JP2005533339A - 誘電膜 - Google Patents
誘電膜 Download PDFInfo
- Publication number
- JP2005533339A JP2005533339A JP2003529515A JP2003529515A JP2005533339A JP 2005533339 A JP2005533339 A JP 2005533339A JP 2003529515 A JP2003529515 A JP 2003529515A JP 2003529515 A JP2003529515 A JP 2003529515A JP 2005533339 A JP2005533339 A JP 2005533339A
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- Prior art keywords
- silicon
- film
- liquid
- capping layer
- dielectric
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 74
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 74
- 239000010703 silicon Substances 0.000 claims abstract description 74
- 239000007788 liquid Substances 0.000 claims abstract description 53
- 239000000758 substrate Substances 0.000 claims abstract description 48
- 230000004888 barrier function Effects 0.000 claims abstract description 19
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 41
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 41
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 39
- 230000005684 electric field Effects 0.000 claims description 31
- 150000002500 ions Chemical class 0.000 claims description 30
- 239000012530 fluid Substances 0.000 claims description 27
- 235000012239 silicon dioxide Nutrition 0.000 claims description 17
- 239000000377 silicon dioxide Substances 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 14
- 150000004767 nitrides Chemical class 0.000 claims description 14
- 239000003989 dielectric material Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 12
- 239000012528 membrane Substances 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 claims description 6
- 229910000314 transition metal oxide Inorganic materials 0.000 claims description 6
- 238000002045 capillary electrochromatography Methods 0.000 claims description 5
- 239000004020 conductor Substances 0.000 claims description 5
- 238000004811 liquid chromatography Methods 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 4
- 238000005251 capillar electrophoresis Methods 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 239000000446 fuel Substances 0.000 claims description 2
- 238000013508 migration Methods 0.000 claims description 2
- 230000005012 migration Effects 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 2
- 238000004587 chromatography analysis Methods 0.000 claims 1
- 239000010408 film Substances 0.000 description 62
- 238000000576 coating method Methods 0.000 description 19
- 239000011248 coating agent Substances 0.000 description 16
- 238000004458 analytical method Methods 0.000 description 13
