PATENT
FOR THE USEFUL MODEL
No. 19900
SILICON EXTRACTION METHOD
Issued pursuant to the Law of Ukraine "On Protection of Rights to Inventions and Useful Models".
Registered with the State Useful Model Patent Register of Ukraine on 15 January 2007.
Head of the State Department of
Intellectual Property (Signature) M.V. Paladiy
Round stamp: Ministry of Education and Science of Ukraine,
State Department of Intellectual Property
(54) Useful model name: SILICON EXTRACTION METHOD
(57) Useful model formula:
1. Silicon extraction method which includes extraction of high-pressure elemental silicon from chemical elements of aluminum and phosphorus by application of electric current with density more than 1011 A/m2 to the mixture of crystalline matters containing oxygen, aluminum, and phosphorus, which differs as follows: batch mixture undergoes preliminary preparation by adding copper and zinc and the subsequent joint alloying.
2. The method described in paragraph 1, which differs as follows: copper and phosphorus are alloyed according to the following percentage ratio: 82% (copper) and 18% (phosphorus).
3. The method described in paragraph 1, which differs as follows: copper and phosphorus are alloyed under the temperature not greater than +1050°C.
4. The method described in paragraph 1, which differs as follows: after alloying of copper and phosphorus, up to 30% of aluminum is infused to the total volume of copper.
5. The method described in paragraph 1, which differs as follows: after the copper + phosphorus + aluminum alloy is obtained, zinc in the amount of 10-15% from the total volume of alloy is infused.
6. The method described in paragraph 1, which differs as follows: after the molten mass has cooled down, silicon is extracted by dissolving in the nitric acid with the subsequent drying until the silicon powder is formed.
(21) i 2006 03009
(22) 21.03.2006
(24) 15.01.2007
(46) 15.01.2007, Bulletin No. 1
(72) …………………….
(57) 1. Silicon extraction method which includes extraction of high-pressure elemental silicon from chemical elements of aluminum and phosphorus by application of electric current with density more than 1011 A/m2 to the mixture of crystalline matters containing oxygen, aluminum, and phosphorus, which differs as follows: batch mixture undergoes preliminary preparation by adding copper and zinc and the subsequent joint alloying.
2. The method described in paragraph 1, which differs as follows: copper and phosphorus are alloyed according to the following percentage ratio: 82% (copper) and 18% (phosphorus).
3. The method described in paragraph 1, which differs as follows: copper and phosphorus are alloyed under the temperature not greater than +1050°C.
4. The method described in paragraph 1, which differs as follows: after alloying of copper and phosphorus, up to 30% of aluminum is infused to the total volume of copper.
5. The method described in paragraph 1, which differs as follows: after the copper + phosphorus + aluminum alloy is obtained, zinc in the amount of 10-15% from the total volume of alloy is infused.
6. The method described in paragraph 1, which differs as follows: after the molten mass has cooled down, silicon is extracted by dissolving in the nitric acid with the subsequent drying until the silicon powder is formed.
Useful model belongs to the methods of obtaining elements, in particular elemental silicon which may be used to obtain new materials.
There are known methods of obtaining silicon by the carbothermal restoration of silicon earth-containing material, subsequent refining, and infusion of alloying additives in the converter, feeding it into the holding furnace, sawing of melted silicon with inert gas, removal of powder from the pulverizing jet and subsequent separation from the inert gas [1].
There is a known method of electro-thermal extraction of silicon [2] and its alloys in ore electrical furnaces.
This method involves supplying of current from the power source to electrodes, submersion into the bath, starting of the arc under the layer of batch mixture materials, renewal and output of silicon from the furnace; in this case, a current fed to the primary output electrodes of the power source is being straightened while current of the same polarity coming from the secondary output electrodes of the power source is being fed to electrodes, and then after the arc was started, current goes through the batch mixture and furnace hearth and fed to the secondary output electrodes of the opposite polarity.
There is a known method of smelting silicon [3] in ore thermal furnace which allows to increase the percentage of its yield from the raw materials. Silicon is being smelted in the three-electrode ore thermal furnace with carbothermal restoration of batch mixture containing silicon earth. During smelting, each 1.5 – 2.0 hours a mixture of carbon-containing reducing agents and quartzite is input into the intra-electrode space in the correlation which ensures mass correlation in the mixture C: SiO2 = 0.5 – 0.75.
