TWI782767B - A methof of mass-producing nanoprobes - Google Patents

A methof of mass-producing nanoprobes Download PDF

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TWI782767B
TWI782767B TW110139826A TW110139826A TWI782767B TW I782767 B TWI782767 B TW I782767B TW 110139826 A TW110139826 A TW 110139826A TW 110139826 A TW110139826 A TW 110139826A TW I782767 B TWI782767 B TW I782767B
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tungsten
protective layer
hole
aqueous solution
tungsten wires
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TW110139826A
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TW202317466A (en
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柳紀綸
林榮君
張仕欣
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汎銓科技股份有限公司
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Abstract

The present invention proposes a novel meth of mass-producing nanoprobes. The diameter of apexes of the obtained nanoprobes falls is 10-100 nm, and the required equipment is simple and easy to operate. There is no need for complicated circuit designs and sensitive galvanometers, thereby personnel is not required to confirm from time to time, and the process is simple and mass-production can be achieved, which greatly improves all the shortcomings of the existing nanoprobe manufacturing methods, and makes the nanoprobes needed for the semiconductor measurement can be provided in large quantities with a cheaper price.

Description

一種大量製作奈米級針尖探針的方法A method for mass production of nanoscale needle-tip probes

本發明乃關於一種大量製作探針的方法,且特別是關於一種大量製作奈米級針尖探針的方法。 The present invention relates to a method for producing probes in large quantities, and in particular to a method for producing nanoscale needle-tip probes in large quantities.

奈米探針是半導體業量測單一電晶體電性的唯一工具,原理是利用數根具有奈米級針尖(10-50nm)的探針(材料為鎢)以一固定下壓力道,分別接觸待測電晶體的電極(如閘極、源極、或汲極),最後藉由外部測試器(Tester)給予測試條件,量測待測電晶體的電壓/電流(IV)特性。上述過程中,探針狀況對於量測有著決定性的影響,例如,1)對先進製程(<16nm)樣品,探針針尖如果太鈍,則探針無法接觸到待測電極,導致無法量測,或2)探針如已量測數個樣品,針尖變鈍之外,針尖表面也會沾附接觸先前樣品之電極的材料,產生接觸電阻,影響量測結果等,探針狀況如有疑慮,更換新且較尖的探針是業界目前唯一的方法;但奈米級針尖探針所費不貲,且越尖越貴,研發出方便且能大量製作奈米級針尖探針的方法,將是半導體業所殷殷期盼的事。 The nanoprobe is the only tool used by the semiconductor industry to measure the electrical properties of a single transistor. The principle is to use several probes (tungsten) with nanometer-scale needle tips (10-50nm) to contact each other with a fixed pressure channel. The electrodes (such as gate, source, or drain) of the transistor to be tested are finally given test conditions by an external tester (Tester) to measure the voltage/current (IV) characteristics of the transistor to be tested. In the above process, the condition of the probe has a decisive impact on the measurement. For example, 1) for advanced process (<16nm) samples, if the probe tip is too blunt, the probe cannot touch the electrode to be tested, resulting in failure to measure. Or 2) If the probe has measured several samples, the needle tip will become blunt, and the surface of the needle tip will also adhere to the material of the electrode that was in contact with the previous sample, resulting in contact resistance and affecting the measurement results. If there is any doubt about the condition of the probe, Replacing new and sharper probes is currently the only method in the industry; however, nano-scale needle-tip probes are expensive, and the sharper the more expensive, the development of a convenient and mass-produced method of nano-scale needle-tip probes will be It's something the semiconductor industry has been waiting for.

圖1A~1D所示為習知一種製作奈米級針尖探針的示意流程圖。如圖1所表示,習知製作奈米級針尖探針的方法主要採用電化學方式,所需材料包含一電源供應器(直流或交流)110、一控制電路120、一電流計130、一碳棒140、一鎢線(一般直徑<0.5mm)150,以及一盛有強鹼水溶液180之容器170, 該強鹼水溶液180為例如但不限於濃度1-2M的氫氧化鉀(KOH)水溶液或氫氧化鈉(NaOH)水溶液,其中鎢線150與電源供應器110之正電極電性連接,碳棒140與電源供應器110之負極電性連接,且碳棒140與鎢線150部分***容器170所盛的強鹼水溶液180內。將電源供應器110之間輸出電壓設定於2-10V之間便可藉由電化學方式開始製作奈米級針尖探針。惟,如圖1A所示,鎢線150因表面張力緣故,與強鹼水溶液180液面L1會有一向上傾角θ,故電化學主要反應位置會在氫氧化鉀水溶液或氫氧化鈉水溶液液面L1附近。電化學反應會在鎢線150靠近強鹼水溶液180的液面L1附近的位置將鎢原子解離成鎢氧離子(WO4 -2),逐漸形成一如圖1B所示內凹弧線。同時,位在強鹼水溶液180的液面L1下方的下鎢線153也會有解離反應,使得下鎢線153變短,變瘦,如圖1C所示。最後,因電化學反應使鎢線150靠近強鹼水溶液180的液面L1附近的位置之剩餘材料越來越少(鎢線半徑變小),最後支撐不住下鎢線153重量,重力拉扯關係,使上、下鎢線151、153分離,形成上鎢針161與下鎢針163,如圖1D所示。 1A-1D are schematic flowcharts of a conventional method for fabricating nanoscale needle-tip probes. As shown in Figure 1, the conventional method for making nano-scale needle tip probes mainly adopts electrochemical methods, and the required materials include a power supply (DC or AC) 110, a control circuit 120, an ammeter 130, a carbon Rod 140, a tungsten wire (generally <0.5mm in diameter) 150, and a container 170 filled with a strong alkaline aqueous solution 180, such as but not limited to potassium hydroxide (KOH) aqueous solution with a concentration of 1-2M or Sodium hydroxide (NaOH) aqueous solution, wherein the tungsten wire 150 is electrically connected to the positive electrode of the power supply 110, the carbon rod 140 is electrically connected to the negative electrode of the power supply 110, and the carbon rod 140 and the tungsten wire 150 are partially inserted into the container 170 In the strong alkali aqueous solution 180 that holds. By setting the output voltage between the power supply 110 between 2-10V, the fabrication of nanoscale needle-tip probes can be started electrochemically. However, as shown in Figure 1A, due to the surface tension, the tungsten wire 150 has an upward inclination angle θ with the liquid level L1 of the strong alkali aqueous solution 180, so the main electrochemical reaction position will be at the liquid level L1 of the potassium hydroxide aqueous solution or the sodium hydroxide aqueous solution nearby. The electrochemical reaction dissociates tungsten atoms into tungsten oxide ions (WO 4 −2 ) at the position near the liquid level L1 of the strong alkali aqueous solution 180 on the tungsten wire 150 , gradually forming a concave arc as shown in FIG. 1B . At the same time, the lower tungsten wire 153 below the liquid level L1 of the strong alkali aqueous solution 180 also undergoes a dissociation reaction, making the lower tungsten wire 153 shorter and thinner, as shown in FIG. 1C . Finally, due to the electrochemical reaction, the remaining material of the tungsten wire 150 near the liquid level L1 of the strong alkali aqueous solution 180 becomes less and less (the radius of the tungsten wire becomes smaller), and finally the weight of the lower tungsten wire 153 cannot be supported, and gravity pulls the relationship , separate the upper and lower tungsten wires 151 and 153 to form an upper tungsten needle 161 and a lower tungsten needle 163, as shown in FIG. 1D.

