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ISSN 1062-7391. Journal of Mining Science, 2011, Vol. 47, No. 6, pp. 850—860. © Pleiades Publishing, Ltd., 2011. Original Russian Text © A.P. Kuz’menko, I.Yu. Rasskazov, N.A. Leonenko, G.G. Kapustina, I.V. Silyutin, J. Li, N.A. Kuz’menko, I.V. Khrapov, 2011, published in Fiziko-Tekhnicheskie Problemy Razrabotki Poleznykh Iskopaemykh, 2011, No. 6 pp. 131—143.

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Thermocapillary Extraction and Laser-Induced Agglomeration of Fine Gold out of Mineral and Waste Complexes A. P. Kuz’menkoa, I. Yu. Rasskazovb, N. A. Leonenkob, G. G. Kapustinac, I. V. Silyutinc, J. Lic, N. A. Kuz’menkoa, and I. V. Khrapova a

South-West State University, ul. 50 Let Oktyabrya, Kursk, 305040 Russia e-mail: [email protected] b Institute of Mining, Far East Branch, Russian Academy of Sciences, ul. Turgeneva 51, Khabarovsk, 680000 Russia e-mail: [email protected] c Pacific State University ul. Tikhookeanskaya 136, Khabarovsk, 680035 Russia e-mail: [email protected], e-mail: [email protected] Received January 20, 2011 Abstract—Interpreted data of the phase analysis of the Far East ore bodies made it possible to characterize rebellious behavior of ores under study. The researchers propose an integrated flow sheet composed of gravitational preparation, flotation and metallurgical processing flow sheets for beneficiation of rebellious auric-arsenical ore, and present the beneficiation parameters for ores of moderate sorption capacity. Key words: rebellious ores, phase analysis, flotation, cyanidation, integrated flow sheet, carbonaceous matter, sorption leaching

INTRODUCTION

The currently sustained high-rate, gross mineral extraction has drastically depleted mineral resources and deteriorated geological and technical conditions of mining operations. It has particularly affected the easily accessed, rich deposits. This calls for involvement of rebellious ore formation, or fine dispersed gold placers into development, or those waste formations appeared as a result of open or underground mining operations. Traditional mineral preparation techniques are not efficient in such cases, governed by crystalline feature and isomorphism of minerals, secondary mineralization impossibility of opening of mineral accretions, etc. [1]. Ore disintegration takes almost 70% of total energy spent to ore processing. The worsened quality of ores, due to greater volume of aggregates (up to 30—45%) and smaller size of mineral inclusions (down to submicrometer dimension; less than 40 μm for gold), initiated the research into improved ore disintegration technique [2, 3]. The use of microwave, electric-pulse, magnetic-pulse and electrochemical treatment, as well as electrodynamic and shock action allows processing of mineral compounds with nanometer size gold inclusions. For instance, the nanosecond electromagnetic-pulse exposure of preparation products results in the maximum gain in gold recovery [3]. The authors [4] offered an integrated solution to the problem of noble metals dissociation and higher sorption of disintegration products under ultrasonic electrons treatment. Higher quality of disintegration of pyrrhotine, for example, as well as improved floatability and sorption activity of defragmentation products can be achieved, alongside with the powerful nanosecond electromagnetic pulse action, by

