CN116655386B - 一次性重结晶圆环状碳化硅加热盘及其制备方法 - Google Patents
一次性重结晶圆环状碳化硅加热盘及其制备方法 Download PDFInfo
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- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 16
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- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 24
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
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- 239000013065 commercial product Substances 0.000 description 1
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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Abstract
本发明属于加热盘及其制备方法的技术领域，具体涉及一次性重结晶圆环状碳化硅加热盘及其制备方法。本发明所述的一次性重结晶圆环状碳化硅加热盘，是由以下原料按照质量百分比制成的：碳化硅：95.3‑97.98％；氮化硼：0.02‑0.20％；水溶胶：2.0‑4.5％；所述的水溶胶为糖和聚乙烯醇的混合物。本发明提供的一次性重结晶圆环状碳化硅加热盘，电气性能稳定性好，合格率高；本发明还提供其制备方法。
Description
技术领域
本发明属于加热盘及其制备方法的技术领域，具体涉及一次性重结晶圆环状碳化硅加热盘及其制备方法。
背景技术
圆环状碳化硅加热盘应用于底部加热且需快速升温、炉温高于800℃的场合。圆环状电加热方式最常见的是金属电热盘，由电阻丝盘旋成蚊香式的现状构成，但是在需要快速升温，且炉温高于800℃，尤其是炉温高于1100℃的应用场合，金属电热盘的功率偏低，难以满足实际需求。为解决此难题，采用圆环状碳化硅加热盘，从功率、使用温度等方面，可以替代金属电热盘，在相同的尺寸前提下，圆环状碳化硅加热盘的功率是金属电热盘的5-6倍，使用温度从金属加热盘的800℃提升至1400℃，但是圆环状碳化硅加热盘是脆性材料，其生产制造难度很大，一是容易断裂，导致合格率低，二是因为形状较复杂，密度难以均一，造成使用时间较短，三是电阻值难以控制。目前，国内尚无批量生产的厂家。
CN113831136A公开了一种一种固相烧结碳化硅制品及其制备方法，将微米级碳化硅粉末与含硼烧结助剂混合并湿法研磨，得到浆料；喷雾造粒：向浆料中加入水溶性炭黑和粘结剂，搅拌均匀，经过喷雾造粒，得到碳化硅造粒粉体；混料；陈腐：将混料得到的湿粉经过陈腐，得到陈腐料；后处理：将陈腐料经过练泥、挤出、干燥、热处理即可。本申请的制备方法制备的碳化硅制品可用作换热管、辊棒、方梁、微反应管等，其制品虽然烧结密度高、抗压强度大。但因其本身不发热，用途与性能也完全不能应用于圆环状加热盘，其生产工艺与烧成原理与本发明有本质区别。
发明内容
本发明要解决的技术问题是克服现有技术存在的上述缺陷，提供一次性重结晶圆环状碳化硅加热盘，电气性能稳定性好，合格率高；本发明还提供其制备方法。
本发明所述的一次性重结晶圆环状碳化硅加热盘，是由以下原料按照质量百分比制成的：
碳化硅：95.3-97.98％；
氮化硼：0.02-0.20％；
水溶胶：2.0-4.5％；
所述的水溶胶为糖和聚乙烯醇的混合物。
糖、聚乙烯醇的混合物的质量比为：(30-70):(70-30)。
碳化硅为高温绿碳化硅，纯度为99.0wt.％以上。
碳化硅的颗粒度型号按照质量比的组成为：粗号40-65wt.％，中号10-20wt.％，细号25-40wt.％；其中粗号为100-300μm，中号为20-50μm，细号为0.5-5μm。
氮化硼的粒度＜2.5μm，纯度≥98.5wt.％。
所述的一次性重结晶圆环状碳化硅加热盘的制备方法，包括以下步骤：
(1)干混料：将原料碳化硅、氮化硼加入搅拌机，搅拌40-60min，得到干混料；
(2)湿混料造粒：将糖、聚乙烯醇混合后的水溶胶，加入干混料中，搅拌60-80min，得到的混合料进行造粒，至粒径为50-350μm；
(3)成型：将造粒放入压机模型，进行压制成型，脱模，得到毛坯件；
(4)烘干：将毛坯件放入干燥箱烘干；