為取得穩定且有一定尖度的奈米級針尖探針,一般手法是在電源供應器110前外加一控制電路120與一高靈敏的電流計130,當電流低於一設定之截止電流時,瞬間(50-100ns)停止電源輸出,避免因上、下鎢線151、153分離後,上鎢針161的針尖因表面張力關係,針尖與強鹼水溶液180接觸,仍會持續解離反應,致使針尖由尖再變鈍。奈米探針都是選用如圖1D所示的上鎢針161當探針,下鎢針163因受化學反應緣故,外型已變形,且在掉落到容器170底部時,針尖先落地,針尖極可能受損,如圖1D所示,並不適合拿來做為奈米 級針尖探針。惟,此改善方法缺點是需要額外搭配一控制電路120與一高靈敏的電流計130,不僅增加不方便性外,且一次也只能製作一根,產量有限。 In order to obtain stable and sharp nano-scale needle probes, the general method is to add a control circuit 120 and a highly sensitive ammeter 130 in front of the power supply 110. When the current is lower than a set cut-off current, Instantaneously (50-100ns) stop the power output to avoid dissociation reaction of the needle tip of the upper tungsten needle 161 due to the surface tension after the upper and lower tungsten wires 151 and 153 are separated, and the needle tip contacts the strong alkali aqueous solution 180. From sharp to blunt. The nanoprobes all use the upper tungsten needle 161 as shown in Figure 1D as the probe, and the lower tungsten needle 163 has been deformed due to the chemical reaction, and when it falls to the bottom of the container 170, the needle tip lands first. The needle tip is very likely to be damaged, as shown in Figure 1D, and is not suitable for use as a nanometer Grade needle tip probes. However, the disadvantage of this improvement method is that an additional control circuit 120 and a high-sensitivity ammeter 130 are required, which not only increases inconvenience, but also can only be produced one at a time, and the output is limited.

有鑒於此,本發明乃提出一個創新的奈米級針尖探針的製備手法,無須繁雜的電路設計與靈敏的電流計,製作過程中也無須人員時時確認,製程容易且可以大量製作。 In view of this, the present invention proposes an innovative method for preparing nano-scale needle-tip probes, which does not require complex circuit design and sensitive ammeters, and does not require constant confirmation by personnel during the production process. The process is easy and mass production is possible.

本發明乃揭示一種大量製作奈米級針尖探針的方法,其步驟包括:提供2N個長度T1的第一鎢線,並以電化學方式去除該等2N個第一鎢線的表面氧化層,以獲得2N個第二鎢線,N為自然數,且T1>0;在該等2N個第二鎢線之一端表面形成一長度T2的保護層,以製備獲得2N個第三鎢線,T1>T2>0;提供一金屬圓盤治具,包括一位在該金屬圓盤治具中心處的第一通孔、2N個等距圍繞該第一通孔的第二通孔以及2N個螺絲孔,每一該等螺絲孔乃分別對應於其中一該等第二通孔,且每一該等螺絲孔乃自該金屬圓盤治具之圓周邊緣朝向其中一該等第二通孔貫穿,其中該第一通孔的直徑為R1,該第二通孔的直徑為R2,每一該等第二通孔之圓心與該第一通孔圓心之距離為R3,R1,R3>R2>0;提供一容器,該容器內盛一強鹼水溶液;將該金屬圓盤治具放置於該容器上方,然後將一碳棒***該第一通孔並以一絕緣材固定於該金屬圓盤治具的該第一通孔內,使該碳棒浸入該強鹼水溶液內,並將該等2N個第三鎢線分別***該等第二通孔內,調整該等2N個第三鎢線的高度,使位在每一該等2N個第三鎢線的一端的該保護層的上緣低於該強鹼水溶液的液面h1之距離,h1>0且每一該等2N個第三鎢線並分別以其中一該等螺絲經由其中一該等螺絲孔固定於其所對應的其中一該等第二通孔上;提供一電源供應器,具有一正電極及一負電極,並以該正電極電性連接該金屬圓盤治具,以該負電極電性連接該碳棒,並於該電源供應 器的輸出電壓為V的條件下進行電化學反應以開始製作奈米級針尖探針,且當該等2N個第三鎢線分離成2N個固定於該金屬圓盤治具的上鎢針與2N個沉入該強鹼水溶液內的下鎢針時,關閉該電源供應器,2

