Hydrated Calcium Silicate Nano-Film via Magnetron Sputtering

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Solution Overview

Problem

Current methods for preparing nano-films of cement-based materials, such as hydrated calcium silicate (C—S—H), lack the ability to effectively control film size and purity, and often require complex and expensive equipment, limiting their application in microscale property investigation.

Innovation Solution

A method involving the synthesis of C—S—H powder with a specific calcium to silicon ratio, followed by calcination and pressing, then using magnetron sputtering to deposit a nano-film on a substrate, with controlled sputtering parameters to achieve a uniform and pure C—S—H nano-film, which is subsequently soaked in a calcium hydroxide solution to enhance hydration.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If physical vapor deposition or chemical vapor deposition methods are used to prepare nano-films, then uniform and dense nano-films can be obtained, but the equipment is complex and expensive

Engineering Contradiction:
Improveuniformity and density of nano-filmVSAvoidcomplexity and cost of equipment
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent replaces complex vapor deposition systems with a magnetron sputtering apparatus, which uses magnetic field and plasma to deposit C-S-H nano-film. This substitution maintains film quality while using more conventional and accessible equipment, reducing system complexity and cost.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

Solution Approach 2:

The patent optimizes sputtering parameters including magnetron power (50-200 W), argon flow rate (10-100 sccm), chamber pressure (0.5-2.5 Pa), and substrate temperature (20-100°C) to achieve uniform and dense C-S-H nano-film deposition, matching the quality of vapor deposition methods.

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If conventional nano-film preparation methods are used, then nano-films can be produced, but the size and purity of the film are difficult to control

Engineering Contradiction:
Improvesize control and purity of nano-filmVSAvoiddifficulty in controlling film properties
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The patent introduces a rotating substrate holder that rotates the substrate during sputtering at controlled speeds (5-50 rpm). This dynamic rotation ensures uniform deposition across the substrate surface, improving size control and film uniformity while maintaining ease of operation.

Inventive Principle:
Principle #15Dynamics

Solution Approach 2:

The patent uses a magnetron sputtering system with magnetic field and plasma as intermediaries to deposit C-S-H nano-film. This intermediary process allows precise control over film thickness, uniformity, and purity by adjusting sputtering parameters, making the manufacturing process more controllable.

Inventive Principle:
Principle #24Intermediary (Mediator)

3Manufacturing precision

If magnetron sputtering is used to prepare C-S-H nano-film, then controllable size and purity can be achieved, but the sputtering process requires precise parameter control

Engineering Contradiction:
Improvecontrollability of film size and purityVSAvoidprecision required for sputtering parameters
Core Design Contradiction:
Manufacturing precisionVSEase of operation

Solution Approach 1:

The patent includes a pre-sputtering step (5-10 minutes) before actual film deposition. This preliminary action cleans the target surface and stabilizes the sputtering process, reducing the precision required during the main deposition phase and making operation easier.

Inventive Principle:
Principle #16Partial or excessive action

Solution Approach 2:

The patent provides specific parameter ranges for magnetron power (50-200 W), argon flow rate (10-100 sccm), chamber pressure (0.5-2.5 Pa), and substrate temperature (20-100°C). These optimized ranges make the process easier to operate while maintaining precise control over film properties.

Inventive Principle:
Principle #35Parameter changes

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

This method allows for the production of controllable, pure, and uniform C—S—H nano-films, enabling convenient observation and mechanical property testing, while being economical and easily implementable with conventional magnetron sputtering devices.

Implementation Method 1

magnetron sputtering that can be used to prepare uniform and dense nano-films and it is one of the PVD methods that has been widely applied to nano-film deposition and surface coating

Methodology Applied
Scientific EffectMagnetron sputtering: Sputtering

Implementation Method 2

physical vapor deposition method (PVD)

Methodology Applied
Scientific EffectPhysical vapor deposition: Physical Vapour Deposition

Implementation Method 3

injecting argon or helium to the sputtering chamber, wherein a flow rate of the argon or helium is controlled to be 10-100 sccm to keep the pressure in the sputtering chamber at 0.5-2.5 pascal

Methodology Applied
Scientific EffectGas pressure control:

Implementation Method 4

soaking the nano-film obtained in 3) into in a saturated aqueous solution of calcium hydroxide at approximately 25° C. for 1-3 days, to yield a hydrated calcium silicate nano-film

Methodology Applied
Scientific EffectHydration: Hydrates

Data Source

PatentUS11466361B2Method of preparing hydrated calcium silicate nano-film
Publication Date: 2022.10.11 WUHAN UNIV
  • US11466361B2 patent drawing
  • US11466361B2 patent drawing
  • US11466361B2 patent drawing

AI summary

A method of preparing a hydrated calcium silicate (C—S—H) nano-film. The method includes: 1) synthesizing a hydrated calcium silicate powder having a calcium to silicon ratio (Ca/Si) of 0.5-3.0; 2) calcining the C—S—H powder obtained in 1) for 2-3 hours under a temperature of 150-250° C., cooling to approximately 25° C., and pressing the C—S—H powder under a pressure of 100-200 megapascal, to yield a target material; 3) fixing a substrate on a sample table of a magnetron sputtering apparatus, placing the target material obtained in 2) in a target position of the magnetron sputtering apparatus, pre-sputtering the target material for 5-10 minutes, rotating the substrate at a constant speed, sputtering the target material for 30-300 minutes, to yield a nano-film; and 4) soaking the nano-film obtained in 3) into in a saturated aqueous solution of calcium hydroxide at approximately 25° C. for 1-3 days.