CN103553625B - Method for preparing silicon carbide micro powder for fine silicon carbide ceramics - Google Patents
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 142
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 101
- 239000000843 powder Substances 0.000 title claims abstract description 63
- 239000000919 ceramic Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000003513 alkali Substances 0.000 claims abstract description 20
- 238000005188 flotation Methods 0.000 claims abstract description 20
- 238000005554 pickling Methods 0.000 claims abstract description 20
- 238000007493 shaping process Methods 0.000 claims abstract description 20
- 239000002270 dispersing agent Substances 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000004806 packaging method and process Methods 0.000 claims abstract description 5
- 238000012216 screening Methods 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims description 32
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 20
- 238000004140 cleaning Methods 0.000 claims description 19
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000047 product Substances 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000006185 dispersion Substances 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 14
- 239000003595 mist Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 239000003921 oil Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000000746 purification Methods 0.000 claims description 9
- 239000013543 active substance Substances 0.000 claims description 6
- 239000007859 condensation product Substances 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 239000008396 flotation agent Substances 0.000 claims description 5
- 238000013467 fragmentation Methods 0.000 claims description 5
- 238000006062 fragmentation reaction Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 230000002000 scavenging effect Effects 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000005245 sintering Methods 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000000725 suspension Substances 0.000 abstract description 2
- 238000005054 agglomeration Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000009966 trimming Methods 0.000 description 1
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Abstract
The invention discloses a method for preparing silicon carbide micro powder for fine silicon carbide ceramics. The method comprises the following steps: crushing and performing jolt ramming on a silicon carbide raw material, subsequently shaping and purifying silicon carbide powder through flotation, acid pickling and alkali wash, dispersing and pulpifying the silicon carbide powder by using a dispersing agent after being purified so as to obtain silicon carbide micro powder pulp, upgrading the silicon carbide micro powder pulp, and finally performing precipitation separation, drying, screening and packaging the silicon carbide micro powder of various specifications obtained through upgrading, so as to obtain the silicon carbide micro powder for fine silicon carbide ceramics. The silicon carbide micro powder grains prepared by using the method are super-clean in surface, high in purity and high in jolt ramming density, have good mobility, shaping process property and sintering property, and can be well applied to the field of fine silicon carbide ceramic production. In the dispersing and pulpifying process, good action is achieved with the silicon carbide grains in a suspension, so that agglomeration among the micron-grade silicon carbide grains in a material liquid is effectively avoided, and meanwhile the adhesion of nano-grade silicon carbide grains to large grains is remarkably weakened.
Description
Technical field
The present invention relates to a kind of preparation method of silicon carbide micro-powder, particularly a kind of silicon carbide fine ceramics silicon carbide micro-powder, also relates to the preparation method of above-mentioned silicon carbide micro-powder.
Background technology
Silicon carbide fine ceramics has high rigidity, high strength, high-wearing feature, the feature such as corrosion-resistant, high temperature resistant, is applied to many technical fields such as aerospace, machinery, metallurgy, the energy, environmental protection, chemical industry, medical science, electronics, military project gradually.The performance of silicon carbide fine ceramics and the quality of sic raw material micro mist closely related, usually require that micro mist purity is high, even particle size distribution, particle shape be subsphaeroidal, not easily reunite there is good mobility, sintering character is good.
Existing silicon carbide micro-powder suitability for industrialized production flow process mainly comprises a series of processes such as smelting, pulverizing, purification, fine grading, need increase trimming for silicon carbide fine ceramics raw material micro mist.In above-mentioned technological process, although the separation of different-grain diameter silicon carbide micro-powder can be realized in theory, but in fact differ very large particle for some particle diameters to be difficult to realize being separated completely, as micron order silicon carbide micro-powder particle surface can adhere to a large amount of nanometer silicon carbide particles, (main component is SiO
2with the SiC of low-purity), and the existence of nanometer silicon carbide particle can reduce the purity of silicon carbide micro-powder, affect the mobility of micro mist, dispersiveness, tap density, and meeting is preferential and sintering aid reacts, cause the processability of silicon carbide micro-powder and sintering character to be deteriorated, and then cause final silicon carbide fine ceramics product properties to decline.
