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    Silicon Production Process

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    7 views7 pages

    Silicon Production Process

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    Puturrú De Fuá
    Silicon Production Process

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    © All Rights Reserved
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    US 200902633071 IM | A us United States a2) Patent Application Publication 10) Pub. No.: US 2009/0263307 Al Nanis et al. (4s) Pub. Date: Oct. 22, 2009 Ga). SILICON PRODUCTION PROC Publication Classification (31) ner, (73) Inventors: Leonard Nanls, San Jose, CA (US): Shi Yuan, Darille. CA (US), coiB 3432 200601) Matthew Sakae Forkin, San Cole 3302 (2005.01) Mateo, CA! Correspondence Address: (2) Us. 423/350; 425/932; 42333 Meyer Solar ‘Attn: Bdward 8, Sherma ‘One Meyer Plaza “7 ABSTRACT Vallejo, CA 94890 (US) An improved process forproducing high purity i (3) Assignee: CIRCULON HUNGARY L fom the reaction of sodium with pure silicon te Budapest (10) ‘28, which produces sodium nore as a by-product. The silicon tetrafluorde pas is formed by decomposing sodium Ql) ApplNos — 12i425.714 fluorosilicat. The sodium furosilicate is produced by pre= cipitation when fuorosilcie acid (FSA) is reacted with the (2) Filed Ape 17,2009 by-product sodium ficride in elosed loop proces, Likewise, r the fuorosilicie acid is preferably formed at high purity usin Related US. Applic ‘source matral that Consist essentally of sia by ating (60) Provisional application No, 61/045,906, filed on Apr, the by-product sodium fluoride with an acid to ereate reactive 17,2008. Fuori ions n Data US 2009/0263307 Al SILICON PRODUCTION PROCESS. (CROSS REFERENCE TO RELATED APPLICATIONS, 10001] The present application claims priority to the US provisional pplication for "DUAL. PURPOSE SILICON” having application Ser. No. 6L/045.906, which was filed on Apr 17,2008, and which s incorporated herein by eference, BACKGROUND OF INVENTION 10002] The present invention relates toa method to make pure luorsilcic acid (FSA) asa precursor feedstock forthe production of pute silicon fnorosiicate (SPS). The invention also relates to an improved process for making metalic sili ton from SES. 10003] "When heated, the pure SFS provides pure gaseous silicon tetrafluoride for reaction with sodium metal, Yielding pure silicon asa product 10003) _Therapidly growing silicon solar cell industry com- Petes withthe semiconductor industry for silicon, which is thus in shor supply. The purity requirements for solar grode silicoa are different ftom those of semiconductor grad sili con, Whereas very low levels of phosphorus (P) and boron (B) fre desirable in semiconductor silicon, less pure silicon with ‘much greater intial Pand B content canbe tolerated for solar arades. A known resction sequence for pricing low cost silicon string with low cost FSA by-product from the phos= phate frilizer industry also carries over P and B to precipi {ated SPS and to end product silicon which thus limits use to solar cells only. 10005] | What is ncoded isan alternative low cost source of clean FSA with low levels of Pand B to replace phosphate Ierilizer by-product FSA. 10005] 11istherefora fit object of thepreseat inventionto provide to increase the supply ofhigh purity silicon whichean serve the dal purpose of meeting the purity requirements of both the semiconductor and solar incites 10007] tis anather object ofthe present invention to pro- Vide an improved process for manafactring seh high purty silicon wherein reaction by-products are reeyeled in a sub- stantially closed loop system, SUMMARY OF INVENTION 0008] _In dhe present invention, the frst object is achieved by providing a process for synthesizing fuorosilicie acid comprising the steps of providing a source of silicon consist- ing essentially of silica, providing a source of huride toa, providing a source of sodium ions, reacting the source of