water is thus of critical importance for the water solution capillary impregnation ofthe wood. The plasma-chemical surface pre-treatment modifies the chemicalactivity of wood surface as well as the its capillary activity and improves suchtechnological characteristics of the impregnation process as the penetration depth,speed of solution spreading and adsorption, and specific quantity of adsorbedsolution per unit of surface area. This allows using the plasma aided retardation as afinishing process and applying it “in situ”. A system of plasma device andapplicators has been created to produce cold technological plasma throughdielectric barrier discharge (DBD) at atmospheric pressure and room temperature[1, 2].It is well known that heat treatments and machining reduce the wood wettabilityand chemical activity by modifying this water-reactive matrix in different ways.We found earlier that the cold plasma pre-treatment of soft wood, like pine (Pinussylvestris), improves technological characteristics such as a solution spreading andadsorption speed, as well as a specific amount of the adsorbed flame retardant. Inthis way, the plasma pre-treatment of pine wood improves its flame retardation andallows “in situ” performance of the procedure [3, 4].Douglas fir (Pseudotzuga) is a largely used wood in a lot of building constructions,flooring, timbers, but its flame retardency by capillary (or surface) impregnation isdifficult due to its relatively high density and surface inactivation. Therefore theimpregnation of this type of wood is often performed under high pressure orvacuum, the procedure requiring complicated apparatus and machines and a simplegeometric shape of the constructions, i.e. lumbers or timbers. In addition, the flameretardency is successful at flame retardant penetration depth of 1015 mm but thanan unacceptable decrease (down to 30 %) of the wood mechanical parametersarises, [5].We investigated the effect of plasma pre-treatment onto the wood surface activation(or functionalization) as well as the effect of different surfactant systems onto theionic activity of the impregnation solution, both aimed at improvement of Douglasfir wood flame retardation. Some experimental results of this investigation arepresented here: alteration the wood surface chemical composition or surfacefunctionalization as a result of the cold plasma pre-treatment at atmosphericpressure and room temperature monitored by X-ray photoelectron spectroscopy(XPS-) analyses; impregnating solution impregnation on bare or plasma pre-treatedDouglas fir wood without or with addition of a surfactant to the impregnatingsolution and the change of wood thermal degradation as a result of a flameretardation under different conditions monitored by thermal analysis (TGA, DTA,DSC).2. ExperimentalDouglas fir soft wood (Pseudotsuga menziesii, Canada), density of 678 g/cm 3 andmoisture content of 7.8 %) and pine soft wood (Pinus Sylvestris, Bulgaria) wereused in this investigation. Capillary impregnation test samples with size of5x30x150 mm were manufactured by heard wood.On the basis of the prior art as well as on a own former experience in the plasma78
aided impregnation of wood and wooden materials, [6, 7], an oxidative surfaceplasma pre-treatment on a part of the test samples was performed for 1 min in a dielectricbarrier air discharge at atmospheric pressure at industrial frequency (50 Hz)and two voltage – 10 and 15 kV, oxygen and ozone or nitrogen oxides (NO x ) respectivelynon-equilibrium cold plasma, and increased frequency (10 kHz) at voltageof 10 kV.The DBD plasma system was consisted of a coplanar shaped rectangular electrodeswith one glass barrier (thickness of 3 mm) arranged closeness to grounded electrodewith operating distance between high voltage electrode and barrier of 6 mm,Fig 1a. The DBD was assured by two different - low frequency (50 Hz) and highfrequency (10 kHz), voltage generators. The wood samples were disposed in operatingvolume and treated for one minute (60 sec) under chosen frequencies andvoltages.Dielectric barrierEarthHV ElectrodeGrounded ElectrodeDischarge Current I AVG , μANon-operatingareaFirst operatingareaSecond operatingarea270024002100180015001200900SN6003.36 W/m 2SO300 2.56 W/m 200 4 8 12 16 20 24a) Voltage V RMS , kV b)Fig. 1. Dielectric barrier discharge coplanar electrode system with one glass barrier (a), staticvolt-ampere characteristic I AVG - V RMS , and regimes of plasma pre-treatment at industrial frequencyof 50 Hz - SO: voltage of 10 kV (RMS); real specific power 2.56 W/m 2 , and SN: voltageof 15 kV (RMS); real specific power 3.36 W/m 2 (b).A tendency to the halogen containing flame retardants replacement by halogen-freeones is observed lately because of the toxicity of the halogens, [8]. A halogen-free,phosphorus and nitrogen containing flame retardant is used in this investigation inform of 30 w. % water solution. The impregnating water solution (FRIS, dry substanceof 30 w. %; phosphorus content of 13 w. %, pH = 78 and density of 1.14g/cm 3 ) was based on a halogen free phosphorus and nitrogen containing flame retardant.A new flame retardant product on the basis of ortho-phosphorous acid, ureaand ammonia was studied.Wood inactivation is a surface phenomenon affecting just a thin outer layer ofwood. An inactivated wood surface does not absorb capillary well an impregnatingsolution containing phosphorous compound as flame retardant. Plasma-chemicalsurface activation (functionalization) with an effective participation of ionicsurfactants and silicone spreaders eliminates the inactivation-impregnating problemcreating a protective flame retardant layer on the wood surface. The air plasmatreatment gives different results from the nitrogen and oxygen treatments. Anionicsurfactants (AS, “Aniticrystallin A“, Chimatech, Ltd., Bulgaria) in quantity of 5vol. %, or silicone super spreader (SSP, Y-17113, Momentive Performance79
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ISSN 1311-0829ГОДИШНИК НА
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