Accepted Manuscript

Characterization of impurities present on Tihimatine (Hoggar) Quartz, Algeria

S. Anas Boussaa, A. Kheloufi, N. Boutarek Zaourar

PII: S1464-343X(17)30351-5
DOI: 10.1016/j.jafrearsci.2017.09.001
Reference: AES 3002

To appear in: Journal of African Earth Sciences

Please cite this article as: S. Anas Boussaa, A. Kheloufi, N. Boutarek Zaourar, Characterization of
impurities present on Tihimatine (Hoggar) Quartz, Algeria, Journal of African Earth Sciences (2017), doi:
10.1016/j.jafrearsci.2017.09.001

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 ACCEPTED MANUSCRIPT
1 Characterization of impurities present on Tihimatine (Hoggar) Quartz, Algeria
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3 S. Anas Boussaaa,b, A. Kheloufia, N. Boutarek Zaourarb
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5 Divion croissance cristalline et procédés métallurgiques
6 Centre de recherche en technologie des semi-conducteurs pour l’énergétique (C.R.T.S.E)
7 02 Bd Frantz Fanon BP. 140 Alger 7 merveilles, Alger 16200
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8 Laboratoire des technologies des matériaux, USTHB, B.P. 32 El Alia, Bab Ezzouar, Alger, Algérie16111.
9 Corresponding author: sabiha.anas@gmail.com anassabiha@crtse.dz
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17 Abstract
18 34 optical Microscopy with reflected and transmitted

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19 Many of today’s advanced materials depend on 35 lights, infra-red spectrometer, Raman spectrometer.
20 quartz as a raw material. 36 Despite the high concentration of SiO2 in studied
21 Quartz usually contains abundant inclusions, both 37 quartz reaching 98%, several harmful inclusions
22 solid and liquid, and due to the number of these 38 were found and identified as hematite, anatase,

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23 inclusions and their small size, complete separation 39 muscovite, graphite, it contains: Fe, Ti, Al, K, Ca.
24 is most difficult. 40 Some fluid inclusions were found. We detect the
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25 Typical properties of raw quartz that must be 41 presence of carbon dioxide and water using raman
26 characterized are: Size and Chemical composition 42 spectroscopy.
27 of inclusions, their spatial distribution, localization 43 The repartition of solid impurities is aleatory and
28 of isomorphic substitutional elements (e.g. Al, Fe). 44 not homogeneous with maximum size of 10 µm.
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29 The aim of this study has been to test experimental 45 Concerning the fluid impurities, their diameter vary
30 methods for investigating some inclusions 46 between 5 to 20 µm and their repartition is aleatory.
31 (impurities) present in the Tihimatine quartz from 47
32 El Hoggar region deposits (southern Algeria) using 48 Key words: Silica, Quartz, Tihimatine, Hoggar,
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33 X Ray Fluorescence, scanning electron microscopy, 49 Inclusions, Characterization.

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66 1. Introduction 95 bound trace elements in quartz either substitute for

67 Quartz is the most abundant mineral in the earth. 96 Si4+ (Al3+, Fe3+, B3+, Ti4+, Ge4+, P5+) or occur at

68 High purity quartz contains less than 50 µ gg-1 of 97 interstitial channel positions (Li+, K+, Na+, H+,

69 impurities. The impurities concentrations in quartz 98 Fe2+), where the ions act predominantly as charge

70 are mainly controlled by their abundance in the 99 compensators for the trivalent and pentavalent

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71 melt, the thermodynamic conditions in the system, 100 substitutional ions Al3+, Fe3+ and P5+. [4]

72 and also by the mass partition between the different 101 Solid and fluid inclusions: frequently, the

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73 phases. [1] 102 quartz grains contain minerals inclusions, silicate

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74 Impurities contents of quartz are its most important 103 melt and fluids. The kind and abundance of the

75 quality criteria (Figure 1), there enter the silicon 104 inclusions depends on the environmental

76 during the carbothermic reduction of quartz, and 105 crystallization. If inclusions are present in large

77 affect the efficiency of final silicon.

