Fabrice Testa, Clémence Coetsier, Emilie Carretier, M. Ennahali, Benoit Laborie, et al.. Reused of Slurry By Membrane Processes for Microelectronic Industry. Water today, 2017, 123, pp.311-320. ⟨hal-01656407⟩ Plus de détails...
Fabrice Testa, Clémence Coetsier, Emilie Carretier, M. Ennahali, Benoit Laborie, et al.. Reused of Slurry By Membrane Processes for Microelectronic Industry. Water today, 2017, 123, pp.311-320. ⟨hal-01656407⟩
Fabrice Testa, Clémence Coetsier, Emilie Carretier, M. Ennahali, B. Laborie, et al.. Recycling a slurry for reuse in chemical mechanical planarization of tungsten wafer: effect of chemical adjustments and comparison between static and dynamic experiments. Microelectronic Engineering, 2014, 113, pp.114-122. ⟨10.1016/j.mee.2013.07.022⟩. ⟨hal-01053254⟩ Plus de détails...
Recycling abrasive slurry that has been used in chemical mechanical polishing (CMP) is one of the options for reducing the cost of manufacturing microchip processors. We use ultrafiltration which is a method of choice to recycle silica (SiO2)-based slurry. Taking into account that the chemical composition of abrasive slurry plays an important role in tungsten CMP (W-CMP), chemical adjustments have to be made so that the concentrated after used slurry can be reused. In this study, we investigate the effects of chemical additives (iron catalyst, oxalic acid as complexing agent and surfactants as stabilizers) in slurry that has been retreated by ultrafiltration. Experiments are conducted both under static and dynamic conditions and results are compared to better understand the effect of chemical adjustments on the main performances of W-CMP. An optimal chemical adjustment is proposed through a design of experiments evaluation to obtain a concentrated after used and chemically adjust slurry comparable to the operational point of use slurry.
Fabrice Testa, Clémence Coetsier, Emilie Carretier, M. Ennahali, B. Laborie, et al.. Recycling a slurry for reuse in chemical mechanical planarization of tungsten wafer: effect of chemical adjustments and comparison between static and dynamic experiments. Microelectronic Engineering, 2014, 113, pp.114-122. ⟨10.1016/j.mee.2013.07.022⟩. ⟨hal-01053254⟩
Clémence Coetsier, Fabrice Testa, Emilie Carretier, M. Ennahali, B. Laborie, et al.. Static dissolution rate of tungsten film versus chemical adjustments of a reused slurry for chemical mechanical polishing. Applied Surface Science, 2011, 257 (14), pp.6163-6170. ⟨10.1016/j.apsusc.2011.02.023⟩. ⟨hal-01026413⟩ Plus de détails...
Tungsten is widely used as deposited layer for the multi-level interconnection structures of wafers. The chemical composition of abrasive slurry plays an important role in chemical mechanical polishing (CMP) process. Removal of tungsten is driven by complex oxidation mechanisms between slurry components. The slurry for tungsten CMP generally contains oxidizer, iron catalyst, complexing agents and stabilizers in a pH adjusted solution of abrasive particles. Interaction between iron complex and H2O2 in the slurry is the main factor governing the chemical mode of material removal, oxidation potencies and kinetics. In this study, we investigate the effects of chemical additives in silica (SiO2)-based slurry on the removal rate of the tungsten film. Experiments were carried out in static batch as a preliminary study to understand and optimize chemical mechanisms in CMP-Tungsten process. Experiment designs were conducted to understand the influence of the chemical additives on the main performances of W-CMP. Used slurry, concentrated and retreated with chemical adjustments, is compared to the original slurry as a reference.
