Ultra-high densification of ZnS for nano-grain optical windows
View Patent ↗A method is provided for producing an article which is transparent to infrared radiation. The method includes the steps of (a) disposing a plurality of nanoparticles on a substrate, wherein said nanoparticles comprise a metal sulfide or a metal selenide; (b) subjecting the nanoparticles to spark plasma sintering, thereby producing a sintered product; and (c) removing the sintered product from the substrate as a self-supporting mass.
1. A process for producing mechanically stable, infra-red and visible light transmissive ZnS disc, comprising:
disposing ZnS nano-particles between two conductive electrodes kept under vacuum inside a chamber;
said nano-particles being subjected to programmed DC plasma treatment that impresses pulse DC current at the start of process and continuous DC current thereafter, resulting in heating of nano-particle;
said chamber being heated gradually and taken through a programmed thermal and pressure cycle;
said thermal cycle and pressure cycle having a temperature increase rate in the range of 60° C./min to 90° C./min and pressure in the range of 70 MPa to 120 Mpa;
said nano-particles being subjected to thermal annealing at the end of pulsed DC plasma treatment resulting in a rigid ZnS planar disc having densely packed ZnS particles with large grain sizes greater than 220 nm;
said ZnS disc being coated with optical anti-reflective coating followed by a protective coating and thus ready for use in various infra-red window applications.
2. The process according to claim 1 wherein the size of ZnS nano-particles prior to the process is in the range of 30 to 50 nm.
3. The process according to claim 1 wherein the said ZnS disc contains ZnS nano-particles whose grain size, after the process is in the range of 220 to 500 nm.
4. The process according to claim 1 wherein the said ZnS disc is used in applications such as infra-red cameras, infra-red sensors, thermal imagers, Fresnel lenses, Fighter Aircraft infra-red windows.
5. The process according to claim 1 wherein the said programmed thermal cycle has a temperature increase rate of 60° C./min up to 450° C. and again with 60° C./min up to 600° C. with applied pressure of 70 Mpa.
6. The process according to claim 1 wherein the said programmed thermal cycle has a temperature increase rate of 90° C./min in up to 600° C. and again with 90° C./min up to 750° C. with applied pressure of 120 Mpa.