U 106 quantities so they have a strong influence on quartz
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78 The production of solar grade silicon is based on 107 chemical quality of quartz raw materials. Because

79 the use of high purity quartz feedstock as well as 108 they are enclosed in quartz crystals, they can be
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80 various silicon refining techniques. Impurities in 109 hardly removed by beneficiation processes.

81 the feedstock materials enter the silicon during the 110 Fluid inclusions are common in
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82 carbothermic reduction of quartz then affect the 111 hydrothermal quartz. It is formed from hot aqueous
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83 final efficiency of the silicon solar cells. 112 solutions percolating through fractures in the

84 The knowledge of the impurity and their 113 earth’s crust. The hot aqueous solutions (p ranging
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85 concentration in the feedstock is necessary for 114 from 1 to 3000 bar, T from 50 to 600 °C) contain

86 targeting less pure and cheaper silicon, in the table 115 primarily ortosilicid acid H4SiO4 with significant
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87 1; we present the average impurities content in 116 quantities of cationic species such as Na+, K+ , Si 4+,
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88 quartz for Si production. 117 Ca2+, Mg2+ and Fe2+ and anionic species such as Cl–

89 Unfortunately, these impurities had not been 118 , HS–, HCO–3, SO2 –4
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90 enough explored. It’s mainly due to the quartz 119 decreases and the solution get saturated with respect

91 crystal structure. [3] 120 to quartz, H4SiO4 decomposes and quartz is formed.

92 121 Hydrothermal fluids are variable in composition

93 These impurities isolated or in chemical association 122 depending on the solubility of the trace elements in

94 can integrate three distinct sets: The lattice: Lattice- 123 the aqueous solutions, the different rocks through

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124 which the fluids have been circulating, the 154 according to it later uses and to envisage it

125 contamination from other types of fluid and the 155 behaviors in these applications.

126 conditions for precipitation. Depending on all these 156 2. Geological setting

127 factors, hydrothermal quartz veins can be host to 157

128 ore deposit or may be extremely pure, containing 158 • Regional geological frame of Hoggar

129 only a few ppm of impurity elements. [5] 159

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130 We can also find the impurities in adsorption in 160 The Hoggar (Figure 2.A) is located in southern

131 network imperfections, on surfaces and of course in 161 Algeria and constitutes the major part of the Tuareg

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132 fully or partially healed fractures. [6] 162 shield, which comprises also the Iforas granulotic

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133 163 unit in Mali to the SW and the Aïr in Niger to the

134 The request of high purity quartz is strongly 164 SE. [11, 12]

135 increasing, especially to be used in electronics and 165 It is composed of well preserved and largely

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136 silicon production for photovoltaic applications 166 reworked Archean (3200–2500 Ma) and
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137 which convert the sun energy directly into the 167 Paleoproterozoic terranes (2000 Ma) and juvenile

138 electrical energy. [7,8 ,9] However, the exploitation 168 Pan-African terranes (750–550 Ma).
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139 of new suitable quartz deposits is hampered by 169 It is subdivided in three different submeridian parts

140 quality specification that applies for high 170 (western, central and eastern). They are limited by
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141 technologies. 171 the two lithosperical accidents NS (4°50" and

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142 172 8°30") of falling components. From east to west, it

143 In view of this, and because of the drastic 173 can be distinguished:
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144 reduction of high purity quartz stocks, which need 174 - Eastern Hoggar: It is the least studied part of the

145 arises for the development of new enrichment 175 Hoggar. It is characterized by two different
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146 quartz for beneficiation technologies of pure silica 176 structural fields the Taffassasset - Djanet block and
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147 with high efficiency and low cost, mainly for 177 the linear chain of Tiririne. This last is composed of

148 photovoltaic field. [10] 178 a detritic serie (pelites and conglomerates) is

149 For this purpose, the aim of this work is to 179 stretched along the 8° 30’ accident. The other block

150 characterize the trace element composition of 180 is composed of a great number of intrusive

151 Tihimatine quartz there for we guide industrials and 181 granitoic orogenic bathollites in a metasedimentary

152 researcher to find an adequate method for it 182 sequence of unknown age.