Summary of the invention
Technical problem to be solved by this invention is for the deficiencies in the prior art, there is provided a kind of production technique simple, efficiency is high, cost is low, easily realize suitability for industrialized production, and the preparation method of super clean, purity is high, tap density the is high silicon carbide fine ceramics silicon carbide micro-powder of particle surface can be obtained.
Technical problem to be solved by this invention is realized by following technical scheme, and the present invention is a kind of preparation method of silicon carbide fine ceramics silicon carbide micro-powder, and be characterized in, its step is as follows:
(1) Feedstock treating: silicon-carbide particle prepared using jet mill grinding machine is carried out fragmentation and classification, obtains the silicon carbide powder that particle diameter D50 is 10 ~ 14 μm, SiC content >=96% in silicon-carbide particle raw material;
(2) shaping: utilize micro mist reshaping machine that above-mentioned silicon carbide powder is carried out shaping, makes its tap density be greater than 1.85 g/ml;
(3) purify: utilize flotation, pickling, alkali cleaning to purify to silicon carbide powder after shaping; Wherein flotation carries out flotation as flotation agent to silicon carbide powder after shaping for adopting Valelinum Liquidum and terebinthine mixture, until no longer emersion uncombined carbon in slurry, wherein Valelinum Liquidum and terebinthine weight ratio are 2 ~ 3:1; Pickling is the mixing acid adopting the vitriol oil and hydrofluoric acid, at 70 ~ 80 DEG C of temperature, and pickling 3 ~ 5 h, wherein the weight ratio of the vitriol oil and hydrofluoric acid is 5 ~ 8:1; Alkali cleaning is adopt sodium hydroxide at 70 ~ 80 DEG C of temperature, alkali cleaning 3 ~ 5h; After flotation, pickling, each procedure of alkali cleaning, silicon carbide powder need be utilized pure water at room temperature to carry out ultrasonic cleaning 3 ~ 5 times, until pH value controls 7.0 ± 0.2, wherein, ultrasonic frequency is 20 KHz, and ultrasonic power is 2 KW, and each scavenging period is 20 ~ 30 min;
(4) pulp is disperseed: at room temperature mixed with pure water by the silicon carbide powder after purification processes, the weight ratio of silicon carbide powder and pure water is 1:1 ~ 2, add chemical dispersant by 0.1 ~ 0.2 % of silicon carbide powder weight fully to stir simultaneously, stirring velocity is 20 ~ 40 rpm, make silicon carbide powder fully dispersion and pulp thus obtain silicon carbide micro-powder slurries in pure water, the mixture of wherein said chemical dispersant to be weight ratio be 1 ~ 2:1 polyocarboxy acid type tensio-active agent and β-sodium sulfonate formaldehyde condensation products;
(5) classification: utilize hydraulic classification equipment to carry out physical dispersion and classification to silicon carbide micro-powder slurries, overflow obtains the silicon carbide micro-powder of different standards model, and wherein the flow velocity of hydraulic classification equipment controls at 300 ~ 800L/ h;
(6) finished product: all size silicon carbide micro-powder classification obtained respectively, through precipitate and separate, oven dry, screening, packaging, namely obtains silicon carbide fine ceramics silicon carbide micro-powder.
In the preparation method of above-described silicon carbide fine ceramics silicon carbide micro-powder of the present invention: in step (5), hydraulic classification equipment is the hydraulic classification equipment that ultrasonic unit is housed, in dispersion and fine graded process, ul-trasonic irradiation mode is continuous action, wherein ultrasonic power is 6 ~ 10KW, and ultrasonic frequency is 20 ~ 30 KHz.
Utilize the silicon carbide micro-powder that preparation method of the present invention obtains, its powder particle surface is super clean, and specific surface area is less than 0.5g/m
2, tap density is greater than 1.85 g/ml, and SiC content is not less than 99 %, and total surface oxygen level is lower than 500 ppm, and total iron content is lower than 500 ppm.
Compared with prior art, beneficial effect of the present invention is as follows:
(1) the silicon carbide micro-powder particle surface that obtains of the present invention is super clean, and purity is high, and tap density is high, has good mobility, moulded manufacturability and sintering character, can be advantageously applied to silicon carbide fine ceramics production field.