There are known methods of obtaining elemental silicon, based on the restoration of silicon oxide by carbon-containing matters upon the following reaction:
SiO2+2C->Si+2CO.
The powder-like mixture of input substances is restored in the electric arc and technical elemental silicon is thus smelted.
However, the main deficiencies of the aforementioned silicon extraction methods is high power consumption and labor content of chemical and physical processes involved in the production technology, which leads to the increased cost of the end products and also large amount of production waste which significantly deteriorates ecological situation on the territory and affects human health.
The closest method of achieving technical result is the method of obtaining compact silicon of other crystalline modification by treating regular silicon under the pressure less than 20 MPa [4]. All technologically used methods of extracting elemental silicon are based on the extraction from silicon-containing oxide materials in the process of restoration, carbothermy. This method is based on the transformation (transmutation) of other chemical elements of aluminum and phosphorus into elemental silicon.
Transformation is achieved by the electric current passing through the mixture of crystalline substances containing main elements O, Al, P with density of the electric current no less than 1011 A/m2.
The goal of the proposed useful model is improvement of silicon extraction technology as a result of reduction of power consumption and labor content by selecting such chemical and physical processes during its production which would have allowed to obtain new technical result and more ecological production process.
This task is resolved as follows: silicon is obtained from chemical elements of aluminum and phosphorus by application of electric current with density not more than 1011 A/m2 to the batch mixture, from crystalline matters containing oxygen, aluminum, and phosphorus; in order to increase the output of silicon copper and phosphorus are preliminary alloyed according to the percentage ratio of 82% copper to 18% (nor more) of phosphorus under the temperature not greater than +1050°C, and after alloying of copper and phosphorus, up to 30% of aluminum is infused to the total volume of copper. After the copper + phosphorus + aluminum molten mass is obtained, zinc in the amount of 10-15% from the total volume of molten mass is infused. After the molten mass has cooled down, it has been dissolved in the nitric acid with the subsequent drying until the solid silicon is obtained in form of a powder.
Thus obtained silicon represents the product of apotropous modification of silicon isosters as a result of nuclear transformation of aluminum phosphide into chemically pure silicon.
Test analysis showed that this type of silicon is quite inert substance which cannot be dissolved in hydrochloric, sulphuric, etching, and other types of acids and even in the nitrohydrochloric acid. It is not dissolved in the fluxes of such metals as aluminum, copper, iron, and others, does not form alloys with them, does not oxidize under the temperature of +3000°C, and does not form carbides.
Silicon obtained using this method is a high-melting matter whichmay resist the impact of temperature of +4000°C but can be melted in the rays of a ultraviolet laser under the temperature of +1415°C.
Fig. shows the appearance of silicon powder after the multiple magnifying by electronic microscope.
Technical result of the proposed useful model is broadening of the arsenal of technical means, namely extraction for the first time of silicon of high-pressure crystalline modification from other chemical elements in conditions of regular atmospheric pressure.
An example.
A mixture of crystalline substances containing main elements O + Al + P was placed in the electrolytic bath, and the impulse electric current with density of 1010 A/m2 was fed to the space between electrodes.
Prior to that, copper was alloyed with phosphorus in the electrolytic bath according to the percentage ratio of 82% to 18% (nor more) under the temperature not greater than +1050°C, and after alloying of copper and phosphorus, up to 30% of aluminum (to the total volume of copper) was infused to the molten mass. After the copper + phosphorus + aluminum molten mass was obtained, zinc in the amount of 10-15% from the total volume of molten mass was infused. Thus obtained molten mass was poured out of the electrolytic bath to a separate crucible. After the molten mass has cooled down, it was dissolved in the nitric acid and then dried until the solid silicon is obtained in form of a powder.
Energy mass analyzer EMAL-2 was used for the purpose of mass spectrometric analysis of the output mixtures and products of transformation upon the method of determination of silicon in the fraction-less sample evaporation mode and registration on the photo film after division of the flow of ions. Peaks of silicon isotope ions were observed in the mass spectra of the product: single-charged 28, 29, 30 and double-charged 14, 14.5, and 15 with relative intensiveness, which corresponds to the master sample of silicon. Trace quantities of silicon were found in the mass spectra of the output mixture.
