CN1027439C - Making method of magnesium silicide - Google Patents
Making method of magnesium silicide Download PDFInfo
- Publication number
- CN1027439C CN1027439C CN 91107558 CN91107558A CN1027439C CN 1027439 C CN1027439 C CN 1027439C CN 91107558 CN91107558 CN 91107558 CN 91107558 A CN91107558 A CN 91107558A CN 1027439 C CN1027439 C CN 1027439C
- Authority
- CN
- China
- Prior art keywords
- magnesium
- reaction zone
- silicide
- steam
- silica flour
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- YTHCQFKNFVSQBC-UHFFFAOYSA-N magnesium silicide Chemical compound [Mg]=[Si]=[Mg] YTHCQFKNFVSQBC-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910021338 magnesium silicide Inorganic materials 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 17
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000011777 magnesium Substances 0.000 claims abstract description 47
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 45
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims abstract description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000001257 hydrogen Substances 0.000 claims abstract description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 36
- 235000013312 flour Nutrition 0.000 claims description 18
- 239000000377 silicon dioxide Substances 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 9
- 230000002194 synthesizing effect Effects 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 4
- 230000002829 reductive effect Effects 0.000 abstract description 3
- 230000001681 protective effect Effects 0.000 abstract description 2
- 239000011863 silicon-based powder Substances 0.000 abstract 2
- 239000012159 carrier gas Substances 0.000 abstract 1
- 239000011261 inert gas Substances 0.000 abstract 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 239000010459 dolomite Substances 0.000 description 2
- 229910000514 dolomite Inorganic materials 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910021332 silicide Inorganic materials 0.000 description 2
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910004261 CaF 2 Inorganic materials 0.000 description 1
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 1
- 229910000551 Silumin Inorganic materials 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- -1 magnesium powder compound Chemical class 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
The present invention relates to a method for preparing magnesium silicide. Magnesium steam and silicon powder are used as raw materials; the silicon powder is put in a reaction region which is heated to 500 to 650 DEG C; vacuum is pumped; the magnesium steam is added into the reaction region; when the vacuum is not pumped, hydrogen/inert gas is used as carrier gas and reaction protective gas for the magnesium steam. When the method is adopted, the raw material cost of the magnesium silicide is reduced by more than 50%, and the yield reaches 98%.
Description
The present invention relates to a kind of preparation method of metal silicide.
Magnesium silicide is a kind of important industrial raw material, is used for production processes such as silane gas, polysilicon, amorphous silicon membrane and silicide powder.Magnesium silicide production method commonly used is mixed silica flour, magnesium powder by a certain percentage, and its compound is sent in the reaction zone, is heated to 500 ℃～550 ℃ under vacuum or protective atmosphere, just synthesizes magnesium silicide, and its reaction formula is:
2Mg+Si→Mg
2Si
German patent DE 1143190 provides a kind of synthesizing magnesium silicide method by the rich invention of Japanese Xiao Song electronic metal company's stone mound, adopt spiral pushing device continuously silica flour, magnesium powder compound to be delivered to 500 ℃～550 ℃ high temperature reaction zone, synthesize magnesium silicide, can continuously feeding and discharging, magnesium silicide output is big, is applicable to production in enormous quantities silane.The shortcoming of this method is:
1. must in advance magnesium ingot be processed into the magnesium powder, this is very uneconomic.No matter the smelting of magnesium adopts electrolytic process or hot reducing method, and its energy consumption is all very big.As refining magnesium with ferrosilicon or silumin as reductive agent, reaction formula commonly used is:
What restore more than 1000 ℃ is gaseous magnesium, becomes crystal magnesium through cryogenic condensation, becomes magnesium ingot through certain purification process founding again.Be synthesizing magnesium silicide, magnesium ingot processed the magnesium powder, because of magnesium powder price far above silica flour, the magnesium silicide cost of being produced is also high.
2. magnesium is the active metal, and the specific surface of magnesium powder is very big, contacts easy deterioration by oxidation with air, and rotten magnesium powder can not react synthesizing magnesium silicide with silica flour, therefore influences the yield of magnesium silicide, and under normal circumstances the yield of magnesium silicide is 95%.
3. in processing and use magnesium powder process, a certain amount of magnesium dust can float in air, when Mg content reaches 30mg/l in the air, can produce blast, blast high temperature impels magnesium silicide to decompose, and the magnesium of the ecosystem that decomposites and silicon produce fiercer blast under air effect.As seen adopt this method to produce magnesium silicide, its security is relatively poor.
4. magnesium powder and silica flour reaction generation magnesium silicide is a kind of thermopositive reaction, and the reaction process temperature of charge can raise automatically, causes burning easily, if temperature surpasses 650 ℃, the vapour pressure of magnesium sharply rises, and magnesium just can be separated from magnesium silicide, side reaction takes place simultaneously, causes the magnesium silicide downgrade.The compound input amount is unsuitable excessive in industrial synthesizer.
The object of the present invention is to provide a kind of is the method that raw material is made magnesium silicide with magnesium steam and silica flour, the magnesium silicide production cost is reduced significantly, less energy consumption, product yield height.