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chemically activated ozone dissolved in a water film at the surface of particles [5]. Copper-nickel ore was used to analyze an electrical blasting treatment that is a combination of disintegration and sizewise separation of conductive products [6]. Disintegration should also account for mineralogicaltechnological versatility of gold-bearing minerals. For instance, for high gold pyrite (more than 9 g/t), it is efficient to use its selective extraction first and then the gravitational flotation scheme [7]. The flotation separation of pyrite involves organic complexing agents [8]. Disperse gold processing may be improved by electromagnetic, including laser, radiation. To intensify opening of gold-bearing mineral phases in the sulphide ore of the Kokpatas deposit, the photoelectrochemical treatment of the pulverized mixture is used [9]. Bacterial oxidation combined with electrical-activated sorption leaching boosts fine gold recovery from sulphide ore to 23%. The ultraviolet exposure of polymethyl acrylate matrix doped with aurichlorohydric acid revealed gold particles 100 nm in size [10]. In [11] the argumentation was presented in support of possible massspectrometric determination of gold micro-inclusion in sand exposed to infrared vaporation by a pulsed laser beam spot 20 μm in size (wavelength 1060 nm). Every 2 ns pulse evaporated ≈ 5·10–4 g gold. A summary of the research of physicochemical characteristics and light-induced reactions with synthesis of nanoparticles of transition elements—copper, silver and gold—from complex compounds is given in [12]. It was found that number and dimension of the resultant clusters are governed by the ultra violet radiation intensity: exposure of a millimeter-thin layer of a complex compound to 1015 quantum/cm2 produced a cluster up to 40 nm. The method of laser treatment of particulates, including gas atomization and exposure to downward and back laser radiation at wavelength other than the wavelength of intense gas absorption line, using fast heating and cooling of particulates by varying the laser radiation parameters was proposed in [13]. The authors of [14] observed agglomeration of ultra fine and colloid-ionic noble metals in mineral associations under radiation by spread-out laser beam 2—5 mm in diameter. Initial, mineral and waste products were subjected to different regime radiation, at different wavelengths and intensities. It was always succeeded to create laser agglomeration conditions for the diverse ultra-fine gold-bearing inclusions. The present study, based on the comparative analysis of examination of mineral and waste compounds in high-clay sands with particulate gold before and after laser treatment, has established the gold particulate shape, structure and composition that allow further gold recovery by conventional gravitation without ecologically unsafe techniques involved [14—16]. The best contributing to the fine gold extraction is suggested to be the thermocapillary mechanism [1]. 1.

THE TEST PROCEDURE AND OUTCOMES

The targeted tests accounted for the wide range of mineral and waste products containing gold impossible to recovery traditionally, as this gold is in ionic, ultra-, fine- and colloid-ionic form, as well as the mineralogical characteristics of different deposits. The samples to be tested are described below: —Sample 1: natural (gold-bearing high-clay sands from Solovievsky placer); —Sample 2: uniform gold (– 1.6—+ 0.63; – 0.63—+ 0.315; – 0.315—+ 0.25; – 0.25—+0.1 mm); —Sample 3: bullion gold, fraction – 0.1 mm; —Sample 4: chemically reduced gold (particle size < 0.050 mm); —Sample 5: model clay, with uniform dust-like gold; JOURNAL OF MINING SCIENCE Vol. 47 No. 6 2011