153 enrichment in order to be able to select the latter

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183 - Central Hoggar : Said polycyclic where dominate 212 Tihimatine site is situated in the NW part of the

184 by the gneissic sets of lower Paleoproterozoic 213 Hoggar about 500Km west of the city of

185 (series of Arechoum and Aleksod) recovered in 214 Tamanrasset.

186 disconcordance by the pharusian volcano 215 Tihimatine area (Figure.2B) is characterized by a

187 sedimentary series (Arefsa and Serouenout). All 216 complex geology, presented by a high level

188 these series are affected by the Pan-African 217 metamorphic Archean formation. These Archean

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189 tectonics expressed in the base nappes (eclogitic 218 sets are composed of various rocks: charnokites,

190 lens) and are largely intruded by syn-orogenic 219 orthogneiss, enderbites, migmatites, quartzites and

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191 granitic batholites. 220 carbonated rocks. The gneiss is varied and

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192 - Western Hoggar : where level off the chain said 221 abundant: they are of pyroxenes, quartz, feldspars,

193 pharusian is composded of two branches (western 222 and of granets. The charnokites are of quartz,

194 and eastern) separated by the In Ouzzal granutic 223 feldspars and granets. In the centre of the quartzites

195 mole of archean age.

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196 The In Ouzzal terrane forms an elongated N–S 225 allotted to the stromatolithes serie.

197 trending block, more than 400 km long and 80 km 226

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198 wide in the north around the In Hihaou massif, 227 3. Experimental

199 thinning out until it disappears in the south near the 228 The focus in this work has been to study the
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200 Malian border, where it is then offset towards the 229 inclusions of Tihimatine quartz.
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201 Iforas granulitic unit (Figure. 2A). The main relief 230 Tihimatine site (fig 2(B)) is situated in the NW part

202 rising several hundreds of meters above the In 231 of the Hoggar (fig 2(A)) about 500Km west of the
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203 Ouzzal granulitic reg (¼ desert pediments with 232 city of Tamanrasset.

204 small pebbles) is made up of ignimbrite massifs da 233 Samples were collected from different pits in the
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205 ted at 530, and the Pan-African granites of In 234 area to represent as much as possible the actual
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206 Hihaou and In Eher in the West, Nahalet and 235 deposits. For this study we used several

207 Tihimatine in the centre and Ihouhaouene in the 236 characterization techniques for finding a maximum

208 East. 237 of inclusions present in our samples and to regroup

209 238 maximum information about them.

210 • Tihimatine geology 239 • The chemical composition was determined

211 240 by the X-Ray Fluorescence (XRF)

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241 • The carbon proportioning was measured 271 remainder of our work, we focused our study on the

242 by a standard carbon batcher ELTRA CS 272 sample which contains the most of the impurities.

243 800 273 According to the results of the table 2, we see that

244 • For our metallographic observations we 274 the chosen quartz samples from Tihimatine deposit

245 used a petrographic microscopy with 275 have a high SiO2 concentration with maximum iron

246 transmitted and reflected light Axio Scope 276 oxide Fe3O4 rate reaching 1.53 % compared to other

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247 A1. 277 oxides.

248 • A scanning electron microscopy model 278

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249 JSM-5500LV/JSM-5500. 279 4.2. Carbon rate

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250 • The Raman analyses were realized using a 280 Carbon is considered among the most undesirable

251 Jobin-Yvon Horiba LabRam HR800 VIS 281 impurities in quartz. It plays a harmful role in the

focal 282 future use of quartz notably in the photovoltaic

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253 microscope and CCD detector. We used 283 field.

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254 two wavelengths at 514 and 532 nm, and 284 We measured the percentage of carbon in our

255 objective lenses of 50× and 100× 285 quartz samples by the carbon analyzer, because we
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256 • The Vickers hardness used is of type OSI 286 can’t measure it by XRF analysis. We recorded

257 with a load applied of 100 gr 287 several values of carbon following five tests carried
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258 • The infra-red spectrometer used is 288 out.

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259 BRUCKER. 289 For each samples the test was done 3 times in order

260 290 to have a precise values (Table 3).

