CN110655399B - 一种钢水定氢探头用透气陶瓷头及其制备方法 - Google Patents
一种钢水定氢探头用透气陶瓷头及其制备方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 38
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 21
- 239000010959 steel Substances 0.000 title claims abstract description 21
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- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 19
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 18
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000005245 sintering Methods 0.000 claims abstract description 23
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 12
- 229910052593 corundum Inorganic materials 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 12
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 8
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 6
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- 239000001095 magnesium carbonate Substances 0.000 claims description 2
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- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 2
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- 239000011777 magnesium Substances 0.000 claims 1
- -1 magnesium aluminate Chemical class 0.000 claims 1
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Abstract
一种钢水定氢探头用透气陶瓷头的制备方法，其特征在于，包括步骤：a)将镁稳定氧化锆粉体、镁铝尖晶石粉体及石墨粉以一定比例混合后，再加入总质量适量的粘结剂，经混匀、造粒后，经双面模压成型，得透气陶瓷头生坯；b)将透气陶瓷头生坯于90～120℃下进行干燥，再缓慢升温至500～700℃下进行排胶，然后缓慢升温至1500～1600℃后烧结1～2小时，再快速降温至800℃后自然冷却至室温，得透气陶瓷头成品。由本方法制得的钢水定氢探头用透气陶瓷头，其烧结后能够形成大量开口气孔，其气孔中位径为250μm左右，开气孔率可达30％，表观密度1.6g/cm3。其能够在良好透气的基础上不透钢水；其在保持良好透气性的基础上，还能够在正常测量状态下坚持70秒以上。
Description
技术领域
本发明涉及材料制备技术领域，具体涉及一种钢水定氢探头用透气陶瓷头及其制备方法。
背景技术
钢铁中的氢含量是钢的重要性能指标，在线实时测量钢水中的氢含量成为提高过程控制精度的重要手段。目前，市场上普遍使用的是在线氢分析仪，其采用为Hydris定氢系统。Hydris定氢系统通过测量载气(氮气)中所带出的氢的含量，然后根据西华特计算钢水中的氢分压。其中，携带氢的氮气需要通过定氢探头上的透气陶瓷头进行集气。由于系统平衡需要一定时间，时间越长，系统状态越接近平衡态，测量数据越接近真实数据。