Roentgenograms were recorded on the X-ray diffraction meter. DRON-4 SiK
a-monochromatic radiation and compared the roentgenograms of the output mixture, product, and the product residuum after the acid treatment.
Results obtained for the product comparing to the output mixture confirm the formation of silicon during nuclear transformation (transmutation) of aluminum and phosphorus. Gravimetrical analysis showed the presence of 18% of silicon in the product obtained.
The experiments conducted by the authors showed that silicon is formed from other chemical elements of the output mixture with density of the electric current less than 1011 A/m2 is discovered by the analysis methods described above.
Silicon obtained upon the proposed method may be used in the lacquer and paint production and in heat-insulating materials, electronics, optics, and jewelry, to process natural minerals and stone, in polishing and grinding pastes and suspensions, in plates and supports of semiconducting materials, fiber optic cables, glass, quartz, glass-ceramic products, and also in nanotechnologies of new materials.
Sources of information used.
1. Karl Forvall. Norwegian patent "Silicon Powder and Method of its Continuous Extraction". Publication 31, No. 2055812 dated 1996.03.10, RU.
2. Patent RU "Method of Smelting Silicon and its Alloys". Publication A1, No. 95100576 dated 1996.12.10, RU.
3. Patent RU "Method of Smelting Silicon". Publication A1, No. 1628443 dated 1996.07.27, RU.
4. Patent RU "Silicon Extraction Method" No. 2140110 CI dated 1997.03.12. Institute of Chemistry and Chemical-Metallurgical Processes of the Russian Academy of Sciences. Kazbanov V.I. and others.
Powyżej tekst Patentu, a poniżej trochę o tym nano krzemie:
Isosters of silicon – it's new material in science, and technology obtained using method of nuclear synthesis. Its unique properties can be used directly, or improve profiles of traditional materials. To distinguish of this material from traditional silicon, we call it “ Nano silicon”.
average size of micro crystals – 2-20nm;
specific surface – 20-400m2
Material passed on to test wasn't purified, and results are presented for alotropic modification of silicon isosters (dark grey powder containing about 90% of silicon isosters), obtained on the way of nuclear influence of pure silicon with other elements, on that interacting components join to silicon, and create mixture of several kinds of pure silicon, and carbides of various elements.
Obtained mixture, is relatively neutral substance, which cannot dissolve in acids (nitrogen, sulphuric, hydrofluoric, hydrochloric), as well cannot dissolve in royal water.
This mixture even don't dissolve in liquid metals (aluminium, copper, iron etc), and don't form alloys with them. It don't oxidize in temperatures up to 3000°C, and don't form to carbides.
Nano silicon have hardness about 9-10 in Moose scale, depend on size of grain. If plotted on cast iron, or ceramic disc, it cut granite, basalt, and ceramics more effectively than Nano disc.
Isosters of silicon are not melting substance, which cannot be melted in graphite melting-pot. Even in temperature of evaporation of graphite (3700-4000°C) this substance remain invariable dark. It looks that it ignore temperature of graphite melting-pot. This property is characteristic for silicon isosters only.
This substance perfectly reflects optical beams, and transforms thermal oscillations into other spectrum of frequency. It's unaffected to bombing by electrons. Thanks to that it could be used as heat insulator, e.g. in space devices, spacesuits, in air and nuclear turbines, in metallurgy.
Nano hardness of silicon isoster crystals is result of method of obtaining them. We have obtained them on the way of within atomic transformations using substances easily undergoing to such transformations: phosphorous, copper, aluminium, and zinc.
There are attached photos (photo 1, 2, 3) that were made in Institute of Super-hard Materials. There were made tests of hardness of crystals.
In that Institute, there were performed tests of two identical samples of alloy of iron-nickel (Fe-70%, Ni-30%). This alloy wasn't pure, and therefore on diagram (photo 4) we can see Zn, Cr, Ni, K, S, P, Si, Al too. Then through alloy were passed pulsating current with density of 100kA/mm2 with frequency of 1 pulse/sec, after transformation it turned out that content of iron and nickel in sample was decreased, but content of titanium, and silicon was increased. However aluminium almost completely disappeared (what can be found in diagram on right side). Besides appeared calcium, that is caused by division of iron into calcium and carbon according to reaction:
26Fe = 20Ca + 6C – W1
On similar way nickel was divided:
28Ni = 22Ti + 6C – W2
As we can see these reactions are endothermic, but we can get simple conclusion, that carbide of titanium, and calcium could be transformed into iron, and nickel with emission of energy, thus they could be one of kind of fuel in chemical-nuclear reactions.
