CN109516820A - 一种氧化锆表面粉末冶金钨涂层保温砖的制备方法 - Google Patents

一种氧化锆表面粉末冶金钨涂层保温砖的制备方法 Download PDF

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CN109516820A
CN109516820A CN201910063081.2A CN201910063081A CN109516820A CN 109516820 A CN109516820 A CN 109516820A CN 201910063081 A CN201910063081 A CN 201910063081A CN 109516820 A CN109516820 A CN 109516820A
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代晓波
解宏伟
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Dushan Zhongke Crystal Element Information Material Co Ltd
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Abstract

本发明公开了一种氧化锆表面粉末冶金钨涂层保温砖的制备方法。按下述步骤制备：a.将氧化锆粉与氧化钇粉混匀，得A品；b.另取氧化锆粉、氧化钇和粉钨粉混匀，得B品；c.将A品与PVA粘结剂混匀，得C品；d.将B品与PVA粘结剂混匀，得D品；e.将C品倒入模具进行预压，得E品；f.在E品上均匀平铺D品并预压，使D品在E品上形成中间过渡层；g.另取钨粉PVA与粘结剂混匀，得F品；h.将F品平铺到中间过渡层的表面，形成钨层，得G品；i.将装有G品的模具静压，制得砖坯；j.将砖坯自然干燥，得H品；k.将H品放入烧结炉中烧结，取出冷却，即得氧化锆砖。本发明具有抗热震性能好和保温性能好的特点。