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—Sample 6: model clay, with introduced ionic gold (yellow tint clay, fraction – 0.05 mm), fraction No. 5; —Sample 7: model clay, with introduced colloid gold (violet tint clay, fraction – 0.001—+ 0.0001 mm), fraction No. 6; —Sample 8: magnetite off high-clay sands from Solovievsky placer; —Sample 9: heavy, nonmagnetic sulfide-bearing, gold-bearing ore concentrate (Tokur deposit), fraction – 0.25—+ 0.1 mm; —Sample 10: heavy concentrate from high-clay Solovievsky placer sands (mineralogical composition of particulates: ilmenite, sphenite, garnet; pyrite, zircon; gold, fraction – 0.100 mm. Preparation of high-clayey Sample 1 involved: water steeping for 96 h; wet screening to fractions + 0.63, – 0.63— + 0.2, – 0.2—+ 0.1, and – 0.1—+ 0.05 mm. Finely dispersed fraction – 0.001—+ 0.0001 mm was extracted through vaporation of solid residual from water. The fractional makeup of Sample 1 is given quantitatively in Table 1. While fractioned, the samples exhibited color change of the particulates belonging to different fractions; for examples, Sample 6 contained violet particles in fraction of 1—0.1 μm, which is an evidence of colloid gold presence, while Sample 1 particles and Sample 5 particulates were yellow color. Assaying determined the content of noble metals in Samples 5 and 9 (Table 2). Sample 5, aside from gold particulates smaller than 50 μm, contains silver 4.6 g/t. The heavy, nonmagnetic sulfidebearing concentrate shows high content of gold, 573 g/t, and silver, 197 g/t (refer to Table 2). RMS error δ in the metal content range (2.0—4.9) g/t is 15.2% for gold and 38.5% for silver; for wider range of metal contents, δ is less than 3.6% and 11.4% for gold and silver, respectively. The laser radiation tests over Samples 1—10 included: (1) СО2-current-wave laser ( λ = 10.6 μm, power to 1.0 kW, transverse mode ТЕМ01); (2) pulsing laser based on neodim-activated ytrrium aluminum garnet (YAG:Nd3+) on machine “Quantum 15” ( λ = 1.06 μm, power from a few MJ to 1 J, pulse duration from micro- to milliseconds, frequency to 10 kHz, transverse mode ТЕМ00); (3) pulsing laser based on neodim-activated ytrrium aluminum garnet (YAG:Nd3+) on machine “Skat-301” (parameters equal to those of the machine “Quantum 15”); (4) fiber-optic ytterbium CW laser LS-06 ( λ = 1.061 μm, power to 600 W, transverse mode ТЕМ00). Table 1. Quantitative fractional makeup of Sample 1 No. of fraction 1 2 3 4 5 6

Size range, mm + 0.63 – 0.63—+ 0.2 – 0.2—+ 0.1 – 0.1—+ 0.05 – 0.05 – 0.001—+ 0.0001—dry residue

Weight, g 29.6 8.5 3.4 8.8 211.3 4.9

Table 2. The assaying results and RMS error δ Sample, fraction 5, fraction – 0.05 mm 9, fraction – 0.25—+ 0.1 mm

Gold g/t 2.3 573.0

Silver

δ ,% 15.2 < 3.6

g/t 4.6 197.2

δ, % 38.5 < 11.4

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The laser beam had nearly normal radiation distribution over cross-section and was defocused to 5 mm depending on the processes observed on each individual sample. Power sources allowed varying the pulse frequency and energy to reach the best efficient regimes of the laser high-speed thermal effect on the mineral particulates. Local laser treatment took no more than 30 s. In any case, the laser radiation intensity provided fast heating, melting and vaporation of the test samples. For instance, laser machine “Skat-301,” equipped with the regime program control, can treat an area 100×100 mm for 5—10 min. The smoothly varied intensity and duration of the machine pulses up to 1 MW/cm2 (at average power of 10 kW) and from 150 μs to 1 ms, respectively, enabled improved examination of interaction between coherent electromagnetic radiation and gold-bearing mineral objects. To find an optimum laser treatment regime, the pulsing energy, duration and frequency, as well as the focal distance and exposure time were varied. As a result, the best efficient laser treatment was under defocused radiation (spot 4—5 mm in diameter) with pulsing at 5 Hz for 40 s. The powdery initial gold-bearing products with fractions less than 1—200 μm were placed in a special-purpose graphite cell with a laser radiation input. The defocusing diameter was set under technological reasoning, to ensure the wider coverage of radiation and minimum gold loss in vaporation. The graphite cell bottom was shaped as a truncated sphere or a cylinder, which allowed additional focusing of the reflected infrared radiation in the middle of the treated dispersed sample. The short-pulsed laser treatment created fast heating conditions (without vaporation). As suggested, chemical reactions were speeded up to the velocities at which oxidation would certainly be behind reducing reactions [12].

Fig. 1. Halftone picture, Sample 10 (heavy concentrate), energy-dispersive spectrograms: Spectrum 1—garnet; Spectrum 2—zircon; Spectrum 3—amalgamated gold; Spectrum 4—particulate (spiny) gold.


