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A method for preparing transparent calcium phosphate bioceramics by sintering under atmospheric pressure

A technology of transparent calcium phosphate and bioceramics, applied in the field of biomedical materials, can solve the problems of cumbersome sintering process, increase production cost, and large equipment investment, avoid decomposition and formation of impurity phases, meet mass production, and reduce equipment investment. Effect

Active Publication Date: 2022-04-29
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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  • A method for preparing transparent calcium phosphate bioceramics by sintering under atmospheric pressure
  • A method for preparing transparent calcium phosphate bioceramics by sintering under atmospheric pressure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[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 sintering under atmospheric pressure under the protection of atmosphere, which belongs to the technical field of biomedical materials. The present invention uses high-purity nano-hydroxyapatite (HA) and / or high-purity nano-β-tricalcium phosphate (β-TCP) powder as raw materials, does not add any sintering aids, and adopts water vapor protection, under atmospheric pressure conditions , The transparent calcium phosphate bioceramics with a light transmittance of 50-95% is obtained by sintering under normal pressure in sections. The phase composition of the transparent calcium phosphate bioceramic is HA single-phase, β-TCP single-phase or HA / β-TCP two-phase mixture. The invention not only has simple process, small equipment investment, short production cycle, and can meet the requirements of mass production, but also obtains a transparent calcium phosphate bioceramic with a relative density greater than 99.5%, uniform and fine crystal grains, no impurity phase, and high mechanical strength , can be used as a good matrix material to observe the interaction between cells, tissues and calcium phosphate bioceramics, and can also be used in the restoration fields of tooth roots, dental pulp and artificial eyes.

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 Patents(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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