As result of analysis of products of pulsating current influence on alloy of iron-nickel, we observed strong structural changes. Crystal form of alloy changed into form with bright navy colour, called by authors “Granatons” (photo 5).
We wish to demonstrate regularity of our research, therefore we will dedicate little space to describe them.
We observed nuclear transformations even on relatively low energies. If we get alloy of copper and phosphorous in such proportion, that after insertion of aluminium, we get following proportion of components: Cu-60%, Al-28%, P-12%, then during insertion of aluminium, we observe self thickening of alloy.
On this process phosphorous is subject of transmutation, there is torn of proton from it, and it transforms into silicon. This transformation begins transformations of other atoms. In our example spectral analysis show presence of large a number of elements: Na, K, Ca, Ti, Fe, Ge, Se, i Mo.
We are convinced, that sodium come into being from aluminium as result of tearing of alpha particle from it, according to formula:
11Na = 13Al – 2He
Calcium arise from copper at the cost of tearing off of fluorine:
20Ca = 29Cu – 9F
If there will be torn off a hydrogen from calcium, then it transforms into potassium:
19K = 20Ca – 1H
Iron can arise from connection of 2 aluminium atoms with 2 neutrons, and molybdenum arise from three atoms of silicon.
As result of our investigations, we observed alloy of copper, phosphorous and aluminium create most favourable conditions for nuclear transformations. In such alloy phosphorous become to be most sensitive to such transformations, and easily lose deuterium transforming itself into silicon. Free deuterium accelerate into high speed, and by collisions force other atoms to transmutation reactions. Following diagram show transformation of alloy of copper with aluminium into other elements. As result we obtained: Na, K, Ca, Ti, Fe, Ge, Se, and Mo.
Above experiment was repeated, but this time there was added potassium chloride into the alloy. On diagram we observed a lot of new elements: Li, Mg, Si, Ca; Fe, Ni, Zn, Sr, In, Eu, and several heavy elements like Ir.
Zinc arise from copper as result of join of deuterium into it:
30Zn = 29Cu + 1D
Zinc and potassium transform into indium:
49In = 30Zn + 19K
Iron and nickel arise as quasi-molecules from aluminium and silicon:
26Fe = 2 13Al 28Ni = 2 14Si
If there would be to indium joined iron or nickel, there will arise rhenium or iridium:
75Re = 49In + 26Fe
77Ir = 49In + 28Ni
We take a note to very interesting property, at the cost of transmutation of phosphorous, there arise atoms with mass bigger that mass of phosphorous.
Above experiment was repeated, but into alloy there was added zinc (ca. 20% of total mass). We observed long series of new elements: Na, Mg, Si, Ca, Sc(AlOH), In, InO (Cs), InOH (Cs), InNa (La),
InAl (Pr), Gd, Tb, Lu, Hf, Ir, IrC, Tl.
Scandium arise as result of joining of calcium with deuterium:
21Sc = 20Ca + 1D
Caesium could arise as result of joining of zinc, sodium, and silicon:
55Cs = 30Zn + 11Na + 14Si
Other elements arise on similar way. We should emphasize, that nuclear transformations occur at the cost of split of nucleus of phosphorous, zinc and chlorine, and this is confirmed by the fact of disappearing of these elements from reaction environment.
As we observed, addition of zinc into alloy of phosphorous increased processes of emission of heat, and production of heavy elements, this means that a pair metal-nonmetal have selective parameters.
We were not satisfied with quantitative course of the reaction in last experiment, because it would be difficult to use these reactions in practice, and therefore we made decision to add iodine into the alloy. Distinct from previous experiment, we provided reaction environment with potassium iodide instead of potassium chloride. Spectrogram shows (as in following picture), that after reaction we observed presence of following elements: Li, Na, Mg, Si, Ca, Sc, Fe, Ni, Ge, As, Se, Pd, Ag, Sn, Sb, Te, Cs, Pm, Tb, Hf, Os, Ir.