Clémence Coetsier, Fabrice Testa, Emilie Carretier, M. Ennahali, B. Laborie, et al.. Static dissolution rate of tungsten film versus chemical adjustments of a reused slurry for chemical mechanical polishing. Applied Surface Science, 2011, 257 (14), pp.6163-6170. ⟨10.1016/j.apsusc.2011.02.023⟩. ⟨hal-01026413⟩
Fabrice Testa, Clémence Coetsier, Emilie Carretier, M. Ennahali, B. Laborie, et al.. Retreatment of silicon slurry by membrane processes. Journal of Hazardous Materials, 2011, 192 (2), pp.440-450. ⟨10.1016/j.jhazmat.2011.05.016⟩. ⟨hal-01026376⟩ Plus de détails...
The purpose of the present study is to develop a process to regenerate the polish liquid used in Chemical and Mechanical Polishing (CMP), called "slurry", and more specifically Silicon CMP slurry. Physico-chemical analyses show a considerable dilution of slurry through washing waters used in polishing. Thus, this effluent has been characterised for a better identification of the deviations from the slurry of reference (Point Of Use). Hence, the principle is to regenerate this effluent by membrane processes. The ultrafiltration results obtained at laboratory scale have led to the development of an industrial prototype. An optimal utilisation of this treatment allows completing a two-step process: the reconcentration by ultrafiltration and a chemical adjustment by addition of concentrated slurry. A stable behaviour of the slurry at the different steps of the process has been observed. Polishing results are similar with retreated and POU slurries. Furthermore, the functioning at industrial scale permits to maintain the performances obtained on the laboratory pilot.
Fabrice Testa, Clémence Coetsier, Emilie Carretier, M. Ennahali, B. Laborie, et al.. Retreatment of silicon slurry by membrane processes. Journal of Hazardous Materials, 2011, 192 (2), pp.440-450. ⟨10.1016/j.jhazmat.2011.05.016⟩. ⟨hal-01026376⟩
Lauren F. Greenlee, Fabrice Testa, Desmond F. Lawler, Benny D. Freeman, Philippe Moulin. Effect of antiscalant degradation on salt precipitation and solid/liquid separation of RO concentrate. Journal of Membrane Science, 2011, 366 (1-2), pp.48-61. ⟨10.1016/j.memsci.2010.09.040⟩. ⟨hal-01026473⟩ Plus de détails...
The key limitation to the application of reverse osmosis (RO) desalination on inland brackish waters is concentrate disposal. Due to precipitation of sparingly soluble salts (CaCO3, CaSO4, BaSO4, SrSO4), RO membrane recovery cannot be increased further; therefore, other strategies must be investigated. Antiscalants are often added to RO feed water to help prevent precipitation and increase RO recovery, but in concentrate treatment, antiscalants may prevent precipitation of problematic constituents. A three-stage process to treat brackish water RO concentrate was investigated; the stages include oxidation of antiscalants with ozone and hydrogen peroxide, precipitation at elevated pH, and solid/liquid separation. A model water concentrate was used to perform laboratory scale experiments for each treatment stage. Experimental results showed that the advanced oxidation process (AOP) of ozonation and hydrogen peroxide on phosphonate antiscalants allowed increased calcium precipitation as well as loss of the solubilizing effects of antiscalants as compared to precipitation without prior ozonation of the antiscalants. The AOP also removed the effect of antiscalant on precipitate particle size distribution and particle morphology. In some cases, the AOP also improved microfiltration performance for the solid/liquid separation stage. The concentrate treatment could increase overall recovery from 80% to 90% for non-ozonated, antiscalant-dosed concentrate and from 80% to 94% for ozonated, antiscalant-dosed concentrate.
Lauren F. Greenlee, Fabrice Testa, Desmond F. Lawler, Benny D. Freeman, Philippe Moulin. Effect of antiscalant degradation on salt precipitation and solid/liquid separation of RO concentrate. Journal of Membrane Science, 2011, 366 (1-2), pp.48-61. ⟨10.1016/j.memsci.2010.09.040⟩. ⟨hal-01026473⟩
Lauren F. Greenlee, Fabrice Testa, Desmond F. Lawler, Benny D. Freeman, Philippe Moulin. The effect of antiscalant addition on calcium carbonate precipitation for a simplified synthetic brackish water reverse osmosis concentrate. Water Research, 2010, 44 (9), pp.2957-2969. ⟨10.1016/j.watres.2010.02.024⟩. ⟨hal-01024800⟩ Plus de détails...
