CN105294108A - Preparation method of low-cost normal pressure-sintered silicon carbide ceramics - Google Patents
Preparation method of low-cost normal pressure-sintered silicon carbide ceramics Download PDFInfo
- Publication number
- CN105294108A CN105294108A CN201510880871.1A CN201510880871A CN105294108A CN 105294108 A CN105294108 A CN 105294108A CN 201510880871 A CN201510880871 A CN 201510880871A CN 105294108 A CN105294108 A CN 105294108A
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- preparation
- raw material
- main raw
- normal pressure
- 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.)
- Pending
Links
Landscapes
- Ceramic Products (AREA)
Abstract
The invention relates to a preparation method of low-cost normal pressure-sintered silicon carbide ceramics. The preparation method is characterized by comprising the following steps: (1) preparing a main raw material; (2) preparing silicon carbide slurry; (3) granulating; (4) molding granulating powder, so as to obtain a biscuit; and (5) sintering, so as to obtain silicon carbide ceramics. Compared with the prior art, the preparation method has the advantages that coarse silicon carbide powder is used as a main raw material for carrying out normal pressure sintering, the density of the coarse silicon carbide powder can reach 3.0g/cm<3>, the average density can reach more than or equal to 94%, and the density and the average density are approximate to the performance of normal pressure sintering density of micro-fine silicon carbide powder, so that application of most fields is met; the cost of coarse-grained silicon carbide powder is much lower than that of the micro-fine silicon carbide powder, so that the production cost of the silicon carbide ceramics is substantially lowered; the preparation method is applicable to industrial batch production.
Description
Technical field
The present invention relates to a kind of preparation method of silicon carbide ceramics.
Background technology
Silicon carbide ceramics has the premium propertiess such as hardness is high, hot strength is large, thermal expansivity is little, chemical stability is good, is widely used at the industrial circles such as machinery, electronics, petrochemical complex, space flight and military field.But silicon carbide has very strong covalent bonds, be typical hard-to-sinter material, make the production cost of high-performance silicon carbide pottery costly, constrain the mass-producing application of silicon carbide ceramics largely.
Normal pressure-sinteredly refer to the method being sintered in an atmosphere by ceramic powder and obtain stupalith, also known as pressureless sintering method, it is by means of sintering aid, the densification sintering of silicon carbide ceramics can be realized at ambient pressure, be applicable to the sintering of different shapes, complex construction goods, be a kind of cost lower, easily realize the industrial sintering method of mass.
Because silicon carbide ceramics rate of diffusion when sintering is lower, therefore the normal pressure-sintered requirement to powder is comparatively strict, mostly adopts particle diameter D
50about 0.5 μm, the comparatively uniform superfine powder of size-grade distribution sinters, and could realize silicon carbide ceramics sintering densification.This kind of document can the referenced patent number Chinese invention patent " preparation method of normal pressure-sintered silicon carbide ceramics " (Authorization Notice No. is CN101555143B) that is ZL200910098377.4; All right referenced patent number is the Chinese invention patent " a kind of normal pressure solid state sintering micro-pore silicon carbide pottery and preparation method thereof " (Authorization Notice No. is CN102765940B) of ZL201110114635.0, and this patent adopts the carborundum powder of 0.1 ~ 1 μm; All right application reference number is open " method of two-step approach solid-phase sintered silicon carbide ceramics with no pressure " (application publication number is CN104446493A) of Chinese invention patent application of 201410728865.X, and the document adopts the carborundum powder of 0.6 μm.
But superfine silicon carbide powder preparation cost is high, and along with the increase of specific surface area, being very easily oxidized when processing, making employing pressureless sintering method prepare silicon carbide ceramics and the cost advantage that reduces receives restriction to a certain degree.