Silicon withthe Mvoride ions to form Morosliie acid (PSA), reacting the sodium ion with FSA to precipitate sodium fuo- rosilicate (SF) and generate hydrofluoric acid, and sepaat- ing the precipitated SES from the reaction mixture of the previous step 10009] A second aspect ofthe invention is characterized by a process for synthesizing silicon comprising the steps of providing a souree of silicon consisting essentially of silica, providing a source of furide ions, providing souree of Soddum ions, reacting the source of silicon with the fluoride jonsto form Muorusilicic acid (FSA). reacting thesodium ions ‘ith FSA to precipitate sodium orosilicate (SES) and gen- eae hydoflooie seid, separating the precipitated SES from, the resction mixture ofthe previous step, decomposing the Oct. 22, 2009 ‘SES to generate silicon etraifuoride pas, reacting the silicon tetraluoride ass with Sodium t produce metallic silicon nd sodium fluoride. [0010] Other aspects ofthe invention include r-cycling the sodium fluoride andor hydroluorie acid by prods for reaction withthe source of silicon that consists essentially of phosphorus and boroa fre sla, [0011] The above and other objects, effects, Features, and advantages ofthe present vention will become more appar fent from the following description of the embodiments thereof taken in conjunction with the accompaaying draw ings. DETAILED DESCRIPTION [W012] One aspect ofthe present invention is @ method to ‘make pre facrsiici aid (FSA) a precursor feedstock forthe production of pur sicon Buowoslicate (SES), When Ingated, the pure SFS provides pure gaseous silicon eral ‘ie for eatin with dium met, yielding pre silicon as 9 pc The rapidly growing sion soar el industry com pees withthe semiconductor industry for icon, hich is thus in short supply. The pity eguiemnts for solar arade silicon ace diffrent. from those of semiconductor grade sl on, Wheres very ow levels of phospoas(P)andboren (3) fre desirable in semiconductor silicon, les pre silicon with ‘och greater inal Pad B content canbe tolerated for salar dgndcs. A known rection sequence fr pradicing lw cont stating with ov cost FSA by-product from the pho ‘phate Ferlize inde aso caries over P and B to peep fated SPS ano end pric silicon which ths imits we 0 solar cll ony. What is needed san alternative low cost Source of clean PSA with low levels of P and B to replace phosphate fertlierby-pduct FSA. The goa of his sven tions inzrease dhe supply of high purity silicon which ean seve the dal purpose of meeting the purity requirements of ‘oth the semicondoctr and solar indies. [0013] There isa plemil supply of FSA. a by-pret of phosphate ferilizer manufacture. The se oF by-product FSA, Bs the hss for several US patents, now expired obtained by SSRI Internationa forthe chemical redction of sion te raflurde by sodium (440.082; 4.584.181; 4.590083 4,597 948; 4 642.228; 4 685,827; 4755,783 and 47,030), all of which are incorporated een by relerence [0014] Commercial grade (23 wejaht perwent) FSA isthe Starting feedstock for the process steps described ia pare ‘ph [0001], a5 reported in FIG. of the joumalaicle ‘ntd “Silicon by Sodium Reduction of Silicon Teeth: de" J. Eleciocherical Society. vol. 128 (981) pp. 179 14 authored by SRI Intemational escrehers, whieh sso incorporate herein by relerece {0013} Porconvenienes the processis herewith ers to fsthe “SRI process” Simi Now chaats ae inchidd i the above-mentioned SR paca, x for example FG. lof US Pat. No. 4.748014, which is also incomporated hersin by reference [W016] As stating input to the SRI process flow chart the profemed foalstock is identiied as commercial ere 23, ‘neiht percent FSA, a by-produet ofthe phosphate flizer ind n the fist sep af the SRI proces, sium ion is sudo PSA to precipitate sodium Moosicate (SES). The properly chemically balanced precipitation reaction using Soli sodium Moride (NaF) asthe source of seu fon is US 2009/0263307 Al 10017] Sodium tluorosiliate, SES, is also avaiable com- ‘mercially