Figure 110139826-A0305-02-0006-12
V
Figure 110139826-A0305-02-0006-11
10;以及取出沉入該強鹼水溶液內的該等2N個下鎢針,去除該等2N個下鎢針表面的該保護層後,便可完成2N個奈米級針尖探針之製備。 The present invention discloses a method for producing a large number of nano-scale needle-tip probes. The steps include: providing 2N first tungsten wires with a length T1, and electrochemically removing the surface oxide layer of the 2N first tungsten wires, 2N second tungsten wires are obtained, N is a natural number, and T1>0; a protective layer with a length T2 is formed on the surface of one end of the 2N second tungsten wires to prepare and obtain 2N third tungsten wires, T1 >T2>0; provide a metal disc jig, including a first through hole at the center of the metal disc jig, 2N second through holes equidistant around the first through hole, and 2N screws holes, each of the screw holes is respectively corresponding to one of the second through holes, and each of the screw holes penetrates from the peripheral edge of the metal disc jig towards one of the second through holes, The diameter of the first through hole is R1, the diameter of the second through hole is R2, and the distance between the center of each of the second through holes and the center of the first through hole is R3, R1, R3>R2>0 ; Provide a container containing a strong alkali aqueous solution; place the metal disk fixture above the container, then insert a carbon rod into the first through hole and fix it on the metal disk fixture with an insulating material In the first through hole of the tool, the carbon rod is immersed in the strong alkali aqueous solution, and the 2N third tungsten wires are respectively inserted into the second through holes, and the 2N third tungsten wires are adjusted Height, so that the upper edge of the protective layer at one end of each of the 2N third tungsten wires is lower than the distance h1 of the liquid level of the strong alkali aqueous solution, h1>0 and each of the 2N third tungsten wires Wires are respectively fixed on one of the corresponding second through holes through one of the screw holes by one of the screws; a power supply is provided, which has a positive electrode and a negative electrode, and uses the The positive electrode is electrically connected to the metal disc jig, the negative electrode is electrically connected to the carbon rod, and the electrochemical reaction is carried out under the condition that the output voltage of the power supply is V to start the production of nano-scale needle tip probes , and when the 2N third tungsten wires are separated into 2N upper tungsten needles fixed on the metal disc jig and 2N lower tungsten needles submerged in the strong alkali aqueous solution, the power supply is turned off, 2
Figure 110139826-A0305-02-0006-12
V
Figure 110139826-A0305-02-0006-11
10; and taking out the 2N lower tungsten needles submerged in the strong alkali aqueous solution, and removing the protective layer on the surface of the 2N lower tungsten needles, the preparation of the 2N nanoscale tip probes can be completed.

如上所述的方法,其中T1例如但不限於介於50-60mm;N例如但不限於介於1至15;T2為例如但不限於20mm。 The above method, wherein T1 is for example but not limited to 50-60 mm; N is for example but not limited to 1 to 15; T2 is for example but not limited to 20 mm.

如上所述的方法,其中當該金屬圓盤治具之直徑為例如但不限於120mm,厚度為例如但不限於10mm,且R1為例如但不限於40mm,R2為例如但不限於1mm,R3例如但不限於介於50-55mm,該容器之直徑為例如但不限於100mm,且0.5mm

Figure 110139826-A0305-02-0006-14
h1
Figure 110139826-A0305-02-0006-5
1mm。 The above-mentioned method, wherein when the diameter of the metal disc jig is, for example, but not limited to 120mm, the thickness is, for example, but not limited to 10mm, and R1 is, for example, but not limited to 40mm, R2 is, for example, but not limited to 1mm, R3 is for example But not limited to between 50-55mm, the diameter of the container is for example but not limited to 100mm, and 0.5mm
Figure 110139826-A0305-02-0006-14
h1
Figure 110139826-A0305-02-0006-5
1mm.

如上所述的方法,其中該強鹼水溶液為例如但不限於濃度1-2M的氫氧化鉀水溶液或氫氧化鈉水溶液。 The above-mentioned method, wherein the strong alkali aqueous solution is, for example but not limited to, an aqueous potassium hydroxide solution or an aqueous sodium hydroxide solution with a concentration of 1-2M.

如上所述的方法,其中該製備獲得2N個第三鎢線之步驟包括:提供一加熱的保護層溶液;將該等2N個第二鎢線部分垂直浸入該加熱的保護層溶液內,使位在被浸入該加熱的保護層溶液內之該等2N個第二鎢線的一端表面形成一長度T2保護層,完成該等2N個第三鎢線之製備。 The above method, wherein the step of preparing and obtaining 2N third tungsten wires includes: providing a heated protective layer solution; vertically immersing the 2N second tungsten wires in the heated protective layer solution, so that A protective layer of length T2 is formed on one end surface of the 2N second tungsten wires immersed in the heated protective layer solution, and the preparation of the 2N third tungsten wires is completed.

如上所述的方法,其中該加熱的保護層溶液為例如但不限於溫度介於攝氏40-50度間的熔蠟或熱熔膠。 The above method, wherein the heated protective layer solution is, for example but not limited to, molten wax or hot melt adhesive at a temperature between 40-50 degrees Celsius.

如上所述的方法,其中該去除該等下鎢針表面的該保護層的步驟包括:提供一丙酮溶劑;將該等2N個下鎢針浸入該丙酮溶劑內攪拌清洗15-30秒;以及將該等2N個下鎢針自該丙酮溶劑中取出,然後浸入一去離子水中,攪拌清洗5-10秒,將該等2N個下鎢針自該去離子水中取出後便可完成2N個奈米級針尖探針之製備。 The above method, wherein the step of removing the protective layer on the surface of the lower tungsten needles comprises: providing an acetone solvent; immersing the 2N lower tungsten needles in the acetone solvent and stirring and cleaning for 15-30 seconds; and The 2N lower tungsten needles are taken out from the acetone solvent, then immersed in deionized water, stirred and cleaned for 5-10 seconds, and the 2N nanometer Preparation of grade needle-tip probes.

