CN105601279A - 注浆成型和固相烧结制备薄壁结构碳化硅陶瓷的方法 - Google Patents
注浆成型和固相烧结制备薄壁结构碳化硅陶瓷的方法 Download PDFInfo
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 40
- 239000000919 ceramic Substances 0.000 title claims abstract description 39
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000005245 sintering Methods 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000007790 solid phase Substances 0.000 title claims abstract description 10
- 238000007569 slipcasting Methods 0.000 title claims abstract description 6
- 239000002002 slurry Substances 0.000 claims abstract description 25
- 239000011230 binding agent Substances 0.000 claims abstract description 12
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract description 3
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 3
- 229910052602 gypsum Inorganic materials 0.000 claims description 21
- 239000010440 gypsum Substances 0.000 claims description 21
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 14
- 235000015895 biscuits Nutrition 0.000 claims description 13
- 150000007530 organic bases Chemical class 0.000 claims description 13
- 229910052580 B4C Inorganic materials 0.000 claims description 12
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000006229 carbon black Substances 0.000 claims description 12
- 238000010276 construction Methods 0.000 claims description 12
- 238000002347 injection Methods 0.000 claims description 12
- 239000007924 injection Substances 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 238000011084 recovery Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 239000013530 defoamer Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 239000011449 brick Substances 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000011505 plaster Substances 0.000 abstract 2
- 239000002518 antifoaming agent Substances 0.000 abstract 1
- 239000006260 foam Substances 0.000 abstract 1
- 238000005238 degreasing Methods 0.000 description 5
- 102220043159 rs587780996 Human genes 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000010792 warming Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000001272 pressureless sintering Methods 0.000 description 2