Summary of the invention
Technical problem to be solved by this invention provides a kind of most crude particle carborundum powder that utilizes to substitute trickle carborundum powder with the preparation method of the normal pressure-sintered silicon carbide ceramics reduced costs for the above-mentioned state of the art.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of preparation method of low cost normal pressure-sintered silicon carbide ceramics, is characterized in that comprising the steps:
1. main raw material prepares, and main raw material comprises the component of following weight percent:
2. silicon carbide slurry preparation, by main raw material be the dehydrated alcohol of main raw material weight 120% ~ 280%, deionized water is main raw material weight 1% ~ 5%, and dispersion agent is that main raw material weight 1% ~ 5% adds in ball mill or sand mill, is mixed with the silicon carbide slurry that solid content is 30% ~ 50%; Aforesaid dispersion agent employing solid content is the aqueous sodium dipersant of 41.5% ~ 43.5%;
3. granulation, silicon carbide slurry, adopts spray drying granulation machine granulation silicon carbide slurry, obtains pelletizing, spray drying condition: inlet temperature is 145 DEG C ~ 195 DEG C, shower nozzle spraying frequency 15Hz ~ 25Hz, temperature out is 75 DEG C ~ 125 DEG C;
4. biscuit obtains, and obtains biscuit by shaping for pelletizing;
5. sinter, biscuit is put into sintering oven, pass into argon gas, at 2200 DEG C ~ 2250 DEG C temperature, be incubated 2h ~ 4h complete normal pressure-sintered, obtain silicon carbide ceramics.Normal pressure-sintered namely material pressurization and make it sinter at atmosheric pressure, preferable range is 1 ± 20% normal atmosphere, and acquiescence refers to 1 normal atmosphere (1.01 × 105Pa) usually,
As preferably, coarse particles carborundum powder purity >=98% that step is 1. described, carbide fine powder purity >=98%, boron carbide powder purity >=95%, alcohol resite solid content >=84%.
As preferably, step 2. in adopt ball milling slurrying, condition is as follows: adopt sphere diameter 10mm ~ 15mm silicon carbide medium ball, ratio of grinding media to material 3 ~ 4:1,3 ~ 7 hours ball mill mixing time, slurry pH value 3 ~ 10, drum's speed of rotation is 180r/min ~ 220r/min.
As preferably, step 2. in be adopted as dispersion agent be the T-61 dispersion agent that Toagosei Co., Ltd produces.
As preferably, step 4. in biscuit by the dry pressure formed or shaping acquisition of cold isostatic pressing process.
Compared with prior art, the invention has the advantages that: adopt thick silicon carbide powder to be that main raw material(s) carries out normal pressure-sintered, density can reach 3.0g/cm
3, density on average reaches more than 94%, substantially can reach 3.17g/cm close to the normal pressure-sintered density of fine silicon carbide powder
3, density reaches the performance of more than 97%, meets the application of most fields, but coarse grained carborundum powder trickleer carborundum powder cost is much lower, reduces shortening by a relatively large margin by making the production cost of silicon carbide ceramics have, and is applicable to industrialized mass production.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1:
By coarse particles carborundum powder (W2.0 μm) 700g, carbide fine powder (W0.5 μm) 270g, alcohol resite 21g, norbide 13g, add T-61 dispersion agent 18.8g, deionized water 30g, dehydrated alcohol 1500ml carries out ball milling slurrying and (controls the ball mill mixing time, drum's speed of rotation, ratio of grinding media to material, the obtained slurry being suitable for spray drying granulation, be specially: adopt the silicon carbide ceramics ball of sphere diameter 10mm ~ 15mm as ball-milling medium ball, ratio of grinding media to material 3:1, 4.5 hours ball mill mixing time, slurry pH value 8 ~ 9, drum's speed of rotation is 220r/min), then after slurry being crossed 60 mesh sieves, spray drying granulation is carried out with spray drying granulation machine, obtain pelletizing, processing parameter is: shower nozzle spraying frequency 16Hz, inlet temperature is 150 DEG C, temperature out is 115 DEG C and obtains pelletizing, gained pelletizing adopts that 150MPa is dry pressure formed obtains biscuit, biscuit is put into vacuum sintering furnace, keeps vacuum tightness in stove to be 10 ~ 600Pa before 1600 DEG C, pass into argon gas when 1600 DEG C to normal pressure, at 2250 DEG C of insulation 2 ~ 3h, after cooling, obtain silicon carbide ceramics.T-61 dispersion agent in the present embodiment is produced by Toagosei Co., Ltd of manufacturers, and commission merchant is Yantai addition chemistry Science and Technology Ltd., and trade mark is called ARON.
The density of this silicon carbide ceramics is 3.02g/cm3, and density is 94.3%.
