Bioactive Borate Glass Synthesis via Freeze-Dried Sol-Gel Processing

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Solution Overview

Problem

Existing methods for producing bioactive borate glasses using the sol-gel technique are complex, require protective atmospheres, and are difficult to scale due to lengthy and uncontrollable sol aging and wet gel aging and drying processes, limiting their industrial applicability.

Innovation Solution

A method involving precursor mixing, freezing, freeze-drying, and controlled thermal treatment to produce bioactive borate glasses, eliminating sol aging and wet gel aging and drying stages, allowing precise control and scalability.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If traditional sol-gel method with sol aging and wet gel aging and drying steps is used, then bioactive borate glasses can be produced, but the synthesis time is excessively long and the process is difficult to control

Engineering Contradiction:
Improvecontrol of synthesis processVSAvoidsynthesis time
Core Design Contradiction:
Manufacturing precisionVSLoss of time

Solution Approach 1:

The patent utilizes freezing and freeze-drying phase transitions to replace the traditional sol aging and wet gel aging and drying steps. By freezing the sol at -10 to -196°C and then freeze-drying, the process achieves the same chemical transformation goals but in a controlled, time-efficient manner without requiring lengthy aging periods

Inventive Principle:
Principle #36Phase transitions

Solution Approach 2:

The patent changes the temperature parameter dramatically by introducing freezing temperatures (-10 to -196°C) and controlled heating rates (1.5 to 3°C/min), replacing the traditional ambient temperature aging process. This parameter change enables precise control over the synthesis process while significantly reducing the time required

Inventive Principle:
Principle #35Parameter changes

2Reliability

If traditional sol-gel method is used, then bioactive borate glasses can be produced, but the process requires protective atmospheres and is complex to scale

Engineering Contradiction:
Improverepeatability of synthesisVSAvoidprocess complexity
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The patent extracts and eliminates the need for protective atmospheres from the synthesis process. By using freezing and freeze-drying followed by controlled heating in air, the process removes the complexity of maintaining inert or controlled atmospheric conditions while maintaining high repeatability and reliability of the synthesis

Inventive Principle:
Principle #2Taking out (Extraction)

3Manufacturing precision

If traditional sol-gel method with lengthy aging and drying steps is used, then bioactive borate glasses can be produced, but the process is difficult to scale to industrial production

Engineering Contradiction:
Improveprecision of glass compositionVSAvoidscalability to industrial production
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The patent performs preliminary action by freezing the sol before drying, which pre-structures the material in a way that maintains composition precision during subsequent processing. This preliminary freezing step enables the process to be scaled to industrial production while maintaining the precision of glass composition, as the frozen structure preserves the precursor distribution during freeze-drying and heating

Inventive Principle:
Principle #10Preliminary action

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

The method significantly shortens synthesis time, ensures high repeatability, and enables the production of amorphous borate glasses with controlled composition and properties, suitable for medical applications, including bone and soft tissue regeneration, angiogenesis, and antibacterial properties.

Implementation Method 1

freezing the sol obtained in step a) in a temperature from -10 to -196 °C

Methodology Applied
Scientific EffectFreezing: Freezing

Implementation Method 2

freeze-drying to obtain an aerogel

Methodology Applied
Scientific EffectFreeze-drying: Freeze Drying

Implementation Method 3

heating the aerogel at a speed ranging from 1,5 to 3 °C/min up to a temperature ranging from 100 to 150 °C

Methodology Applied
Scientific EffectHeating: Heating

Data Source

PatentEP4574784B1A method for producting bioactive borate glasses
Publication Date: 2026.05.20 ACAD GORNICZO HUTNICZA IM STANISLAWA STASZICA
  • EP4574784B1 patent drawingFigure 1a~1b
  • EP4574784B1 patent drawingFigure 2a~2d
  • EP4574784B1 patent drawingFigure 3a~3d

AI summary

The invention relates to a method for producing bioactive borate glasses, comprising the following steps: a) mixing of precursors of B2O3, CaO, Na2O and P2O5 in a solvent for 12-48 hours, in a temperature from 20 to 40°C, to obtain a sol; b) freezing the sol obtained in step a) in a temperature from -10 to -196 °C, and then freeze-drying to obtain an aerogel; c) grinding the aerogel obtained in step b) and sieving through a sieve with a mesh size of 40-100 µm; d) heating the aerogel sieved in step c) according to the following temperature treatment scheme: - heating the aerogel at a speed ranging from 1,5 to 3 °C/min up to a temperature ranging from 100 to 150 °C; - maintaining the aerogel in a temperature ranging from 100 to 150 °C, over time from 24 to 72 hours; - heating the aerogel at a speed ranging from 1,5 to 3 °C/min, up to a temperature ranging from 400 to about 600 °C; - maintaining the aerogel in a temperature ranging from 400 to about 600 °C, over time from 1,5 to 6 hours; - free cooling of the furnace.