TWI601851B - Tungsten oxide film hydrogen sensor - Google Patents
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- TWI601851B TWI601851B TW105124324A TW105124324A TWI601851B TW I601851 B TWI601851 B TW I601851B TW 105124324 A TW105124324 A TW 105124324A TW 105124324 A TW105124324 A TW 105124324A TW I601851 B TWI601851 B TW I601851B
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本發明係有關於一種氧化鎢薄膜氫氣感測器，特別係設有矽基板經清洗後固定置入真空腔體；氧化鎢(WO3)薄膜，係利用熱蒸發將蒸鍍靶材蒸鍍於該矽基板，其中，該蒸鍍靶材為氧化鎢(WO3)粉末，首先透過加熱使氧化鎢(WO3)粉末所含水氣先揮發掉，再加熱使氧化鎢(WO3)粉末完全昇華蒸鍍於該矽基板形成氧化鎢(WO3)薄膜；白金(Pt)電極，係利用射頻(RF)磁控濺鍍沉積濺鍍靶材於該氧化鎢(WO3)薄膜，其中，該濺鍍靶材為白金(Pt)靶材；如此，感測氫氣(H2)時，可提供最佳之感測能力。 The invention relates to a tungsten oxide thin film hydrogen sensor, in particular, a tantalum substrate is fixed and placed in a vacuum chamber after being cleaned; a tungsten oxide (WO 3 ) film is used to evaporate the vapor deposition target by thermal evaporation. The ruthenium substrate, wherein the vapor deposition target is a tungsten oxide (WO 3 ) powder, firstly, the water of the tungsten oxide (WO 3 ) powder is first volatilized by heating, and then heated to make the tungsten oxide (WO 3 ) powder completely Sublimation vapor deposition on the germanium substrate to form a tungsten oxide (WO 3 ) film; platinum (Pt) electrode is deposited by sputtering (RF) magnetron sputtering on the tungsten oxide (WO 3 ) film, wherein The sputtering target is a platinum (Pt) target; thus, the best sensing capability is provided when sensing hydrogen (H 2 ).
按，目前之氣體感測器，常使用在生活、工業環境中偵測有危險性之氣體，而氫氣在常溫常壓下是一種無色、無味、無臭、無毒的可燃性氣體，不容易察覺它的存在，卻因為其閃火點低，使其極容易燃燒，而燃燒之火焰肉眼難見，燃燒時會跟氧產生劇烈的化學作用，可能會導致***，所以氫氣感測器不可或缺，但尚未見有氧化鎢(WO3)薄膜氫氣感測器對氫氣(H2)氣體之感測，更未見其如何具備最佳感測能力；緣此，本發明人有鑑於習知存在有如上述之缺失，乃潛心研究、改良，遂得以首先發明本發明。 According to the current gas sensor, it is often used to detect dangerous gases in living and industrial environments. Hydrogen is a colorless, odorless, odorless, non-toxic flammable gas under normal temperature and pressure, which is not easy to detect. The existence of the flash, because of its low flash point, makes it extremely easy to burn, and the burning flame is hard to see, burning will have a strong chemical reaction with oxygen, which may cause an explosion, so the hydrogen sensor is indispensable. However, no tungsten oxide (WO 3 ) thin film hydrogen sensor has been used to sense hydrogen (H 2 ) gas, and it has not been seen how to have the best sensing capability. Therefore, the present inventors have The above-mentioned deficiencies are painstakingly studied and improved, and the invention can be first invented.
本發明之主要目的係在：對氫氣(H2)感測時，可提供最佳感測能力之氧化鎢薄膜氫氣感測器。 The main object of the present invention is a tungsten oxide thin film hydrogen sensor which provides optimum sensing capability when sensing hydrogen gas (H 2 ).