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261 4. Results and Discussion 291 The results indicate that the values of the carbon

262 4.1. XRF analysis 292 concentrations in five samples converge despite
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263 We began our work by the analysis of 293 slight difference that really indicates the non-
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264 12 quartz samples by X-Ray fluorescence because 294 uniformity of carbon distribution in the quartz.

265 the elemental analysis composition of studied 295 The percentage of carbon come probably from fluid

266 samples can give us important information about 296 inclusions and carbonates or graphite distributed in

267 the mineral. [14] 297 a no uniform way in our samples. [15]

268 We note that the concentration of impurities was 298

269 practically the same. In The table 2, the result of 299 4.3. Microscopy observations

270 five quartz samples are represented. For the

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300 4.3.1 Optical microscopy 330 In the (Figure 5b) we observed the presence of

301 observations 331 graphite in the quartz sample.

302 Optical microscopic analysis of raw quartz 332 The microscopic investigations of the quartz

303 allows rapid detection and a first overview of the 333 samples from Tihimatine deposit (Fig 6) revealed

304 sample texture and structure as well as impurities 334 primary hydrothermal origin. The crystals were

305 such as fluid and solid phase inclusions. 335 strongly affected by brittle and ductile deformation

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306 The micrographics observation with reflected 336 as suggested by the presence of numerous cracks

307 revealed the presence of solids inclusions with 337 (Fig. 3a) and crystals with undulatory extinction or

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308 various morphologies: nodular, lengthened, 338 deformation bands.

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309 unspecified; distributed in a random way in the 339 4.3.2 Scanning electron microscopy observations

310 quartz matrix. 340 Scanning Electron Micrograph (SEM) of quartz

311 We observed the presence of microscopic cracks 341 sample (Fig 7, Fig 8) shows the presence of several

312 and fluid inclusions too Fig (3a, 3b and 3c).

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313 Fluid inclusions present in hydrothermal quartz 343 matrix in a random manner.

314 may be the reason for the higher volatility 344 These agglomerated particles have an average size
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315 presented. During heating of quartz, the internal 345 lower than 50 nm. In the Figure 7, we can see the

316 partial pressure of the fluid inclusions increases and 346 fluid inclusions, with their irregular shape and their
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317 they decrepitate; so cracks develop in the quartz 347 dimensions.

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318 enabling degassing of water and CO2 from the 348 The Scanning Electron Microscopy (SEM)

319 inclusions. 349 combined with energy-dispersive X-ray

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320 Decrepitation occurs in the temperature range from 350 spectrometry (EDX) yields an elemental analysis of

321 200 to 600 °C depending on the fluid composition 351 individual particles.
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322 and size. 352 In Fig 8, we show that the existence of iron oxides
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323 In the figure 4 we show several fluid inclusion 353 particles which covered the quartz surface.

324 indicate that their distribution is in random and their 354

325 dimensions vary between 5 to 20 µm. 355 4.4. Raman spectroscopy

326 To be able to identify the mineral inclusions we use 356 In order to explore more inclusions, we use the

327 a polarized and reflected light micrograph (Fig 5). 357 Raman spectroscopy. Raman spectroscopy

328 The micrograph in (Figure 5a) shows the presence 358 revealed the presence of solid inclusions as

329 of muscovite KAl2Si3AlO10(OH,F)2. 359 hematite and anatase (Figure 9 and 10).

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360 In the figure 11, a H2O-CO2 mixed inclusion is 390 infrared spectrum of natural quartz are around 450

361 illustrated , it is the only inclusion that we could 391 cm-1 ; 690cm-1 ; 800cm-1 and finally at 1000cm-1.

362 identify by Raman spectroscopy it’s measure 20 392 The band at 459 cm-1 corresponds to the

363 µm. 393 movements of deformation of the quartz.

364 The H2O-CO2 mixtures have a very steep P-T 394 The band at 690 cm-1 corresponds to the vibrational

365 path, and decrepitate early during heating. 395 mode of the link Si-O.

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366 396 The presence of isolated links (Si-O) shows the

367 4.4. Vickers hardness 397 existence of bonds Si-O engaged in a chain − [Si -O

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368 398 - Si -O] –.