Embodiment 2:
By coarse particles carborundum powder (W2.0 μm) 720g, carbide fine powder (W0.5 μm) 250g, alcohol resite 22g, norbide 13.1g, add T-61 dispersion agent 19g, deionized water 35g, dehydrated alcohol 1500ml carries out ball milling slurrying and (controls the ball mill mixing time, drum's speed of rotation, ratio of grinding media to material, the obtained slurry being suitable for spray drying granulation, be specially: adopt the silicon carbide ceramics ball of sphere diameter 10mm ~ 15mm as ball-milling medium ball, ratio of grinding media to material 3:1, 4.5 hours ball mill mixing time, slurry pH value 8 ~ 9, drum's speed of rotation is 220r/min), then after slurry being crossed 60 mesh sieves, spray drying granulation is carried out with spray drying granulation machine, obtain pelletizing, processing parameter is: shower nozzle spraying frequency 16Hz, inlet temperature is 150 DEG C, temperature out is 110 DEG C and obtains pelletizing, gained pelletizing adopts that 150MPa is dry pressure formed obtains biscuit, biscuit is put into vacuum sintering furnace, keeps vacuum tightness in stove to be 10 ~ 600Pa before 1600 DEG C, pass into argon gas when 1600 DEG C to normal pressure, at 2250 DEG C of insulation 2 ~ 3h, after cooling, obtain silicon carbide ceramics.
The density of this silicon carbide ceramics is 3.01g/cm
3, density is 94.1%.
Embodiment 3:
By coarse particles carborundum powder (W2.0 μm) 700g, carbide fine powder (W0.5 μm) 280g, alcohol resite 23g, norbide 13.1g, add T-61 dispersion agent 19.5g, deionized water 40g, dehydrated alcohol 1500ml carries out ball milling slurrying and (controls the ball mill mixing time, drum's speed of rotation, ratio of grinding media to material, the obtained slurry being suitable for spray drying granulation, be specially: adopt the silicon carbide ceramics ball of sphere diameter 10mm ~ 15mm as ball-milling medium ball, ratio of grinding media to material 3:1, 4.5 hours ball mill mixing time, slurry pH value 8 ~ 9, drum's speed of rotation is 220r/min), then after slurry being crossed 60 mesh sieves, spray drying granulation is carried out with spray drying granulation machine, obtain pelletizing, processing parameter is: shower nozzle spraying frequency 16Hz, inlet temperature is 160 DEG C, temperature out is 115 DEG C and obtains pelletizing, gained pelletizing adopts that 150MPa is dry pressure formed obtains biscuit, biscuit is put into vacuum sintering furnace, keeps vacuum tightness in stove to be 10 ~ 600Pa before 1600 DEG C, pass into argon gas when 1600 DEG C to normal pressure, at 2250 DEG C of insulation 2 ~ 3h, after cooling, obtain silicon carbide ceramics.
The density of this silicon carbide ceramics is 3.0g/cm
3, density is 93.7%.
Claims (5)
1. a preparation method for low cost normal pressure-sintered silicon carbide ceramics, is characterized in that comprising the steps:
1. main raw material prepares, and main raw material comprises the component of following weight percent:
2. silicon carbide slurry preparation, by main raw material be the dehydrated alcohol of main raw material weight 120% ~ 280%, deionized water is main raw material weight 1% ~ 5%, and dispersion agent is that main raw material weight 1% ~ 5% adds in ball mill or sand mill, is mixed with the silicon carbide slurry that solid content is 30% ~ 50%; Aforesaid dispersion agent employing solid content is the aqueous sodium dipersant of 41.5% ~ 43.5%;
3. granulation, silicon carbide slurry, adopts spray drying granulation machine granulation silicon carbide slurry, obtains pelletizing, spray drying condition: inlet temperature is 145 DEG C ~ 195 DEG C, shower nozzle spraying frequency 15Hz ~ 25Hz, temperature out is 75 DEG C ~ 125 DEG C;
4. biscuit obtains, and obtains biscuit by shaping for pelletizing;
5. sinter, biscuit is put into sintering oven, pass into argon gas, at 2200 DEG C ~ 2250 DEG C temperature, be incubated 2h ~ 4h complete normal pressure-sintered, obtain silicon carbide ceramics.
2. preparation method according to claim 1, is characterized in that coarse particles carborundum powder purity >=98% that step is 1. described, carbide fine powder purity >=98%, boron carbide powder purity >=95%, alcohol resite solid content >=84%.