Germanium arise as result of joining of copper atom with lithium atom:
32Ge = 29Cu + 3Li
Palladium arise when atom of germanium joins with silicon atom:
46Pd = 32Ge + 14Si
Silver arise as result of joining of palladium with deuterium:
47Ag = 46Pd + 1D
Iridium is a result of fusion of silver atom with zinc atom:
77Ir = 47Ag + 30Zn
Phosphorous, zinc, and iodine disappeared almost completely.
Insertion of iodine into phosphorous model of atoms increases process of transmutation. Iodine by lose of proton transforms into tellurium, and tellurium ion thanks to its activity, have ability to join other atoms.
Thanks to carrying out of enormous scientific job (fragment of that we shown in this short study), we got knowledge and experience that allow us to say, that we are able to:
- Produce isosters (silicon first of all) in industrial scale;
- Produce in industrial scale green, clean energy using chemical-nuclear reactions (transformation reactions), as well new inexhaustible fuel, e.g.:
40Zr + 2 8O = 36Kr + 2 10Ne + e1 = 32Ge + 2 12Mg + e2 = 28Ni + 2 14Si + e3
where: e1, e2, and e3 – energy emitted during transmutation reaction.
Because our job wasn't financed by any source, we spent our all energy to base research, as we realized that any doubts in understanding of phenomenon we researched, doesn't allow us to get effective results on field of practical use of knowledge we got.
Actually when we got experience necessary to design results of experiments, we are ready to put our knowledge to practice.
Initial, modest experiments in range of usefulness of silicon isosters for practical use, allow us to make a suppose that humankind can receive a material, that will find application in many branches of industry, and human activity, as:
- Electronics, optics, precision engineering, jewellery, and stone processing:
polishing pastes, and suspensions for precise processing of micro-crystals, gems, silicon, semiconductor plates, and matrix, optical products (with roughness not exceeding 2nm).
- Processing of metals and ceramic materials:
sanding finishing/polishing powders, suspensions, and pastes for precise processing of details mad from special, construction, or instrumental alloys, ceramics, and other materials resistant to mechanical processing.
- Processing of metals:
addition to technical greases reducing friction, greases for matrix and stretch processing, cold and hot metal press-processing, or lubricating/cooling mixtures for cutting;
- Machine, automotive, and petrochemical industry:
additive for reduction of friction into transmission and engine oils;
- Chemistry of polymers, production of technical rubbers, active filler of composite polymers facilitating forming of three-dimensional structures, and increasing durability, resistance for sanding, thermal, radiant, and chemical stability;
- Electronics:
pressing of this material, leaded to creation of new types of ceramic materials similar to Nano, we received homogeneous, poorly porous material (with R=1014 – 1016 Ω/cm2, ε= 6-8, tgΔ =102-103), with high heat conductivity. Ceramic materials on base of Nano silicon, could be used to build active and passive elements for radio engineering;
- Medicine, and biology:
very effective sorbents, immuno-stabilizers of active substances, substance accelerating ripen of prototypes of micro-organisms, transport of antibodies into parts of body affected by cancer cells.
This material could be used in light bulbs instead of tungsten, in high temperature transistors and thyristors as electrodes, because it have conductivity of silver. It could be used as facing of tungsten or molybdenum thread to protect it against oxygen, and to increase losing of heat. In such case there is possibility of production of lamps without balloons.
Nano silicon could find application in efficient lubricating materials. Insertion of fraction of percent of this material into lubricating oil increases endurance of moving parts in mechanisms for one order.
Addition of Nano silicon into various paints or varnishes reduces their heat conductivity.
Alloy of aluminium with silicon with reinforced with this material take hardness comparable to corundum. It cut perfectly glass, but at the same time could be processed like ordinary alloy.
Iron reinforced with Nano silicon, better magnetic profiles. Copper become beautiful jewellery material.
Crystal glass, and porcelain mixed with nano silicon have unusual tint.
by
MSc. engineer Waldemar Mordkowicz
W tym tekście o Nano krzemie wytłuściłem jeden fragment, ale wart wszystkie pieniądze świata: to jest ta reakcja, według której już dzsiiaj możemy uzyskiwać energię z przekształceń atomowych (transmutacji). mam yjuż opracowane ponad sto kompozycji "paliwowych"
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