JP2007316001A - TiCl4中の金属不純物の分析方法及び高純度チタンの製造方法 - Google Patents
TiCl4中の金属不純物の分析方法及び高純度チタンの製造方法 Download PDFInfo
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- JP2007316001A JP2007316001A JP2006148015A JP2006148015A JP2007316001A JP 2007316001 A JP2007316001 A JP 2007316001A JP 2006148015 A JP2006148015 A JP 2006148015A JP 2006148015 A JP2006148015 A JP 2006148015A JP 2007316001 A JP2007316001 A JP 2007316001A
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- 239000010936 titanium Substances 0.000 title claims abstract description 118
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 76
- 239000012535 impurity Substances 0.000 title claims abstract description 67
- 238000004458 analytical method Methods 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title claims description 66
- 229910003074 TiCl4 Inorganic materials 0.000 title 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 title 1
- 238000000034 method Methods 0.000 claims abstract description 71
- 229910052751 metal Inorganic materials 0.000 claims abstract description 62
- 239000002184 metal Substances 0.000 claims abstract description 62
- 238000005259 measurement Methods 0.000 claims abstract description 34
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000460 chlorine Substances 0.000 claims abstract description 25
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001704 evaporation Methods 0.000 claims abstract description 17
- 238000005349 anion exchange Methods 0.000 claims abstract description 15
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 9
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 claims abstract 3
- 238000000926 separation method Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 238000011946 reduction process Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 11
- 230000008020 evaporation Effects 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract 1
- 235000011149 sulphuric acid Nutrition 0.000 abstract 1
- 239000001117 sulphuric acid Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 14
- 239000000523 sample Substances 0.000 description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000003957 anion exchange resin Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 239000012488 sample solution Substances 0.000 description 7
- 238000005342 ion exchange Methods 0.000 description 6
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- 150000002500 ions Chemical class 0.000 description 4
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- 229920005989 resin Polymers 0.000 description 4
- 238000004611 spectroscopical analysis Methods 0.000 description 4
- 229910052720 vanadium Inorganic materials 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000004886 process control Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000012086 standard solution Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- MGSRCZKZVOBKFT-UHFFFAOYSA-N thymol Chemical compound CC(C)C1=CC=C(C)C=C1O MGSRCZKZVOBKFT-UHFFFAOYSA-N 0.000 description 2