110:電源供應器 110: Power supply

120:控制電路 120: control circuit

130:電流計 130: ammeter

140:碳棒 140: carbon rod

150:鎢線 150: Tungsten wire

151:上鎢線 151: Upper tungsten wire

153:下鎢線 153: Lower tungsten wire

161:上鎢針 161: Upper tungsten needle

163:下鎢針 163: Lower tungsten needle

170:容器 170: container

180:強鹼水溶液 180: Aqueous solution of strong alkali

210:電源供應器 210: Power supply

240:碳棒 240: carbon rod

251:第一鎢線 251: The first tungsten wire

252:第二鎢線 252: Second tungsten wire

253:第三鎢線 253: The third tungsten wire

260:表面氧化層 260: surface oxide layer

270:保護層 270: protective layer

281:上鎢針 281: Upper tungsten needle

283:下鎢針 283: Lower tungsten needle

2831:下鎢針283的奈米級針尖 2831: The nanoscale tip of the lower tungsten needle 283

300:容器 300: container

350:強鹼水溶液 350: Aqueous solution of strong alkali

400:容器 400: container

450:保護層溶液 450: protective layer solution

500:金屬圓盤治具 500: metal disc jig

505:圓周邊緣 505: Circumferential edge

510:第一通孔 510: the first through hole

520:第二通孔 520: the second through hole

530:螺絲孔 530: screw hole

540:絕緣材 540: insulating material

550:螺絲 550: screw

R1:第一通孔直徑 R1: Diameter of the first through hole

R2:第二通孔直徑 R2: second through hole diameter

R3:第二通孔之圓心與該第一通孔圓心之距離 R3: The distance between the center of the second through hole and the center of the first through hole

T1:第一鎢線之長度 T1: Length of the first tungsten wire

T2:保護層270之長度 T2: the length of the protective layer 270

θ:向上傾角 θ: upward inclination

L1:液面 L1: liquid level

h1:保護層270的上緣與液面L1之距離 h1: the distance between the upper edge of the protective layer 270 and the liquid surface L1

圖1A~1D所繪示的是習知一種製作探針的製程示意圖。 1A-1D are schematic diagrams of a conventional manufacturing process for making probes.

圖2A~2K所繪示的是根據本發明實施例所揭示的一種大量製作奈米級針尖探針的製程示意圖。 2A to 2K are schematic diagrams of a mass production process of nano-scale needle-tip probes disclosed according to an embodiment of the present invention.

為了使本發明揭示內容的敘述更加詳盡與完備,下文針對了本發明的實施態樣與具體實施例提出了說明性的描述;但這並非實施或運用本發明具體實施例的唯一形式。以下所揭露的各實施例,在有益的情形下可相互組合或取代,也可在一實施例中附加其它的實施例,而無須進一步的記載或說明。 In order to make the description of the disclosed content of the present invention more detailed and complete, the following provides an illustrative description of the implementation aspects and specific embodiments of the present invention; but this is not the only form for implementing or using the specific embodiments of the present invention. The various embodiments disclosed below can be combined or replaced with each other when beneficial, and other embodiments can also be added to one embodiment, without further description or illustration.

在以下描述中,將詳細敘述許多特定細節以使讀者能夠充分理解以下的實施例。然而,可在無此等特定細節之情況下實踐本發明之實施例。在其它情況下,為簡化圖式,熟知的結構與裝置僅示意性地繪示於圖中。 In the following description, numerous specific details will be set forth in order to enable readers to fully understand the following embodiments. However, embodiments of the invention may be practiced without these specific details. In other instances, well-known structures and devices are only schematically shown in order to simplify the drawings.

實施例 Example

根據本發明實施例所揭示的一種大量製作奈米級針尖探針的製程乃以圖2A~2K作例示說明。 A process for manufacturing a large number of nanoscale needle-tip probes according to an embodiment of the present invention is illustrated in FIGS. 2A-2K .

首先,提供2N個如圖2A所示的第一鎢線251,其長度T1為例如但不限於50-60mm,且其直徑為例如但不限於0.5mm。本實施例所提供的第一鎢線251之數量為12個(即N=6),在根據本發明的其它實施例中,所提供的第一鎢線251之數量可為2以上的偶數數量,即N為自然數,且N較佳的是介於1~15。如圖2A所示,每一該等第一鎢線251之表面具有一表面氧化層260。 First, 2N first tungsten wires 251 as shown in FIG. 2A are provided, the length T1 of which is, for example but not limited to, 50-60 mm, and the diameter thereof is, for example but not limited to, 0.5 mm. The number of the first tungsten wires 251 provided in this embodiment is 12 (that is, N=6), and in other embodiments according to the present invention, the number of the first tungsten wires 251 provided can be an even number of more than 2 , that is, N is a natural number, and N is preferably between 1 and 15. As shown in FIG. 2A , the surface of each of the first tungsten wires 251 has a surface oxide layer 260 .