The present invention directly adopts magnesium steam and silica flour to generate magnesium silicide at the reaction zone internal reaction, silica flour placed in the reaction zone, and 500～650 ℃ of reaction zone heating and vacuumizing, the magnesium that adds reaction zone is magnesium steam; Perhaps silica flour is placed in the reaction zone, the reaction zone Heating temperature is 560 ℃～700 ℃, and the magnesium that adds reaction zone is magnesium steam, with the shielding gas that carry gas and synthesizing magnesium silicide of hydrogen/rare gas element as magnesium steam.Used magnesium steam is provided by the heating liquid magnesium, perhaps adopts in the hot reducing method reduction magnesium ore process to obtain.
Adopt cheap rhombspar ore and thick silicon as raw material, with lower energy consumption and easy processing step, directly synthetic high-grade magnesium silicide can become the high quality raw material of producing silane.
With prior art relatively, the present invention has following advantage:
1. magnesium raw material adopts magnesium steam and without the magnesium powder, particularly adopts the magnesium steam synthesizing magnesium silicide that produces in the smelting magnesium by thermal reduction process process, can make the cost of magnesium silicide raw material reduce more than 50%.
2. with magnesium steam and silica flour reaction synthesizing magnesium silicide, wherein send into the magnesium quantity of steam of reaction zone and control easily, can eliminate reaction process heat up automatically problem and magnesium powder deterioration by oxidation problem, both guaranteed the magnesium silicide quality, the yield of magnesium silicide can be brought up to more than 98% again.
3. do not use the magnesium powder, eliminated the possibility that produces blast because magnesium dust floats in the atmosphere.
Embodiment 1:
Solid magnesium 17.5 grams are put into vacuum electric furnace, and silica flour 10 grams are put into the reaction zone that links to each other with electric furnace, vacuumize the air of getting rid of the inside, fill hydrogen to normal pressure.To electric furnace and reaction zone energising heating, the control electric furnace is 800 ℃ respectively, and reaction zone is 600 ℃, feeds hydrogen simultaneously in electric furnace, and magnesium steam is delivered to reaction zone.After 1 hour, synthesizing magnesium silicide 27 grams.
Embodiment 2:
Rhombspar CaCO
3MgCO
3Calcined 2 hours down at 1100 ℃, its reaction formula is
Pulverize behind the dolomite calcination is got ground dolomite 26 grams, silica flour (purity 99%) 4 gram and fluorspar powder CaF
2The trace mixing is made bulk under the pressure about 50MPa, dough and 3.5 gram silica flours are placed the different sites of tubular reactor respectively and vacuumize, to 1250 ℃ of calcinings of dough heating, 600 ℃ of position, silica flour place heating through 3 hours, get magnesium silicide 9.5 grams.Product is even blue fine powder.X-ray energy spectrometer analytical results, magnesium silicide content are 98%.
Claims (4)
1, a kind of method of making magnesium silicide is a raw material with magnesium and silica flour, and silica flour places in the reaction zone, and reaction zone is heated and vacuumizes, and it is characterized in that the reaction zone Heating temperature is 500 ℃～650 ℃, and the magnesium that adds reaction zone is magnesium steam.
2, according to the method for claim 1, described magnesium steam is provided by the heating liquid magnesium.
3, according to the method for claim 1, described magnesium steam adopts hot reducing method reduction magnesium ore to obtain.
4, a kind of method of making magnesium silicide; with magnesium and silica flour is raw material; silica flour places in the reaction zone; reaction zone is heated; it is characterized in that the reaction zone Heating temperature is 500～650 ℃; the magnesium that adds reaction zone is magnesium steam, and with the shielding gas that carry gas and synthesizing magnesium silicide of hydrogen/rare gas element as magnesium steam.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91107558 CN1027439C (en) | 1991-12-14 | 1991-12-14 | Making method of magnesium silicide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91107558 CN1027439C (en) | 1991-12-14 | 1991-12-14 | Making method of magnesium silicide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1062710A CN1062710A (en) | 1992-07-15 |
| CN1027439C true CN1027439C (en) | 1995-01-18 |
Family
ID=4908892
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91107558 Expired - Fee Related CN1027439C (en) | 1991-12-14 | 1991-12-14 | Making method of magnesium silicide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1027439C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101306818B (en) * | 2008-07-01 | 2010-06-09 | 浙江理工大学 | Method for preparing magnesium silicide and device |
| CN101928004B (en) * | 2010-03-31 | 2013-02-20 | 清华大学 | Method for preparing Mg2Si crystal and fluidized bed reactor |
| CN101928006B (en) * | 2010-09-13 | 2012-03-14 | 化学工业第二设计院宁波工程有限公司 | Equipment and method for producing magnesium silicide |
| CN103193234B (en) * | 2013-04-12 | 2014-07-23 | 太原理工大学 | Method for preparing magnesium silicide-based powder thermoelectric material by utilizing polysilicon byproduct |
| CZ2016108A3 (en) * | 2016-02-25 | 2017-05-17 | Ústav Chemických Procesů Av Čr, V. V. I. | The method of production of magnesium silicide and its processing |
| CN112479211B (en) * | 2020-12-17 | 2022-10-04 | 烟台万华电子材料有限公司 | Method for continuously producing disilane |
-
1991
- 1991-12-14 CN CN 91107558 patent/CN1027439C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1062710A (en) | 1992-07-15 |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |