CN102718217A - High purity linear silicon carbide powder and preparation method - Google Patents
High purity linear silicon carbide powder and preparation method Download PDFInfo
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Abstract
The invention relates to a high purity linear silicon carbide powder and a preparation method, the linear silicon carbide powder product presents light green color and has a cubic crystal system, a microstructure presents a linear state, and the content of the silicon carbide is no less than 99%. The preparation method provided by the present invention comprises the following steps: silica sol and oxidized graphene are uniformly mixed, then subjected to ultrasonic treatment, and completely stirred to obtain a composite precursor. The composite precursor is subjected to solidification, drying and grinding to obtain a powdery precursor with fine and uniform quality. Argon is introduced in the powdery precursor, a carbon thermal reduction is carried out under high temperature in a high temperature tubular furnace to obtain the carbonized silicon powder crude product; the carbonized silicon powder crude product is immersed in inorganic acid and then the pumping filtration is carried out, the unreacted carbon is removed, and cooled to obtain the silicon carbide powder with content of less than 99%. According to the invention, a silicon source is silica sol, a carbon source is oxidized grapheme, the invention has the advantages of no requirement of subsequent processing, no requirement of pressurization, addition of metal catalyst, simple process and short production period; the precursor with homogeneousness is prepared in advance, then the carbon thermal reduction is carried out, the product purity is high, and the method provided by the invention enables large-scale industrial production.
Description
Technical field
The invention belongs to the ceramics processing field, be specifically related to a kind of high-purity wire carborundum powder and preparation method thereof.
Background technology
Silit (SiC) material be continue two generation a kind of novel semiconductor material of growing up of semi-conductor.Its peculiar broad-band gap (Eg>2.3ev), high heat conductance (θ
K=4.9W cm
-1K
-1), high critical breakdown electric field (V=3.0MV cm
-1), the saturated drift of high carrier (ζ sat=2.0 * 10
7Cm S
-1) etc. characteristics, bigger at the application potential of aspects such as high temperature, high-power, high frequency, photoelectron and radioprotective.Its high temperature and radiation-resistant property have been used as fields such as geothermal drilling, oil, aerospace, nuclear energy exploitations; For high frequency, superpower, the SiC device then is to be used in radar, communication and field of broadcast televisions.Can find out that the SiC material will represent its important use value with its excellent physics and chemical property future in high-tech area.
Typical SiC crystalline structure generally is divided into two big types: one type is cube SiC crystal formation that is called the zincblende lattce structure of 3C or β-SiC, and another kind of is the large period structure that is called hexangle type or the diamond structure of α-SiC, and 6H, 4H, 15R etc. are typically arranged.Because the bond energy of β-SiC is minimum, the lattice free energy is maximum, so its also nucleation the most easily, and the needed temperature of growing is also minimum relatively.On chemical property, because spacing is equal basically between the carbon silicon stack lamination, different SiC polytypes are identical in the lattice arrangement of the double-deck solid matter face of Si-C, so the chemical property that they had is basic identical; And for physical properties, owing to have very high energy barrier between these homogeneity polytypes, and therefore, even under the identical situation of basal component, the physical properties between them, particularly characteristic of semiconductor also has nothing in common with each other.In addition, β-SiC is one of the hardest high performance material that is only second to diamond, and its ultrahigh hardness and density make it can be ideally suited for standing the parts of high wearing and tearing and skimming wear, are applicable to especially ultraprecision grinding of various grindings.
Carbothermic reduction reaction is one of main method of present synthesizing silicon carbide powder, is called the Acheson method in the industrial production, and traditional method is to adopt silica sand, silicon-dioxide powdery, silica flour as the silicon source; Graphite, carbon dust and some contain carbon macromolecule such as starch, resol, pitch as carbon source; For also having, the silicon carbide powder that obtains different-shape adopt resinous material in recent years as carbon source with fibrous texture; Can find out; The own foreign matter content in silicon source that is used in this method is many, is unfavorable for obtaining the purity high product, and employed carbon source is also very limited; And the solid state reaction contact area that when using powder body material as reaction carbon source and silicon source, is taken place is limited, is unfavorable for abundant reaction.There are problems such as silicon source foreign matter content is high, reaction is insufficient, income rate is low,
The patented claim of relevant silicon carbide powder preparation is more, like the patented claim of publication number CN101597059, CN101704523, CN101215187, CN101177268, CN101876095, CN1844493, CN1834309, CN1724351, CN101850972, CN1472136.It is the silicon source that these methods adopt silica flour, silicon dioxide powder mostly, and graphite, carbon black, gaseous hydride are carbon source, and what have has also used metal as catalyzer, methods such as pressurization, and the labor energy and preparation process are complicated.
Also do not appear in the newspapers as yet as carbon source with graphene oxide.And because the excellent properties of graphene oxide will have crucial meaning to its many-sided applied research
Summary of the invention
The objective of the invention is to above-mentioned present situation, aim to provide that a kind of preparation technology is simple, production cost is low, with short production cycle, a kind of high-purity wire carborundum powder that product purity is high and preparation method thereof.
The implementation of the object of the invention does, a kind of high-purity wire carborundum powder is light green, isometric system, and microtexture is wire, and the content of silit is not less than 99%.
A kind of preparation method of high-purity wire carborundum powder, concrete steps are following:
(1) silicon sol and graphene oxide are mixed by the weight percent of 100:16-36 after, earlier through ultrasonication 15-30 minute, ultrasonic frequency 20-120kHz, powerful again the stirring 2-4 hour, composite precursor;
Described silicon sol is dioxide-containing silica 5%-30%, pH value 2-7, and size is the acidic silicasol between the 6-30nm;
Described graphene oxide is the carbon material with good laminated structure;
(2) composite precursor is solidified dry 48h in loft drier after, adopt high speed ball mill to grind 2 hours, the fine and smooth and Powdered presoma of homogeneous;
Said drying means is vacuum-drying, forced air drying or lyophilize,
(3) Powdered presoma is put into high temperature process furnances, feed purity and reach 99.99% argon gas, under 1400-1600 ℃, carried out carbothermic reduction reaction 2-8 hour, obtain the silicon carbide micro-powder bullion;
(4) the silicon carbide micro-powder bullion is soaked suction filtration after 2-4 hour in mineral acid, filter residue in 400-700 ℃ of following sintering 1-9 hour, is removed unreacted carbon under the air existence condition, obtains content after the cooling and is not less than 99% silicon carbide powder;
Described mineral acid is that concentration is hydrofluoric acid and/or the nitric acid of 10%-20%, the ratio of mixture of hydrofluoric acid and nitric acid be arbitrarily than.
The used silicon source of the present invention is the silicon sol that contains the Nano particles of silicon dioxide of high reaction activity, carbon source is the graphene oxide with laminated structure, has not only avoided polymer carbon source residual harmful verivate in reduction reaction, need not subsequent disposal; Entire reaction does not relate to pressurization and uses metal catalyst, thereby has further simplified production craft step.Utilize the good dispersion and the silicon sol thorough mixing of graphene oxide, make the uniformity presoma earlier, carry out carbothermic reduction reaction again, thereby guaranteed the adequacy of follow-up reduction reaction, productive rate is high.
Technology of the present invention is simple, production cost is low, with short production cycle, product purity is high, can mass industrialized production.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) figure of the β-SiC of instance 1 preparation,
Fig. 2 is sem (SEM) figure of the β-SiC of instance 1 preparation.
Embodiment
Graphene oxide is a kind of important derivatives of Graphene, is to be a kind of plates that hexagonal annular is arranged between the carbon atom, is made up of one deck carbon atom; Can infinitely extend at two-dimensional space; Be connected with some oxygen-containing functional groups on the two dimension basal plane, this makes it can absorb large quantity of moisture, has good hydrophilicity; Dispersed, with the compatibility of polymkeric substance, thereby in the present invention can with the silicon sol thorough mixing.
Product of the present invention is light green, isometric system, and microtexture is wire, and the content of silit is not less than 99%.
Preparing method of the present invention is, silicon sol and graphene oxide mix, ultrasonication, the powerful stirring, composite precursor.Composite precursor grinds fine and smoothly and the Powdered presoma of homogeneous after solidifying drying.Powdered presoma feeds argon gas, carries out carbothermic reduction under the high temperature and gets the silicon carbide micro-powder bullion; The silicon carbide micro-powder bullion is the back suction filtration in mineral acid, and the filter residue sintering is removed unreacted carbon, obtains content after the cooling and is not less than 99% silicon carbide powder.
Below in conjunction with embodiment the present invention is detailed.
Embodiment one:
(1) after graphene oxides mixed with 1.15 grams with 5.0 gram silicon sol, through ultrasonication 30 minutes, ultrasonic frequency 20-120kHz stirred 3 hours under powerful mechanical stirring again, got composite precursor earlier; Dioxide-containing silica is 30% in the acidic silicasol of being selected for use, and the pH value is 2.0, and size is 6nm;
(2) composite precursor that obtains is solidified in air dry oven adopt behind the dry 48h high speed ball mill to grind 2 hours, obtain exquisiteness and the Powdered presoma of homogeneous;
(3) Powdered presoma is put into high temperature process furnances, feed high-purity argon gas, under 1500 ℃, carried out carbothermic reduction reaction 6 hours; Obtain the silicon carbide micro-powder bullion;
(4) with gained silicon carbide micro-powder bullion suction filtration after concentration is to soak 2 hours in 20% the hydrofluoric acid, filter residue is under the air existence condition, and 400 ℃ of sintering 9 hours are removed unreacted carbon, obtain purified silicon carbide powder after the cooling.
Embodiment two:
(1) after graphene oxides mixed with 1.15 grams with 7.2 gram silicon sol, through ultrasonication 15 minutes, ultrasonic frequency 20kHz stirred 2 hours under powerful mechanical stirring again, got composite precursor earlier; Dioxide-containing silica is 20% in the acidic silicasol of being selected for use, and the pH value is 2.4, and size is 20nm;
(2) composite precursor that obtains is solidified in vacuum drying oven adopt behind the dry 24h high speed ball mill to grind 2 hours, obtain exquisiteness and the Powdered presoma of homogeneous;
(3) Powdered presoma is put into high temperature process furnances, feed high-purity argon gas, under 1400 ℃, carried out carbothermic reduction reaction 8 hours; Obtain the silicon carbide micro-powder bullion;
(4) with gained silicon carbide micro-powder bullion suction filtration after concentration is to soak 2 hours in 10% the hydrofluoric acid, filter residue is under the air existence condition, and 700 ℃ of sintering 5 hours are removed unreacted carbon, obtain purified silicon carbide powder after the cooling.
Embodiment three:
(1) after graphene oxides mixed with 1.8 grams with 5.0 gram silicon sol, through ultrasonication 20 minutes, ultrasonic frequency 80kHz stirred 4 hours under powerful mechanical stirring again, got composite precursor earlier; Dioxide-containing silica is 30% in the acidic silicasol of being selected for use, and the pH value is 2.0, and size is 6nm;
(2) composite precursor that obtains is solidified in air dry oven adopt behind the dry 24h high speed ball mill to grind 2 hours, obtain exquisiteness and the Powdered presoma of homogeneous;
(3) Powdered presoma is put into high temperature process furnances, feed high-purity argon gas, under 1600 ℃, carried out carbothermic reduction reaction 2 hours; Obtain the silicon carbide micro-powder bullion;
(4) with gained silicon carbide micro-powder bullion suction filtration after concentration is to soak 3 hours in the mixing acid formed of the nitric acid acid of 10% hydrofluoric acid and 10%; Filter residue is under the air existence condition; 500 ℃ of sintering 8 hours are removed unreacted carbon, obtain purified silicon carbide powder after the cooling.
Embodiment four:
(1) after graphene oxide mixed with 0.8 gram with 5.0 gram silicon sol, through ultrasonication 15 minutes, ultrasonic frequency 60kHz stirred 3 hours under powerful mechanical stirring again, got composite precursor earlier; Dioxide-containing silica is 10% in the acidic silicasol of being selected for use, and the pH value is 7.0, and size is 20nm;
(2) composite precursor that obtains is solidified in freeze drying box adopt behind the dry 24h high speed ball mill to grind 2 hours, obtain exquisiteness and the Powdered presoma of homogeneous;
(3) Powdered presoma is put into high temperature process furnances, feed high-purity argon gas, under 1600 ℃, carried out carbothermic reduction reaction 2 hours; Obtain the silicon carbide micro-powder bullion;
(4) with gained silicon carbide micro-powder bullion suction filtration after concentration is to soak 4 hours in 20% the nitric acid, filter residue is under the air existence condition, and 600 ℃ of sintering 5 hours are removed unreacted carbon, obtain purified silicon carbide powder after the cooling.
Embodiment five:
(1) after graphene oxide mixed with 0.8 gram with 5.0 gram silicon sol, through ultrasonication 25 minutes, ultrasonic frequency 120kHz stirred 4 hours under powerful mechanical stirring again, got composite precursor earlier; Dioxide-containing silica is 5% in the acidic silicasol of being selected for use, and the pH value is 6.0, and size is 20nm;
(2) composite precursor that obtains is solidified in vacuum drying oven adopt behind the dry 24h high speed ball mill to grind 2 hours, obtain exquisiteness and the Powdered presoma of homogeneous;
(3) Powdered presoma is put into high temperature process furnances, feed high-purity argon gas, under 1500 ℃, carried out carbothermic reduction reaction 7 hours; Obtain the silicon carbide micro-powder bullion;
(4) with gained silicon carbide micro-powder bullion suction filtration after concentration is to soak 3.5 hours in 8% the hydrofluoric acid, filter residue is under the air existence condition, and 700 ℃ of sintering 1 hour are removed unreacted carbon, obtain purified silicon carbide powder after the cooling.
Embodiment six:
(1) after graphene oxides mixed with 1.15 grams with 5.0 gram silicon sol, through the UW place 20 minutes earlier, ultrasonic frequency 120kHz stirred 2 hours under powerful mechanical stirring again, got composite precursor; Dioxide-containing silica is 20% in the acidic silicasol of being selected for use, and the pH value is 3.0, and size is 30nm;
(2) composite precursor that obtains is solidified in vacuum drying oven adopt behind the dry 24h high speed ball mill to grind 2 hours, obtain exquisiteness and the Powdered presoma of homogeneous;
(3) Powdered presoma is put into high temperature process furnances, feed high-purity argon gas, under 1400 ℃, carried out carbothermic reduction reaction 7 hours; Obtain the silicon carbide micro-powder bullion;
(4) with gained silicon carbide micro-powder bullion suction filtration after concentration is to soak 3 hours in 10% the nitric acid, filter residue is under the air existence condition, and 600 ℃ of sintering 4 hours are removed unreacted carbon, obtain purified silicon carbide powder after the cooling.
Claims (3)
1. a high-purity wire carborundum powder is characterized in that being light green, isometric system, and microtexture is wire, and the content of silit is not less than 99%.
2. method for preparing the described high-purity wire carborundum powder of claim 1 is characterized in that concrete steps are following:
(1) silicon sol and graphene oxide are mixed by the weight percent of 100:16-36 after, earlier through ultrasonication 15-30 minute, ultrasonic frequency 20-120kHz stirred 2-4 hour in brute force again, composite precursor;
Described silicon sol is dioxide-containing silica 5%-30%, pH value 2-7, and size is the acidic silicasol between the 6-30nm;
Described graphene oxide is the carbon material with good laminated structure;
(2) composite precursor is solidified dry 48h in loft drier after, adopt high speed ball mill to grind 2 hours, the fine and smooth and Powdered presoma of homogeneous;
Said drying means is vacuum-drying, forced air drying or lyophilize,
(3) Powdered presoma is put into high temperature process furnances, feed purity and reach 99.99% argon gas, under 1400-1600 ℃, carried out carbothermic reduction reaction 2-8 hour, obtain the silicon carbide micro-powder bullion;
(4) the silicon carbide micro-powder bullion is soaked suction filtration after 2-4 hour in mineral acid, filter residue in 400-700 ℃ of following sintering 1-9 hour, is removed unreacted carbon under the air existence condition, obtains content after the cooling and is not less than 99% silicon carbide powder;
Described mineral acid is that concentration is hydrofluoric acid and/or the nitric acid of 10%-20%, the ratio of mixture of hydrofluoric acid and nitric acid be arbitrarily than.
3. a kind of method for preparing high-purity wire carborundum powder according to claim 2 is characterized in that presoma is to put into high temperature process furnances feeding argon gas after placing corundum crucible, carries out carbothermic reduction reaction.
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| CN103834988A (en) * | 2014-03-24 | 2014-06-04 | 中国科学院山西煤炭化学研究所 | Preparation method of nano silicon carbide whisker |
| CN103864076A (en) * | 2012-12-11 | 2014-06-18 | 河南工业大学 | Preparation method of silicon carbide aerogel on basis of SiO2 aerogel as template |
| CN103964439A (en) * | 2014-04-25 | 2014-08-06 | 北方工业大学 | Surface purification treatment method for abrasive grade SiC particles |
| CN104973873A (en) * | 2015-06-11 | 2015-10-14 | 中国科学院山西煤炭化学研究所 | High temperature oxidization-resistant graphene-based composite film and preparation method thereof |
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| CN103864076A (en) * | 2012-12-11 | 2014-06-18 | 河南工业大学 | Preparation method of silicon carbide aerogel on basis of SiO2 aerogel as template |
| CN103834988A (en) * | 2014-03-24 | 2014-06-04 | 中国科学院山西煤炭化学研究所 | Preparation method of nano silicon carbide whisker |
| CN103834988B (en) * | 2014-03-24 | 2016-06-15 | 中国科学院山西煤炭化学研究所 | A kind of method preparing nanometer silicon carbide whiskers |
| CN103964439A (en) * | 2014-04-25 | 2014-08-06 | 北方工业大学 | Surface purification treatment method for abrasive grade SiC particles |
| CN104973873A (en) * | 2015-06-11 | 2015-10-14 | 中国科学院山西煤炭化学研究所 | High temperature oxidization-resistant graphene-based composite film and preparation method thereof |
| CN106219549B (en) * | 2016-07-29 | 2019-01-01 | 苏州大学 | The method that vacuum-sintering prepares silicon carbide nanometer line |
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| CN106219549A (en) * | 2016-07-29 | 2016-12-14 | 苏州大学张家港工业技术研究院 | The method of silicon carbide nanometer line is prepared in vacuum-sintering |
| CN106890724A (en) * | 2017-03-12 | 2017-06-27 | 郑州睿科生化科技有限公司 | A kind of production technology of silicon carbide micro-powder |
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| CN108285145A (en) * | 2018-04-27 | 2018-07-17 | 中国人民解放军国防科技大学 | Three-dimensional multi-level structure nano silicon carbide, preparation method and application thereof |
| CN111232983A (en) * | 2020-03-27 | 2020-06-05 | 泉州师范学院 | Method for large-scale preparation of SiC nanowires by using spongy graphene or derivatives thereof as carbon source |
| CN111533131A (en) * | 2020-06-22 | 2020-08-14 | 黑龙江冠瓷科技有限公司 | Based on CaCl2Preparation method of nano silicon carbide particles of shape regulator |
| CN111591995A (en) * | 2020-06-22 | 2020-08-28 | 黑龙江冠瓷科技有限公司 | Preparation method of nano silicon carbide particles based on NaF shape regulator |
| CN111533131B (en) * | 2020-06-22 | 2021-08-13 | 黑龙江冠瓷科技有限公司 | Based on CaCl2Preparation method of nano silicon carbide particles of shape regulator |
| CN111591995B (en) * | 2020-06-22 | 2021-08-13 | 黑龙江冠瓷科技有限公司 | Preparation method of nano silicon carbide particles based on NaF shape regulator |
| CN113897130A (en) * | 2021-09-30 | 2022-01-07 | 西安特种设备检验检测院 | Silicon carbide graphene nylon composite coating for elevator guide shoe liner and preparation method thereof |
| CN113897130B (en) * | 2021-09-30 | 2023-02-17 | 西安特种设备检验检测院 | Silicon carbide graphene nylon composite coating for elevator guide shoe liner and preparation method thereof |
| CN115521162A (en) * | 2022-10-17 | 2022-12-27 | 峨眉山市鑫锐新材料有限公司 | Preparation method of hollow silicon carbide microspheres |
| CN115521162B (en) * | 2022-10-17 | 2023-08-22 | 峨眉山市鑫锐新材料有限公司 | Preparation method of hollow silicon carbide microbeads |
| CN116023145A (en) * | 2022-12-29 | 2023-04-28 | 湖南福德电气有限公司 | Preparation method of silicon carbide series piezoresistor |
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