(5)烧成：将烘干后的毛坯件，进行重结晶烧成，冷却后获得成品。
步骤(2)将糖、聚乙烯醇混合配制成浓度为30wt.％-50wt.％的水溶胶。
步骤(3)将造粒放入压机模型，按1:(2.5-2.8)的压缩比进行压制成型。
步骤(4)烘干温度为110-170℃，烘干时间6-8h。
步骤(5)的烧成温度2250-2550℃，烧成时间为1-3h。
具体的，所述的一次性重结晶圆环状碳化硅加热盘的制备方法，包括以下步骤：
(1)干混料：将原料95.3-97.98％碳化硅、0.02-0.20％氮化硼加入搅拌机，搅拌40-60min，得到干混料；其中碳化硅的颗粒度型号按照质量比的组成为：粗号40-65wt.％，中号10-20wt.％，细号25-40wt.％。
(2)湿混料造粒：将糖、聚乙烯醇按照质量比为：(30-70):(70-30)混合，配制成浓度为30wt.％-50wt.％的溶液，即水溶胶，将2.0-4.5％的水溶胶加入干混料中，搅拌60-80min，得到的混合料进行造粒，至粒径为50-350μm。
(3)成型：将造粒放入压机模型，按1:(2.5-2.8)的压缩比进行压制成型，脱模，得到毛坯件。
(4)烘干：将毛坯件在110-170℃放入干燥箱烘干6-8h。
(5)烧成：将烘干后的毛坯件，在2250-2550℃进行重结晶烧成1-3h，冷却后获得成品。
本发明采用以特定颗粒粒度的质量比的碳化硅为主要原料，结合氮化硼作为辅助原料，协同特定比例的糖、聚乙烯醇的混合物为水溶胶，将原料按照本发明的顺序经过干混、湿混、成型，然后进行烤干、烧成，制得产品。本发明的一次性重结晶圆环状碳化硅加热盘适用于医疗设备及其他精密设备加热场合。
与现有技术相比，本发明具有的有益效果是：
(1)本发明的一次性重结晶圆环状碳化硅加热盘的制备方法，工艺简单，可操作性强；
(2)采用本发明的制备方法制得的圆环状碳化硅加热盘，电气性能好，延长使用时间。
附图说明
图1为本发明制备的一次性重结晶圆环状碳化硅加热盘的示意图。
具体实施方式
下面结合具体实施例对本发明作进一步说明。以下实施例与对比例中的原料与试剂均来自正常市售产品。其中碳化硅为高温绿碳化硅，纯度为99.0wt.％以上。氮化硼的粒度＜2.5μm，纯度≥98.5wt.％。碳化硅的颗粒度型号的粗号为100-300μm，中号为20-50μm，细号为0.5-5μm。
实施例1
所述的一次性重结晶圆环状碳化硅加热盘的制备方法，包括以下步骤：
(1)干混料：将原料96％碳化硅、0.15％氮化硼加入搅拌机，搅拌50min，得到干混料；其中碳化硅的颗粒度型号按照质量比的组成为：粗号50wt.％，中号15wt.％，细号35wt.％。
(2)湿混料造粒：将糖、聚乙烯醇按照质量比为：50:50混合，配制成浓度为40wt.％的溶液，即水溶胶，将3.85％加入干混料中，搅拌70min，得到的混合料进行造粒，至粒径为50-90μm。
(3)成型：将造粒放入压机模型，按1:2.6的压缩比进行压制成型，脱模，得到毛坯件。
(4)烘干：将毛坯件在150℃放入干燥箱烘干7h。
(5)烧成：将烘干后的毛坯件，在2350℃进行重结晶烧成2h，冷却后获得成品。
实施例2
所述的一次性重结晶圆环状碳化硅加热盘的制备方法，包括以下步骤：
(1)干混料：将原料97.98％碳化硅、0.02％氮化硼加入搅拌机，搅拌40min，得到干混料；其中碳化硅的颗粒度型号按照质量比的组成为：粗号60wt.％，中号15wt.％，细号25wt.％。
(2)湿混料造粒：将糖、聚乙烯醇按照质量比为：30:70混合，配制成浓度为50wt.％的溶液，即水溶胶，将2.0％加入干混料中，搅拌60min，得到的混合料进行造粒，至粒径为120-200μm。
(3)成型：将造粒放入压机模型，按1:2.8的压缩比进行压制成型，脱模，得到毛坯件。
(4)烘干：将毛坯件在170℃放入干燥箱烘干6h。
(5)烧成：将烘干后的毛坯件，在2250℃进行重结晶烧成3h，冷却后获得成品。
实施例3
所述的一次性重结晶圆环状碳化硅加热盘的制备方法，包括以下步骤：
(1)干混料：将原料95.3％碳化硅、0.20％氮化硼加入搅拌机，搅拌60min，得到干混料；其中碳化硅的颗粒度型号按照质量比的组成为：粗号40wt.％，中号20wt.％，细号40wt.％。
(2)湿混料造粒：将糖、聚乙烯醇按照质量比为：60:40混合，配制成浓度为30wt.％的溶液，即水溶胶，将4.5％加入干混料中，搅拌80min，得到的混合料进行造粒，至粒径为200-300μm。
(3)成型：将造粒放入压机模型，按1:2.5的压缩比进行压制成型，脱模，得到毛坯件。
(4)烘干：将毛坯件在110℃放入干燥箱烘干8h。
(5)烧成：将烘干后的毛坯件，在2550℃进行重结晶烧成1h，冷却后获得成品。
实施例4
