CN1059182C - 高频低损耗微晶玻璃材料的制造方法 - Google Patents
高频低损耗微晶玻璃材料的制造方法 Download PDFInfo
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- CN1059182C CN1059182C CN96116647A CN96116647A CN1059182C CN 1059182 C CN1059182 C CN 1059182C CN 96116647 A CN96116647 A CN 96116647A CN 96116647 A CN96116647 A CN 96116647A CN 1059182 C CN1059182 C CN 1059182C
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- 239000011521 glass Substances 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 239000000463 material Substances 0.000 title claims description 5
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 13
- 238000002425 crystallisation Methods 0.000 claims abstract description 13
- 230000008025 crystallization Effects 0.000 claims abstract description 13
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000002241 glass-ceramic Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000002844 melting Methods 0.000 claims abstract description 3
- 230000008018 melting Effects 0.000 claims abstract description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 11
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 5
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 4
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 4
- 239000004408 titanium dioxide Substances 0.000 claims description 4
- JRIGVWDKYXCHMG-UHFFFAOYSA-N (5-arsoroso-2-hydroxyphenyl)azanium;chloride Chemical compound Cl.NC1=CC([As]=O)=CC=C1O JRIGVWDKYXCHMG-UHFFFAOYSA-N 0.000 claims description 3
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 3
- 239000006004 Quartz sand Substances 0.000 claims description 3
- 229910000413 arsenic oxide Inorganic materials 0.000 claims description 3
- 229960002594 arsenic trioxide Drugs 0.000 claims description 3
- KTTMEOWBIWLMSE-UHFFFAOYSA-N diarsenic trioxide Chemical compound O1[As](O2)O[As]3O[As]1O[As]2O3 KTTMEOWBIWLMSE-UHFFFAOYSA-N 0.000 claims description 3
- 229950008475 oxophenarsine Drugs 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 239000003989 dielectric material Substances 0.000 abstract description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003317 industrial substance Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 229910001051 Magnalium Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000006066 glass batch Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0036—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents
- C03C10/0045—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents containing SiO2, Al2O3 and MgO as main constituents
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
一种高频低损耗微晶玻璃介质材料的制造方法，属于微晶玻璃领域，本发明提供的系统为SiO2-Al2O3-MgO-TiO2系统。具体组成范围(wt%)为SiO236-47，Al2O318.28，MgO15.27，TiO215.20。玻璃熔制温度为1460-1510℃保温3小时，第一阶段晶化温度为730℃±10℃，第二阶段为1250℃±10℃。所得微晶玻璃介电常数介于7.0～7.5，介电损耗＞2X10-4，是一类较理想的高频低损耗微晶玻璃介质材料。
Description
本发明是关于高频低损耗微晶玻璃材料的制造方法，更确切地说涉及一种高强度耐候性好的微波介质材料的制造方法。属于微晶玻璃领域。
众所周知，微晶玻璃又称玻璃陶瓷，是一种性能优良的材料，在工业、国防、军工许多领域中有广泛的应用。其中MgO-Al2O3-SiO2-TiO2系统是一种性能优良的微波介质材料。据美国专利USP 4304603和USP 5013605A报导SiO2含量48～53％，Al2O3 21-25％ MgO 15-18，TiO2 9.5-11.5％，其介电常数为5.0-6.0。如何使MgO-Al2O3-SiO2-TiO2系统的介电常数进一步提高到7.2-7.5，而介电损耗tgδ＜2×10-4，成为许多科技工作者长期追求的目标之一。
本发明的目的在于使掺杂TiO2的MgO-Al2O3-SiO2的微晶玻璃系统的TiO2含量从文献报导的8.9-11.5％提高到15-20％，使制成的堇青石微晶玻璃具有高频低损耗的特点，使介电常数ε从6提高到7。由于TiO2含量的提高，导致玻璃的析透现象，因此需相应改变SiO2含量，采用高温熔制的快冷措施获得透明玻璃。
表1为本发明提供的高频低损耗微晶玻璃介质材料的组分与美国专利的对比。
表1 本发明与相应文献组分比较(wt％)
| 类别USP 4304603USP 5013605A本发明 | SiO2 Al2O3 MgO TiO248-53 21-25 15-18 9.5-11.556.1 19.7 14.9 8.936-47 18-28 15-27 15-20 |