in the form of dry. non-hygroscopic powder. pe cipitate from commercial grade FSA by the addition of som ion in a manner similae tothe first stp of the SRT process, the above-written chemical equation {W018} Other investigators of the reactions underlying the SSRI process also consider by-praduets ofthe phosphate fer tlizer industry as the source of silicon. In U.S. Pat. No, 4446,120, which is ineooporated herein by reference Schmidt ct al. begin with almeady precipitated SES and describe heated SPS as asouree for gascous silicon tetrafhuo- Fide for redvetive reaction with sodium metal (see present Equation 2) Schmidt etal. note {col lines 34-36] tat “One readily available source of silicon is sodium fvorosilicate (Na,SiF,) which is a by-product ofthe phosphate fertilizer 10019] As stated in the background section, a purpose of this invention is to obisin low cost, clean FSA (and SPS) ‘which will avoid the P and B impurities associated with F by-product of the phosphate frilizer industry. 10020) However the "we-process” forphosphate fertilizer ‘manufacture contributes phosphorous and boron as impuri- ties to PSA and ultimately to SPS and to sodium reduced silicon, The wet process is yo-named because sullurie acid reaets with phosphate oreto yield the desired phosphoric acid snd difficult to dispose by-products FSA and ealium sll (eypsum). The present invention recognizes that the ehemis- ley of the side eaetions that yield by product Tiguid FSA and solid gypsum may be isolated and hamessed so as to produce loan FSA and thas clean SFS and silicon, 10024) The present invention uses naturally occuring pure silicon dioxide (silica) asa low cost sourceof FSA, Pure ica js abundant and is less expensive per weight of contained silicon than commercially available FSA, Thekey ingredients to produce elean FSA ate the combination of stiea, an oid, preferably sulfuric acid anda source of uoride on, prefer- bly ealeium fluoride uorte) or more preferably sodium fMuoride. By-product sodium fluoride from the sodium metal reduction of silicon terafluoride (Equation 3) can provide a recycled source of sodinm fluoride. Conversion steps of FSA lw SFS tosiicon will beable to avoid phosphorus and boron, ‘other impurities associated with phosphate by-product FSA. The purty of silicon produced starting with the PSA of this invention may qualify it for dual purpose use oth for semiconductor devices and solar cells BACKGROUND 10022] 11s attractive to consider the ecological benoit of oblaining silicon from the waste material penerated fom the Phosphate fertilizer industry. In addition, the cost per ilo- fram of contained silicon is remarkably Jow when waste Muorosliie cid, FSA, serves as the source. While fuorosi- lici aed derived from the fertilizer process is an admirable source on an ecological basis and also a cost basis, impurities tre present because of the very nature of the source materi These impurities can be tolerated inthe conventional uses for PSA such as sn alive to Adoridate municipal water sup plies and in ceramics technology. However, fr silicon po duced with FSA as a stating feedstock, seemingly minor mounts of eeriin impurities are detrimental to performance in solar cells and also semiconductors. 10023] In brie, silicon obtained from waste by-product FSA contains high proportion ofthe elements boron, B, and phosphorus, P. Roth Band P are active ingrients diffe Oct. 22, 2009 purposely into silicon waters (doping) inthe fbrication of Solar cells For example, Pis frequently diffused into silicon te define the n-p junction, typically 10 a depth of about 4000 "Angstrom, The requirements for low background B and P ‘concentration levels in semiconductor stactures are more ‘Stringent than for solar applications, For semicondictors, 3 Jow initial level of impurity Band P is desirable as a comve- nient reference starting point for controlled process doping additions. 0024] When by-product commercial grade FSA is the feedstock, the elements B and P transfer t precipitated sodium fnrosiicate (SS). The mechanism of tansfer from FSA to SFS and then to silicon has aot been studied in any reat detail [0025] _ goal ofthe present invention sto developa simple cans to get the P and Boutofthesilcon inonder to have dul pParpose material for both photoveltaies and semiconductor ‘wafer fabrication, Methods have been suggested in the itera ture for purifying commercial ESA such as the use of mem- ‘branes. However, the present invention is a simple and srsightforward method to reduce [and P content by com pletely avoiding these elements atthe very frontend of pro 0026] ‘The present invention provides a novel path to get clean PSA by modifying and. controlling the secondary ‘chemical retions that wenerate FSA asa phosphate fertilizer Iy-product. lasted of phosphate rock, the starting material forthe present invention is clean, lowcost silica asthe pri- mary source of slieon, Better eontol of the FSA procing reactions is oblained by starting with a defined amount of siliea and fluoride ion rather than depend on the highly vari- ablecuotent of siliceous material in phosphate rock ore. Addi tionally, the present invention permits improved control of the reaction rtey pre-selection ofthe particle sizeof puresiica and also of solid Auride compound added to provide the fluoride ion required forthe formation of FSA by acid diges- tion of silica aecording to Fgn 2B. Fluoride ion for silica digestion may also be obtained from the solution of NaF resulting from aqueous Feahing used to separate the mixture ‘of solid NaF and Siproivced by the Na Si reaction Eqn 4 ‘Source Chemistry 0027] It is helpful to briefly consider the mineralogy and chemisey of phosphate rock mining as baekground forthe present invention for obtaining extra pure FSA and SPS. The key ingredient in phosphate fertilizer ore i the mineral “apa lite” also known as “uoroapatite”, which i ealeium Buoro- phosphate with the chemical form [0028] Nore that silicon is not part of the apatite crystal seture, The silicon isin different rock, principally sil cates and silicon dioxide (quartz) which just happens to be ‘naturally mixed in with the phosphate-bearing rock. In adi tion to the minerals quartz and apatite, the ore may also ‘contain calejum carbonate, CaCO, the mineral “caeite™ 0029} Inthe wet process" of phosphate fertilizer proiue- tioa, wo rections aceur simultaneously whea sulfuric acids ‘added to apatite in the ore. The first reaction is shown in Ea, 2A the second in Egn 28, (Ca4PO,sF8H, 90,731, PO CSO HE) 2a) S0,61"46F 8921.0 es) US 2009/0263307 Al 10080) As spatite minerals tteked by sue seid gn 2), the Morne component ofthe apatite ofthe mineral is solubilized ino the aqueous aidsolutionas orien. Egn 2A is a plasibl overall chemical sequence tsefl forthe purpose material balance calelations altho its wader ‘ood that he overall chemistry may be composed o vera dntermediate eaction steps Its pono thatthe foride jon released fom the apatite and some ofthe hydrogen fon from the sure acd temporarily associat in solton, pro viding a chemical activity equivalent hydrolase GF). The aeidfed faords Yon immediatly proceeds 10 attack ay silica present to form the by-product FSA acon dng othe reaetion in Egn 2B. The reaction beeen sulurc acid and apatite forms phosphoric acd (he desired fertilizer product) and also by-product ealeum sulle CaSO, (asp Ss) [031] White sulfric acid is the source of hydrogen ions conventional used in phosphate processing, the hydrogen Jon can come ftom other acids 28 well {0032} there were mo silica inthe ore there would Be 0 wanted by-product FSA from the "welproces” acid digestion of apatte-bearing phosplate feliz ore. The pesca inenton focuses on silica othe main constituent br Shemicalreaetion aevoning 1 gn 2B, essentially com- pletely removing any source of phosphors. The Muon no Ionger available fom apatite is provided separately throvah fvorde compounds added tothe reaction in amounts eae Into etetvey match the mass