(2) the present invention adopts novel surface activity chemistry dispersion agent, this chemical dispersant can form good effect with the silicon-carbide particle in suspension, effectively prevent the reunion between micron order silicon-carbide particle in feed liquid, obviously weaken the adhesive attraction of nanometer silicon carbide particle on macrobead simultaneously.
(3) the present invention introduces ultrasonic wave field effect in classification process, realize product fine graded while complete the sepn process of micron order silicon-carbide particle nano surface level micro mist, in conjunction with the chemical dispersion effect of novel dispersant, the super clean high-quality silicon carbide micro mist in surface can be obtained.
Accompanying drawing explanation
The particle size distribution figure of Fig. 1 F500, F600, F800 product powder prepared by the present invention;
The stereoscan photograph of Fig. 2 F600 product powder particle obtained by the embodiment of the present invention 4;
The stereoscan photograph of Fig. 3 F600 product powder particle prepared by the embodiment of the present invention 5;
The stereoscan photograph of Fig. 4 F600 product powder particle prepared by the embodiment of the present invention 6.
Embodiment
Below further describe concrete technical scheme of the present invention, so that those skilled in the art understands the present invention further, and do not form the restriction to its right.
Embodiment 1, a kind of preparation method of silicon carbide fine ceramics silicon carbide micro-powder, its step is as follows:
(1) Feedstock treating: silicon-carbide particle prepared using jet mill grinding machine is carried out fragmentation and classification, obtains the silicon carbide powder that particle diameter D50 is 10 ~ 14 μm, SiC content >=96% in silicon-carbide particle raw material;
(2) shaping: utilize micro mist reshaping machine that above-mentioned silicon carbide powder is carried out shaping, makes its tap density be greater than 1.85 g/ml;
(3) purify: utilize flotation, pickling, alkali cleaning to purify to silicon carbide powder after shaping; Wherein flotation carries out flotation as flotation agent to silicon carbide powder after shaping for adopting Valelinum Liquidum and terebinthine mixture, until no longer emersion uncombined carbon in slurry, wherein Valelinum Liquidum and terebinthine weight ratio are 2:1; Pickling is the mixing acid adopting the vitriol oil and hydrofluoric acid, at 70 DEG C of temperature, and pickling 3 h, wherein the weight ratio of the vitriol oil and hydrofluoric acid is 5:1; Alkali cleaning is adopt sodium hydroxide at 70 DEG C of temperature, alkali cleaning 3h; After flotation, pickling, each procedure of alkali cleaning, silicon carbide powder need be utilized pure water at room temperature to carry out ultrasonic cleaning 3 times, until pH value controls 7.0 ± 0.2, wherein, ultrasonic frequency is 20 KHz, and ultrasonic power is 2 KW, and each scavenging period is 20 min;
(4) pulp is disperseed: at room temperature mixed with pure water by the silicon carbide powder after purification processes, the weight ratio of silicon carbide powder and pure water is 1:1, add chemical dispersant by 0.1 % of silicon carbide powder weight fully to stir simultaneously, stirring velocity is 20 rpm, make silicon carbide powder fully dispersion and pulp thus obtain silicon carbide micro-powder slurries in pure water, the mixture of wherein said chemical dispersant to be weight ratio be 1:1 polyocarboxy acid type tensio-active agent and β-sodium sulfonate formaldehyde condensation products;
(5) classification: utilize hydraulic classification equipment to carry out physical dispersion and classification to silicon carbide micro-powder slurries, overflow obtains the silicon carbide micro-powder of different standards model, and wherein the flow velocity of hydraulic classification equipment controls at 300 ~ 800L/ h;
(6) finished product: all size silicon carbide micro-powder classification obtained respectively, through precipitate and separate, oven dry, screening, packaging, namely obtains silicon carbide fine ceramics silicon carbide micro-powder.