The primary limitations to inland brackish water reverse osmosis (RO) desalination are the cost and technical feasibility of concentrate disposal. To decrease concentrate volume, a side-stream process can be used to precipitate problematic scaling salts and remove the precipitate with a solid/liquid separation step. The treated concentrate can then be purified through a secondary reverse osmosis stage to increase overall recovery and decrease the volume of waste requiring disposal. Antiscalants are used in an RO system to prevent salt precipitation but might affect side-stream concentrate treatment. Precipitation experiments were performed on a synthetic RO concentrate with and without antiscalant; of particular interest was the precipitation of calcium carbonate. Particle size distributions, calcium precipitation, microfiltration flux, and scanning electron microscopy were used to evaluate the effects of antiscalant type, antiscalant concentration, and precipitation pH on calcium carbonate precipitation and filtration. Results show that antiscalants can decrease precipitate particle size and change the shape of the particles; smaller particles can cause an increase in microfiltration flux decline during the solid/liquid separation step. The presence of antiscalant during precipitation can also decrease the mass of precipitated calcium carbonate.
Lauren F. Greenlee, Fabrice Testa, Desmond F. Lawler, Benny D. Freeman, Philippe Moulin. The effect of antiscalant addition on calcium carbonate precipitation for a simplified synthetic brackish water reverse osmosis concentrate. Water Research, 2010, 44 (9), pp.2957-2969. ⟨10.1016/j.watres.2010.02.024⟩. ⟨hal-01024800⟩
Lauren F. Greenlee, Fabrice Testa, Desmond F. Lawler, Benny D. Freeman, Philippe Moulin. Effect of antiscalants on precipitation of an RO concentrate: metals precipitated and particle characteristics for several water compositions. Water Research, 2010, 44 (8), pp.2672-2684. ⟨10.1016/j.watres.2010.01.034⟩. ⟨hal-01024814⟩ Plus de détails...
Inland brackish water reverse osmosis (RO) is economically and technically limited by the large volume of salty waste (concentrate) produced. The use of a controlled precipitation step, followed by solid/liquid separation (filtration), has emerged as a promising side-stream treatment process to treat reverse osmosis concentrate and increase overall system recovery. The addition of antiscalants to the RO feed prevents precipitation within the membrane system but might have a deleterious effect on a concentrate treatment process that uses precipitation to remove problematic precipitates. The effects of antiscalant type and concentration on salt precipitation and precipitate particle morphology were evaluated for several water compositions. The primary precipitate for the synthetic brackish waters tested was calcium carbonate; the presence of magnesium, sulfate, minor ions, and antiscalant compounds affected the amount of calcium precipitated, as well as the phases of calcium carbonate formed during precipitation. Addition of antiscalant decreased calcium precipitation but increased incorporation of magnesium and sulfate into precipitating calcium carbonate. Antiscalants prevented the growth of nucleated precipitates, resulting in the formation of small (100-200 nm diameter) particles, as well as larger (6-10 μm) particles. Elemental analysis revealed changes in composition and calcium carbonate polymorph with antiscalant addition and antiscalant type. Results indicate that the presence of antiscalants does reduce the extent of calcium precipitation and can worsen subsequent filtration performance.
Lauren F. Greenlee, Fabrice Testa, Desmond F. Lawler, Benny D. Freeman, Philippe Moulin. Effect of antiscalants on precipitation of an RO concentrate: metals precipitated and particle characteristics for several water compositions. Water Research, 2010, 44 (8), pp.2672-2684. ⟨10.1016/j.watres.2010.01.034⟩. ⟨hal-01024814⟩