由于其使用环境较为恶劣，测量环境通常在1600℃左右，并且在实际使用过程中，透气陶瓷头的透气孔会逐渐被钢水堵住。现有的定氢探头在使用时，透气陶瓷头仅能在钢水中坚持30～70秒。
发明内容
本要解决的技术问题是，提供一种钢水定氢探头用透气陶瓷头的制备方法，使其制备的透气陶瓷头能够在测量状态下坚持更长时间。
本解决技术问题采用的技术方案是：
一种钢水定氢探头用透气陶瓷头的制备方法，包括步骤：a)将镁稳定氧化锆粉体、镁铝尖晶石粉体及石墨粉以一定比例混合后，再加入总质量适量的粘结剂，经混匀、造粒后，经双面模压成型，得透气陶瓷头生坯；b)将透气陶瓷头生坯于90～120℃下进行干燥，再缓慢升温至500～700℃下进行排胶，然后缓慢升温至1500～1600℃后烧结1～2小时，再快速降温至800℃后自然冷却至室温，得透气陶瓷头成品。
优选地，所述镁稳定氧化锆粉体由在基粉中添加0.1～5％质量比例的烧结促进剂后经混匀、过筛制得；
其中，所述基粉由摩尔百分比为80％～99％：0.1％～10％：0.1％～5％：0.1％～5％的ZrO2、MgO、Y2O3、CaO混合得到；所述烧结促进剂由摩尔百分比10％～40％，30％～60％：20％～50％：0.5％～20％的Al2O3、SiO2、TiO2、Fe2O3混合得到。
优选地，所述镁铝尖晶石粉体由MgCO3、Al2O3以摩尔比1：0.85～1.15混合，并经1000～1200℃预烧1.5～3小时后粉磨、过筛制得。
优选地，所述镁稳定氧化锆粉体、所述镁铝尖晶石粉体及所述石墨粉的混合比例为质量百分比10％～30％：60％～75％：5％～20％。
优选地，所述粘结剂为PVA，其加入量为所述镁稳定氧化锆粉体、所述镁铝尖晶石粉体及所述石墨粉的总质量的0.2％～0.6％。
优选地，透气陶瓷头生坯在干燥后，其含水率控制为3％～5％。
优选地，双面模压成型时的压力控制为35MPa～70MPa。
本发明还要求保护由上述制备方法所制得的钢水定氢探头用透气陶瓷头。
本发明具有以下优点：由本方法制得的钢水定氢探头用透气陶瓷头，其烧结后能够形成大量开口气孔，其气孔中位径为250μm左右，开气孔率可达30％，表观密度1.6g/cm3。其能够在良好透气的基础上不透钢水；其在保持良好透气性的基础上，还能够在正常测量状态下坚持70秒以上。
具体实施方式
实施例1：
1、将ZrO2、MgO、Y2O3、CaO以摩尔百分比为80％：10％：5％：5％的比例混合，得基粉；
将Al2O3、SiO2、TiO2、Fe2O3以摩尔百分比19.5％，30％：50％：0.5％的比例混合，得烧结促进剂；
在基粉中添加和占基粉质量3％的烧结促进剂，混匀后过80目筛，得镁稳定氧化锆粉体；
2、将MgCO3、Al2O3以摩尔比1：1.05混合，并经1150℃预烧2小时后，粉磨后过80目筛，得镁铝尖晶石粉体；
3、将上述镁稳定氧化锆粉体、镁铝尖晶石粉体及石墨粉以质量百分比10％：70％：20％混合后，再加入总质量0.3％的粘结剂PVA(聚乙烯醇)，经混匀、造粒后，于60MPa压力下双面模压成型，得透气陶瓷头生坯；
4、将透气陶瓷头生坯于110℃下进行干燥，使之含水率降至3％，再缓慢升温至650℃下排胶64小时，然后缓慢升温至1570℃后烧结1小时，再快速降温至800℃后自然冷却至室温，得透气陶瓷头成品。
实施例2：
1、将ZrO2、MgO、Y2O3、CaO以摩尔百分比为87％：10％：2.9％：0.1％的比例混合，得基粉；
将Al2O3、SiO2、TiO2、Fe2O3以摩尔百分比10％，60％：20％：10％的比例混合，得烧结促进剂；
在基粉中添加和占基粉质量0.1％的烧结促进剂，混匀后过80目筛，得镁稳定氧化锆粉体；
2、将MgCO3、Al2O3以摩尔比1：0.85混合，并经1000℃预烧2.5小时后，粉磨后过80目筛，得镁铝尖晶石粉体；
3、将上述镁稳定氧化锆粉体、镁铝尖晶石粉体及石墨粉以质量百分比20％：75％：5％混合后，再加入总质量0.5％的粘结剂PVA(聚乙烯醇)，经混匀、造粒后，于35MPa压力下双面模压成型，得透气陶瓷头生坯；