Embodiment 2, in the preparation method according to embodiment 1, its step is as follows:
(1) Feedstock treating: silicon-carbide particle prepared using jet mill grinding machine is carried out fragmentation and classification, obtains the silicon carbide powder that particle diameter D50 is 10 ~ 14 μm, SiC content >=96% in silicon-carbide particle raw material;
(2) shaping: utilize micro mist reshaping machine that above-mentioned silicon carbide powder is carried out shaping, makes its tap density be greater than 1.85 g/ml;
(3) purify: utilize flotation, pickling, alkali cleaning to purify to silicon carbide powder after shaping; Wherein flotation carries out flotation as flotation agent to silicon carbide powder after shaping for adopting Valelinum Liquidum and terebinthine mixture, until no longer emersion uncombined carbon in slurry, wherein Valelinum Liquidum and terebinthine weight ratio are 3:1; Pickling is the mixing acid adopting the vitriol oil and hydrofluoric acid, at 80 DEG C of temperature, and pickling 5 h, wherein the weight ratio of the vitriol oil and hydrofluoric acid is 8:1; Alkali cleaning is adopt sodium hydroxide at 80 DEG C of temperature, alkali cleaning 5h; After flotation, pickling, each procedure of alkali cleaning, silicon carbide powder need be utilized pure water at room temperature to carry out ultrasonic cleaning 5 times, until pH value controls 7.0 ± 0.2, wherein, ultrasonic frequency is 20 KHz, and ultrasonic power is 2 KW, and each scavenging period is 30 min;
(4) pulp is disperseed: at room temperature mixed with pure water by the silicon carbide powder after purification processes, the weight ratio of silicon carbide powder and pure water is 1:2, add chemical dispersant by 0.2 % of silicon carbide powder weight fully to stir simultaneously, stirring velocity is 40 rpm, make silicon carbide powder fully dispersion and pulp thus obtain silicon carbide micro-powder slurries in pure water, the mixture of wherein said chemical dispersant to be weight ratio be 2:1 polyocarboxy acid type tensio-active agent and β-sodium sulfonate formaldehyde condensation products;
(5) classification: utilize hydraulic classification equipment to carry out physical dispersion and classification to silicon carbide micro-powder slurries, overflow obtains the silicon carbide micro-powder of different standards model, and wherein the flow velocity of hydraulic classification equipment controls at 300 ~ 800L/ h;
(6) finished product: all size silicon carbide micro-powder classification obtained respectively, through precipitate and separate, oven dry, screening, packaging, namely obtains silicon carbide fine ceramics silicon carbide micro-powder.
Embodiment 3, in preparation method according to embodiment 1 and 2, in step (5), hydraulic classification equipment is the hydraulic classification equipment that ultrasonic unit is housed, in dispersion and fine graded process, ul-trasonic irradiation mode is continuous action, wherein ultrasonic power is 6 ~ 10KW, and ultrasonic frequency is 20 ~ 30 KHz.
Embodiment 4: the experiment of the preparation method of silicon carbide fine ceramics silicon carbide micro-powder; Its step is as follows, first the silicon-carbide particle prepared using jet mill grinding machine of SiC content >=96% is carried out fragmentation and preliminary classification, and obtaining particle diameter D50 is 10 ~ 14 μm of powder.Utilize micro mist reshaping machine to carry out corner angle, shaping in gained powder subsequently, make powder tap density (TPD) reach 1.85 more than g/ml.
Then the powder after shaping is carried out flotation, pickling, alkali cleaning purification processes successively, after per pass purification processes operation, pure water is all utilized by silicon carbide powder at room temperature to carry out ultrasonic cleaning 4 times, each scavenging period is 25 min, until pH value controls about 7, ultrasonic frequency is 20 KHz, and ultrasonic power is 2 KW.Wherein flotation carries out flotation for adopting Valelinum Liquidum and terebinthine mixture as flotation agent, until no longer emersion uncombined carbon in slurry, wherein Valelinum Liquidum and terebinthine weight ratio are 2:1; Pickling is the mixing acid adopting the vitriol oil and hydrofluoric acid, at 75 DEG C of temperature, and pickling 4h, wherein the weight ratio of the vitriol oil and hydrofluoric acid is 5:1; Alkali cleaning is adopt sodium hydroxide at 75 DEG C of temperature, alkali cleaning 4h.