osiicabeing ote, The balancing of reaction chemistry will desirably provide for close contol ofthe Fan 28 reaction 10033} Asstaedthepreseatinventonisto purposely make TSA asa primary reaction product without geting involved ‘with phosphate ore chemist. Carefully selected sic wil Servers the source of silicon and a selected Maori come pound will provide Suorine foe ISH, (FSA), Paty wl be ‘ainsind nthe subsequent reaction fo forma precipitate of STS by the use of selected pure sourees of sodium ion. Recycle by-prstct sodium boride (NaF) frm the eaction| oF Fan 4, that is the process of using the SPS w generate (SiCI4 Si, for ection with iid sodium wo produce Sic con metal aso frie (NaF), will preferably serveas a suitable source in preference wo the NAF residue of STS thermal decomposition (Eqn 3) which wil retain any’ non volatile imports, Impurities 10034) The main impurities of concer for semiconductor applications are Band P Typical concentrations of B and Pia have been reported by Chioti(The Pseudobinary System NaF-—Na.Sif,, 1. Less Common Motals, 80 (1981) pp. 105-113. Chiotti analyzed two commercial sources of SES by indvetively coupled plsina spectroscopy and found 3120 parts per milion by weight (ppmt}of I in. sample from the first source and 65 ppm B from the second source. The frst sample aso had 3000 ppmvt P, while the second source sample had 2050 ppmst P-Chiot also reported aluminum as ‘umajor impurity in commercial rade SFS with 1250 pprmwt ‘AL inthe fist source sample and 930 ppm inthe second ‘source sample, 1 js noted tat aluminum is aso a frequently used dopant for silicon in semiconductor technology: 10035] "Anadvantageofusing the dermal decomposition of SS (Lign 3) to provide silicon tetrafluoride as the silicon= ‘containing reactant for reaction with sodium (Eqn 4) i that ‘non-volatile impurity compounds remain in the NaP revue Oct. 22, 2009 ‘and do not transfer over into the rector However, some Band P is known to transfer to the silicon produced by’ reaction between sodium and silicon totauoride (Eqn 4) Following ‘generation of Si. from thermal decomposition of SFS (Eqn 3) NSS ONE ® sNassie- Sie oy 0036] An indication ofthe amount of B and P that ean be transferred to Si in the sodium reaction (Eqn 4) (3s reported by the SRI group, J. Electrochem Soe.v 128, 1981 p 179) is, shown in Table I, together with ata determined by Chioti for ‘commercially prepared STS. [0037] While relatively high levels of B and P may be tolerable for photovoltaic silicon itis instructive 1 compare ‘them in Table I with the B and P levels customarily encoun- tered in “pure” silicon vsed for semicondictor device pro- cessing. ‘able 1 also includes concentrations of B and P in 'SESprecipitated fom commercial grade FSA, as reported by SSRI, supra TABLE 1 Boron Photons SHISTS pipe yan ao us ‘SRisiion, tom Nave wit SF, Rge-4 at 02 Low impunity sensoniasorS (Dio th DOS 2 toms pres} 10038] ‘There are major differences shown in Table | for impurity levels in commercial SPS (Chiot) as compared ‘with SS precipitated by SRI from commercial grade FSA. In, “addition, the coacentrations of B and P reported by SRI ia, Silicon produced by reaction of sodium with Si. (Pn) are ‘well above the levels in semiconductor grade silicon. For the purpose oF comparison, Table I lists ppmavt for dopant eon- ‘centration, converted from number of atoms per cubie cent ‘meter, he units preferred by the semiconductor industry 0039] Forsemiconductorgradesiliconat the start of wafer processing, Le. before B and P doping, impurity levels are Iypieally slow as 10to the [Shor Lath (10" of 10") atoms per cubic centimeter, Highly refined float zone silicon can Ihave as Tile as 10 0 the Lh (10") atoms per ee of boron, For the phosphorus example shown in Table 1, 10 the 1th (10°) atoms per cubie centimeter isthe equivalent of 0.002, parts pee million by weight, clearly well below the P levels in silicon produced bythe reaction in Eqn 4, a8 reported by SRL [0040] Silica as he Source OF