其次,如圖2B~2C所示,利用電化學法去除每一該等第一鎢線251表面之表面氧化層260,以獲得如圖2C所示的去除表面氧化層260的第二鎢線252。此步驟乃將每一該等第一鎢線251平放入一盛有強鹼水溶液350的容器300內,該強鹼水溶液350為例如但不限於濃度1-2M的氫氧化鉀水溶液或氫氧化鈉水溶液,將每一該等第一鎢線251分別接上電源供應器210的正極,並將一接上電源供應器210的負極的碳棒240部分***盛有強鹼水溶液350的容器300內,並使電源供應器210施加5V電壓,維持為時15-20秒,以獲得如圖2C所示的去除表面氧化層260的第二鎢線252。 Next, as shown in FIGS. 2B-2C , the surface oxide layer 260 on the surface of each of the first tungsten wires 251 is removed by electrochemical method, so as to obtain the second tungsten wire 252 with the surface oxide layer 260 removed as shown in FIG. 2C . In this step, each of the first tungsten wires 251 is put into a container 300 filled with a strong alkali aqueous solution 350. The strong alkali aqueous solution 350 is, for example but not limited to, a potassium hydroxide aqueous solution or an aqueous potassium hydroxide solution with a concentration of 1-2M. Sodium aqueous solution, connect each of the first tungsten wires 251 to the positive pole of the power supply 210, and insert a part of the carbon rod 240 connected to the negative pole of the power supply 210 into the container 300 containing the strong alkali aqueous solution 350 , and make the power supply 210 apply a voltage of 5V for 15-20 seconds to obtain the second tungsten wire 252 with the surface oxide layer 260 removed as shown in FIG. 2C .

然後,如圖2D~2E所示般,提供一盛有加熱的保護層溶液450的容器400,並將該等第二鎢線252部分垂直浸入該加熱的保護層溶液450內,使位在被浸入該加熱的保護層溶液450內之該等第二鎢線252的一端表面形成一長度T2保護層270,完成該等第三鎢線253之製備。該加熱的保護層溶液450為例如但不限於溫度介於攝氏40-50度間的熔蠟或熱熔膠,且保護層270之長度T2為例如但不限於20mm。 Then, as shown in Figures 2D-2E, a container 400 containing a heated protective layer solution 450 is provided, and the parts of the second tungsten wires 252 are vertically immersed in the heated protective layer solution 450, so that A length T2 protection layer 270 is formed on one end surface of the second tungsten wires 252 immersed in the heated protection layer solution 450 , and the preparation of the third tungsten wires 253 is completed. The heated protective layer solution 450 is, for example, but not limited to, melted wax or hot melt adhesive at a temperature between 40-50 degrees Celsius, and the length T2 of the protective layer 270 is, for example, but not limited to 20 mm.

接著,如圖2F-1~2F-2所示般,提供一金屬圓盤治具500,其中圖2F-1為該金屬圓盤治具500之俯視圖,而圖2F-2為該金屬圓盤治具500之側視圖。如圖2F-1~2F-2所示,該金屬圓盤治具500包括一位在該金屬圓盤治具中心處的第一通孔510、2N個等距圍繞該第一通孔510的第二通孔520以及2N個螺絲孔530,每一該等螺絲孔530乃分別對應於其中一該等第二通孔520,且每一該等螺絲孔530乃自該金屬圓盤治具500之圓周邊緣505朝向其中一該等第二通孔520貫穿。其中,該第一通孔510的直徑為R1,該第二通孔的直徑為R2,每一該等第二通孔之圓心與該第一通孔圓心之距離為R3,R1,R3>R2>0。在本實施例中,R1為例如但不限於40mm,R2為例如但不限於1mm,R3為例如但不限於50-55mm,且 螺絲孔為例如但不限於螺紋牙徑:M1.4之螺絲孔。在根據本發明的其它實施例中,R1、R2、R3之尺寸以及螺絲孔之螺紋牙徑可視實際需要加以調整。此外,本實施例所提供的第一通孔510、第二通孔520以及螺絲孔530之數量分別為12個(即N=6),在根據本發明的其它實施例中,所提供的第一通孔510、第二通孔520以及螺絲孔530之數量可分別為2以上的偶數數量,即N為自然數,且N較佳的是介於1~15。 Next, as shown in Figures 2F-1~2F-2, a metal disk fixture 500 is provided, wherein Figure 2F-1 is a top view of the metal disk fixture 500, and Figure 2F-2 is the metal disk A side view of the fixture 500. As shown in Figures 2F-1~2F-2, the metal disc jig 500 includes a first through hole 510 at the center of the metal disc jig, 2N equidistantly surrounding the first through hole 510. The second through hole 520 and 2N screw holes 530, each of the screw holes 530 is respectively corresponding to one of the second through holes 520, and each of the screw holes 530 is formed from the metal disc jig 500 The peripheral edge 505 penetrates toward one of the second through holes 520 . Wherein, the diameter of the first through hole 510 is R1, the diameter of the second through hole is R2, and the distance between the center of each of the second through holes and the center of the first through hole is R3, R1, R3>R2 >0. In this embodiment, R1 is for example but not limited to 40mm, R2 is for example but not limited to 1mm, R3 is for example but not limited to 50-55mm, and The screw holes are, for example but not limited to, thread diameter: M1.4 screw holes. In other embodiments according to the present invention, the sizes of R1, R2, R3 and the thread diameter of the screw holes can be adjusted according to actual needs. In addition, the number of the first through hole 510, the second through hole 520 and the screw hole 530 provided in this embodiment is 12 respectively (that is, N=6). In other embodiments of the present invention, the provided first The number of the first through hole 510 , the second through hole 520 and the screw hole 530 can be an even number greater than 2, ie N is a natural number, and N is preferably between 1-15.

然後,如圖2G所示,提供另一內盛強鹼水溶液350的容器300,該強鹼水溶液350為例如但不限於濃度1-2M的氫氧化鉀水溶液或氫氧化鈉水溶液,然後將該金屬圓盤治具500放置於該容器300上方。 Then, as shown in FIG. 2G , another container 300 containing a strong alkali aqueous solution 350 is provided. The strong alkali aqueous solution 350 is, for example but not limited to, an aqueous potassium hydroxide solution or an aqueous sodium hydroxide solution with a concentration of 1-2M, and then the metal The disc jig 500 is placed above the container 300 .