Again the silicon carbide powder after purification processes is at room temperature mixed by weight 1:1 with pure water, add polyocarboxy acid type tensio-active agent and β-sodium sulfonate formaldehyde condensation products mixture as chemical dispersant by 0.2 % of solid materials weight simultaneously, abundant stirring, stirring velocity is 30 rpm, obtains silicon carbide micro-powder slurries.Then the hydraulic classification equipment that ultrasonic unit is housed is utilized silicon carbide micro-powder slurries at room temperature to be carried out physical dispersion and fine graded, ultrasonic power is 8.4 KW, frequency is 20KHZ, the mode of action is continuous action, flow velocity selects 300L/h, 500L/h, 800L/h successively, and overflow obtains the silicon carbide micro-powder of different standards model respectively.Then through precipitate and separate, oven dry, sieve pine, obtain the silicon carbide micro-powder series product of F500, F600, F800, the performance index of product are as shown in table 1 and Fig. 1, and Fig. 2 gives the high power stereoscan photograph of prepared F600 product powder.
The performance index of table 1 F500, F600, F800 product powder prepared by the present invention
| Product | SiC （%） | C （%） | SiO 2 （%） | Si （%） | Fe 2O 3 （%） | Al 2O 3 （%） | CaO （%） | D 50 （μm） | T.P.D. （g/ml） |
| F500 | 99.75 | 0.07 | 0.12 | 0.04 | 0.015 | 0.03 | 0.002 | 11.8-13.8 | 1.95 |
| F600 | 99.70 | 0.07 | 0.15 | 0.04 | 0.015 | 0.005 | 0.002 | 8.3-10.3 | 1.90 |
| F800 | 99.60 | 0.10 | 0.20 | 0.04 | 0.015 | 0.005 | 0.005 | 5.5-7.5 | 1.85 |
Embodiment 5: the experiment of the preparation method of silicon carbide fine ceramics silicon carbide micro-powder, this experiment as different from Example 4: the ultrasonic wave diverting device of uneasy dress continuous action in hydraulic classification equipment, other step and parameter identical with embodiment 4.The high power stereoscan photograph of prepared F600 product powder as shown in Figure 3.
Embodiment 6: the experiment of the preparation method of silicon carbide fine ceramics silicon carbide micro-powder, this experiment is as different from Example 4: the chemical dispersant added in the silicon carbide powder dispersion slurrying process after purification processes is not mixed by polyocarboxy acid type tensio-active agent and β-sodium sulfonate formaldehyde condensation products and forms, but the conventional chemical dispersant used, other step and parameter identical with embodiment 4.The high power stereoscan photograph of prepared F600 product powder as shown in Figure 4.
Claims (1)
1. a preparation method for silicon carbide fine ceramics silicon carbide micro-powder, is characterized in that, its step is as follows:
(1) Feedstock treating: silicon-carbide particle prepared using jet mill grinding machine is carried out fragmentation and classification, obtains the silicon carbide powder that particle diameter D50 is 10 ~ 14 μm, SiC content >=96% in silicon-carbide particle raw material;
(2) shaping: utilize micro mist reshaping machine that above-mentioned silicon carbide powder is carried out corner angle, shaping, makes its tap density be greater than 1.85 g/mL;
(3) purify: utilize flotation, pickling, alkali cleaning to purify to silicon carbide powder after shaping; Wherein flotation carries out flotation as flotation agent to silicon carbide powder after shaping for adopting Valelinum Liquidum and terebinthine mixture, until no longer emersion uncombined carbon in slurry, wherein Valelinum Liquidum and terebinthine weight ratio are 2:1; Pickling is the mixing acid adopting the vitriol oil and hydrofluoric acid, at 75 DEG C of temperature, and pickling 4 h, wherein the weight ratio of the vitriol oil and hydrofluoric acid is 5:1; Alkali cleaning is adopt sodium hydroxide at 75 DEG C of temperature, alkali cleaning 4h; After flotation, pickling, each procedure of alkali cleaning, silicon carbide powder need be utilized pure water at room temperature to carry out ultrasonic cleaning 4 times, until pH value controls 7.0 ± 0.2, wherein, ultrasonic frequency is 20 kHz, and ultrasonic power is 2 kW, and each scavenging period is 25 min;
(4) pulp is disperseed: at room temperature mixed with pure water by the silicon carbide powder after purification processes, the weight ratio of silicon carbide powder and pure water is 1:1, add chemical dispersant by 0.2 % of silicon carbide powder weight fully to stir simultaneously, stirring velocity is 30 rpm, make silicon carbide powder fully dispersion and pulp thus obtain silicon carbide micro-powder slurries in pure water, the mixture of wherein said chemical dispersant to be weight ratio be 1:1 polyocarboxy acid type tensio-active agent and β-sodium sulfonate formaldehyde condensation products;
(5) classification: utilize the hydraulic classification equipment that ultrasonic unit is housed to carry out physical dispersion and classification to silicon carbide micro-powder slurries, in dispersion and fine graded process, ul-trasonic irradiation mode is continuous action, wherein ultrasonic power is 8.4kW, ultrasonic frequency is 20kHz, the flow velocity of hydraulic classification equipment selects 300L/h, 500L/h, 800L/h successively, and classification obtains 3 kinds of silicon carbide micro-powders;
(6) finished product: all size silicon carbide micro-powder classification obtained respectively, through precipitate and separate, oven dry, screening, packaging, namely obtains 3 kinds of silicon carbide fine ceramics silicon carbide micro-powders.
