CN102810462A - A kind of preparation method of semiconductor rectifier device with large breakdown voltage - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 230000003647 oxidation Effects 0.000 claims abstract description 10
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 10
- 239000002071 nanotube Substances 0.000 claims description 34
- 239000010936 titanium Substances 0.000 claims description 23
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 20
- 229910052719 titanium Inorganic materials 0.000 claims description 20
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 18
- 229910052782 aluminium Inorganic materials 0.000 claims description 18
- 239000002131 composite material Substances 0.000 claims description 17
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 14
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 8
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 8
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 8
- 238000003491 array Methods 0.000 claims description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 6
- 229960003280 cupric chloride Drugs 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- DPZKMHVEGIUXGE-UHFFFAOYSA-N [NH4+].[F-].OCCO Chemical compound [NH4+].[F-].OCCO DPZKMHVEGIUXGE-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 6
- 239000004408 titanium dioxide Substances 0.000 abstract 3
- 239000008367 deionised water Substances 0.000 abstract 2
- 229910021641 deionized water Inorganic materials 0.000 abstract 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract 1
- 238000000137 annealing Methods 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 abstract 1
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 abstract 1
- 229940056932 lead sulfide Drugs 0.000 abstract 1
- 229910052981 lead sulfide Inorganic materials 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 229910052979 sodium sulfide Inorganic materials 0.000 abstract 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 abstract 1
- 239000011593 sulfur Substances 0.000 abstract 1
- 229910052717 sulfur Inorganic materials 0.000 abstract 1
- 238000000576 coating method Methods 0.000 description 10
- 239000011248 coating agent Substances 0.000 description 9
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 238000003917 TEM image Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 2
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- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 1
- 241000973497 Siphonognathus argyrophanes Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 1
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Abstract
Description
技术领域 technical field
本发明涉及半导体整流器件的制备，特别是一种具有明显整流效应、大击穿电压的半导体整流器件制备方法。The invention relates to the preparation of a semiconductor rectifying device, in particular to a method for preparing a semiconductor rectifying device with obvious rectifying effect and large breakdown voltage.
背景技术 Background technique
具有整流效应的半导体整流器件是许多重要半导体器件的核心，利用其可制备二极管、太阳电池、场效应晶体管、太阳电池、激光器等众多器件。正向开启电压、反向击穿电压和反向电流是半导体整流器件的重要参数，对于设计不同功率、不同用途的半导体器件尤为重要。其中，外加反向电压超过某一数值时，反向电流会突然增大，这种现象称为电击穿。引起电击穿的临界电压称为半导体整流器反向击穿电压。电击穿时半导体整流器失去单向导电性。如果半导体整流器没有因电击穿而引起过热，则单向导电性不一定会被永久破坏，在撤除外加电压后，其性能仍可恢复，否则半导体整流器就损坏了，因而使用时应避免半导体整流器外加的反向电压过高。如果半导体整流器不能承受高的反向电压，不仅会影响其在半导体器件中的应用，而且会影响其寿命。The semiconductor rectifier device with rectification effect is the core of many important semiconductor devices, which can be used to prepare many devices such as diodes, solar cells, field effect transistors, solar cells, and lasers. Forward turn-on voltage, reverse breakdown voltage and reverse current are important parameters of semiconductor rectifier devices, which are especially important for designing semiconductor devices with different power and different uses. Among them, when the applied reverse voltage exceeds a certain value, the reverse current will suddenly increase. This phenomenon is called electrical breakdown. The critical voltage that causes electrical breakdown is called the reverse breakdown voltage of the semiconductor rectifier. Semiconductor rectifiers lose unidirectional conductivity during electrical breakdown. If the semiconductor rectifier is not overheated due to electrical breakdown, the unidirectional conductivity may not be permanently damaged, and its performance can still be restored after the external voltage is removed, otherwise the semiconductor rectifier will be damaged, so semiconductor rectifiers should be avoided when using The applied reverse voltage is too high. If the semiconductor rectifier cannot withstand high reverse voltage, it will not only affect its application in semiconductor devices, but also affect its life.
发明内容 Contents of the invention
鉴于现有技术的以上缺点，本发明的目的是提供一种具有大击穿电压的半导体整流器件的制备方法，以进一步提高二半导体整流器在电子、电工中的实用化性能。In view of the above shortcomings of the prior art, the object of the present invention is to provide a method for preparing a semiconductor rectifier device with a large breakdown voltage, so as to further improve the practical performance of the semiconductor rectifier in electronics and electrical engineering.
