Sulphur-Free Anti-Stokes Crystals via Sol-Gel Synthesis
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Solution Overview
Problem
Existing anti-Stokes crystals based on yttrium and gadolinium oxysulphides, doped with rare earths, pose issues due to the release of sulphur compounds, non-uniform particle size, high cost of ultra-pure metal oxides, and limited production flexibility, making them unsuitable for various applications.
Innovation Solution
A crystalline material with the formula We1(We2)Ta(Do1Do2)HalO(x)Te(y)Se(z), doped with rare earth elements like erbium, ytterbium, and thulium, produced through sol-gel or hydro processes, eliminating sulphur and enabling uniform crystal formation for enhanced luminescence.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Ease of manufacture
If solid-phase synthesis is used to produce anti-Stokes crystals, then the crystals can be manufactured, but sulphur compounds are released causing odour and physiological harm
Solution Approach 1:
The invention extracts and removes sulphur from the crystal composition entirely. The new crystal structure uses oxide materials (yttrium oxide, gadolinium oxide) instead of oxysulphides, completely eliminating the source of harmful sulphur compound release while maintaining the anti-Stokes luminescence properties.
Solution Approach 2:
The invention changes the chemical composition parameters by replacing sulphur-containing compounds with sulphur-free oxide materials. This parameter change transforms the crystal from containing reactive sulphur groups to stable oxide structures, eliminating harmful emissions while preserving optical functionality.
2Ease of manufacture
If solid-phase synthesis is used, then crystals can be produced, but uniform particle size is not achieved
Solution Approach 1:
The invention applies preliminary action by using sol-gel processing to pre-form uniform nanoscale precursors before final crystal formation. This preliminary structuring at the molecular level ensures uniform nucleation and growth, resulting in monodisperse crystal particles with controlled size distribution.
Solution Approach 2:
The invention utilizes phase transitions in the sol-gel process, transitioning from sol to gel state, then through controlled drying and calcination phases. These sequential phase transitions enable precise control over crystal formation, particle size, and uniformity that cannot be achieved through conventional solid-phase synthesis.
3Length of moving object
If crystals are ground to achieve small sizes, then small crystal particles can be obtained, but the crystals are broken down and quantum yield drops
Solution Approach 1:
The invention performs preliminary action by controlling crystal growth at the nanoscale during synthesis rather than attempting to reduce larger crystals afterward. This top-down approach of growing small uniform crystals directly prevents mechanical damage and maintains structural integrity, preserving high quantum yield.
Solution Approach 2:
The invention replaces the mechanical grinding process with a chemical synthesis approach. Instead of mechanically crushing crystals (which causes damage), the sol-gel process chemically forms crystals at the desired small size from molecular precursors, eliminating mechanical stress and preserving crystal perfection.
4Manufacturing precision
If ultra-pure metal oxides with 5-nine grade purity are used, then high purity crystals can be produced, but the cost increases and availability decreases
Solution Approach 1:
The invention applies preliminary purification through the sol-gel process itself, which forms a homogeneous gel matrix that incorporates impurities. Subsequent controlled calcination removes these impurities, achieving high purity crystals from lower purity starting materials, thus reducing the need for expensive ultra-pure reagents.
Solution Approach 2:
The gel matrix acts as an intermediary that facilitates purification. The gel structure traps and concentrates impurities during formation, and the controlled thermal treatment of the gel selectively removes these impurities, enabling high purity crystal production from more readily available, lower cost precursor materials.
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 new crystalline material is free of sulphur, allows for the production of uniform crystals of varying sizes, and improves luminescence performance, making it suitable for marking agents in diverse applications without the limitations of previous technologies.
Implementation Method 1
When excited with IR radiation of a particular wavelength, they exhibit distinct luminescence
Implementation Method 2
Pang et al., Material Letters, 2008, 62, 2500 discloses up-conversion luminescence of trivalent-rare-earth ion-doped LnTaO 4 materials
Implementation Method 3
heating a mixture produced in step c) to a temperature of 50-150° C, preferably 60-120° C, to form a gel
Implementation Method 4
heating the gel to a temperature of at least 175° C, preferably in a furnace, to convert the gel into a powder
Implementation Method 5
annealing the powder obtained in step e) at a temperature of at least 500° C, preferably 500-2,000° C
Implementation Method 6
a crystalline material comprising a basic crystal based on at least one host element
Data Source
AI summary
The present invention relates to a crystalline material comprising a basic crystal based on at least one host element (We), which basic crystal is doped with at least one element of the rare earths (Do), the crystalline material having the formula: We1(a)We2(b)Ta(c)Do1(d)Do2(e)Hal(w)O(x)Te(y)Se(z), where We1 and We2 are independently and differently selected from elements from the group consisting of niobium, aluminium, scandium, barium, gadolinium, lanthanum, yttrium, cerium, calcium and titanium; Do1 and Do2 are independently and differently selected from elements of the group of rare earths; Hal is fluoride, chloride, bromide or iodide; the indices (a)-(z) each being 0 to 3 independently of one another, though at least one of (a) and (b) is greater than 0, at least one of (d) and (e) is greater than 0, and at least one of (w), (x), (y) and (z) is greater than 0; wherein the sum of (a)+(b)+(c)=1-2, preferably 1 or 2, and the sum of (w)+(x)+(y)+(z)=2-3, preferably 2 or 3, with the proviso that (c) is > 0 if - We1 = Ca, We2 = Sc, Do1 = Yb or Tm and (e)=(w)=(y)=(z)=0, or - We1 = Ce, Do1 = Eu or Er and (b) = (e) = (w) = (y) = (z) = 0, wherein (x) is >0.