3. preparation method according to claim 1, it is characterized in that adopting ball milling slurrying during step 2., condition is as follows: adopt sphere diameter 10mm ~ 15mm silicon carbide medium ball, ratio of grinding media to material 3 ~ 4:1,3 ~ 7 hours ball mill mixing time, slurry pH value 3 ~ 10, drum's speed of rotation is 180r/min ~ 220r/min.
4. preparation method according to claim 1, is characterized in that being adopted as dispersion agent during step is 2. the T-61 dispersion agent that Toagosei Co., Ltd produces.
5. preparation method according to claim 1, is characterized in that biscuit during step is 4. by the dry pressure formed or shaping acquisition of cold isostatic pressing process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510880871.1A CN105294108A (en) | 2015-12-03 | 2015-12-03 | Preparation method of low-cost normal pressure-sintered silicon carbide ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510880871.1A CN105294108A (en) | 2015-12-03 | 2015-12-03 | Preparation method of low-cost normal pressure-sintered silicon carbide ceramics |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105294108A true CN105294108A (en) | 2016-02-03 |
Family
ID=55192046
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510880871.1A Pending CN105294108A (en) | 2015-12-03 | 2015-12-03 | Preparation method of low-cost normal pressure-sintered silicon carbide ceramics |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105294108A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107043259A (en) * | 2017-03-17 | 2017-08-15 | 宁波伏尔肯陶瓷科技有限公司 | A kind of reaction sintering silicon carbide ceramic selective laser sintering forming method |
| CN109180195A (en) * | 2018-09-30 | 2019-01-11 | 威海威林特电控科技有限公司 | One kind is based on adding obdurability porous ceramic composite and its preparation process made of infiltrated metal method |
| CN111875384A (en) * | 2020-08-11 | 2020-11-03 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of silicon carbide plug for hot piercing of seamless steel tube |
| CN112830798A (en) * | 2021-01-19 | 2021-05-25 | 黑龙江冠瓷科技有限公司 | A kind of preparation method of boron carbide granulated powder for pressureless sintering |
| CN113121239A (en) * | 2021-03-03 | 2021-07-16 | 山东君道高温材料有限公司 | Preparation process of large-size pressureless sintered silicon carbide ceramic material |
| CN113372096A (en) * | 2020-03-09 | 2021-09-10 | 江苏省宜兴非金属化工机械厂有限公司 | Preparation method of low-temperature normal-pressure sintered silicon carbide composite ceramic, silicon carbide composite ceramic product prepared by preparation method and application of silicon carbide composite ceramic product |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10291857A (en) * | 1997-04-22 | 1998-11-04 | Hitachi Chem Co Ltd | High specific resistance sic sintered compact |
| CN103641482A (en) * | 2013-10-25 | 2014-03-19 | 宁夏机械研究院（有限责任公司） | Preparation method for self-lubricating silicon carbide ceramic sealing material |
| CN104291827A (en) * | 2014-10-14 | 2015-01-21 | 中国钢研科技集团有限公司 | Process for preparing silicon carbide ceramic in complicated shape from phenolic resin serving as carbon source by adopting solid phase sintering |
-
2015
- 2015-12-03 CN CN201510880871.1A patent/CN105294108A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10291857A (en) * | 1997-04-22 | 1998-11-04 | Hitachi Chem Co Ltd | High specific resistance sic sintered compact |
| CN103641482A (en) * | 2013-10-25 | 2014-03-19 | 宁夏机械研究院（有限责任公司） | Preparation method for self-lubricating silicon carbide ceramic sealing material |
| CN104291827A (en) * | 2014-10-14 | 2015-01-21 | 中国钢研科技集团有限公司 | Process for preparing silicon carbide ceramic in complicated shape from phenolic resin serving as carbon source by adopting solid phase sintering |
Non-Patent Citations (1)
| Title |
|---|
| 刘维良等: ""无压烧结制备SiC密封件的工艺与性能研究"", 《中国陶瓷工业》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107043259A (en) * | 2017-03-17 | 2017-08-15 | 宁波伏尔肯陶瓷科技有限公司 | A kind of reaction sintering silicon carbide ceramic selective laser sintering forming method |
| CN107043259B (en) * | 2017-03-17 | 2020-03-10 | 宁波伏尔肯科技股份有限公司 | Selective laser sintering forming method for reactive sintering silicon carbide ceramic |