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Fig. 2. Halftone picture, laser-treated Sample 10 (heavy concentrate), elemental analysis of titanium-zircon fractal formations (Spectrums 1 and 3) and spectrogram of agglomerated gold (Spectrum 2). The experiment was carried out with a fiber-optic ytterbium laser radiation source.

The elemental analysis of minerals composing the initial samples was carried out on the electronscan microscope “LEO EVO 40HV” and energy-dispersive analyzer “INCA-ENERGY” with the SEdetector and QBS-detector. The nano-scale of data on qualitative and quantitative distribution of the chemical elements was supported by the localization of the electron beam to ~ 20—30 nm diameter spot and its penetration depth to ~ 1 μm. Figures 1 and 2 show half pictures of the initial heavy concentrate before and after laser treatment. The laser radiation revealed structural changes in all the tested samples in the form of the agglomerated gold. Moreover, it was found that the agglomeration involved the whole sample, not gold only (refer to Fig. 2): for example, titan-zircon skeleton structures in the form of snow-flakes. Structure and size of particles in the samples before and after the laser treatment were examined using the electron-scan microscope “LEO EVO 40HV” and the atomic-force microscope “NTEGRA Prima”. The structural characteristics of Samples 4 and 5 are show in Figs. 3 and 4, respectively. The shown formations were observed under defocused pulsed laser beam (source 3), at frequency of 5 Hz, diameter of 2 mm and treatment duration for 40 s. Initial Sample 5 contained particles – 100—+ 10 μm of 1 g clay and 10 mg of plate-shaped gold, and was put in a graphite cell as a thin layer (to 3 mm thick). After the laser treatment, fused spheres 500 to 1000 μm in diameter appeared; at their surfaces semispherical formations 100—500 μm were observed, with gold-typical color and glitter (see Fig. 4b). JOURNAL OF MINING SCIENCE Vol. 47 No. 6 2011


Fig. 3. Structures in Sample 4 (reduced gold): (a) initial sample; magnification 4000; (b) a fragment of a large gold agglomerate after laser treatment, magnification 790; (c) agglomerated gold surface, magnification 8000.

Fig. 4. Pictures of Samples 1 and 5 (gold-bearing high-clay sands) before (a) and after (b—e) laser treatment; (b) Sample 1 pulsing laser radiation source “Quant 15”; (c—e) Sample 5, continuous laser radiation source “LS-06”.


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The same regime of the defocused laser radiation (beam diameter 3 mm, frequency 5 Hz, duration 50 s) of Sample 5 containing bullion plate-shaped gold – 100—+ 50 μm in size, with inclusions of quartz, zeolite, zircon and other minerals resulted in the formation of fused spheres with particles of 400—800 μm and melt tear drop-shaped gold at the surface of the spheres. The same-regime laser treatment of Sample 4 (reduced gold) with fractions smaller than 50 μm yielded also tear drop-shaped formations (Fig. 3). The diameters of the laser-generated spherical formations in the studied mineral and waste samples range from 500 to 300 μm, while the same shape granules that appear at their surfaces are much smaller (50—500 μm). Some of them are covered with a thin sheet (to a few microns thick) of agglomerated gold (initially fine) as follows from the energy-dispersion elemental analysis (refer to Figs. 3b and 3c). The defocused laser treatment of plate-shaped gold (Sample 2) resulted in the formation of spherical gold for monofractions – 0.63—+ 0.315; – 0.315—+ 0.25; – 0.25—+ 0.1 mm, while gold fractions 1.6—0.63 mm deformed. The defocused laser radiation of Samples 6 and 7 generated roast “buttons” with a visible purple transition zone, which indicates the reduced ionic and colloid gold. The laser treatment of Samples 8 and 9 also formed “buttons” composed of the sintered top part and the heavy metal bottom. According to the pulsed laser radiation results obtained on fine gold inclusions in the mineral and waste samples, the largest gold agglomeration is achieved under the defocused laser beam (spot diameter 1—2 mm) at the frequency of 5 Hz for 40 s. Depending on the treated sample composition, the laser power density and duration were varied up to 1 MW/cm2 (average power was to 10 kW) and from 150 μs to 1 ms, respectively. The parameters and regimes of the pulsed laser treatment are under Russian Federation patent [14]. The experiments on the laser agglomeration under continuous radiation using ytterbium fiber optic laser source “LS-06” allowed establishment of the efficient regimes. 2. DISCUSSION OF THE RESULTS