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 11
- 235000012431 wafers Nutrition 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 10
- 239000002184 metal Substances 0.000 description 10
- 230000015556 catabolic process Effects 0.000 description 9
- 238000000926 separation method Methods 0.000 description 9
- 239000012491 analyte Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 8
- 238000007787 electrohydrodynamic spraying Methods 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- 230000008901 benefit Effects 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 6
- 238000000151 deposition Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 230000010354 integration Effects 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 239000010409 thin film Substances 0.000 description 5
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- 238000004377 microelectronic Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000004593 Epoxy Substances 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000000137 annealing Methods 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 2
- 238000000132 electrospray ionisation Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000005350 fused silica glass Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000005459 micromachining Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- -1 moisture Substances 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000009509 drug development Methods 0.000 description 1
- 238000007876 drug discovery Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000002330 electrospray ionisation mass spectrometry Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000002032 lab-on-a-chip Methods 0.000 description 1
- 238000013178 mathematical model Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000004452 microanalysis Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/447—Systems using electrophoresis
- G01N27/44704—Details; Accessories
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- H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
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Abstract
Description
本発明は、誘電膜および、導電材料上の液体用の被覆・絶縁層(coating and insulation layer)としてのその使用とに関する。特に、本発明は、誘電膜および、電気絶縁を必要とする微量流体装置および電気噴霧装置を含む、装置の被覆・絶縁層としてのその使用とに関する。
「ラボ・オン・チップ(lab-on-a-chip)」または「マイクロ全分析システム」としても知られる小型化微量流体技術の分野は、化学分析の革新および生命科学における有効ツールおよび有効技術の提供の見込みと共に、急速に発展している。生命科学における関心対象の分子および化合物の大部分は液相中にあり、通常、溶液中のこれらの分析物を定量的および定性的に微量分析するのに分析測定が用いられる。しかし、分析中の材料の性質および由来のために、試料の量および体積は伝統的に不十分であり、かつこれらの量は絶えず減少している。さらに、薬物動態学的な用途およびプロテオミクス用途を含む創薬および薬物開発に見られるように、より少ない量および体積の試料しか必要としないより優れた分析測定の必要性が増している。本質的には、マイクロ流体は、試料を小型化し体積を少なくする要件に「合致」している。実際、小型化の主要な理由とは、装置の物理的なサイズを小さくするためというよりもむしろ装置の分析性能を高めるためである。さらに、マイクロ流体を用いて分析を小型化できれば、並行処理を可能にする複数の分離技術を統合することが可能になると共に、いくつかの種類の分析測定(試料操作、噴射、2D分離、反応チャンバなど)を単一の装置に組み込むことが可能になる。本質的には、試薬および廃棄物の処理の削減ならびに装置フットプリントの縮小のような、小型化に伴うその他の利点がある。