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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Abstract
一种注浆成型和固相烧结制备薄壁结构碳化硅陶瓷的方法，属于陶瓷制备领域。选用SiC粉体为主要原料，以去离子水为溶剂，添加适量分散剂、粘结剂后混合均匀，然后加入适量消泡剂除泡，制备出高固相含量陶瓷浆料，然后倒入石膏模具注浆，静置一段时间后倒出石膏模具中剩余浆料并回收，继续静置一段时间后经脱模、干燥直接于2100-2200℃烧成。优点在于，该工艺周期短，简单易行，制备出的薄壁结构SiC陶瓷壁厚为3-8mm，密度可达3.08-3.15g/cm3，强度为360-400MPa之间。
Description
技术领域
本发明属于陶瓷技术领域，特别是涉及一种注浆成型和固相烧结制备薄壁结构碳化硅陶瓷的方法。
背景技术
为了获得性能稳定均匀、表面质量好的钢板，一般要求热处理制度下的温度均匀性高，因此越来越多的中厚板厂采用辐射管加热无氧化辊底式炉，而碳化硅陶瓷材料热导率高，热震稳定性好，是辐射管的首选材料。
由于辐射管形状复杂，且多为薄壁结构，因此采用注浆成型较为适宜。
目前市场上常用反应烧结SiC制备辐射管，而由于反应烧结SiC陶瓷中含有大量的游离硅(10～20vol％)，因此力学性能一般，尤其是高温性能差，使其工程应用受到了很大限制。
发明内容
本发明的目的在于提供一种注浆成型和固相烧结制备的薄壁结构碳化硅陶瓷的方法，将注浆成型和无压固相烧结工艺相结合，制备性能优异的薄壁结构SiC陶瓷，碳化硅陶瓷制品壁厚为3-8mm，密度达3.08-3.15g/cm3，强度达360MPa-400MPa，这在薄壁结构碳化硅陶瓷中并不常见，较注浆成型制备的反应烧结SiC陶瓷也有较大提高。
本发明选用SiC粉体为主要原料，以去离子水为溶剂，经混料、消泡、注浆、干燥、固相烧结等工艺制备出表面光洁度高的、力学性能和高温性能更优的薄壁结构碳化硅陶瓷。本发明避免了采用注浆成型反应烧结碳化硅陶瓷的表面光洁度差、高温性能差问题，可大大提高薄壁碳化硅陶瓷的应用领域。具体工艺步骤如下：
(1)注浆成型：以碳化硅粉为原料，炭黑为碳源，碳化硼为烧结助剂，以去离子水为溶剂，以有机碱为分散剂，以改性PVA和液体石蜡为粘结剂，将陶瓷粉体原料和分散剂球磨混合0.5-3h后，加入粘结剂继续球磨0.5-3h后倒出加入消泡剂，经机械搅拌0.5-2h后，制备出固相含量为65-72vol％的浆料，将浆料倒入石膏模具中注浆，静置1-2.5h后倒出石膏模具中剩余浆料并回收，继续静置1-2h打开石膏模具脱模获得碳化硅陶瓷素坯；
(2)干燥和烧结：于115-125℃干燥5-12h，然后于2100-2200℃1-4h烧成，其中1800℃以上的升温速率不超过1.5℃/min。
优选的是，粘结剂加入量为2-6％，改性PVA和液体石蜡的比例为1:2-2:1；
优选的是，分散剂为有机碱，加入量为1-2％；
优选的是，步骤(1)所述的消泡剂为正辛醇，加入量为0.1-0.5％。
本发明的有益效果
本发明采用注浆成型和无压烧结制备薄壁结构碳化硅陶瓷制品，较反应烧结碳化硅陶瓷相比，性能更为优异：壁厚为3-8mm，密度3.08～3.15g/cm3，强度达360MPa以上。
附图说明
图1为一种薄壁结构的固相烧结碳化硅陶瓷制品的制备工艺流程图。
图2为薄壁结构的碳化硅陶瓷制品的剖面图。
图3为图2的俯视图。
具体实施方式
下面结合具体实施例本发明做进一步详细的说明。
实施例1：
SiC原料粒度D50＝1.6μm；以炭黑为碳源，添加1％碳化硼，粘结剂为改性PVA和液体石蜡的混合物，其中改性PVA:液体石蜡＝1:1，加入量为3.5％，分散剂有机碱加入量为1％。
将2000gSiC粉体，40g炭黑、20g碳化硼以及20g有机碱等放入球磨罐，加入去离子水球磨1h，然后加入35g改性PVA和35g液体石蜡，继续球磨3h后倒出浆料至除泡罐中，加入5g正辛醇，缓慢搅拌2h除泡，得到固相含量为66％的浆料。
将浆料倒入石膏模具注浆，静置1.5h后倒出石膏模具中剩余浆料并回收，继续静置1.5h后打开石膏模具脱模获得素坯；
将SiC陶瓷素坯置入干燥箱中于118℃保温6h；
将干燥后的SiC陶瓷生坯放入真空烧结炉中，脱脂和烧结一体化进行，升至1750℃后以0.8℃/min升至2175℃，保温2h烧成。
制备出的SiC陶瓷制品壁厚为4.1mm，密度可达3.09g/cm3，强度为362MPa。
实施例2：
SiC原料粒度D50＝2μm；以炭黑为碳源，添加0.6％碳化硼，粘结剂为改性PVA:液体石蜡＝1.2:1，加入量为5％。分散剂有机碱加入量为1.1％。
将2000gSiC粉体，45g炭黑、12g碳化硼、22g有机碱放入球磨罐，加入去离子水球磨1.5h，然后加入54.5g改性PVA、45.5g液体石蜡，继续球磨2h后倒出浆料至除泡罐中，加入4g正辛醇，缓慢搅拌1.5h除泡，得到固相含量为68％的浆料。