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| CN103923605B (en) * | 2014-03-14 | 2015-12-02 | 唐山圣诺纳微科技有限公司 | A kind of making method of silicon carbide ball |
| CN104923805A (en) * | 2015-07-03 | 2015-09-23 | 渤海大学 | Micro-nano-silver base material preparation method and micro-nano-silver base material thereof |
| CN105127009B (en) * | 2015-08-26 | 2018-04-06 | 连云港龙塔研磨材料有限公司 | The flotation unit and method of free carbon in a kind of removal carborundum powder |
| CN106698435A (en) * | 2016-12-16 | 2017-05-24 | 苏州金仓合金新材料有限公司 | Silicon carbide particle and preparation method thereof |
| CN106966732B (en) * | 2017-03-09 | 2021-03-23 | 平顶山学院 | Fine powder silicon carbide ceramic and preparation method thereof |
| CN108394903B (en) * | 2018-04-23 | 2021-04-09 | 刘焕新 | Preparation method of nano-scale silicon carbide micro powder |
| CN108752003B (en) * | 2018-08-17 | 2021-06-22 | 宁夏和兴碳基材料有限公司 | Preparation method of silicon carbide micro powder for silicon carbide fine ceramic |
| CN110860223A (en) * | 2019-12-05 | 2020-03-06 | 南京工业大学东海先进硅基材料研究院 | Grading method of superfine silicon carbide micro powder with narrow particle size distribution |
| CN111318352A (en) * | 2020-03-03 | 2020-06-23 | 宁夏和兴碳基材料有限公司 | Method for producing silicon carbide high-bulk density granularity sand |
| CN111302397B (en) * | 2020-03-13 | 2022-06-24 | 中国科学院城市环境研究所 | Method and device for recovering waste denitration catalyst |
| CN113680462B (en) * | 2021-10-27 | 2021-12-31 | 苏州锦艺新材料科技有限公司 | Production process of spherical silicon micropowder |
| CN113956048B (en) * | 2021-11-24 | 2022-10-14 | 唐山圣诺纳微科技有限公司 | Preparation method for silicon carbide ceramic powder by slip casting, injection and extrusion molding |
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| CN102849737A (en) * | 2011-06-28 | 2013-01-02 | 比亚迪股份有限公司 | Preparation method for silicon carbide micropowder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101920959A (en) * | 2009-06-15 | 2010-12-22 | 南京工业大学 | Process for purifying silicon carbide micro powder for linear cutting |
| CN101823712A (en) * | 2010-04-02 | 2010-09-08 | 河南新大新材料股份有限公司 | Recovery processing method of silicon slice cut waste mortar |
| CN102849737A (en) * | 2011-06-28 | 2013-01-02 | 比亚迪股份有限公司 | Preparation method for silicon carbide micropowder |
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Denomination of invention: Preparation Method of Silicon Carbide Micropowder for Silicon Carbide Fine Ceramics Effective date of registration: 20231030 Granted publication date: 20150422 Pledgee: Bank of Nanjing Co.,Ltd. Lianyungang Branch Pledgor: LIANYUNGANG ROTA GRINDING MATERIALS CO.,LTD. Registration number: Y2023980062866 |