本発明の一局面は、ベース層およびキャッピング層を含む誘電体膜に関し、これは、、導電基板と、基板の電位とは異なる電位を有する液体との間に配置されたときに効果的な水分・イオン障壁(mositure and ion barrier)となる。
本発明は、高湿度下および/または直接液体に接触した状態で直接電圧印加および高電界強度に供されたときに、電気特性を維持する誘電膜に関する。
図1のデータは、以下の実験の設定および条件を用いて生成されたものである。半導体洗浄プロトコル(MOS洗浄)を用いてシリコンウェハを洗浄した。低圧化学蒸着炉内でシリコンウェハ上に100nmの低応力窒化物を付着させた。次いで、試料をへき開し、電気試験装置に入れて薄膜の絶縁破壊強度を評価した。導電エポキシを用いてシリコン基板(ウェハのへき開された縁部)と接地された金属段とを適切に電気接触させた。乾性条件下で金属電極、または湿性条件下で流体電極を用いて正(または負)電圧を印加した。電圧を段階的に上昇させ、同時に、膜を通ってシリコン基板に漏れる電流を監視した。曲線を記録した。このデータは図1に見ることができる。このデータから、低応力窒化ケイ素膜の電流−電圧特性は乾性状況(金属電極)と湿性状況(液体電極)とで著しく異なり、液体電気接触実施例の場合の方が絶縁耐力がずっと低いことが分かる。
図2ののデータは、以下の実験の設定および条件を用いて生成されたものである。半導体洗浄プロトコル(MOS洗浄)を用いてシリコンウェハを洗浄した。低圧化学蒸着炉内でシリコンウェハ上に100nmの高応力窒化物を付着させた。次いで、試料をへき開し、電気試験装置に入れて薄膜の絶縁破壊強度を評価した。導電エポキシを用いてシリコン基板(ウェハのへき開された縁部)と接地された金属段とを適切に電気接触させた。乾性条件下で金属電極、または湿性条件下で流体電極を用いて正(または負)電圧を印加した。電圧を段階的に上昇させ、同時に、膜を通ってシリコン基板に漏れる電流を監視した。曲線を記録した。このデータは図2に見ることができる。このデータから、金属(乾性)電気接触よりも液体(湿性)電気接触の方が絶縁耐力がずっと低いことが分かる。アニーリングの前にはこのような差はなかった。このデータは、応力によって膜にナノスケールクラック(nano-scale cracking)が生じたことを意味している。高応力窒化ケイ素膜の電流−電圧特性は乾性状況(金属電極)と湿性状況(液体電極)とで著しく異なり、液体電気接触実施例の場合の方が絶縁耐力がずっと低いことが分かる。
図3のデータは、以下の実験の設定および条件を用いて生成されたものである。半導体洗浄プロトコル(MOS洗浄)を用いてシリコンウェハを洗浄した。低圧化学蒸着炉内でシリコンウェハ上に1.5μmの低応力窒化物を付着させた。次いで、ウェハをへき開し、1つの破片を、低応力窒化物のみによって電気試験することが可能になるように保存し、他の破片をさらに加工し、その後100nmのオキシナイトライドを付着させた。次いで、これらの試料をへき開し、電気試験装置に入れて薄膜の絶縁破壊強度を評価した。導電エポキシを用いてシリコン基板(ウェハのへき開された縁部)と接地された金属段とを適切に電気接触させた。両方の試料について、乾性条件下で金属電極、または湿性条件下で流体電極を用いて、正(または負)電圧を印加した。電圧を段階的に上昇させ、同時に、膜を通ってシリコン基板に漏れる電流を監視した。曲線を記録した。このデータは図3に見ることができる。オキシナイトライドキャッピングをコーティングした後、液体電極に接触した膜の絶縁耐力が著しく向上している。絶縁耐力は、100%以上改善されている。
酸化物/低応力窒化物/オキシナイトライドの誘電膜スタックを有するシリコン電気噴霧装置を以下の手順に従って作製する。
シリコン基板を洗浄し、シリコンを熱酸化させて2.5μmの二酸化ケイ素を成長させる準備をする。二酸化ケイ素層の成長は、大気炉内で、蒸気酸化物を用いて、炉を約11000Cから12000Cに保持した状態で行う。膜が成長した後、窒素雰囲気でアニール段階を実施する。
二酸化ケイ素が成長した後、基板を低圧化学蒸着炉に移し、約1.5μmの低応力窒化物を付着させる。低応力窒化物を付着させるための炉気体にはジクロロシランおよびNH3が含まれる。炉条件には、温度約800〜9000Cおよび圧力300mTorrが含まれる。低応力窒化物の屈折率は約2.2である。
低応力窒化物を付着させた後、低圧化学蒸着炉内で(同一の炉または異なる炉内で)0.3μmのオキシナイトライドを付着させる。炉気体にはNH3、N2O、およびシラン(またはジクロロシラン)が含まれる。炉条件には、温度約800〜9000Cおよび圧力260mTorrが含まれる。オキシナイトライドの屈折率は約1.71である。
Claims (22)
- ベース層およびキャッピング層を含む誘電膜であり、導電基板と、基板の電位とは異なる電位を有する液体との間に配置されたときに効果的な水分・イオン障壁となる誘電膜。
- キャッピング層が凝縮膜を含む、請求項1記載の誘電膜。
- キャッピング層が、シリコンオキシナイトライド、非化学量論的シリコンオキシナイトライド、水素を含むシリコンオキシナイトライド、ドーピングされたシリコンオキシナイトライド、屈折率が約1.4から約2であるオキシナイトライド、屈折率が約2から約2.09である窒化ケイ素、ダイヤモンドライクカーボン、セラミック系の誘電材料、または遷移金属酸化物系の誘電材料を含む、請求項1記載の誘電膜。
