Capítulo IV. Cuerpo y precarización
4.2. Cuerpo, Estado y violencia: el caso de la diabetes
The reactions described were initially carried out in the manner described below for zinc sulfide. In each case, the alkali metal chalcogenide was Jfreshly prepared fi*om direct combination o f the elements in liquid ammonia, with all manipulation undertaken using Schlenk techniques to avoid exposure to either air or water moisture (as described below). Once isolated, product work-up and characterisation of all products were carried out as for the solid state metathetical products described in chapter 5.
Reaction o f zinc sulfide (from the reaction o f sodium sulfide with zinc chloride)
The same general reaction scale and procedure was adopted for all these reactions, as exemplified here for ZnS.
Freshly prepared disodium sulfide (100 mg, 1.28 mmol.) and zinc chloride (175 mg, 1.28 mmol.) were ground together inside a glove box, using an agate pestle and mortar, until intimately mixed. The mixture was added to a Youngs-type pressure tube containing ca. 15 cm^ at ca.-l% °C using Schlenk techniques. The tube was then sealed at allowed to warm to room temperature with continuous stirring o f the reaction mixture. In each case, although the liquid ammonia was observed to change colour upon addition o f the reagents (suggesting the presence o f solvated species), the bulk o f the mixture remained solid state in nature throughout the course o f the reaction. After 12-18 h (or once the liquid ammonia was observed to turn colourless) the ammonia was allowed to evaporate under dinitrogen gas flow. Part o f the product (typically a mixture o f black and white material) was then triturated with 3x20 cm^ o f distilled water, typically yielding a black material, before being dried under vacuum. The isolated product was then annealed for 2 h at 200-250 °C. The isolated product was typically analysed (before and after annealing) by XRD, SEM / EDXA and IR spectroscopy. XRD analysis was also carried out on the pre-washed reaction product.
Slight modifications to the general experimental procedure were then developed. First, condensation o f the ammonia over either the sodium sulfide or selenide resulted in complete dissolution o f the material, thereby affording excellent contact between the reagents. It should be noted, however, that such a procedure only resulted in partial dissolution o f sodium telluride. Finally, as described earlier, the synthesis o f ternary materials may be sensitive to mode o f addition o f the metal halides (possibly resulting firom a differential in reagent solubilities). In an attempt to limit this effect, these precursors were added as an intimately ground mix, with the least soluble halides available being used.
Preparation o f sodium chalcogenide
Na2E (E = S, Se, Te) was prepared by the direct combination o f stoichiometric quantities o f
sodium metal and elemental chalcogen in liquid ammonia. These reactions were carried at room temperature in teflon-in-glass Youngs-type pressure vessels, using Schlenk techniques. Once prepared, the sodium chalcogenide was used immediately in the liquid ammonia metathesis without exposure to atmospheric conditions.
Table 6.8 SEM / EDXA data of Binary metal chalcogenides synthesised by metathetical reaction in liquid ammonia at room temperature
R e a g e n t s ' P a r tic le m o r p h o lo g y ^ R a t io o f e le m e n t s ( e x p t . e r ro r ± 2 - 3 atm .% )^ p m = m ic r o n s n m = n a n o m e te r s E le m e n t a l r a tio E x p t v a lu e s T h e o r e tic a l v a lu e s