从表1可知，本发明的组成范围与相应的专利文献报导不同，尤其是TiO2含量提高，使工艺难度增加，SiO2含量的降低，快冷措施的实施，不至于产生析透现象。
本发明主要采用国产化工原料(氧化镁、氢氧化铝、钛白粉)以及石英砂，按表1所示成份，采用熔制后在浇铸模具中快速冷却方法成型，冷加工后再晶化处理，即可获得介电常数为7.0-7.5系统的微波介质材料。
具体地说，以氧化镁、氢氧化铝、钛白粉以及石英砂等化工原料作为玻璃配合料，加入1wt％氧化砷和1wt％硝酸铵作为澄清剂，玻璃熔制温度为1460-1510℃保温3小时，晶化分二阶段进行，第一阶段晶化温度为730±10℃，第二阶段为1250℃±10℃保温时间分别为1小时和5小时，其他工艺条件与一般玻璃制作工艺相同。
本发明的特点是使用原料来源是丰富而廉价的化工原料，只需控制含铁量低于0.05wt％，碱金属含量＜0.5wt％氧化钙含量1％即可。
特点之二是配料，混合，溶制，晶化工艺条件要求简单，采用常规微晶玻璃工艺。
特点之三是制得微晶玻璃含有镁铝钛相和堇青石相，主要性能如表2所示。
表2本发明提供的微晶玻璃性能
| 性 能 | 单位 | |
| 密度 | g/cm3 | 3.00 |
| 耐碱性(5％NaOH，6h) | kg/g | 0.36 |
| 吸水率 | ％ | 0 |
| 抗折强度 | MPa | 100 |
| 膨胀系数(25-500℃) | 10-7/℃ | 52 |
| 硬度HV | kg/mm2 | 1000 |
| 介电常数 | 7.2±0.2 | |
| 介电损耗 | ＜2×10-4 |
实施例1
玻璃组成(wt％)为 SiO2 47 MgO 15
Al2O318 TiO2 20
澄清剂加人量为1wt％硝酸铵和1wt％氧化砷以石英砂、氧化镁、氢氧化铝和钛白粉为原料按上述组分称量、混合然后在1510℃溶融保温3小时，熔制后浇铸在模具中快速冷却成为棕色透明的玻璃，然后经740℃保温1小时再升温至1250℃保温5小时，冷却至室温即成高频低损耗微晶玻璃介质材料其性能如表2所示。介电常数ε＝7.5，介电损耗＜2×10-4。实施例2、3
微晶玻璃组成和性能如表3所示，熔融保温温度分别为1460℃和1480℃，保温3小时，晶化时第一阶段温度分别为730℃和750℃，第二阶段为1240℃其余条件同实施例1。
表3 实施例2、3组成(wt％)和性能
实施例 SiO2 Al2O3 MgO TiO2 介电常数 介电损耗
2 42 21 19 18 7.2 ＜1.5×10-4
3 36 28 27 15 7.0 ＜1.5×10-4
Claims (3)
1、一种高频低损耗微晶玻璃材料的制造方法，属于掺杂TiO2的MgO-Al2O3-SiO2系统，其特征在于
(1)各组分的重量百分含量是：
SiO2 36-47
Al2O3 18-28
MgO 15-27
TiO2 15-20
(2)TiO2含量的提高造成的玻璃析透现象通过改变SiO2含量，采用熔制后浇铸在模具中快速冷却方法，予以避免；
(3)加入1wt％硝酸铵和1wt％氧化砷为澄清剂；
(4)熔制温度为1460-1510℃保温3小时；
(5)二阶段晶化，第一阶段晶化温度为730℃±10℃，保温1小时；
第二阶段晶化温度为1250℃±10℃，保温5小时；
(6)以国间氧化镁、氢氧化铝、钛白粉及石英砂为主要原料。
2、按权利要求1所述的微晶玻璃制造方法，其特征在于
(1)玻璃组成(wt％)为：SiO2 47，MgO 15，Al2O3 18，TiO2 20；
(2)熔融温度为1510℃，保温3小时；
(3)第一阶段晶化温度为740℃，保温1小时；
第二阶段晶化温度为1250℃，保温5小时；
3、按权利要求1所述的制造方法，其特征在于
(1)玻璃的组成范围为(1wt％)：SiO2 42，MgO 19，Al2O3 21，TiO2 18；
(3)第一阶段晶化温度为730℃，保温1小时；
第二阶段晶化温度为1240℃，保温5小时。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96116647A CN1059182C (zh) | 1996-12-30 | 1996-12-30 | 高频低损耗微晶玻璃材料的制造方法 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96116647A CN1059182C (zh) | 1996-12-30 | 1996-12-30 | 高频低损耗微晶玻璃材料的制造方法 |
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| Publication Number | Publication Date |
|---|---|
| CN1186781A CN1186781A (zh) | 1998-07-08 |
| CN1059182C true CN1059182C (zh) | 2000-12-06 |
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| CN96116647A Expired - Fee Related CN1059182C (zh) | 1996-12-30 | 1996-12-30 | 高频低损耗微晶玻璃材料的制造方法 |
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| KR20210035828A (ko) | 2018-07-23 | 2021-04-01 | 코닝 인코포레이티드 | 마그네슘 알루미노실리케이트 유리 세라믹 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4304603A (en) * | 1980-08-11 | 1981-12-08 | Corning Glass Works | Glass-ceramic compositions designed for radomes |
| EP0742019A1 (en) * | 1994-11-30 | 1996-11-13 | TDK Corporation | Glass material, substitution material of living tissue and teeth-straightening material |
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1996
- 1996-12-30 CN CN96116647A patent/CN1059182C/zh not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4304603A (en) * | 1980-08-11 | 1981-12-08 | Corning Glass Works | Glass-ceramic compositions designed for radomes |
| EP0742019A1 (en) * | 1994-11-30 | 1996-11-13 | TDK Corporation | Glass material, substitution material of living tissue and teeth-straightening material |
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| Publication number | Publication date |
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| CN1186781A (zh) | 1998-07-08 |
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