| CN109180195A (en) * | 2018-09-30 | 2019-01-11 | 威海威林特电控科技有限公司 | One kind is based on adding obdurability porous ceramic composite and its preparation process made of infiltrated metal method |
| CN113372096A (en) * | 2020-03-09 | 2021-09-10 | 江苏省宜兴非金属化工机械厂有限公司 | Preparation method of low-temperature normal-pressure sintered silicon carbide composite ceramic, silicon carbide composite ceramic product prepared by preparation method and application of silicon carbide composite ceramic product |
| CN113372096B (en) * | 2020-03-09 | 2022-08-02 | 江苏省宜兴非金属化工机械厂有限公司 | Preparation method of low-temperature normal-pressure sintered silicon carbide composite ceramic, silicon carbide composite ceramic product prepared by preparation method and application of silicon carbide composite ceramic product |
| CN111875384A (en) * | 2020-08-11 | 2020-11-03 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of silicon carbide plug for hot piercing of seamless steel tube |
| CN112830798A (en) * | 2021-01-19 | 2021-05-25 | 黑龙江冠瓷科技有限公司 | A kind of preparation method of boron carbide granulated powder for pressureless sintering |
| CN112830798B (en) * | 2021-01-19 | 2022-05-06 | 哈尔滨工业大学 | Preparation method of boron carbide granulation powder for pressureless sintering |
| CN113121239A (en) * | 2021-03-03 | 2021-07-16 | 山东君道高温材料有限公司 | Preparation process of large-size pressureless sintered silicon carbide ceramic material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105294108A (en) | Preparation method of low-cost normal pressure-sintered silicon carbide ceramics | |
| KR100462274B1 (en) | A method of manufacturing tungsten- copper based composite powder and sintered alloy for heat sink using the same | |
| CN100445235C (en) | A kind of aluminum nitride reinforced silicon carbide ceramics and preparation method thereof | |
| CN104150882B (en) | A kind of aluminum oxide preparation of microbeads | |
| KR101208896B1 (en) | Manufacturing method of alumina abrasive grains and alumina abrasive grains manufactured by the method | |
| CN104291827A (en) | Process for preparing silicon carbide ceramic in complicated shape from phenolic resin serving as carbon source by adopting solid phase sintering | |
| CN107651965A (en) | A kind of silicon nitride ceramic material and preparation method thereof | |
| CN102311268A (en) | Highly compact ceramic ball of silicon carbide and preparation process thereof | |
| CN102115330A (en) | Preparation method of solid phase sintering silicon carbide ceramics taking phenolic resin as carbon source | |
| CN105294138A (en) | Doublet aluminum oxide micropowder and preparation method thereof | |
| CN104788083B (en) | A kind of polycrystalline silicon reducing furnace high-heat resistance shock resistant aluminium oxide ceramics ring and preparation method | |
| CN116947499B (en) | Silicon carbide ceramic material and preparation method and application thereof | |
| CN104387073A (en) | Method for manufacturing ultrafine high-toughness silicon carbide ceramic material based on reaction sintering technology | |
| CN106032323B (en) | A kind of preparation method of Ti2AlC ceramic powder using TiAl powder as raw material | |
| CN101734920B (en) | Titanium nitride porous ceramics and preparation method thereof | |
| CN103194631B (en) | Preparation method of high-volume fraction alumina ceramic particle enhanced composite material | |
| JP2015501775A (en) | Production method of transparent ceramic body by fluidized bed granulation | |
| CN103693646B (en) | Method for spheroidizing and purifying silicon carbide micropowder | |
| CN104788094B (en) | A kind of preparation method of bismuth titanate ceramics material | |
| CN117164345B (en) | Low-cost preparation method of sintered microcrystalline corundum sand raw material | |
| CN101585701A (en) | Method for manufacturing superfine alpha-alumina powder suitable for various ceramic molding technics | |
| CN107628814A (en) | A kind of silicon carbide ceramics valve and preparation method thereof | |
| CN104016668A (en) | Preparation method of mullite ceramic powder | |
| CN104591743B (en) | The preparation method of silicon nitride-silicon carbide hafnium complex phase ceramic | |
| JP2013023745A (en) | Titanium nitride sputtering target and method of manufacturing the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160203 |