Description

一种氧化锆表面粉末冶金钨涂层保温砖的制备方法
技术领域
本发明涉及晶体生长炉保温材料领域，特别是一种氧化锆表面粉末冶金钨涂层保温砖的制备方法。
技术背景
二氧化锆(化学式：ZrO2)是锆的主要氧化物，通常状况下为白色无臭无味晶体，难溶于水、盐酸和稀硫酸。一般常含有少量的二氧化铪。化学性质不活泼，且具有高熔点、高电阻率、高折射率和低热膨胀系数的性质，使它成为重要的耐高温材料、陶瓷绝缘材料和陶瓷遮光剂，亦是人工钻的主要原料。
由于氧化锆的耐高温性能，良好的保温性能，目前在晶体生长领域，多采用氧化锆做温场保温层，来实现晶体的定向生长。但在晶体生长的设备内，尤其是高熔点的晶体生长炉，其温场温度梯度大及温度变化快，容易导致由氧化锆制作的保温砖容易发生断裂(即抗热震性能差)。断裂后将导致温场的均匀性能变差，影响产品质量。因此，如何提高氧化锆的高温抗热震性能成为急需解决的技术难题。研究人员对此做了很多研究工作，其中向陶瓷中添加金属颗粒制备金属陶瓷是一个很好的解决方法。但是，添加金属颗粒后，将整体改变保温层的热导系数，氧化锆砖的保温性能变差。
发明内容：
本发明的目的在于，提供一种氧化锆表面粉末冶金钨涂层保温砖的制备方法。本发明具有抗热震性能好和保温性能好的特点。
为解决上述技术问题，本发明采用以下技术方案实现。一种氧化锆表面粉末冶金钨涂层保温砖的制备方法，按下述步骤制备：
a.将氧化锆粉与氧化钇粉按重量比5.6:1混匀，得A品；
b.另取氧化锆粉、氧化钇和粉钨粉按重量比6～7∶1～2∶2～3混匀，得B品；
c.将A品与PVA粘结剂按重量比20～30∶1～0.5混匀，得C品；
d.将B品与PVA粘结剂按重量比20～30∶1～0.5混匀，得D品；
e.将C品倒入模具进行预压，得E品；
f.在E品上均匀平铺D品并预压，使D品在E品上形成中间过渡层；
g.另取钨粉PVA与粘结剂按重量比20～30∶1～0.5混匀，得F品；
h.将F品平铺到中间过渡层的表面，形成钨层，得G品；
i.将装有G品的模具静压，制得砖坯；
j.将砖坯自然干燥，得H品；
k.将H品放入烧结炉中烧结，取出冷却，即得氧化锆砖。
具体地，前述的氧化锆表面粉末冶金钨涂层保温砖的制备方法中，所述氧化锆粉的粒度为1～2mm，氧化钇粉的粒度为800～1000目，钨粉的粒度为200～400目。
具体地，前述的氧化锆表面粉末冶金钨涂层保温砖的制备方法中，所述的步骤e中预压的压力为5～10Mpa，预压时间为3～5min。
具体地，前述的氧化锆表面粉末冶金钨涂层保温砖的制备方法中，所述的步骤f具体为：在E品上均匀平铺D品，其中E品与D品的厚度比为30:1，并使用5～10Mpa的压力预压3～5min，使D品在E品上形成中间过渡层。
具体地，前述的氧化锆表面粉末冶金钨涂层保温砖的制备方法中，所述的步骤h中，钨层的厚度为10mm。
6.根据权利要求1或2所述的氧化锆表面粉末冶金钨涂层保温砖的制备方法，其特征在于，所述的步骤i具体为：将装有G品的模具在60～100Mpa的压力下静压5～10min，制得砖坯。
具体地，前述的氧化锆表面粉末冶金钨涂层保温砖的制备方法中，所述的步骤j中，自然干燥的时间为24～48h。
具体地，前述的氧化锆表面粉末冶金钨涂层保温砖的制备方法中，所述的步骤k具体为，将H品放入烧结炉中，以50～100℃/h的升温速率升到1500℃，保温5～10h后进行降温，降温速率为50～100℃/h，降到室温，取出即得氧化锆砖。
有益效果
与现有技术相比，本发明在氧化锆砖表面形成一层粉末冶金钨涂层，有效提高了氧化锆砖的抗热震性能，使得氧化锆砖能更好地适应温场温度梯度大及温度变化快的使用环境。由于本发明的氧化锆砖其震性能优良，有效防止氧化锆在温场温度梯度大及温度变化快的使用环境中出现断裂，因而有效提高了晶体生长时，晶体生长炉的保温效果，降低了晶体生长炉的能耗，提升了晶体生长的成品率，同时也延长了晶体生长炉的使用寿命。
使用本发明制备的氧化锆砖，能够将晶体生长炉的使用温度提升至1800℃以上，且在使用中，温度梯度在1000℃～1800℃时，氧化锆砖未出现断裂情况，大大提高了晶体生长成品率，降低生产成本。
本发明采用原料中，氧化锆粉的粒度为1～2mm，氧化钇粉的粒度为800～1000目，钨粉的粒度为200～400目。通过上述粒度的原料制得的氧化锆砖，其致密度更均匀，进一步确保了氧化锆砖的保温性能。
本发明涂覆钨层前，先在砖基体(E品)上涂覆一层由氧化锆粉、氧化钇和粉钨粉制成的中间过渡层，再将钨层涂覆在中间过渡层上，通过该方法，能够更好地使得砖基体与钨层结合更牢固，有效防止了钨层的脱落，进一步提高了保温效果，也进一步防止了氧化锆砖的断裂。
本发明中将自然干燥后的砖坯放入烧结炉中，以50～100℃/h的升温速率升到1500℃，保温5～10h后进行降温，降温速率为50～100℃/h，降到室温；通过该方法，能够有效防止升温过快导致的砖体断裂，又能避免升温慢导致的高能耗，进而在确保砖体烧结质量的前提下，降低了能耗，即降低了制作成本。
具体实施方式
实施例1：
一种氧化锆表面粉末冶金钨涂层保温砖的制备方法，按下述步骤制备：
a.将氧化锆粉与氧化钇粉按重量比5.6:1混匀，得A品；
b.另取氧化锆粉、氧化钇和粉钨粉按重量比6～7∶1～2∶2～3混匀，得B品；
c.将A品与PVA粘结剂按重量比20～30∶1～0.5混匀，得C品；
d.将B品与PVA粘结剂按重量比20～30∶1～0.5混匀，得D品；
e.将C品倒入模具进行预压，得E品；
f.在E品上均匀平铺D品并预压，使D品在E品上形成中间过渡层；
g.另取钨粉PVA与粘结剂按重量比20～30∶1～0.5混匀，得F品；
h.将F品平铺到中间过渡层的表面，形成钨层，得G品；
i.将装有G品的模具静压，制得砖坯；
j.将砖坯自然干燥，得H品；
k.将H品放入烧结炉中烧结，取出冷却，即得氧化锆砖。
具体地，前述氧化锆粉的粒度为1～2mm，氧化钇粉的粒度为800～1000目，钨粉的粒度为200～400目。
具体地，前述的步骤e中预压的压力为5～10Mpa，预压时间为3～5min。经过反复试验，该压力及时间可以保证密度达到使用要求，也可以保证砖的涂层厚度和保温性能。
具体地，前述的步骤f具体为：在E品上均匀平铺D品，其中E品与D品的厚度比为30:1，并使用5～10Mpa的压力预压3～5min，使D品在E品上形成中间过渡层。30:1的厚度比，可以保证砖有良好的不开裂性能，也可以保证涂层的均匀性，且通过该条件下的预压使得中间过渡层的均匀性更好。
具体地，前述的步骤h中，钨层的厚度为10mm。该厚度的钨层，在确保涂层的均匀性能的同时，能够降低成本。
具体地，前述的步骤i具体为：将装有G品的模具在60～100Mpa的压力下静压5～10min，制得砖坯。
具体地，前述的步骤j中，自然干燥的时间为24～48h。
具体地，前述的步骤k具体为，将H品放入烧结炉中，以50～100℃/h的升温速率升到1500℃，保温5～10h后进行降温，降温速率为50～100℃/h，降到室温，取出即得氧化锆砖。