Visual observation of the laser treatment results shows 5 stages of the process (see Fig. 5). Stage I (t = 0 s, T = 300°С): laser source radiates special formed mineral or waste samples containing fine gold particles, placed in a graphite cell. In t = 5—10 s, T ~ 600 K (Stage II), after the easy-melt silicate phases have been melted, fine gold particles, like Brownian particles, start disordered motion over the surface of the appeared spheres, probably, under the greatly different surface forces of the melted material and unmelted gold particles. Under continued heat the gold particles melt and agglomerate due to mutual wetting under the chaotic collisions. Stage III (t = 10—15 s, T ~ 900°С): the particle motion decelerates by a factor of 2—3, and the particles grow in size. As known, with higher dispersion of gold, its melting temperature decreases to 200—300°С for the nano-particle, which probably would promote the decrease in the laser radiation temperature. Stage IV (t = 15—20 s, T ~ 1100°С) is characterized by formation of larger gold particles (Figs. 2 and 3), which is associated with the heating and higher energy of motion of the particles. In 25—40 s the laser treatment is ceased (Stage V) and the treatment products naturally cool down. The agglomerated gold particles predominantly have spherical shape corresponding to the minimum surface energy (refer to Figs 2—4). To explain qualitatively the obtained data, it is necessary to recall that the inner energy of the multicomponent substances depends on the surface tension energy of all of the included phases. The laser radiation power was set to be sufficient to melt all of the studied samples (e.g. continuous laser radiation power was set between 60 and 450 W). The observed structural transformations are thought to be caused due to the change in the entropy and volume of the treated samples, and the change in the mass (due to vaporation) or charge (during plasma formation) could be neglected. JOURNAL OF MINING SCIENCE Vol. 47 No. 6 2011


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Fig. 5. Stages of the laser generated agglomeration.

The total energy U for the discussed experimental conditions obeys the Gibbs—Helmholtz equation: U = [σ + qs ] S , where σ is the surface tension, qs is the heat of formation of a unit surface, and S is the surface area. This approach is feasible for the tested systems, in particular, since the noble metal melts have usually rather high surface energy, e.g., Pt and Au have 1.82 and 1.1 J/m2, respectively, whereas Pb has 0.453 J/m2. The tested ultra-dispersed mixtures contained particles larger than the critical dimension (smaller than a few nm [18]) when the dimension versus free surface energy relationship is better described with the Tolman equation. In liquid state n the tested systems, the boundary between phases should form according to the additivity concept (sol called Antonov’s rule): σ 12 = σ 1 − σ 2 , where σ 12 , σ 1 , σ 2 are the surface tensions of separate phases and their associations. Let us analyze the obtained results (refer to Figs. 2—4) in terms of the contact angle between the liquid gold and the melted mass. The surface tension of the liquid-phase heavy concentrate, σ 1 (Fig. 2a), is slightly less than σ 2 of the agglomerated gold melt. In this case it is partial wetting as the contact angle is somewhat smaller than π / 2 (Fig. 2a). The by-phase are alumina silicates as they dominate in the most examined goldbearing systems. The surface tension of the alumina silicates appears much less than the noble metals have. The laser cakes of high-clay sands with inclusions of fine gold (see Figs. 3b and 4b) have greatly larger contact angle as compared to π / 2 , since σ 1 is much lower than σ 2 . For the comparison: the heavy concentrates and high-clay sands have twofold differing contact angles, which agrees with their difference in σ 1 . Nearly in every tested system, it was noticed that products of laser melting had clear inter-phase boundaries. The fractal structures of zircon on the melted surface of the heavy concentrate in Fig. 2b are in good compliance with the conclusion that agglomeration process depends on the dispersion level of particles [19]. The nano-size gold film formed during agglomeration was within a few micron range thickness (Fig. 2c). On this basis, according to [20], it is assumable that one of the two capillary phenomena takes place, either the thermal-capillary or the thermal-gravitational capillary. Each phenomenon is proportional to the surface tension gradient ( ∂σ / ∂x ). Dominancy of this or that phenomenon is JOURNAL OF MINING SCIENCE Vol. 47 No. 6 2011