接著,如圖2H所示,提供一電源供應器210,以該電源供應器210正電極電性連接該金屬圓盤治具500,並將一與電源供應器210之負極電性連接的碳棒240部分***該第一通孔510並以一絕緣材540,例如但不限於壓克力,固定於該金屬圓盤治具500的該第一通孔510內,並使該碳棒240部分浸入該強鹼水溶液350內,然後再將該等第三鎢線253分別***該等第二通孔520內,調整該等第三鎢線520的高度,使位在每一該等第三鎢線253的一端的該保護層270的上緣低於該強鹼水溶液350的液面h1之距離,h1為例如但不限於0.5-1mm,且每一該等第三鎢線253並分別以其中一該等螺絲550經由其中一該等螺絲孔530固定於其所對應的其中一該等第二通孔520上。本實施例之螺絲550為例如但不限於螺紋牙徑:M1.4之螺絲。然後,該電源供應器210的輸出電壓設定為V的條件下進行電化學反應以開始製作奈米級針尖探針,其中電源供應器210的輸出電壓V乃例如但不限於介於2~10伏特之間。電化學反應只會發生在鎢線253與強鹼水溶液350的液面附近,液面下的鎢線253因有保護層270緣故,此部分鎢線253不會接 觸到強鹼水溶液350,並不會有電化學反應,因此在整個奈米級針尖探針製作過程中,形狀並不會改變。如圖2I所示,當圖2H所示的12個第三鎢線253分離成12個固定於該金屬圓盤治具500的上鎢針281與12個沉入該強鹼水溶液350內的下鎢針283時,關閉該電源供應器210。下鎢針283在脫離上鎢針281的瞬間,因為下鎢針283沒有接電源供應器,不會再有電化學反應,因此所獲得的針尖2831是最尖的狀態。且下鎢針283在沉入該強鹼水溶液350內的過程中,因有保護層270緣故,不會造成下鎢針283具有奈米級針尖2831受損。圖2H乃繪示將一第三鎢線253***一第二通孔520內作例示說明,其餘的第三鎢線253乃同樣***如圖2H所示的其餘的第二通孔520內,在此不再贅述。 Next, as shown in FIG. 2H , a power supply 210 is provided, and the positive electrode of the power supply 210 is electrically connected to the metal disk tool 500, and a carbon rod is electrically connected to the negative electrode of the power supply 210. 240 is partially inserted into the first through hole 510 and fixed in the first through hole 510 of the metal disk tool 500 with an insulating material 540, such as but not limited to acrylic, and the carbon rod 240 is partially immersed The strong alkali aqueous solution 350, and then insert the third tungsten wires 253 into the second through holes 520 respectively, adjust the height of the third tungsten wires 520, so that each of the third tungsten wires The upper edge of the protective layer 270 at one end of 253 is lower than the distance h1 of the liquid surface of the strong alkali aqueous solution 350, h1 is for example but not limited to 0.5-1mm, and each of the third tungsten wires 253 is connected with one of them The screws 550 are fixed on the corresponding one of the second through holes 520 through one of the screw holes 530 . The screw 550 in this embodiment is, for example but not limited to, a thread diameter: M1.4 screw. Then, the electrochemical reaction is carried out under the condition that the output voltage of the power supply 210 is set to V to start the production of nano-scale needle tip probes, wherein the output voltage V of the power supply 210 is, for example but not limited to, between 2~10 volts between. The electrochemical reaction will only occur near the liquid surface between the tungsten wire 253 and the strong alkali aqueous solution 350, and the tungsten wire 253 under the liquid surface will not be connected to the tungsten wire 253 because of the protective layer 270. There will be no electrochemical reaction when it comes into contact with a strong alkaline aqueous solution 350, so the shape of the nanoscale needle-tip probe will not change during the entire fabrication process. As shown in FIG. 2I, when the 12 third tungsten wires 253 shown in FIG. 2H are separated into 12 upper tungsten needles 281 fixed on the metal disc jig 500 and 12 lower tungsten needles immersed in the strong alkali aqueous solution 350 When the tungsten needle 283 is turned off, the power supply 210 is turned off. When the lower tungsten needle 283 is detached from the upper tungsten needle 281, because the lower tungsten needle 283 is not connected to the power supply, there will be no electrochemical reaction, so the obtained needle tip 2831 is in the sharpest state. In addition, when the lower tungsten needle 283 sinks into the strong alkali aqueous solution 350 , due to the protection layer 270 , the nanoscale needle tip 2831 of the lower tungsten needle 283 will not be damaged. FIG. 2H shows that a third tungsten wire 253 is inserted into a second through hole 520 for illustration, and the remaining third tungsten wires 253 are similarly inserted into the remaining second through holes 520 as shown in FIG. 2H . This will not be repeated here.