N iC lz + NazS 1-5 pm aggregates. Irregular particles < 50 nm N i : S 5 0 : 5 0 5 0 : 5 0 ( N i S )
Z n C la + N a 2 S 1-5 pm aggregates. Spherical particles < 50 nm Z n : S 5 0 : 5 0 5 0 : 5 0 ( Z n S )
CdCh + NazS 1-5 pm aggregates. Spherical particles < 50 nm C d : S 5 0 : 5 0 5 0 : 5 0 ( C d S )
2 C u B r + N a2S 1-8 pm aggregates. Irregular particles < 100 nm C u : S 6 7 : 3 3 6 7 : 3 3 (C U2S )
C u : S 6 4 : 3 6 C u2.xS 2 p h a s e s
C u C l2 + N a 2 S 1-8 pm aggregates. Spherical particles < 100 nm C u : S 5 0 : 5 0 5 0 : 5 0 ( C u S )
C u : S 6 7 : 3 3 6 7 : 3 3 ( CU2S )
C u C l2 + N a 2 S e 1-8 pm aggregates. Irregular particles < 100 nm C u : S e 5 0 : 5 0 5 0 : 5 0 ( C u S e )
C u C l2 + N a 2 T e 1-8 pm aggregates. Spherical particles < 100 nm C u : T e 42 : 58 C u4T e3 2 p h a s e s
2 A g F + N a 2 S 1-5 pm aggregates. Spherical particles < 50 nm A g : S 6 7 : 3 3 6 7 : 3 3 ( A g z S )
2 A g F + N a 2 S e 1-5 pm aggregates. Spherical particles < 50 nm A g : S e 6 7 : 3 3 6 7 : 3 3 ( A g 2 S e )
2 A g F + N a 2 T e 1 -5 pm aggregates. Spherical particles < 50 nm A g : T e 6 7 : 3 3 6 7 : 3 3 ( A g 2 T e )
H g C l2 + N a 2 S 1 -5 pm aggregates. Spherical particles < 50 nm H g : S 5 0 : 5 0 5 0 : 5 0 ( H g S )
H g C l2 + N a 2 S e 1 -5 pm aggregates. Spherical particles < 50 nm H g : S e 5 0 : 5 0 5 0 : 5 0 ( H g S e )
H g C l2 + N a 2 T e 1-5 pm aggregates. Spherical particles < 50 nm H g : T e 5 0 : 5 0 5 0 : 5 0 ( H g T e )
2 G a C l3 + 3 N a 2 S 1 -5 pm aggregates. Spherical particles < 50 nm G a : S 4 0 : 6 0 4 0 : 6 0 (G a 2 S 3 )
2 G a C l3 + 3 N a 2 S e 1-5 pm aggregates. Spherical particles < 50 nm G a : S e 4 0 : 6 0 4 0 : 6 0 (G a 2 S e 3 )
2 G a C l3 + 3 N a 2 T e 1-5 pm aggregates. Spherical particles < 50 nm G a : T e 4 0 : 6 0 4 0 : 6 0 (G a 2 S 3 )
2 I n C l3 + 3 N a 2 S 1-5 pm aggregates. Spherical particles < 50 nm I n : S 4 0 : 6 0 4 0 : 6 0 (In2S3)
2 I n C l3 + 3 N a 2 S e 1-5 pm aggregates. Spherical particles < 50 nm In : S e 4 0 : 6 0 4 0 : 6 0 (In 2 S e3 )
2 I n C l3 + 3 N a 2 T e 1-5 pm aggregates. Spherical particles < 50 nm In : T e 4 0 : 6 0 4 0 : 6 0 (In2S3)
2T1C1 + N a 2 S 1 -8 pm aggregates. Irregular particles < 200 nm T l : S 5 0 : 5 0 5 0 : 5 0 (T I S )
2T1C1 + N a 2 S e 1 -8 pm aggregates. Irregular particles < 200 nm T l : S e 5 0 : 5 0 5 0 : 5 0 ( T l S e )
2T1C1 + N a 2 T e 1 -8 pm aggregates. Irregular particles < 200 nm T l : T e 6 3 : 3 7 6 3 : 3 7 ( T ls T e s )
P b C l + N a 2 S 1-5 pm aggregates. Spherical particles < 50 nm P b : S 50 : 50 50 : 50 (PbS)
PbCl + Na2Se 1-5 pm aggregates. Spherical particles < 50 nm Pb : Se 5 0 : 5 0 50 : 50 (P bSe) PbCl + Na2Te 1-5 pm aggregates. Spherical particles < 50 nm P b : T e 50 : 50 50 : 50 (PbT e)
3M Cl2+3Na3Pn 1-5 pm aggregates. Irregular particles 50-1 OOnm M : Pn 6 0 : 4 0 4 0 : 60 (M3Pn2)
M = Fe, Co, Ni; Pn = As, Sb
3M Cl2+3Na3Pn 1-8 pm aggregates. Irregular particles 50-1 OOnm M : Pn 6 0 : 4 0 4 0 : 60 (M3Pn2)
M = Zn, Cd; Pn = As, Sb Free elements (M, Pn) detected as minor phase
' M olar ratios o f reagents given for the room temperature, liquid amm onia m etathesis reaction o f transition m etal halides w ith sodium chalcogenides. Subsequent analyses were obtained from sam ples w a sh ed with distilled water, and refer to both pre-annealed and annealed material (unless stated).
^ A ssessed by SEM at m axim um m agnification.
^ Elem ental com p osition o f phase assessed by E D X A (spot size - 1 m icron). A pproxim ate surface abundance o f m ultiple phases (assessed qualitatively using back-scattered electrons) is expressed either as a percentage or as m a jo r / m in or phases.