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governed by the Bond number that is the ratio of the Rayleigh and Marangoni numbers: ρ gβ h 4 / σ , where ρ is density, g is free acceleration, β is temperature conductivity, h is the layer thickness, σ is surface tension. The estimate of the Bond number, considering the known values of ρ , g, β , σ and the experimental data on the gold layer thickness (within a few microns range) appears much under 1. Based on this, it is concluded that the laser agglomeration of fine gold (and noble metals as like as not) includes the thermal capillary mechanism. The analysis of Figs. 2a and 4b shows that the gold macro-agglomerates are evenly distributed over the melting surface. The laser treatment necessitates high temperature difference in the treated products, that, in its turn, causes the surface tension force gradient. The said gradient would be noticeably higher in line of the tangent of the laser radiation beam acting as the heat source. The thermal capillary transition of particles may e oriented along the laser radiation beam if dσ / dT > 0 , and across it if dσ / dT < 0 , when thermophoresis is eventual [19]. The surface tension force gradient makes the fine gold particles move toward the melting surface; this motion will go with the uniform agglomeration of the particles until the visible thin gold layer is formed (see Fig. 2c). The more comprehensive analysis of processes happening during the fine gold agglomeration under the laser radiation is possible using the atomic force microscopy. Figure 6 shows the atomic force image of a fragment of the thin gold sheet (size 10×10 μm), obtained with the help of lateral forces method intended to detect and study deformations at a studied surface, which are clearly seen in Fig. 6. The goffering of the surface of semispheres and thermoelastic deformations at the surface of the agglomerated gold sheets (refer to Fig. 6) are associated with the thermal capillary mechanisms too. The surface tension forces, always directed to the free surface or inter-phase surface (the melting surface in the case discussed) may evidently cause volume convection. The convection goes with the changes in the normal stresses of the surface layer, which results in fine deformations. The observed deformations are size-comparable with the gold sheet thickness, the ruptures on the sheet are proportional in size to the sheet thickness square, which is in accord with the conclusions drawn in [20]. In a general case, such deformations may apprise under the effect of the local drops in temperature and due to inhomogeneity of compositions, which can partially explain the unevenness of the distribution and shapes (Fig. 6).

Fig. 6. The atomic-force image of a fragment of the agglomerated gold sheet generated by the laser radiation: (a) lateral force method, scan 10×10 μm; (b) the same fragment 500×500 nm in dimension, nano-structure formations not larger than 20 nm. JOURNAL OF MINING SCIENCE Vol. 47 No. 6 2011


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CONCLUSION

1. In the course of agglomeration of fine gold in mineral and waste products exposed to laser radiation, almost spherical submillimeter gold granules are formed. This method is of practical value, in the authors’ opinion, due to higher recovery of gold (above 90% as against presently 50%) and ecological safety, which will allow waste dumps to be included into the production process, as well as will mitigate environmental impact. 2. The proposed quantitative physical model validates fine gold recovery under laser radiation follows the thermal capillary mechanism that is higher efficient and rests upon natural processes, and favorably conditions the agglomeration. ACKNOWLEDGMENTS

This work was supported by the RF Ministry of Education and Science, State Contract no. 16.552.11.7027 for the research and development.

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