最後,如圖2J所示取出沉入該強鹼水溶液350內的該等下鎢針,去除該等下鎢針283表面的該保護層270後,便可獲得如圖2K所示具有奈米級針尖2831的探針283。根據本實施例所製作好的下鎢針283經過電子顯微鏡確認其針尖2831直徑為10-100nm。針對不同製程尺寸的待分析樣品,可以選用具有適合奈米級針尖探針進行量測。本實施例去除該等下鎢針283表面的該保護層270之步驟,包括提供一丙酮溶劑;將該等2N個下鎢針浸入該丙酮溶劑內攪拌清洗15-30秒;以及將該等下鎢針283自該丙酮溶劑中取出,然後浸入一去離子水中,攪拌清洗5-10秒,將該等下鎢針283自該去離子水中取出後便可完成該等具奈米級針尖2831的探針283之製備。本實施例雖使用丙酮溶劑去除該等下鎢針283表面的該保護層270,惟根據本發明的其它實施例,也可視該保護層270之材質選擇其它適合的有機溶劑,在此不再贅述。 Finally, take out the lower tungsten needles immersed in the strong alkali aqueous solution 350 as shown in FIG. 2J , and remove the protective layer 270 on the surface of the lower tungsten needles 283, and then obtain nanometer-scale tungsten needles as shown in FIG. 2K . Tip 2831 of probe 283 . The lower tungsten needle 283 fabricated according to this embodiment is confirmed by an electron microscope that the diameter of the needle tip 2831 is 10-100 nm. For samples to be analyzed with different process sizes, a suitable nano-scale needle tip probe can be selected for measurement. In this embodiment, the step of removing the protective layer 270 on the surface of the lower tungsten needles 283 includes providing an acetone solvent; immersing the 2N lower tungsten needles in the acetone solvent and stirring and cleaning them for 15-30 seconds; The tungsten needles 283 are taken out from the acetone solvent, then immersed in a deionized water, stirred and cleaned for 5-10 seconds, and the lower tungsten needles 283 are taken out of the deionized water to complete the nanoscale needle tip 2831 Preparation of probe 283. Although this embodiment uses acetone solvent to remove the protective layer 270 on the surface of the lower tungsten needles 283, but according to other embodiments of the present invention, other suitable organic solvents can also be selected depending on the material of the protective layer 270, and will not be repeated here. .

如上所述,本實施例所揭示的大量製作奈米級針尖探針的方法,所獲得的探針針尖直徑為10-100nm,且所需設備簡便、操作簡單,無 須繁雜的電路設計與靈敏的電流計,製作過程中也無須人員時時確認,製程容易且可以大量製作,大幅改善現有製作奈米級針尖探針製程的所有缺點,使半導體量測所需要的奈米級針尖探針可以以更便宜的價格被大量提供。 As mentioned above, in the method for producing a large number of nano-scale needle-tip probes disclosed in this embodiment, the diameter of the obtained probe tip is 10-100nm, and the required equipment is simple and easy to operate, without Complicated circuit design and sensitive galvanometer are required, and there is no need for constant confirmation by personnel during the production process. The process is easy and can be mass-produced, which greatly improves all the shortcomings of the existing nano-scale needle-tip probe process, and enables semiconductor measurement. Nanoscale needle-tip probes are available in large quantities at a cheaper price.

雖然本發明已以實施例揭露如上,然其並非用以限定本發明,任何熟習此技藝者,在不脫離本發明之精神和範圍內,當可作各種之更動與潤飾,因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。 Although the present invention has been disclosed as above with the embodiments, it is not intended to limit the present invention. Anyone skilled in this art can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the protection of the present invention The scope shall be defined by the appended patent application scope.

210:電源供應器 210: Power supply

240:碳棒 240: carbon rod

270:保護層 270: protective layer

281:上鎢針 281: Upper tungsten needle

283:下鎢針 283: Lower tungsten needle

2831:下鎢針283的奈米級針尖 2831: The nanoscale tip of the lower tungsten needle 283

300:容器 300: container

350:強鹼水溶液 350: Aqueous solution of strong alkali

500:金屬圓盤治具 500: metal disc jig

510:第一通孔 510: the first through hole

520:第二通孔 520: the second through hole

530:螺絲孔 530: screw hole

540:絕緣材 540: insulating material

550:螺絲 550: screw

Claims (10)