Claims (8)

1.一种氧化锆表面粉末冶金钨涂层保温砖的制备方法，其特征在于，按下述步骤制备：
a.将氧化锆粉与氧化钇粉按重量比5.6:1混匀，得A品；
b.另取氧化锆粉、氧化钇和粉钨粉按重量比6～7∶1～2∶2～3混匀，得B品；
c.将A品与PVA粘结剂按重量比20～30∶1～0.5混匀，得C品；
d.将B品与PVA粘结剂按重量比20～30∶1～0.5混匀，得D品；
e.将C品倒入模具进行预压，得E品；
f.在E品上均匀平铺D品并预压，使D品在E品上形成中间过渡层；
g.另取钨粉PVA与粘结剂按重量比20～30∶1～0.5混匀，得F品；
h.将F品平铺到中间过渡层的表面，形成钨层，得G品；
i.将装有G品的模具静压，制得砖坯；
j.将砖坯自然干燥，得H品；
k.将H品放入烧结炉中烧结，取出冷却，即得氧化锆砖。
2.根据权利要求1所述的氧化锆表面粉末冶金钨涂层保温砖的制备方法，其特征在于，所述氧化锆粉的粒度为1～2mm，氧化钇粉的粒度为800～1000目，钨粉的粒度为200～400目。
3.根据权利要求1或2所述的氧化锆表面粉末冶金钨涂层保温砖的制备方法，其特征在于，所述的步骤e中预压的压力为5～10Mpa，预压时间为3～5min。
4.根据权利要求1或2所述的氧化锆表面粉末冶金钨涂层保温砖的制备方法，其特征在于，所述的步骤f具体为：在E品上均匀平铺D品，其中E品与D品的厚度比为30:1，并使用5～10Mpa的压力预压3～5min，使D品在E品上形成中间过渡层。
5.根据权利要求1或2所述的氧化锆表面粉末冶金钨涂层保温砖的制备方法，其特征在于，所述的步骤h中，钨层的厚度为10mm。
6.根据权利要求1或2所述的氧化锆表面粉末冶金钨涂层保温砖的制备方法，其特征在于，所述的步骤i具体为：将装有G品的模具在60～100Mpa的压力下静压5～10min，制得砖坯。
7.根据权利要求1或2所述的氧化锆表面粉末冶金钨涂层保温砖的制备方法，其特征在于，所述的步骤j中，自然干燥的时间为24～48h。
8.根据权利要求1或2所述的氧化锆表面粉末冶金钨涂层保温砖的制备方法，其特征在于，所述的步骤k具体为，将H品放入烧结炉中，以50～100℃/h的升温速率升到1500℃，保温5～10h后进行降温，降温速率为50～100℃/h，降到室温，取出即得氧化锆砖。
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