & Authority Patents(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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