本發明之主要特徵係在：矽基板，係經清洗後固定置入真空腔體；氧化鎢(WO3)薄膜，係利用熱蒸發將蒸鍍靶材蒸鍍於該矽基板，其中，該蒸鍍靶材為氧化鎢(WO3)粉末，首先透過加熱使氧化鎢(WO3)粉末所含水氣先 揮發掉，再加熱使氧化鎢(WO3)粉末完全昇華蒸鍍於該矽基板形成氧化鎢(WO3)薄膜；白金(Pt)電極，係利用射頻(RF)磁控濺鍍沉積濺鍍靶材於該氧化鎢(WO3)薄膜，其中，該濺鍍靶材為白金(Pt)靶材；如此，在對氫氣(H2)感測時，通入氫氣(H2)1000ppm，電阻值R(Ω)會從100kΩ隨著時間慢慢增加，即表示有感測到氫氣(H2)，在氫氣(H2)感測之電阻值R(Ω)增加至1800kΩ即抽掉氫氣(H2)，再通入空氣(Air)，電阻值R(Ω)則會漸漸下降至180kΩ，響應值Response(Ra/Rg)為10，連續三次進行氫氣(H2)與空氣(Air)之感測發現都是感測到氫氣(H2)時，電阻值R(Ω)會增加，抽掉氫氣(H2)通入空氣(Air)時，電阻值R(Ω)會減少，故，可提供最佳之感測能力。 The main feature of the present invention is that the ruthenium substrate is fixed and placed in the vacuum chamber after being cleaned; the tungsten oxide (WO 3 ) film is vapor deposited on the ruthenium substrate by thermal evaporation, wherein the steam is evaporated. The plating target is a tungsten oxide (WO 3 ) powder. First, the moisture of the tungsten oxide (WO 3 ) powder is first volatilized by heating, and then heated to form a tungsten oxide (WO 3 ) powder which is completely sublimated and vapor-deposited on the crucible substrate. a tungsten oxide (WO 3 ) film; a platinum (Pt) electrode is deposited on the tungsten oxide (WO 3 ) film by radio frequency (RF) magnetron sputtering, wherein the sputtering target is platinum (Pt) The target; thus, when hydrogen (H 2 ) is sensed, hydrogen (H 2 ) is introduced at 1000 ppm, and the resistance value R (Ω) is gradually increased from 100 kΩ over time, indicating that hydrogen gas is sensed ( H 2 ), the resistance value R(Ω) sensed by hydrogen (H 2 ) is increased to 1800kΩ, that is, the hydrogen gas (H 2 ) is taken out, and then the air (Air) is introduced, and the resistance value R (Ω) is gradually decreased to 180kΩ, response value response (Ra / Rg) is 10, three consecutive hydrogen gas (H 2) of the sensed air found (air) are sensed hydrogen gas (H 2), the resistance value R (Ω) will increase , pumping off hydrogen (H 2 ) When the air is introduced, the resistance value R(Ω) is reduced, so that the best sensing capability can be provided.
本發明氧化鎢薄膜氫氣感測器，其中，該矽基板係為P型矽基板，該矽基板之大小為1.5cmx1.5cm，該矽基板係以超音波清洗5分鐘。 In the tungsten oxide thin film hydrogen sensor of the present invention, the germanium substrate is a P-type germanium substrate having a size of 1.5 cm x 1.5 cm, and the germanium substrate is ultrasonically cleaned for 5 minutes.
本發明氧化鎢薄膜氫氣感測器，其中，該氧化鎢(WO3)粉末係為0.35克。 The tungsten oxide thin film hydrogen sensor of the present invention, wherein the tungsten oxide (WO 3 ) powder is 0.35 g.
本發明氧化鎢薄膜氫氣感測器，其中，射頻(RF)磁控濺鍍沉積濺鍍靶材於該氧化鎢(WO3)薄膜時，設定濺鍍功率為100W，濺鍍時間為3分鐘。 In the tungsten oxide thin film hydrogen sensor of the present invention, the radio frequency (RF) magnetron sputtering deposition sputtering target is set to a sputtering power of 100 W and a sputtering time of 3 minutes when the tungsten oxide (WO 3 ) film is used.
