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Method for in situ growth for preparing nano-composite material of carbon nano-tube and hydroxyapatite

A nano-composite material and hydroxyapatite technology, which is applied in the field of nano-composite material preparation, can solve the problems of high price, affect the mechanical properties of HA/CNT composite materials, low crystallinity, etc., and achieve uniform distribution and good biological safety. , the effect of improving dispersion

Inactive Publication Date: 2011-07-27
SOUTHWEST JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method uses a surfactant to treat the CNT powder surface, it can improve its dispersion in the HA matrix to a certain extent; however, the composite material prepared by this method has a low crystallinity due to the deposition of HA, which affects The mechanical properties of the HA / CNT composite
Moreover, both preparation methods require commercially available nanoscale CNT powders, which are expensive

Method used

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  • Method for in situ growth for preparing nano-composite material of carbon nano-tube and hydroxyapatite
  • Method for in situ growth for preparing nano-composite material of carbon nano-tube and hydroxyapatite
  • Method for in situ growth for preparing nano-composite material of carbon nano-tube and hydroxyapatite

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Experimental program
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specific Embodiment approach

[0031] A kind of specific embodiment of the present invention is:

[0032] A method for preparing carbon nanotubes and hydroxyapatite nanocomposites by in-situ growth, the specific method is:

[0033] a. Wet synthesis of hydroxyapatite solution to prepare calcium nitrate solution with calcium ion concentration of 0.835mol / L, adjust its pH value to 12 with ammonia water; prepare diammonium hydrogen phosphate solution with phosphate ion concentration of 0.50mol / L , the molar ratio of calcium and phosphorus is 1.67: 1, under stirring, the diammonium hydrogen phosphate solution is dripped in the calcium nitrate solution with a titration rate of 3ml / min, and reacts. The reaction temperature is room temperature, and the reaction is adjusted with ammonia water simultaneously. The pH value at the time was 12; after the titration was completed, it was allowed to stand for aging for 24 hours to obtain a hydroxyapatite slurry solution.

[0034] b, adding metal salts In the hydroxyapatit...

Embodiment 2

[0039] The method in this example is basically the same as the method in Embodiment 1, the difference is:

[0040] (1) in a step, the calcium ion concentration is 0.01mol / L, and the phosphate ion concentration is 0.01mol / L, and the rate of addition is 10ml / min, and the pH of adjusting the reaction solution with sodium hydroxide is 14, and the reaction temperature is 80 ℃.

[0041] (2) In step b, when the mixed liquid is filtered, the suction filtration method is used to filter (the suction filtration method is faster than the filtration); and the hydroxyapatite powder containing metal salts is first sintered to form a hydroxyapatite matrix and sintered The specific method of treatment is: raise the temperature from room temperature to 1100°C at a heating rate of 3°C / min, keep it warm for 2 hours, and then cool it down naturally.

[0042] (3) When growing carbon nanotubes in situ by step c chemical vapor deposition, when the temperature rises to 780°C at a rate of 5°C / min, hyd...

Embodiment 3

[0045] The method in this example is basically the same as that in Example 1, the difference is:

[0046] (1) The metal salt-containing hydroxyapatite powder prepared in step b is first subjected to porous forming treatment by an organic foam coating method. That is: the HA powder containing metal salt prepared in step b is coated on the polymer organic foam, dried and sintered at 300°C for 2 hours, and the polymer foam is fully burned to form a porous HA scaffold. Then sinter the HA scaffold, raise the temperature from room temperature to 1200°C at a rate of 5°C / min, keep it warm for 2 hours, and then cool it naturally to obtain the HA matrix. (2) When growing carbon nanotubes in situ by chemical vapor deposition, ethylene gas is used as the carbon source gas.

[0047] The CNT / HA composite material prepared by the method in this example is mainly composed of HA crystals and CNT crystals. The grain size of HA is about 63nm, the diameter of CNT is about 100nm, and the growth c...

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Abstract

The invention discloses a method for preparing a carbon nano tube and hydroxylapatite nanocomposite material by root position growth. The specific preparation method comprises the steps as follows: a. the hydroxylapatite slurry solution is synthesized by a wet method; b. metal salt is added: under the stirring by magnetic force, one or more than one compound in metal salts of iron, magnesium, cobalt or nickel are addedin the solution of step a, filtering is carried out, the PH value is regulated to be neutrality, and dryness is carried out; c. root position growth of carbon nano tube: the powder in step b is put into the tube-type furnace, the temperature is increased as 5-10 DEG C / min to 780 DEG C-800 DEG C, and the gas of nitrogen or argon is inlet; after the temperature is raised, hydrogen is inlet for deoxidization for 1-2 hours, the temperature is increased to 700 DEG C-1200 DEG C again, gaseous substance containing carbon is inlet and kept for 1-2 hours; the temperature is lowered to room temperaturein the gas of nitrogen or argon. The compound material and the carbon nano tube prepared by the method has the advantages that the distribution in hydroxylapatite is even, the combination of interfaces between the compound material and the carbon nano tube is good, the purity of the carbon nano tube is high, and the nanometer structure is kept completely.

Description

technical field [0001] The invention relates to the preparation of nanocomposite materials, in particular to a preparation method of carbon nanotube and hydroxyapatite nanocomposite materials. Background technique [0002] The chemical formula of hydroxyapatite (hydroxyapatite, HA) is Ca 10 (PO 4 ) 6 (OH) 2 , is the main inorganic component of human bone tissue and teeth, has good biocompatibility and osteogenic activity, and can form a tight combination with human tissue in a short period of time after being implanted in the human body, so it has become a modern bone repair and replacement field. Recognized as a good bone replacement biomaterial. However, HA is brittle and has low strength, which limits its clinical application to a large extent. In order to improve its mechanical properties, a variety of hydroxyapatite-based composite materials have been developed. As a new nanoscale material, carbon nanotubes (CNT) have excellent mechanical properties, electrical pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61L27/42A61L27/12A61L27/08
Inventor 卢晓英翁杰
Owner SOUTHWEST JIAOTONG UNIV