将浆料倒入石膏模具，静置2h后倒出石膏模具中剩余浆料并回收，继续静置1.6h后打开石膏模具脱模获得素坯；
将SiC陶瓷素坯置入干燥箱中于120℃保温10h；
将干燥后的SiC陶瓷生坯放入真空脱脂炉中以2.5℃/分的速率升温至850℃，保温2.5h后取出放置真空烧结炉中，1800℃后升温速率为1.5℃/min，于2190℃保温2.5h烧成。
制备出的SiC陶瓷制品壁厚为5.2mm，密度可达3.10g/cm3，强度为371MPa。
实施例3：
SiC原料粒度D50＝1.8μm；以炭黑为碳源，添加1.2％碳化硼，粘结剂为改性PVA:液体石蜡＝3:4，加入量为6％。分散剂有机碱加入量为1.8％。
将2000gSiC粉体，60g炭黑、24g碳化硼以及36g有机碱等放入球磨罐，加入去离子水球磨1.5h，然后加入51.4g改性PVA、68.6g液体石蜡，继续球磨1.8h后倒出浆料至除泡罐中，加入6g正辛醇，缓慢搅拌1h除泡，得到固相含量为70％的浆料。
将浆料倒入石膏模具，静置1.6h后倒出石膏模具中剩余浆料并回收，继续静置2h后打开石膏模具脱模获得素坯；
将SiC陶瓷素坯置入干燥箱中于115℃保温12h；
将干燥后的SiC陶瓷生坯放入真空脱脂炉中以3℃/分的速率升温至800℃，保温3h后取出放入真空烧结炉中，以5℃/分升至1800℃，然后以1℃/分升至2160℃保温2h烧成。
制备出的SiC陶瓷制品壁厚为4.3mm，密度可达3.11g/cm3，强度为380MPa。
实施例4：
SiC原料粒度D50＝1.8μm；以炭黑为碳源，添加1.8％碳化硼，粘结剂为改性PVA:液体石蜡＝1.2:1，加入量为5.5％。分散剂有机碱加入量为2％。
将2000gSiC粉体，50g炭黑、36g碳化硼以及40g有机碱等放入球磨罐，加入去离子水球磨1.5h，然后加入60g改性PVA、50g液体石蜡，继续球磨1.5h后倒出浆料至除泡罐中，加入8g正辛醇，缓慢搅拌1h除泡，得到固相含量为70％的浆料。
将浆料倒入石膏模具，静置1h后倒出石膏模具中剩余浆料并回收，继续静置1.5h后打开石膏模具脱模获得素坯；
将SiC陶瓷素坯置入干燥箱中于115℃保温11h；
将干燥后的SiC陶瓷生坯放入真空脱脂炉中以2.5℃/分的速率升温至800℃，保温3h后取出放入真空烧结炉中，以5℃/分升至1800℃，然后以1.2℃/分升至2160℃保温2h烧成。
制备出的SiC陶瓷制品壁厚为3.4mm，密度可达3.11g/cm3，强度为388MPa。
实施例5：
SiC原料粒度D50＝2μm；以炭黑为碳源，添加2％碳化硼，粘结剂为改性PVA:液体石蜡＝1:1.8，加入量为6％。分散剂有机碱加入量为1.5％。
将2000gSiC粉体，36g炭黑、40g碳化硼以及30g有机碱等放入球磨罐，加入去离子水球磨2h，然后加入42.86g改性PVA、77.14g液体石蜡，继续球磨1.6h后倒出浆料至除泡罐中，加入10g正辛醇，缓慢搅拌1h除泡，得到固相含量为70％的浆料。
将浆料倒入石膏模具，静置1.4h后倒出石膏模具中剩余浆料并回收，继续静置1.6h后打开石膏模具脱模获得素坯；
将SiC陶瓷素坯置入干燥箱中于120℃保温9h；
将干燥后的SiC陶瓷生坯放入真空脱脂炉中以3℃/分的速率升温至800℃，保温3h后取出放入真空烧结炉中，以5℃/分升至1800℃，然后以1.3℃/分升至2175℃保温2h烧成。
制备出的SiC陶瓷制品壁厚为4.1mm，密度可达3.11g/cm3，强度为391MPa。
本发明采用注浆成型和无压烧结制备薄壁结构碳化硅陶瓷制品，较反应烧结碳化硅陶瓷相比，性能更为优异：壁厚为3-8mm，密度3.08～3.15g/cm3，强度达360MPa以上。
Claims (4)
1.一种注浆成型和固相烧结制备薄壁结构碳化硅陶瓷的方法，其特征在于：工艺步骤及技术参数如下：
(1)注浆成型：以碳化硅粉为原料，炭黑为碳源，碳化硼为烧结助剂，以去离子水为溶剂，以有机碱为分散剂，以改性PVA和液体石蜡为粘结剂，将陶瓷粉体原料和分散剂球磨混合0.5-3h后，加入粘结剂继续球磨0.5-3h后倒出加入消泡剂，经机械搅拌0.5-2h后，制备出固相含量为65-72vol％的浆料，将浆料倒入石膏模具中注浆，静置1-2.5h后倒出石膏模具中剩余浆料并回收，继续静置1-2h打开石膏模具脱模获得碳化硅陶瓷素坯；
(2)干燥和烧结：将成型后的陶瓷素坯于115-125℃干燥5-12h后，于2100-2200℃保温1-4h烧成，其中1800℃以上的升温速率不超过1.5℃/min。
2.根据权利要求1所述的方法，其特征在于，步骤(1)中粘结剂的加入量为2-6％，改性PVA和液体石蜡的比例为1:2-2:1。
3.根据权利要求1所述方法，其特征在于，步骤(1)中的分散剂为有机碱，加入量为1-2％。
4.根据权利要求1所述的方法，其特征在于，步骤(1)中的消泡剂为正辛醇，加入量为0.1-0.5％。
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