本發明氧化鎢薄膜氫氣感測器，其中，該白金(Pt)電極係為矩形陣列，該白金(Pt)電極之大小為1mm x2mm、左右間距為3.5mm、上下間距為1mm。 In the tungsten oxide thin film hydrogen sensor of the present invention, the platinum (Pt) electrode is a rectangular array, and the platinum (Pt) electrode has a size of 1 mm x 2 mm, a left-right pitch of 3.5 mm, and a pitch of 1 mm.
本發明氧化鎢薄膜氫氣感測器，其中，利用熱蒸發使氧化鎢(WO3)粉末完全昇華蒸鍍於該矽基板形成氧化鎢(WO3)薄膜後，係進行真空快速熱退火，溫度為400℃。 Tungsten oxide film hydrogen sensor according to the present invention, wherein, by thermal evaporation of tungsten oxide (WO 3) powder of tungsten oxide is completely sublimated vapor form (WO 3) after the film, vacuum-based rapid thermal annealing to the silicon substrate, the temperature is 400 ° C.
1‧‧‧氧化鎢薄膜氫氣感測器 1‧‧‧Tungsten Oxide Thin Film Hydrogen Sensor
10‧‧‧矽基板 10‧‧‧矽 substrate
11‧‧‧氧化鎢(WO3)薄膜 11‧‧‧Tungsten oxide (WO 3 ) film
12‧‧‧白金(Pt)電極 12‧‧‧Platinum (Pt) electrode
2‧‧‧蒸鍍設備 2‧‧‧vapor deposition equipment
20‧‧‧真空腔體 20‧‧‧vacuum chamber
21‧‧‧泵浦 21‧‧‧ pump
22‧‧‧電流源 22‧‧‧current source
23‧‧‧鎢舟 23‧‧‧Tungsten boat
3‧‧‧氧化鎢(WO3)粉末 3‧‧‧Tungsten oxide (WO 3 ) powder
第一圖所示係為本發明實施例之組合局部剖視圖。 The first figure shows a partial cross-sectional view of a combination of embodiments of the present invention.
第二圖所示係為本發明實施例之組合俯視圖。 The second figure shows a combined top view of an embodiment of the invention.
第三圖所示係為本發明實施例之蒸鍍設備示意圖。 The third figure is a schematic view of an evaporation apparatus according to an embodiment of the present invention.
第四圖所示係為本發明實施例之流程圖。 The fourth figure is a flow chart of an embodiment of the present invention.
第五圖所示係為本發明實施例之未熱退火之氫氣感測圖。 The fifth figure is a hydrogen sensing diagram of the unheated annealing of the embodiment of the present invention.
第六圖所示係為本發明實施例之已熱退火之氫氣感測圖。 The sixth figure shows a hydrogen annealing diagram of the thermally annealed embodiment of the present invention.
有關本發明為達上述之使用目的與功效，所採用之技術手段，茲舉出較佳可行之實施例，並配合圖式所示，詳述如下：本發明之實施例，請配合參閱第一~三圖所示，主要係設有氧化鎢薄膜氫氣感測器1，該氧化鎢薄膜氫氣感測器1設有矽基板10、氧化鎢(WO3)薄膜11及白金(Pt)電極12所組成，其中，該矽基板10係為P型矽基板，該矽基板10之大小為1.5cm x1.5cm，該矽基板10係以超音波清洗5分鐘後固定置入蒸鍍設備2之真空腔體20，該蒸鍍設備2設有泵浦21及電流源22，該電流源22電性連接鎢舟23；氧化鎢(WO3)薄膜11，係利用熱蒸發將蒸鍍靶材蒸鍍於該矽基板10，其中，該蒸鍍靶材為氧化鎢(WO3)粉末3；白金(Pt)電極12，係利用射頻(RF)磁控濺鍍沉積濺鍍靶材於該氧化鎢(WO3)薄膜11，其中，該濺鍍靶材為白金(Pt)靶材，設定濺鍍功率為100W，濺鍍時間為3分鐘，該白金(Pt)電極12係為矩形陣列，該白金(Pt)電極12之大小為1mm x2mm、左右間距為3.5mm、上下間距為1mm。 For the purpose of the present invention, the preferred embodiments of the present invention are set forth in the accompanying drawings. As shown in the three figures, a tungsten oxide thin film hydrogen sensor 1 is mainly provided, and the tungsten oxide thin film hydrogen sensor 1 is provided with a tantalum substrate 10, a tungsten oxide (WO 3 ) thin film 11 and a platinum (Pt) electrode 12 The ruthenium substrate 10 is a P-type ruthenium substrate having a size of 1.5 cm x 1.5 cm. The ruthenium substrate 10 is ultrasonically cleaned for 5 minutes and then