阅读说明：本技术 一种生物玻璃的冷等静压烧结制备方法 (Cold isostatic pressing sintering preparation method of bioglass ) 是由 胡春峰 徐强 蒋安娜 索尔沃托瑞·格拉索 于 2020-05-11 设计创作，主要内容包括：一种生物玻璃的冷等静压烧结制备方法,包括以下步骤：步骤1：将作为冷压烧结原料的生物玻璃粉和液相助烧剂混合均匀,得到混合浆料；所述步骤1中使用的生物玻璃粉粒径为20 nm～500nm；生物玻璃粉和液相助烧剂的体积分数比为12:3~8;步骤2：将混合浆料放入模具中后置于冷等静压机中进行冷烧结处理；冷等静压压力为300～500 MPa,保压时间为5～120 min;步骤3：将经过步骤2的混合浆料进行干燥处理;温度为40～60℃,湿度为50%,时间为24～48 h。(A cold isostatic pressing sintering preparation method of bioglass comprises the following steps: step 1: uniformly mixing bioglass powder serving as a cold-pressed sintering raw material and a liquid-phase sintering aid to obtain mixed slurry; the particle size of the bioglass powder used in the step 1 is 20 nm-500 nm; the volume fraction ratio of the bioglass powder to the liquid-phase sintering aid is 12: 3-8, and the step 2: placing the mixed slurry into a mold and then placing the mold into a cold isostatic press for cold sintering treatment; cold isostatic pressure of 300-500 MPa, pressure maintaining time of 5-120 min, step 3: and (3) drying the mixed slurry obtained in the step (2), wherein the temperature is 40-60 ℃, the humidity is 50%, and the time is 24-48 h.)

1. The cold isostatic pressing sintering preparation method of the bioglass is characterized by comprising the following steps of:

step 1: uniformly mixing bioglass powder serving as a cold-pressed sintering raw material and a liquid-phase sintering aid to obtain mixed slurry; the particle size of the bioglass powder used in the step 1 is 20 nm-500 nm; the volume fraction ratio of the bioglass powder to the liquid-phase sintering aid is 12: 3-8;

step 2: placing the mixed slurry into a mold and then placing the mold into a cold isostatic press for cold sintering treatment; the cold isostatic pressure is 300-500 MPa, and the pressure maintaining time is 5-120 min;

and step 3: and (3) drying the mixed slurry obtained in the step (2), wherein the temperature is 40-60 ℃, the humidity is 50%, and the time is 24-48 h.

2. The method as claimed in claim 1, wherein the liquid sintering aid in step 1 is deionized water or NaOH solution.

3. The method for preparing bioglass through cold isostatic pressing sintering according to claim 1, wherein in the step 1, bioglass powder and liquid-phase sintering aid are uniformly mixed through a vortex mixer for 5-100 min.

4. The method for preparing bioglass according to claim 1, wherein the mould in step 2 is a flexible rubber mould.

Technical Field

The invention relates to a cold isostatic pressing sintering preparation method of bioglass, in particular to a cold isostatic pressing sintering preparation method for preparing bioglass with a certain shape by sintering at room temperature.

Background

Bioglass (bioglass) refers to a glass material that performs a specific biological or physiological function. Bioglass research dates back to the end of the last 60's century. Professor Larry l. Hench, university of florida, invented bioglass material first in 1969. Wherein the bioglass has about 45% Na as the main component₂O, CaO 25%, SiO 25%₂And 5% of P₂O₅. If a small amount of K is added₂O、MgO、CaF₂、B₂O₃And other components to obtain a series of practical bioglasses. Because the bioglass has good bioactivity and biocompatibility, the material has no rejection, inflammation and tissue necrosis after being implanted into a human body, can form osseointegration with bones, and has good interface binding capacity and faster osteogenesis. At present, the bioglass material has wide application in medical fields such as medical tissue engineering scaffold materials, orthopedic materials, dental materials, middle ear and drug carrier materials and the like.

Up to now, many sintering methods for producing bioglass are available, such as two-phase sintering, SPS sintering, hydrothermal reaction sintering, and the like. Although the preparation method of the bioglass has good mechanical structure performance, processability and the like. However, in the above sintering preparation process, the biological activity and toxicity of the material are greatly affected in view of the crystallization of the material and the higher sintering temperature. Therefore, the search for a bioglass material with a lower sintering temperature and suitable for 3D forming technology is the direction of research in the field of biomedical materials. The invention relates to a cold isostatic pressing sintering preparation method of bioglass, which is a sintering preparation method capable of realizing efficient low-temperature forming and not destroying bioactivity. The medical biological glass material with complex three-dimensional shape can be made at room temperature. The preparation method not only saves energy and protects the environment, but also has high production efficiency and low cost, and the preparation process undoubtedly has very wide biomedical application prospect.

Disclosure of Invention

The invention provides a cold isostatic pressing sintering preparation method which is simple and convenient in preparation process and low in cost and can prepare a bioglass sample by sintering at room temperature.

In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:

the cold isostatic pressing sintering preparation method of the bioglass is characterized by comprising the following steps of:

step 1: uniformly mixing bioglass powder serving as a cold-pressed sintering raw material and a liquid-phase sintering aid to obtain mixed slurry; the particle size of the bioglass powder used in the step 1 is 20 nm-500 nm; the volume fraction ratio of the bioglass powder to the liquid-phase sintering aid is 12: 3-8;

step 2: placing the mixed slurry into a mold and then placing the mold into a cold isostatic press for cold sintering treatment; the cold isostatic pressure is 300-500 MPa, and the pressure maintaining time is 5-120 min;

and step 3: and (3) drying the mixed slurry obtained in the step (2), wherein the temperature is 40-60 ℃, the humidity is 50%, and the time is 24-48 h.

As a preferable technical scheme, the liquid-phase sintering aid in the step 1 is deionized water or NaOH solution, wherein the concentration of the NaOH solution is 1 mol/L-10 mol/L.

As a preferable technical scheme, in the step 1, the bioglass powder and the liquid-phase sintering aid are uniformly mixed by a vortex mixer, and the mixing time is 5-100 min.

As a preferred technical scheme, the mould in the step 2 is a flexible rubber mould.

As a preferable embodiment, the three-dimensional shape of the flexible rubber mold is not limited, and may be a cylindrical shape, a triangular prism shape, a quadrangular prism shape, a hexagonal prism shape, or the like.

The invention has the beneficial effects that:

(1) the invention adopts deionized water or NaOH solution as the liquid-phase sintering aid, and prepares the bioglass by cold sintering under ultrahigh cold isostatic pressure, and the preparation process is very simple.

(2) The invention can be used for manufacturing the bioglass material with a complex three-dimensional shape. Not only saves energy and protects environment, but also has high production efficiency and low cost, and the preparation process undoubtedly has very wide biomedical application prospect.

Drawings

FIG. 1 is a density chart of bioglass samples prepared in examples 1 to 6 of the present invention.

FIG. 2 is a graph showing Vickers hardness of bioglass samples prepared in examples 1 to 6 of the present invention.

Fig. 3 is an XRD pattern of the bioglass sample and bioglass raw material prepared in example 3 of the present invention.

FIG. 4 is an SEM image of the fracture surface of a bioglass sample prepared in example 3 of the invention.

Fig. 5 is an FTIR-ATR infrared spectrum of a bioglass sample prepared in example 3 of the present invention.

Detailed Description

The invention is further described with reference to the following figures and specific embodiments.