所述的一次性重结晶圆环状碳化硅加热盘的制备方法，包括以下步骤：
(1)干混料：将原料96％碳化硅、0.1％氮化硼加入搅拌机，搅拌50min，得到干混料；其中碳化硅的颗粒度型号按照质量比的组成为：粗号65wt.％，中号10wt.％，细号25wt.％。
(2)湿混料造粒：将糖、聚乙烯醇按照质量比为：70:30混合，配制成浓度为40wt.％的溶液，即水溶胶，将3.9％加入干混料中，搅拌70min，得到的混合料进行造粒，至粒径为350-360μm。
(3)成型：将造粒放入压机模型，按1:2.8的压缩比进行压制成型，脱模，得到毛坯件。
(4)烘干：将毛坯件在150℃放入干燥箱烘干7h。
(5)烧成：将烘干后的毛坯件，在2450℃进行重结晶烧成2h，冷却后获得成品。
实施例5
所述的一次性重结晶圆环状碳化硅加热盘的制备方法，包括以下步骤：
(1)干混料：将原料97％碳化硅、0.18％氮化硼加入搅拌机，搅拌60min，得到干混料；其中碳化硅的颗粒度型号按照质量比的组成为：粗号50wt.％，中号20wt.％，细号30wt.％。
(2)湿混料造粒：将糖、聚乙烯醇按照质量比为：40:60混合，配制成浓度为50wt.％的溶液，即水溶胶，将2.82％加入干混料中，搅拌80min，得到的混合料进行造粒，至粒径为50-150μm。
(3)成型：将造粒放入压机模型，按1:2.5的压缩比进行压制成型，脱模，得到毛坯件。
(4)烘干：将毛坯件在120℃放入干燥箱烘干7h。
(5)烧成：将烘干后的毛坯件，在2550℃进行重结晶烧成1h，冷却后获得成品。
对比例1
本对比例与实施例1相同，只是将水溶胶只采用聚乙烯醇，制得一种加热盘成品。
对比例2
本对比例与实施例1相同，只是将步骤(1)的氮化硅去掉，全部采用碳化硅原料，制得一种加热盘成品。
对比例3
本对比例与实施例1相同，只是将碳化硅的颗粒度型号质量比的组成替换为：粗号70wt.％，中号15wt.％，细号15wt.％，制得一种加热盘成品。
对比例4
本对比例与实施例1的加热盘的原料相同，将所有原料共混，其制备方法包括以下步骤：
(1)混料、造粒：将原料96％碳化硅、0.15％氮化硼、3.85％水溶胶(糖、聚乙烯醇按照质量比为：50:50混合)加入搅拌机，搅拌70min，得到混合料，得到的混合料进行造粒，至粒径为60μm；其中碳化硅的颗粒度型号按照质量比的组成为：粗号50wt.％，中号15wt.％，细号35wt.％。
(2)成型：将造粒放入压机模型，按1:2.6的压缩比进行压制成型，脱模，得到毛坯件。
(3)烘干：将毛坯件在150℃放入干燥箱烘干7h。
(4)烧成：将烘干后的毛坯件，在2350℃进行重结晶烧成2h，冷却后获得成品。
对比例5
采用正常市售的产品金属加热盘，其标注性能参数为电阻率：1.42Ωmm2m-1，微观结构：铁素体，耐温：1350℃。
将以上实施例1至实施例5与对比例1至对比例4制备的碳化硅加热盘成品，在不同使用温度下，对其性能进行检测，检测结果如表1所示。
表1测试条件与测试结果
当然，上述内容仅为本发明的较佳实施例，不能被认为用于限定对本发明的实施例范围。本发明也并不仅限于上述举例，本技术领域的普通技术人员在本发明的实质范围内所做出的均等变化与改进等，均应归属于本发明的专利涵盖范围内。
Claims (1)
1.一种一次性重结晶圆环状碳化硅加热盘的制备方法，其特征在于：包括以下步骤：
(1)干混料：将原料碳化硅、氮化硼加入搅拌机，搅拌40-60min，得到干混料；
(2)湿混料造粒：将糖、聚乙烯醇混合制成浓度为30wt.％-50wt.％的水溶胶，加入干混料中，搅拌60-80min，得到的混合料进行造粒，至粒径为50-350μm；
(3)成型：将造粒放入压机模型，按1:(2.5-2.8)的压缩比进行压制成型，脱模，得到毛坯件；
(4)烘干：将毛坯件放入干燥箱110-170℃烘干6-8h；
(5)烧成：将烘干后的毛坯件，进行重结晶烧成，烧成温度2250-2550℃，烧成时间为1-3h，冷却后获得成品；
一次性重结晶圆环状碳化硅加热盘是由以下原料按照质量百分比制成的：
碳化硅：95.3-97.98％；
氮化硼：0.02-0.20％；
水溶胶：2.0-4.5％；
所述的水溶胶为糖和聚乙烯醇的混合物，质量比为：(30-70):(70-30)；
碳化硅的颗粒度型号按照质量比的组成为：粗号40-65wt.％，中号10-20wt.％，细号25-40wt.％；其中粗号为100-300μm，中号为20-50μm，细号为0.5-5μm；
碳化硅为高温绿碳化硅，纯度为99.0wt.％以上；
氮化硼的粒度＜2.5μm，纯度≥98.5wt.％。
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