placed in a vacuum chamber of the vapor deposition apparatus 2. The vapor deposition device 2 is provided with a pump 21 and a current source 22. The current source 22 is electrically connected to the tungsten boat 23; the tungsten oxide (WO 3 ) film 11 is used to evaporate the vapor deposition target by thermal evaporation. The germanium substrate 10, wherein the vapor deposition target is tungsten oxide (WO 3 ) powder 3; and the platinum (Pt) electrode 12 is deposited by a radio frequency (RF) magnetron sputtering on the tungsten oxide (WO) 3) film 11, wherein the sputtering target of platinum (Pt) target, the sputtering power was set to 100W, the sputtering time was 3 minutes, and the platinum (Pt) electrode 12 A rectangular array, the platinum (Pt) as the size of the electrode 12 of 1mm x2mm, about 3.5mm pitch, the vertical spacing of 1mm.
本發明製作、設定及感測之流程，請配合參閱第三、四圖所示，主要步驟為：(a)清洗矽基板10：係對該矽基板10進行超音波清洗5分鐘；(b)置入真空腔體：係將該矽基板10固定置入蒸鍍設備2之真空腔體20；(c)將0.35克之氧化鎢(WO3)粉末3放置蒸鍍設備2之鎢舟23，泵浦21抽真空至8×10-3Pa， 電流源22進行加熱，透過加熱使鎢舟23上的氧化鎢(WO3)粉末3所含水氣先揮發掉；(d)蒸鍍氧化鎢(WO3)薄膜11：係利用熱蒸發將蒸鍍靶材蒸鍍於該矽基板10，其中，該蒸鍍靶材為氧化鎢(WO3)粉末3，係以電流源22進行再加熱，透過再加熱使鎢舟23上的氧化鎢(WO3)粉末3逐漸昇華蒸鍍於該矽基板10，直到氧化鎢(WO3)粉末3完全昇華蒸鍍於該矽基板10形成氧化鎢(WO3)薄膜11；(e)熱退火：係透過熱退火爐以溫度400℃進行真空快速熱退火，待降溫至常溫(RT)25℃即完成熱退火；(f)濺鍍白金(Pt)電極12：係利用射頻(RF)磁控濺鍍沉積濺鍍靶材於該氧化鎢(WO3)薄膜11，其中，該濺鍍靶材為白金(Pt)靶材(純度：99.99%)，首先設定濺鍍參數，即設定真空腔體功率及時間，例如：濺鍍功率為100W，濺鍍時間為3分鐘；(g)氫氣感測：請參閱第五、六圖所示，第五圖係未熱退火之氫氣感測圖，第六圖係已熱退火之氫氣感測圖，由第五圖可知，當通入氫氣(H2)1000ppm時，電阻值R(Ω)會從100kΩ隨著時間Time(e)慢慢增加，即表示有感測到氫氣(H2)，在氫氣(H2)感測之電阻值R(Ω)增加至1800kΩ即抽掉氫氣(H2)，再通入空氣(Air)，電阻值R(Ω)則會漸漸下降至180kΩ，響應值Response(Ra/Rg)為0.1，而響應定義係為通入感測氣氛前後的電阻值改變率，即Res=Ra/Rg，Ra為空氣(Air)中氧化鎢薄膜氫氣感測器1之電阻值，Rg為氫氣(H2)下氧化鎢薄膜氫氣感測器1之電阻值，故，連續三次進行氫氣(H2)與空氣(Air)之感測發現電阻值R(Ω)之增加及減少一致，都是感測到氫氣(H2)時，電阻值R(Ω)會增加，抽掉氫氣(H2)通入空氣(Air)時，電阻值R(Ω)會減少，即表示具有感測能力；另由第六圖可知，連續三次進行氫氣(H2)與空氣(Air)之感測發現都是感測到氫氣(H2)時，電阻值R(Ω)會增加，抽掉氫氣(H2)通入空氣(Air)時，電阻值R(Ω)會減少，表示同樣具有感測能力；如此，本發明係藉由熱蒸發將氧化鎢(WO3)粉末3完全昇華蒸鍍於該矽基板10形成氧化鎢(WO3)薄膜11，來提供最佳之感測能力。 For the process of fabrication, setting and sensing of the present invention, please refer to the third and fourth figures. The main steps are as follows: (a) cleaning the substrate 10: ultrasonic cleaning the substrate 10 for 5 minutes; (b) Inserting the vacuum chamber: fixing the crucible substrate 10 into the vacuum chamber 20 of the vapor deposition apparatus 2; (c) placing 0.35 g of tungsten oxide (WO 3 ) powder 3 on the tungsten boat 23 of the vapor deposition apparatus 2, pump The pump 21 is evacuated to 8×10 -3 Pa, and the current source 22 is heated, and the moisture of the tungsten oxide (WO 3 ) powder 3 on the tungsten boat 23 is first volatilized by heating; (d) vapor deposition of tungsten oxide ( WO 3 ) Thin film 11 : The vapor deposition target is vapor-deposited on the tantalum substrate 10 by thermal evaporation, wherein the vapor deposition target is tungsten oxide (WO 