一種大量製作奈米級針尖探針的方法,其步驟包括:提供2N個長度T1的第一鎢線,並以電化學方式去除該等2N個第一鎢線的表面氧化層,以獲得2N個第二鎢線,N為自然數,且T1>0;在該等2N個第二鎢線之一端表面形成一長度T2的保護層,以製備獲得2N個第三鎢線,T1>T2>0;提供一金屬圓盤治具,包括一位在該金屬圓盤治具中心處的第一通孔、2N個等距圍繞該第一通孔的第二通孔以及2N個螺絲孔,每一該等螺絲孔乃分別對應於其中一該等第二通孔,且每一該等螺絲孔乃自該金屬圓盤治具之圓周邊緣朝向其中一該等第二通孔貫穿,其中該第一通孔的直徑為R1,該第二通孔的直徑為R2,每一該等第二通孔之圓心與該第一通孔圓心之距離為R3,R1,R3>R2>0;提供一容器,該容器內盛一強鹼水溶液;將該金屬圓盤治具放置於該容器上方,然後將一碳棒***該第一通孔,並以一絕緣材固定於該金屬圓盤治具的該第一通孔內,使該碳棒浸入該強鹼水溶液內,並將該等2N個第三鎢線分別***該等第二通孔內,調整該等2N個第三鎢線的高度,使位在每一該等2N個第三鎢線的一端的該保護層的上緣低於該強鹼水溶液的液面h1之距離,h1>0且每一該等2N個第三鎢線並分別以其中一該等螺絲經由其中一該等螺絲孔固定於其所對應的其中一該等第二通孔上;提供一電源供應器,具有一正電極及一負電極,並以該正電極電性連接該金屬圓盤治具,以該負電極電性連接該碳棒,並於該電源供應器 的輸出電壓為V的條件下進行電化學反應以開始製作奈米級針尖探針,且當該等2N個第三鎢線分離成2N個固定於該金屬圓盤治具的上鎢針與2N個沉入該強鹼水溶液內的下鎢針時,關閉該電源供應器,2
Figure 110139826-A0305-02-0015-6
V
Figure 110139826-A0305-02-0015-8
10;以及取出沉入該強鹼水溶液內的該等2N個下鎢針,去除該等2N個下鎢針表面的該保護層後,便可完成2N個奈米級針尖探針之製備。
A method for producing a large number of nano-scale needle-tip probes, the steps comprising: providing 2N first tungsten wires with a length T1, and electrochemically removing the surface oxide layer of the 2N first tungsten wires to obtain 2N The second tungsten wire, N is a natural number, and T1>0; a protective layer with a length T2 is formed on the surface of one end of the 2N second tungsten wires to prepare 2N third tungsten wires, T1>T2>0 ; Provide a metal disc jig, including a first through hole at the center of the metal disc jig, 2N second through holes equidistant around the first through hole and 2N screw holes, each The screw holes correspond to one of the second through holes respectively, and each of the screw holes penetrates from the peripheral edge of the metal disc jig towards one of the second through holes, wherein the first The diameter of the through hole is R1, the diameter of the second through hole is R2, the distance between the center of each of the second through holes and the center of the first through hole is R3, R1, R3>R2>0; provide a container , the container contains a strong alkali aqueous solution; the metal disc jig is placed above the container, and then a carbon rod is inserted into the first through hole, and an insulating material is fixed to the metal disc jig In the first through hole, the carbon rod is immersed in the strong alkali aqueous solution, and the 2N third tungsten wires are respectively inserted into the second through holes, and the height of the 2N third tungsten wires is adjusted so that The upper edge of the protective layer at one end of each of the 2N third tungsten wires is lower than the liquid level h1 of the strong alkali aqueous solution, h1>0 and each of the 2N third tungsten wires is respectively Fix one of the screws to one of the corresponding second through holes through one of the screw holes; provide a power supply with a positive electrode and a negative electrode, and use the positive electrode to Connect the metal disc jig, connect the carbon rod electrically with the negative electrode, and perform an electrochemical reaction under the condition that the output voltage of the power supply is V to start making nano-scale needle tip probes, and when When the 2N third tungsten wires are separated into 2N upper tungsten needles fixed on the metal disk jig and 2N lower tungsten needles submerged in the strong alkali aqueous solution, turn off the power supply, 2
Figure 110139826-A0305-02-0015-6
V
Figure 110139826-A0305-02-0015-8
10; and taking out the 2N lower tungsten needles submerged in the strong alkali aqueous solution, and removing the protective layer on the surface of the 2N lower tungsten needles, the preparation of the 2N nanoscale tip probes can be completed.
如請求項1所述的方法,其中T1介於50-60mm。 The method according to claim 1, wherein T1 is between 50-60mm. 如請求項1所述的方法,其中N介於1至15。 The method according to claim 1, wherein N is between 1 and 15. 如請求項2所述的方法,其中T2為20mm。 The method as claimed in item 2, wherein T2 is 20mm. 如請求項2所述的方法,其中該金屬圓盤治具之直徑為120mm,厚度為10mm。 The method as claimed in item 2, wherein the diameter of the metal disk jig is 120mm, and the thickness is 10mm. 如請求項5所述的方法,其中R1為40mm,R2為1mm,R3介於50-55mm,該容器之直徑為100mm,且0.5mm
Figure 110139826-A0305-02-0015-17
h1
Figure 110139826-A0305-02-0015-19
1mm。
The method as described in claim 5, wherein R1 is 40mm, R2 is 1mm, R3 is between 50-55mm, the diameter of the container is 100mm, and 0.5mm
Figure 110139826-A0305-02-0015-17
h1
Figure 110139826-A0305-02-0015-19
1mm.
如請求項1所述的方法,其中該強鹼水溶液為濃度1-2M的氫氧化鉀水溶液或氫氧化鈉水溶液。 The method as claimed in claim 1, wherein the strong alkali aqueous solution is an aqueous potassium hydroxide solution or an aqueous sodium hydroxide solution with a concentration of 1-2M. 如請求項1所述的方法,其中該製備獲得2N個第三鎢線之步驟包括:提供一加熱的保護層溶液;將該等2N個第二鎢線部分垂直浸入該加熱的保護層溶液內,使位在被浸入該加熱的保護層溶液內之該等2N個第二鎢線的一端表面形成一長度T2保護層,完成該等2N個第三鎢線之製備。 The method as described in claim 1, wherein the step of preparing and obtaining 2N third tungsten wires comprises: providing a heated protective layer solution; immersing the 2N second tungsten wires vertically in the heated protective layer solution , forming a protective layer with a length T2 on one end surface of the 2N second tungsten wires immersed in the heated protective layer solution, and completing the preparation of the 2N third tungsten wires. 如請求項8所述的方法,其中該加熱的保護層溶液為溫度介於攝氏40-50度間的熔蠟或熱熔膠。 The method according to claim 8, wherein the heated protective layer solution is melted wax or hot melt adhesive at a temperature between 40-50 degrees Celsius. 如請求項9所述的方法,其中該去除該等下鎢針表面的該保護層的步驟包括:提供一丙酮溶劑;將該等2N個下鎢針浸入該丙酮溶劑內攪拌清洗15-30秒;以及將該等2N個下鎢針自該丙酮溶劑中取出,然後浸入一去離子水中,攪拌清洗5-10秒,將該等2N個下鎢針自該去離子水中取出後便可完成2N個奈米級針尖探針之製備。 The method as described in claim item 9, wherein the step of removing the protective layer on the surface of the lower tungsten needles comprises: providing an acetone solvent; immersing the 2N lower tungsten needles in the acetone solvent and stirring and cleaning for 15-30 seconds and taking out the 2N lower tungsten needles from the acetone solvent, then immersing them in deionized water, stirring and cleaning them for 5-10 seconds, and taking out the 2N lower tungsten needles from the deionized water to complete the 2N Preparation of a nanoscale needle-tip probe.
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TW200611996A (en) * 2004-10-07 2006-04-16 Academia Sinica Single-atom sharp atomic tip and preparation method thereof
US20120186998A1 (en) * 2006-09-25 2012-07-26 Andre Hermans Microelectrode, Microelectrode formation, and methods of utilizing microelectrodes for charaterizing properties of localized environments and substrates
US20140033374A1 (en) * 2012-07-27 2014-01-30 Academia Sinica System for fabricating nanoscale probe and method thereof
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