369 The defects found in quartz are regarded as 399 While bands located at 780cm-1 and 795cm-1 are

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370 concentrations, heterogeneities of stresses and the 400 also assigned to the torsional vibration of the group

371 presence of impurities, thus they support the 401 Si-O-Si.

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372 defragmentation and the breaking of silica during 402 The band at 1080 cm-1 is due of stretching
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373 the heating. To display this heterogeneity of stress, 403 vibrations of the group Si-O-Si.

374 we had recourse to the micro Vickers pyramid 404 The different small peaks appearing due to the
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375 hardness as average of analysis. 405 presence of impurities such as iron (almost

376 It is noted that the hardness of pure quartz 406 1200cm-1) and water (1600 cm-1 and 3450 cm-1) ;
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377 varies very little; it is on average about 407 1900 and 2000 cm-1 Format defects developed
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378 1050HV0.1.This value agrees with the values of 408 specifically AlO4 and other inclusions. [17-19]

379 hardness according to the Mohs scale of hardness. 409 5. Conclusion

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380 [16] Besides, the presence of solid inclusions in the 410 The study of the quartz from Tihimatine (Hoggar)

381 matrix affects the entire hardness because of the 411 deposits reveals quite important initial
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382 solid inclusions hardness itself. 412 concentrations of SiO2 up to 97.8%, with oxides
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383 The Table 4 represents the hardness of three chosen 413 impurities which rate varies from trace to 1.6%

384 representative samples QT1, QT2 and QT3. 414 Fe2O3. However, these concentrations are not

385 In the figure 12, we show different solid inclusions 415 sufficient to be used as raw material for solar grade

386 referred to their specified hardness. 416 silicon production;

387 4.5. IR Spectroscopy 417 - The optical and spectroscopic characterizations

388 The infrared spectrum of quartz is shown 418 show the presence of different “defects” in terms of

389 in Figure 13. The main peaks observed in the 419 morphology, structure and mineral inclusions;

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420 - Concerning the mineralogy of solid inclusions, we 449 Funding was provided by the General Direction of

421 have identified the presence of muscovite, graphite, 450 research and development technologies / Ministry

422 anatase, hematite using petrographic microscope 451 of Higher

423 and the Raman spectroscopy, H2O-CO2 fluid 452 Education and Research Sciences DGRSDT/MERS

424 inclusion was detected. We note that the size of the 453 (ALGERIA).

425 observed inclusions does not exceed 30 microns. 454 We thank the department of geology of the National

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426 -Employing a scanning electron microscope, we 455 Office of Research in Geology and Mineralogy

427 observed fluid inclusions and hematite solid 456 (ORGM, Boumerdes, Algeria) for the XRF

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428 inclusion. 457 analysis.

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429 -The mineral phases present in the quartz contain 458 We thank the metallurgy laboratory of the national

430 the following elements: Fe; Al; Mn; Mg; Ti; K and 459 company of the industrial vehicles (SNVI) in

431 Ca. 460 Rouiba (Algiers, Algeria) for the carbon and

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432 - By measuring the rise of carbon, we were able to 461 Vickers hardness measuring.
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433 find several values. These values can be explained 462 Raman analyses were per-formed at Ecole Normale

434 by the presence of fluid inclusions wish contain 463 Supérieure (ENS) Lyon. The Raman facility in
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435 carbon, solid inclusions as graphite and carbonates. 464 Lyon is supported by the “Institut des Sciences de

436 - The infrared spectrum of the silica allows us to 465 l’Univers (INSU) ENS. We thank Gilles Montagnac
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437 define the main peaks of natural quartz. The values 466 for assistance.
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438 are detected around 450 cm-1; 690 cm-1; 800 cm-1 467 For our metallographic observations we used a

439 and finally to 1000 cm-1. The analysis allows us to 468 petrographic microscopy with transmitted and
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440 identify the presence of inclusions especially iron, 469 reflected light Axio Scope A1.

441 aluminum and water which confirm the XRF and 470 We thank also the department of Materials Science
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442 microscopic results. 471 of the University of Biskra, Algeria for the SEM
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443 On the other hand several micro-hardness values of 472 observations.