- 210000002268 wool Anatomy 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000005844 Thymol Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920001467 poly(styrenesulfonates) Polymers 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229960000790 thymol Drugs 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
【解決手段】(1)TiCl4中の金属不純物の濃度をICP−MSで測定する。前記の測定を、TiCl4を硫酸と反応させ、続いて蒸発乾固させることにより塩素分を除去し、更に、フッ化水素酸溶液を加え、陰イオン交換カラムを通してTi分を除去した後に行えば、不純物としてのVの濃度を、定量下限が0.015ppmという高い精度で測定することができる。
(2)TiCl4をサンプリングし、(1)の方法でTiCl4中の金属不純物(特に、V)濃度を測定し、その測定結果を製造工程へフィードバックして製品中の金属不純物が所定濃度以下となるように製造工程を制御する。高純度のチタンを安定して製造することができる。
【選択図】図7
Description
2:陰イオン交換樹脂
3:テフロン(登録商標)ウール
Claims (7)
- TiCl4中の金属不純物の濃度をICP−MSで測定することを特徴とするTiCl4中の金属不純物の分析方法。
- 前記金属不純物がVであり、このVの濃度を、前記TiCl4を硫酸と反応させ、続いて蒸発乾固させることにより塩素分を除去した後、測定することを特徴とする請求項1に記載のTiCl4中の金属不純物の分析方法。
- 前記V濃度の測定を、蒸発乾固させた後にフッ化水素酸溶液を加え、陰イオン交換カラムを通してTi分を除去した後に行うことを特徴とする請求項2に記載のTiCl4中の金属不純物の分析方法。
- クロール法による高純度チタンの製造方法であって、蒸留工程で精製された高純度TiCl4の一部をサンプリングして、当該TiCl4中の金属不純物濃度をICP−MSで測定し、その測定結果を製造工程へフィードバックして製品中の金属不純物が所定濃度以下となるように製造工程を制御することを特徴とする高純度チタンの製造方法。
- 前記金属不純物がVであり、このVの濃度を、前記TiCl4を硫酸と反応させ、続いて蒸発乾固させることにより塩素分を除去した後、測定することを特徴とする請求項4に記載の高純度チタンの製造方法。
- 前記V濃度の測定を、蒸発乾固させた後にフッ化水素酸溶液を加え、陰イオン交換カラムを通してTi分を除去した後に行うことを特徴とする請求項5に記載の高純度チタンの製造方法。
- 前記一部をサンプリングした高純度TiCl4をクロール法の還元工程で用いてスポンジチタンを生成させ、その後に真空分離工程、冷却工程を経て反応容器から取り出すよりも前に、サンプリングした高純度TiCl4中のV濃度を測定することを特徴とする請求項6に記載の高純度チタンの製造方法。
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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KR100977991B1 (ko) | 2009-12-17 | 2010-08-25 | 테크노세미켐 주식회사 | 염화티타늄의 분석 방법 |
CN104677883A (zh) * | 2015-02-02 | 2015-06-03 | 海南中航特玻科技有限公司 | 一种测定锡样中杂质含量的分析方法 |
Families Citing this family (1)
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CN108267498A (zh) * | 2017-12-28 | 2018-07-10 | 中核北方核燃料元件有限公司 | 一种铀钆锆合金中硼铝杂质元素含量的测定方法 |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH07207591A (ja) * | 1994-01-17 | 1995-08-08 | Babcock Hitachi Kk | 塩化物を含む物質から塩素を除去する方法 |
JPH11322343A (ja) * | 1998-05-21 | 1999-11-24 | Toshin Kagaku Kogyo Kk | 塩化鉄の硫酸塩転換と塩基性硫酸第二鉄製造の方法 |
JP2002187718A (ja) * | 2000-12-20 | 2002-07-05 | Sumitomo Titanium Corp | TiCl4の精製方法 |
JP2003057225A (ja) * | 2001-08-21 | 2003-02-26 | Kurita Water Ind Ltd | バナジウムの分析方法、分析装置および分析キット |
JP2003293050A (ja) * | 2002-04-04 | 2003-10-15 | Sumitomo Metal Ind Ltd | チタンのフッ化物イオンを含む水溶液中の不純物金属イオンの除去方法 |
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH07207591A (ja) * | 1994-01-17 | 1995-08-08 | Babcock Hitachi Kk | 塩化物を含む物質から塩素を除去する方法 |
JPH11322343A (ja) * | 1998-05-21 | 1999-11-24 | Toshin Kagaku Kogyo Kk | 塩化鉄の硫酸塩転換と塩基性硫酸第二鉄製造の方法 |
JP2002187718A (ja) * | 2000-12-20 | 2002-07-05 | Sumitomo Titanium Corp | TiCl4の精製方法 |
JP2003057225A (ja) * | 2001-08-21 | 2003-02-26 | Kurita Water Ind Ltd | バナジウムの分析方法、分析装置および分析キット |
JP2003293050A (ja) * | 2002-04-04 | 2003-10-15 | Sumitomo Metal Ind Ltd | チタンのフッ化物イオンを含む水溶液中の不純物金属イオンの除去方法 |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR100977991B1 (ko) | 2009-12-17 | 2010-08-25 | 테크노세미켐 주식회사 | 염화티타늄의 분석 방법 |
CN104677883A (zh) * | 2015-02-02 | 2015-06-03 | 海南中航特玻科技有限公司 | 一种测定锡样中杂质含量的分析方法 |
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