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Method for preparing transparent calcium phosphate bioceramics by normal-pressure sintering under atmosphere protection

A technology of transparent calcium phosphate and bioceramics, applied in the field of biomedical materials, can solve the problems of increasing production costs, large equipment investment, and high production costs, and achieve the effects of mass production, small equipment investment, and short production cycles.

Active Publication Date: 2020-02-21
SUZHOU DINGAN ELECTRONICS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method needs to be pre-sintered first, and then sintered by hot isostatic pressing at 150MPa, 1000-1100°C. Ar-20vol%O is used in the sintering process. 2 Mixed gas protection, not only the sintering process is cumbersome, but also the investment in equipment is large, and mass production cannot be realized
CN1793022 has announced a kind of preparation method of transparent β-tricalcium phosphate bioceramics material, and this method has obtained dense and transparent β-tricalcium phosphate bioceramics by spark plasma sintering technology, but still needs to adopt pressure-assisted sintering in the sintering process of this method
At the same time, this method requires a special graphite mold, which not only has high production costs, but also cannot achieve mass production
[0007] It can be seen that traditional hot pressing sintering, hot isostatic pressing sintering, microwave sintering and pulse current sintering technologies often require sintering under special conditions such as vacuum, argon, nitrogen atmosphere or electric pulse, pressure assist and microwave. High investment and technical requirements not only make it impossible to achieve mass production, but also greatly increase the difficulty of the process and increase the production cost

Method used

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  • Method for preparing transparent calcium phosphate bioceramics by normal-pressure sintering under atmosphere protection
  • Method for preparing transparent calcium phosphate bioceramics by normal-pressure sintering under atmosphere protection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] (100wt% β-TCP+0wt% HA) transparent calcium phosphate bioceramics

[0051] Weigh and measure 100wt% high-purity nano-β-TCP powder and ball mill it for pulping and spray granulation, put the granulated powder into the mold, pre-press molding at 20MPa, and then cold isostatic pressing molding at 250MPa, and the molded billet The body was sintered in a box-type electric furnace. The sintering system is: 2°C / min to 550°C for 2 hours, then 10°C / min to 820°C for 5 hours, then 10°C / min to 950°C for 10 hours, and finally 2°C / min The temperature was lowered to 600° C. and then naturally cooled to room temperature to prepare a β-TCP single-phase transparent calcium phosphate bioceramic with an average grain size of 235 nm and a relative density of 99.5%. The light transmittance is 95%, and the bending strength is 178MP.

Embodiment 2

[0053] (0wt% β-TCP+100wt% HA) transparent calcium phosphate bioceramics

[0054] Weigh the measured 100wt% high-purity nano-HA powder and ball mill it for slurrying and spray granulation, put the granulated powder into the mold, pre-press molding at 30MPa and then cold isostatic pressing at 280MPa, place the green body after molding Sintered in a box-type electric furnace. The sintering system is: 2°C / min heating up to 550°C for 2 hours, then heating up to 700°C at a rate of 15°C / min. ℃ for 5 hours, then heated at 15℃ / min to 1250℃ for 1 hour, and finally cooled to 600℃ at 4℃ / min, stopped feeding deionized water, and cooled naturally to room temperature to prepare HA single-phase hyaluronic acid Calcium bioceramics, the average grain size is 156nm, and the relative density is 99.5%. The light transmittance is 92%, and the bending strength is 125MP.

Embodiment 3

[0056] (10wt% β-TCP+90wt% HA) transparent calcium phosphate bioceramic

[0057] 90wt% high-purity nano-HA and 10wt% high-purity nano-β-TCP powder are mixed and ball milled for slurrying and spray granulation. The granulated powder is put into the mold, pre-pressed at 40MPa and then subjected to 300MPa cold isostatic Press molding, put the formed green body in a box-type electric furnace for sintering. The sintering system is: 2°C / min to 550°C for 2 hours, and then 20°C / min to 700°C, then pour deionized water at a rate of 4ml / min, and continue to heat up to 1000°C for 8 hours, and then Raise the temperature at a rate of 15 °C / min to 1250 °C for 4 hours, and finally cool down to 600 °C at a rate of 3 °C / min. Phase transparent calcium phosphate bioceramics, wherein the average grain size of the β-TCP phase is 360nm, the average grain size of the HA phase is 260nm, and the relative density is 99.5%. The light transmittance is 90%, and the bending strength is 135MP.

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Abstract

The invention provides a method for preparing transparent calcium phosphate bioceramics by normal-pressure sintering under atmosphere protection, and belongs to the technical field of biomedical materials. According to the method, high-purity nano hydroxyapatite (HA) and / or high-purity nano beta-tricalcium phosphate (beta-TCP) powder are taken as raw materials, no sintering auxiliary agent is added, steam is adopted for protection, and the transparent calcium phosphate biological ceramic with light transmittance of 50-95% can be obtained by multi-step normal pressure sintering under a condition of atmospheric pressure. The phase composition of the transparent calcium phosphate bioceramic is an HA single phase, a beta-TCP single phase or a HA / beta-TCP two-phase mixture. The method has simple process, small equipment investment and short production period, and can meet requirements of batch production. The obtained transparent calcium phosphate bioceramic has the advantages that relativedensity is more than 99.5%, crystal grains are uniform and fine, no impurity phase exists, and mechanical strength is high. The transparent calcium phosphate bioceramic can be used as a good matrix material for observing interaction among cells, tissues and calcium phosphate bioceramic, and can also be used in repair fields of tooth roots, dental pulp, artificial eyes and the like.

Description

technical field [0001] The invention relates to the technical field of biomedical materials, in particular to a method for preparing transparent calcium phosphate bioceramics by sintering under atmospheric protection and normal pressure. Background technique [0002] Hydroxyapatite (HA), β-tricalcium phosphate (β-TCP) and hydroxyapatite / β-tricalcium phosphate biphase composite ceramics (Biphase Calcium Phosphate, BCP for short) have excellent biocompatibility and can be It conducts bone cell regeneration quickly, and can directly bond with bone without passing through an intermediate medium. As a good biological hard tissue filling, repairing and replacing material, it has been widely used in clinical practice. [0003] When calcium phosphate bioceramics with certain light transmission properties are used as cell culture substrates, the biological properties such as cell growth, proliferation and differentiation can be directly observed in real time by using a transmission o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/447C04B35/622C04B35/626C04B35/638
CPCC04B35/447C04B35/622C04B35/62605C04B35/62695C04B35/638C04B2235/6562C04B2235/6565C04B2235/6567C04B2235/786C04B2235/661C04B2235/96C04B2235/9653
Inventor 徐传艳李亚东朱阳光李亚军
Owner SUZHOU DINGAN ELECTRONICS TECH
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