- ベース層が2.5μmの酸化物膜および1.5μmの窒化物膜であり、キャッピング層が0.3μmのシリコンオキシナイトライド膜である、請求項1記載の誘電膜。
- ベース層が、酸化ケイ素系の材料、二酸化ケイ素系の誘電膜、二酸化ケイ素、非化学量論的二酸化ケイ素、ドーピングされた二酸化ケイ素、窒化ケイ素系の誘電膜、窒化ケイ素、非化学量論的窒化ケイ素、ドーピングされた窒化ケイ素、屈折率が約2.1から約3である窒化ケイ素、セラミック系の誘電材料、または遷移金属酸化物系の誘電材料を含む、請求項1記載の誘電膜。
- 導電基板と液体との電位差が約1200Vから約5000Vであるときに効果的な水分・イオン障壁となる、請求項1記載の誘電膜。
- 導電基板と液体との電位差が約4300Vであるときに効果的な水分・イオン障壁となる、請求項6記載の誘電膜。
- 導電基板と液体との電位差が約1200Vであるときに効果的な水分・イオン障壁となる、請求項6記載の誘電膜。
- キャッピング層が、屈折率が約1.6から約1.8であるシリコンオキシナイトライドを含む、請求項1記載の誘電膜。
- ベース層が2.5μmの酸化物膜であり、キャッピング層が1μmのシリコンオキシナイトライド膜である、請求項1記載の誘電膜。
- 少なくとも一部がベース層およびキャッピング層を含む誘電層で被覆された、導電基板;ならびに
誘電層に接触する液体
を含む装置。 - マイクロ流体装置が、電気噴霧装置、流体クロマトグラフィー装置、液体クロマトグラフィー/電気噴霧装置の組合せ、キャピラリー電気泳動、キャピラリー電気クロマトグラフィー、キャピラリー電気泳動/電気噴霧装置の組合せ、キャピラリー電気クロマトグラフィー/電気噴霧装置の組合せ、シリコン装置上の静電作動、電界を用いた導体上の液滴供給装置、またはシリコン系の燃料噴射装置である、請求項11記載の装置。
- キャッピング層が凝縮膜を含む、請求項11記載の装置。
- キャッピング層は、シリコンオキシナイトライド、非化学量論的シリコンオキシナイトライド、水素を含むシリコンオキシナイトライド、ドーピングされたシリコンオキシナイトライド、屈折率が約1.4から約2であるオキシナイトライド、屈折率が約2から約2.09である窒化ケイ素、ダイヤモンドライクカーボン、セラミック系の誘電材料、または遷移金属酸化物系の誘電材料を含む、請求項11記載の装置。
- ベース層が2.5μmの酸化物膜および1.5μmの窒化物膜であり、キャッピング層は0.3μmのシリコンオキシナイトライド膜である、請求項11記載の装置。
- ベース層が、酸化ケイ素系の材料、二酸化ケイ素系の誘電膜、二酸化ケイ素、非化学量論的二酸化ケイ素、ドーピングされた二酸化ケイ素、窒化ケイ素系の誘電膜、窒化ケイ素、非化学量論的窒化ケイ素、ドーピングされた窒化ケイ素、屈折率が約2.1から約3である窒化ケイ素、セラミック系の誘電材料、または遷移金属酸化物系の誘電材料を含む、請求項11記載の装置。
- 膜が、導電基板と液体との電位差が約1200Vから約5000Vであるときに効果的な水分・イオン障壁となる、請求項11記載の装置。
- 膜が、導電基板と液体との電位差が約4300Vであるときに効果的な水分・イオン障壁となる、請求項17記載の装置。
- 膜が、導電基板と液体との電位差が約1200Vであるときに効果的な水分・イオン障壁となる、請求項17記載の装置。
- キャッピング層が、屈折率が約1.6から約1.8であるシリコンオキシナイトライドを含む、請求項11記載の装置。
- ベース層が2.5μmの酸化物膜であり、キャッピング層が1μmのシリコンオキシナイトライド膜である、請求項11記載の装置。
- 溶液の電位とは異なる電位を有する導電基板への、溶液からの、イオンの移動を防止する方法であって、以下の段階を含む方法:
基板と溶液との間に挿入されたベース層およびシリコンオキシナイトライド・キャッピング層を含む、誘電膜層を設ける段階。
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2002
- 2002-09-17 EP EP10180014A patent/EP2261956A3/en not_active Withdrawn
- 2002-09-17 US US10/246,150 patent/US6891155B2/en not_active Expired - Lifetime
- 2002-09-17 WO PCT/US2002/029505 patent/WO2003025992A1/en active Application Filing
- 2002-09-17 JP JP2003529515A patent/JP2005533339A/ja active Pending
- 2002-09-17 AT AT02766293T patent/ATE533177T1/de active
- 2002-09-17 EP EP02766293A patent/EP1442476B1/en not_active Expired - Lifetime
Also Published As
Publication number | Publication date |
---|---|
EP1442476A1 (en) | 2004-08-04 |
EP2261956A3 (en) | 2011-03-30 |
ATE533177T1 (de) | 2011-11-15 |
WO2003025992A1 (en) | 2003-03-27 |
EP1442476B1 (en) | 2011-11-09 |
EP1442476A4 (en) | 2008-03-12 |
US20030057506A1 (en) | 2003-03-27 |
US6891155B2 (en) | 2005-05-10 |
EP2261956A2 (en) | 2010-12-15 |
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