3 ) powder 3, which is reheated by the current source 22 to pass through Reheating causes the tungsten oxide (WO 3 ) powder 3 on the tungsten boat 23 to be gradually sublimated and evaporated on the tantalum substrate 10 until the tungsten oxide (WO 3 ) powder 3 is completely sublimated and evaporated on the tantalum substrate 10 to form tungsten oxide (WO 3 ) Film 11; (e) Thermal annealing: rapid thermal annealing at a temperature of 400 ° C through a thermal annealing furnace, to be cooled to room temperature (RT) 25 ° C to complete thermal annealing; (f) sputtering platinum (Pt) Pole 12: system using radio frequency (RF) magnetron sputter deposition sputtering target tungsten oxide (WO 3) film 11, wherein the sputtering target of platinum (Pt) target (purity: 99.99%), First set the sputtering parameters, that is, set the vacuum chamber power and time, for example: sputtering power is 100W, sputtering time is 3 minutes; (g) hydrogen sensing: please refer to the fifth and sixth figures, the fifth figure The hydrogen sensing pattern is not thermally annealed, and the sixth figure is the hydrogen sensing pattern of the thermal annealing. As shown in the fifth figure, when hydrogen (H 2 ) is introduced at 1000 ppm, the resistance value R (Ω) will be from 100 kΩ. with time time (e) gradually increases to a sensing means that the hydrogen (H 2), hydrogen (H 2) sensing the resistance value R (Ω) is increased to 1800kΩ deprived i.e. hydrogen (H 2), then Air (Air), the resistance value R (Ω) will gradually drop to 180kΩ, the response value Response (Ra / Rg) is 0.1, and the response is defined as the rate of change of resistance before and after the sensing atmosphere, that is, Res =Ra/Rg, Ra is the resistance value of the tungsten oxide film hydrogen sensor 1 in air (Air), and Rg is the resistance value of the tungsten oxide film hydrogen sensor 1 under hydrogen (H 2 ), so hydrogen is continuously performed three times. (H 2 ) and The sensing of air (Air) finds that the increase and decrease of the resistance value R(Ω) are consistent. When hydrogen (H 2 ) is sensed, the resistance value R (Ω) increases, and the hydrogen (H 2 ) is extracted. In the case of air, the resistance value R(Ω) is reduced, which means that it has sensing capability. According to the sixth figure, the sensing of hydrogen (H 2 ) and air (Air) is detected three times in succession. When hydrogen (H 2 ) is applied, the resistance value R (Ω) is increased. When the hydrogen (H 2 ) is drawn into the air (Air), the resistance value R (Ω) is decreased, indicating that the sensing capability is also the same; In the present invention, tungsten oxide (WO 3 ) powder 3 is completely sublimated by thermal evaporation onto the tantalum substrate 10 to form a tungsten oxide (WO 3 ) film 11 to provide optimum sensing capability.