Table 6.9 SEM / EDXA data of Ternary metal chalcogenides synthesised by metathetical reactions in liquid ammonia at room temperature
Reagents' Particle morphology^ Ratio o f elements (expt error ± 2-3 atm %Ÿ
p m = m ic ro n s; a g g . = a g gregates n m = n a n o m e ters; pts = particles Elemental ratio Expt values Theoretical values
CuBr + GaBi3 + 2NazS 1-5 p m a g g . S p h erical p ts < 5 0 nm Cu:Ga:S 25:25:50 25:25:50 CuGaS]
Cu:Ga:S 65:2:33 64:0:36 CU7S4
CuBr + GaBr3 + 2Na2Se 1-5 p m a g g . S p h er ica l p ts < 5 0 nm Cu:Ga:Se 25:25:50 25:25:50 CuGaSe:
CuBr + InCl3 + 2NazS 1-5 p m a g g . S p h er ica l p ts < 5 0 nm Cu:In:S 25:25:50 25:25:50 CuInSz
CuBr + InCl3 + 2Na2Se 1 -5 p m a g g . S p h erica l p ts < 5 0 nm Cu:In;Se 25:25:50 25:25:50 CuInSez
AgF + GaBr3 + 2Na2S 1 -5 p m a g g . S p h erica l p ts < 5 0 nm Ag:Ga:S 25:25:50 25:25:50 AgGaSz
AgF + GaBr3 + 2Na2Se 1 -5 p m a g g . S p h erica l p ts < 5 0 nm Ag:Ga:Se 25:25:50 25:25:50 AgGaSez
AgF + InCl3 + 2Na2S 1-5 p m a g g . S p h erica l p ts < 5 0 nm Ag:In:S 25:25:50 25:25:50 AglnSz
AgF + InCl3 + 2Na2Se 1-5 p m a g g . S p h erica l p ts < 5 0 nm Ag;In;Se 25:25:50 25:25:50 AglnSea
CuBr + AICI3 + 2Na2S 1-7 p m a g g . irregular p ts < 2 0 0 nm Cu:Al:S* 50:0:50 50:0:50 CuS
CuBr + AICI3 + 2Na2Se 1-7 p m a g g . irregular p ts < 2 0 0 nm Cu;Al:Se* 50:0:50 50:0:50 CuSe
AgF + AlBr3 + 2Na2S 1 -7 p m a g g . irregular p ts < 2 0 0 nm Ag;Al:S* 67:0:33 67:0:33 AgjS
AgF + AlBr3 + 2Na2Se 1 -7 p m a g g . irregular pts < 2 0 0 nm Ag:Al;Se* 67:0:33 67:0:33 AgjSe
* Aluminium was only detected in sub-micron regions of > 95 atm % abundance.
In addition, regions of free chalcogen (> 95 % atm. %) were also detected.
3CuBr + SbBr3 + 3Na2S 2 -7 p m a g g . irregular p ts < 2 0 0 nm Cu:Sb:S 42:13:46 43:14:43 Cu3SbS3
CuBr + SbBr3 + 2Na2S 1-7 p m a g g . Irregular pts < 1 5 0 nm Cu:Sb:S 25:25:50 25:25:50 CuSbSz
CuBr + SbBr3 + 2Na2Se 1 -7 p m a g g . irregular p ts < 1 50 nm Cu:Sb:Se 25:25:50 25:25:50 CuSbSc2
CuBr + SbCl3 + 2Na2Te 1 -7 p m a g g . irregular p ts < 150 nm Cu:Sb;Te 25:25:50 25:25:50 CuSbTcz
CuBr + FeCl3 + 2Na2S 1-5 p m a g g . irregular p ts < 100 nm Cu:Fe:S 25:25:50 25:25:50 CuFeS^
Cu:Fe:S** 50:10:40 50:10:40 CusFeS4 MCI2 + FeCb + 2Na2S M - Zn, Cd 1-5 p m a g g . S p h erica l p ts < 150 nm M:Fe:S 50:2:48 50:0:50 MS M:Fe:S 2:32:66 0:33:67 FeS; MCI2 + CrCl3 + 2Na2S M = Zn, Cd 1 -5 p m a g g . Irregular p ts < 100 nm M:Cr:S 50:1:49 50:0:50 MS M;Cr;S 2:48:50 0:50:50 CrS MCI2 + VCI3 + 2Na2Se M - Zn, Cd
1-8 p m a g g . Irregular p ts < 1 0 0 nm M:V:Se 50:0:50 50:0:50 MSe
M:V:Se 0:50:50 0:50:50 VSe
M;V:Se** 2:30:68 0:33:67 VSe;
CdCl2 + HgCl2 + 2Na2Te 1 -5 p m a g g . S p h er ica l p ts < 5 0 nm Cd:Hg:Te 47:3:50 50:0:50 CdTe
Cd:Hg:Te 3:48:49 0:50:50 HgTe
** Minor phases
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