444 different order of magnitude (from 400 to 1900 473 Finally we thank our institution CRTSE for all the

445 HV0.1) were identified indicating the variety of solid 474 facilities to be able to realize this work.

446 inclusions in quartz. 475

447 476 References

448 Acknowledgements 477

478 [1] Karel Breiter , Martin Svojtka , Lukáš Ackerman ,

479 Kateřina Švecová Trace element composition of

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606 FIGURES CAPTIONS
607 Figure 1. Schematic quartz structure showing the configuration of different trace elements in the quartz lattice.

608 Also it isproposed that substitution of Si4+ by four H+ is possible (silanol groups). Because of the two-

609 dimensional illustration thefourth H+ is not shown on the figure. [2]

610 Figure 2. (A) Schematic map of the tuareg shiel showing the setting of the In Ouzzal terrane . (B) Geological

611 map showing the localization of Tihimatine.[13]

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612 Figure 3. Quartz inclusions micrograph (solid and fluid inclusions)

613 Figure 4. fluid inclusions on Tihimatine quartz

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614 Figure 5. Mineral inclusions using polarized and reflected light micrograph

615 Figure 6. Quartz micrograph using polarized and transmitted light

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616 Figure 7. Scanning electron micrograph of fluid inclusions on quartz

617 Figure 8. Scanning electron micrograph of iron inclusion with EDS presentation

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618 Figure 9. Hematite mineral inclusion in Tihimatine quartz
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619 Figure 10. Anatase mineral inclusion from Tihimatine quartz

620 Figure 11. Carbon fluid inclusion from Tihimatine quartz

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621 Figure 12. Micro hardness micrographs

622 (a) Quartz micro hardness micrograph 1050HV0.1 , (b) Anatase inclusion micro hardness micrograph 570 ,
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623 (c) alumina inclusion micro hardness micrograph 1930 HV0,1 and (d) Hematite inclusion micro
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624 hardness 370 HV0,1

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626 Figure 13. Infra -red spectrum of Tihimatine quartz

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Solid inclusion
Fluid inclusion Solid inclusion

Micro crack

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Fig 4.
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Muscovite

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Fluid inclusion

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Fig .9

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LIST OF TABLES
Table 1. The average impurities content in quartz for Si production .[5]
Table 2. Oxide composition of Tihimatine quartz % (QT1, QT2, QT3, QT4, QT5).

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Table 3. Carbon rate

Table 4. Vickers hardness

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Table 1

Element Quartz
P <5-50
B <10-45
Fe 1000-1500
Al 300-3200

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Ca <75-160
Ti 20-200
Mn 3-600

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K <75-1700
Mg 20-140
Na 50-170

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Table 2
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Samples SiO2 Al2O3 Fe2O3 CaO MgO Na2O K2O TiO2 MnO P2O5

QT1 97.72 0.25 1.46 0.06 0.05 0.10 0.05 0.05 0.01 0.05
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QT2 98.08 0.25 1.28 0.05 0.05 0.14 0.05 0.05 0.01 0.05
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QT3 97.80 0.23 1.45 0.05 0.05 0.12 0.05 0.05 0.01 0.05
QT4 97.88 0.30 1.53 0.06 0.05 0.15 0.05 0.05 0.01 0.05
QT5 98.10 0.28 1.26 0.05 0.05 0.10 0.05 0.05 0.05 0.05
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Table 3
C

Samples QT1 QT2 QT3 QT4 QT5

0,055 0.050 0.040

0,059 0,039
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0,045 0.045 0.044

C (%) 0,060 0,045
0,065 0.049 0.053
0.055 0,068

Table 3

Samples QT1 QT2 QT3

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881,5 554 922 ,2
932 858 548,5
HV 552,8 388 402
0,1
400,38 900 1850
1900 1800 899,9

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Highlights

Quartz is the most abundant mineral in the earth

Geology of Tihimatine (HOGGAR) was study.

Traces elements impurities in quartz are its most important quality criteria in the silica for it suitable
uses.

Anatase, muscovite, hematite, graphite was determined by several characterization technics.

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