本發明所採用之氧化鎢(WO3)粉末3為N型金屬氧化物半導體，具有優異的電色、光色及氣色等特性，可應用於氣體感測器；又透過熱退火爐以溫度400℃進行真空快速熱退火，因此，可快速完成氧化鎢(WO3)粉末3完全昇華蒸鍍於該矽基板10形成氧化鎢(WO3)薄膜11之熱退火。 The tungsten oxide (WO 3 ) powder 3 used in the present invention is an N-type metal oxide semiconductor, and has excellent characteristics of electrochromic, light color and gas color, and can be applied to a gas sensor; and a temperature of 400 through a thermal annealing furnace. The vacuum rapid thermal annealing is performed at ° C. Therefore, the thermal annealing of the tungsten oxide (WO 3 ) powder 3 is completely sublimated and vapor deposited on the tantalum substrate 10 to form the tungsten oxide (WO 3 ) thin film 11.
綜上所述，本發明確實已達到所預期之使用目的與功效，且更較習知者為之理想、實用，惟，上述實施例僅係針對本發明之較佳實施例進行具體說明而已，該實施例並非用以限定本發明之申請專利範圍，舉凡其它未脫離本發明所揭示之技術手段下所完成之均等變化與修飾，均應包含於本發明所涵蓋之申請專利範圍中。 In view of the above, the present invention has achieved the intended use and efficacy, and is more desirable and practical than the prior art, but the above embodiments are only specifically described for the preferred embodiment of the present invention. The present invention is not intended to limit the scope of the invention, and all other equivalents and modifications may be included in the scope of the invention covered by the invention.
1‧‧‧氧化鎢薄膜氫氣感測器 1‧‧‧Tungsten Oxide Thin Film Hydrogen Sensor
10‧‧‧矽基板 10‧‧‧矽 substrate
11‧‧‧氧化鎢(WO3)薄膜 11‧‧‧Tungsten oxide (WO 3 ) film
12‧‧‧白金(Pt)電極 12‧‧‧Platinum (Pt) electrode
Claims (6)
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| TW105124324A TWI601851B (en) | 2016-08-01 | 2016-08-01 | Tungsten oxide film hydrogen sensor |
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| TW105124324A TWI601851B (en) | 2016-08-01 | 2016-08-01 | Tungsten oxide film hydrogen sensor |
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| TWI601851B true TWI601851B (en) | 2017-10-11 |
| TW201805482A TW201805482A (en) | 2018-02-16 |
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| TW105124324A TWI601851B (en) | 2016-08-01 | 2016-08-01 | Tungsten oxide film hydrogen sensor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI650553B (en) * | 2017-10-20 | 2019-02-11 | 行政院原子能委員會核能硏究所 | Gas sensor device and manufacturing method thereof |
| CN109768121A (en) * | 2018-12-29 | 2019-05-17 | 浙江师范大学 | The method that monocrystalline silicon surface is passivated with tungsten oxide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI528031B (en) * | 2014-10-28 | 2016-04-01 | Indium gallium oxide thin film hydrogen sensor |
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2016
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI528031B (en) * | 2014-10-28 | 2016-04-01 | Indium gallium oxide thin film hydrogen sensor |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI650553B (en) * | 2017-10-20 | 2019-02-11 | 行政院原子能委員會核能硏究所 | Gas sensor device and manufacturing method thereof |
| CN109768121A (en) * | 2018-12-29 | 2019-05-17 | 浙江师范大学 | The method that monocrystalline silicon surface is passivated with tungsten oxide |
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| Publication number | Publication date |
|---|---|
| TW201805482A (en) | 2018-02-16 |
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