FSA and SES 0041] As mentioned, the present invention will minimize Pana impurity levels inthe final silicon product by making ‘lean FSA and SFS. The staightforward approach of pener- ating Hresly made FSA starts wih pure silica as feedstock Pure silica with 99.7 weight percent or hotter SiO. is com- ‘mercially available in several forms aod is in abundance throughout the world [0043] "Silica is reacted with an ac, such as hydrofluoric acid orsulfurie eid plus NaP to forma wource of fuoride ions that react with the silica o form several by-products that can ‘be used or purified o fom Silioon Tetrathuoride STF), When the acid is sulfuric acid (H,S0,) there are three reaction US 2009/0263307 Al pathways possible, Fans 5-7. The approximate yields forthe ‘Muorine compound products dseussed below are based on ‘ypieal yields experienced for similar reactions in te indus teal production oF SFS, SOI, SOg4NAE Sy ° $10,120,590 +684F +N, Sif tN SO2,0 6 Si0,31,90,¢68AF o,f, S0 2140 o 10043] The silicon tetafluoride gas liberated in Eqn 3 ‘ight represent only about 13% to 28% ofthe Muorine from the Na starting component, with the SFS produced in gn 6 might cepresent about 40-50% of the fvoine from the NaF starting component. The silicon tetrafivorde gas can be wsed directly w produce silicon if sulieiently pure, or reacted further to produce SPS by frst reacting With water to form FSAae Sg i2ILO=21LSiFeAS0, ® and then precipitating SFS fom the FSA a in Eqn 1, orn saturated sodiim chloride to form SES sad LIC, a H,Siyr2NiCI-Na, SHC » [0044] Likewise, the FSA formedin ga 7 canbe converted {SPS asin Fgn 9. Fgn 7 might account forabout 35%%-45% of Muorine available in the starting compound, 10045] It should be apparent that SES ean be derived from, ny of the three reactions in Eqns 8, 6 and 7 10046) tis most preferable from an economic standpointto derive the SFS from allof these reaction, bu may'be es haa prictical depending on the actual yield in production and the dificult in separating out the by product acid sats, such a5 sium sulfate i the above examples 10047] Tt should be noted that although the above com= pounds and routes are preferred, the sodium salts may be replaced by other alkali earth metal silts such as cal for ‘non-limiting example. [0048] There are many grades of silica that may be suitable orrevction according to Eqn 2B, ranging fom finely divided silea flour” to clean quartz sand used in plas prosetion While the preset invention offers path to proce a dal purpose solar-semiconductor Si with B and P at lor levels, Some silica soures almost certainly include other impurities Such as Glanium andl iron that are known to be undesirable for photovoltaic use. Trace amounts of impurity elements with multiple valence states reduce solr cell efceney by trap- Ping the electrons produced by solar photons. Slice as a Source for dual use silicon can be selected to have minimal traces of any undesirable impurity elements 10049] As an example of typical impurity levels i silica, the unground silica sand grade supplied by USS. Silica Corp. as #1 DRY has panieles with more than 80 percent inthe size ange from 0.2 t 0.3 mm. Chemical analysis indicates 99.7 ‘weight percent SiO, with Fe,O,, 80.024 weight percent (wt 6), xO, 210.07 wi % and TiO, a 0.01 8% Otherelements reported oxides ator below’ 0.01 wt % include ealeinm, ‘magnesium, sodium and potassium, Any impurity elements eatried over into the grantlar silicon peediced by eacton of SIP, with Na gn 4) will havean opportunity for additional removal during the growth of large ingots by the refining provided typially by the Czochralski (C2) ingot grovth method. 