4、将透气陶瓷头生坯于90℃下进行干燥，使之含水率降至3.5％，再缓慢升温至500℃下排胶48小时，然后缓慢升温至1500℃后烧结1.4小时，再快速降温至800℃后自然冷却至室温，得透气陶瓷头成品。
实施例3：
1、将ZrO2、MgO、Y2O3、CaO以摩尔百分比为84％：7％：4.5％：16％的比例混合，得基粉；
将Al2O3、SiO2、TiO2、Fe2O3以摩尔百分比16％，36％：28％：20％的比例混合，得烧结促进剂；
在基粉中添加和占基粉质量1.0％的烧结促进剂，混匀后过80目筛，得镁稳定氧化锆粉体；
2、将MgCO3、Al2O3以摩尔比1：0.95混合，并经1100℃预烧1.5小时后，粉磨后过80目筛，得镁铝尖晶石粉体；
3、将上述镁稳定氧化锆粉体、镁铝尖晶石粉体及石墨粉以质量百分比25％：68％：7％混合后，再加入总质量0.2％的粘结剂PVA(聚乙烯醇)，经混匀、造粒后，于45MPa压力下双面模压成型，得透气陶瓷头生坯；
4、将透气陶瓷头生坯于100℃下进行干燥，使之含水率降至4.5％，再缓慢升温至550℃下排胶56小时，然后缓慢升温至1530℃后烧结1.6小时，再快速降温至800℃后自然冷却至室温，得透气陶瓷头成品。
实施例4：
1、将ZrO2、MgO、Y2O3、CaO以摩尔百分比为90％：7.9％：0.1％：2％的比例混合，得基粉；
将Al2O3、SiO2、TiO2、Fe2O3以摩尔百分比40％，33％：22％：5％的比例混合，得烧结促进剂；
在基粉中添加和占基粉质量5％的烧结促进剂，混匀后过80目筛，得镁稳定氧化锆粉体；
2、将MgCO3、Al2O3以摩尔比1：1.15混合，并经1200℃预烧3小时后，粉磨后过80目筛，得镁铝尖晶石粉体；
3、将上述镁稳定氧化锆粉体、镁铝尖晶石粉体及石墨粉以质量百分比30％：60％：10％混合后，再加入总质量0.6％的粘结剂PVA(聚乙烯醇)，经混匀、造粒后，于70MPa压力下双面模压成型，得透气陶瓷头生坯；
4、将透气陶瓷头生坯于120℃下进行干燥，使之含水率降至5％，再缓慢升温至700℃下排胶72小时，然后缓慢升温至1600℃后烧结2小时，再快速降温至800℃后自然冷却至室温，得透气陶瓷头成品。
上述各实施例所得的透气陶瓷头，通过LP07-XQK-04显气孔体密测定仪测量试样的开气孔率、容重，通过压汞仪测量其孔径分布，结果如表1所示：
表1
以上仅是本的优选实施方式，应当指出，对本技术领域的普通技术人员来说，在不脱离本原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本的保护范围。
Claims (2)
1.一种钢水定氢探头用透气陶瓷头的制备方法，其特征在于，包括步骤：
a)将镁稳定氧化锆粉体、镁铝尖晶石粉体及石墨粉以一定比例混合后，再加入总质量适量的粘结剂，经混匀、造粒后，在35MPa～70MPa压力下经双面模压成型，得透气陶瓷头生坯；
b)将透气陶瓷头生坯于90～120℃下干燥至含水率控制为3％～5％，再缓慢升温至500～700℃下进行排胶，然后缓慢升温至1500～1600℃后烧结1～2小时，再快速降温至800℃后自然冷却至室温，得透气陶瓷头成品；
所述粘结剂为PVA，其加入量为所述镁稳定氧化锆粉体、所述镁铝尖晶石粉体及所述石墨粉的总质量的0.2％～0.6％；
其中，所述镁稳定氧化锆粉体由在基粉中添加0.1～5％质量比例的烧结促进剂后经混匀、过筛制得；所述基粉由摩尔百分比为80％～99％：0.1％～10％：0.1％～5％：0.1％～5％的ZrO2、MgO、Y2O3、CaO混合得到；所述烧结促进剂由摩尔百分比10％～40％，30％～60％：20％～50％：0.5％～20％的Al2O3、SiO2、TiO2、Fe2O3混合得到；
所述镁铝尖晶石粉体由MgCO3、Al2O3以摩尔比1：0.85～1.15混合，并经1000～1200℃预烧1.5～3小时后粉磨、过筛制得。
2.一种钢水定氢探头用透气陶瓷头，其特征在于，其由权利要求1中的制备方法制得。
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