10050] 1tis of interest to now that silica serves a the Feed- stock for “pure silicon made by purification of metallurgical Oct. 22, 2009 ade silicon (abbreviated as mgt), Metallurgical grades cons made by carbothermic reduction ofa mixtureof carbon and silica in high temperature fumace. However, mgSi has relatively low purty, typically 97 weight percent Si Refin- ing treatment is require to improve the purity of mig. High {temperature mgSi prodtion and purification requie a sab- ‘tamil energy input. By comparison, the present invention involves low temperature aqueous reactions ator near oom ‘temperature in tanks constricted of reatvely'Tow cost mate als, [0051] FSA generation takes place in an aqusows mixture ‘faci, silica and fluoride. Likewise, precipitation of SS by ‘adding sodium ion to FSA takes place in an aquecs medium, Tow temperature processing minimizes the opportunity for impurity transfer tothe produet which ca occur i. high Temperature operations. Its also noted that the Na Si, reaction (Eqn ) is exothermic and provides is own heat 35 reaction prococds, The present iavention contributes 10 ‘energy savings a= wells theoppartanity to obi igh party Starting materials FSA and SES forthe prodction of pure silicon. 0082] | Cost Comparison: PSA from Silica vs. Commercial FSA 0083] Since FSA is the starting point for precipitation of ‘SPS and sodium reduction of gaseous Sif, an equivalent way To evaluate silica as silicon source isto compare the present ‘cot of commercial FSA (and SPS) with the ras material cost for pricing florosicie seid by the method of the present inveation, This is not an exact comparison because process costs and profit margin are inchided inthe price of commer cial FSA and SPS and aot in the present cost calculations ‘hich are based on materials only. However, reactant costs ‘permit he calculation ofa minimum base line cost to produce lean FSA. [0084] Table 2 shows the cost benefit for using silica as Silicon source by comparing the amount of silicon avaiable fom various sources and the associate cost per kilogram of available silicon, Other reagent costs are also included to ‘oblain an overal estimate forthe pure silica approach of the present inveation, Tape? Dalamig pasta an sows Maia swasctu Sion “Avtigst horse Ase ame ass coed FS 0% Gina san, iis, S103) cu Intelsat lee 0) 0038 EsSiiedtD (SO) 00 Bem eam mea emensl 020 am ‘sigue herman {0085} Soures of stcon tht consist essentially of silica inchude, without limitation, glass sand, filler sand, industrial snd, diatomaceous earth, reeycled ground glass and the like. From Table 2, iis clear that silica is literally dirt cheap 2s 8 source of silicon on the basis ofthe cost of sila suicient 0 Yield I kgof silicon, As mentioned, the present invention does US 2009/0263307 Al not noo apatites a source of ore on for the revetons described in Fans 24 and 2B. The chemist of Ean 2A is simplified by substiuting a seevted soure of rie on in the formof a eadily soluble compound with no phosphorous [0056] For the purpose of calcultion based on Euston 2B, thorpar (CaP) designated a Te source of foride ions Acid grade Nuorsparn97% CaF ndcots $220 perton (2o06 price). Theamotnt of CaF, noodod is 2324 kamal for 28 kamal of silicon or 144 kg-iol of 10026 FSA, Since 4.9 ig of H,S0, are nowded foreach kg of SiO, according to Equation 21 the cost of sulfrie aids 80.635 per Kilogram, of Stand the cost of Morspar is $2,022 per Kilogram ofS. [087] Adingthe costo! sfc acd and caleium fooide toreavtwithslca, the oa costs 82.706 foronekilogramot Sitshen silica s US Sica Comp. #1Dry. The major cost tem the Muorpae followed by slr eed, with ica at less than 2% of mater costs, The eleuated 82.706 perk Sis shout half the cost of either commercial FSA oF SFS on a comparable bass aw source foe 1h Si [0038] Forspar is considered asthe forine source only asan example Inmore prefered enbeximents of the inven- tion the sodium Muoedeby- proce rom the Na—SiP, reve tion (Eg 4) is recycled serve as the Moorne source the gn 2 silica digestion reaction. This embestiment provides the potential fora substantially closed loop manfctring process wlere the re-eyeling of sich by-products reduces fosts andthe ned fr shiaent of the by-product © other Users Likewise, HF produced in Bg | ean be re-

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