本发明的目的是通过如下的手段实现的。The object of the present invention is achieved by the following means.
一种具有大击穿电压的半导体整流器件的制备方法，利用窄带半导体对TiO2纳米管阵列进行修饰，包括以下步骤：A method for preparing a semiconductor rectifier device with a large breakdown voltage, using a narrow-band semiconductor to modify the TiO nanotube array, comprising the following steps:
A)阳极氧化法制备TiO2纳米管阵列A) Preparation of TiO2 nanotube arrays by anodic oxidation
将铂片作为阴极、钛片(1cm宽×3cm长)作为阳极，将钛片沿长边方向2cm(露1cm钛片在液面上以留作电极)浸入在0.25％wt(即重量百分比为0.25％)氟化铵的乙二醇溶液中进行阳极氧化，电压为55v，氧化时间13小时，即在钛片表面生长出TiO2纳米管阵列。Platinum sheet is used as cathode, titanium sheet (1cm wide * 3cm long) is used as anode, titanium sheet is immersed in 0.25%wt (that is, weight percentage is 0.25%) ammonium fluoride in ethylene glycol solution for anodic oxidation, the voltage is 55v, and the oxidation time is 13 hours, that is, TiO2 nanotube arrays grow on the surface of the titanium sheet.
B)水热合成CuS/TiO2纳米管阵列复合材料B) Hydrothermal synthesis of CuS/TiO nanotube array composites
将A步骤生长有TiO2纳米管阵列的钛片放入装有氯化铜和硫代硫酸钠的混合溶液中，混合溶液的氯化铜和硫代硫酸钠的摩尔浓度相同，浓度均为0.005-0.02mol/L；用高压釜封好后，放入炉中加温，时间为17小时，温度为100℃。Put the titanium sheet with TiO2 nanotube array grown in step A into the mixed solution containing copper chloride and sodium thiosulfate, the molar concentration of copper chloride and sodium thiosulfate in the mixed solution is the same, the concentration is 0.005 -0.02mol/L; After sealing with an autoclave, put it into a furnace to heat for 17 hours at a temperature of 100°C.
C)制作条形铝电极C) Making strip aluminum electrodes
在CuS/TiO2纳米管阵列复合材料表面蒸镀铝电极，铝电极垂直于钛片的长边，蒸镀时真空度为5-10-4pa，铝电极的厚度为100nm，宽度为3mm，长度即钛片的宽度10mm，铝电极之间间隔2mm。以铝电极为正极，裸露的钛基底为负极，整个体系即构成具有大击穿电压的半导体整流器件。Evaporate aluminum electrodes on the surface of the CuS/ TiO2 nanotube array composite material. The aluminum electrodes are perpendicular to the long side of the titanium sheet. The vacuum degree during evaporation is 5-10-4 Pa. The thickness of the aluminum electrodes is 100nm and the width is 3mm. The length, that is, the width of the titanium sheet is 10mm, and the interval between the aluminum electrodes is 2mm. With the aluminum electrode as the positive electrode and the exposed titanium substrate as the negative electrode, the whole system constitutes a semiconductor rectifier device with a large breakdown voltage.
采用本发明的具有大击穿电压的半导体整流器件，可广泛应用于二极管、太阳电池、场效应晶体管、太阳电池、激光器等众多半导体电子器件。The semiconductor rectifying device with large breakdown voltage of the present invention can be widely used in many semiconductor electronic devices such as diodes, solar cells, field effect transistors, solar cells, and lasers.
附图说明 Description of drawings
图1、CuS/TiO2纳米管阵列复合材料正面SEM图像。Figure 1. Front SEM images of CuS/TiO 2 nanotube array composites.
图2、CuS/TiO2纳米管阵列复合材料断面SEM图像。Figure 2. SEM images of the cross-section of the CuS/TiO 2 nanotube array composite.
图3、CuS/TiO2纳米管阵列复合材料TEM图像。Figure 3. TEM images of CuS/TiO 2 nanotube array composites.
图4、CuS/TiO2纳米管阵列复合材料XRD图像。Figure 4. XRD image of CuS/TiO 2 nanotube array composite.
图5、CuS/TiO2纳米管阵列复合材料TEM图像。Figure 5. TEM images of CuS/TiO 2 nanotube array composites.
图6、Ti/CuS/TiO2纳米管阵列复合材料/Al半导体整流器件的I-V曲线图。Figure 6. IV curve of Ti/CuS/TiO 2 nanotube array composite/Al semiconductor rectifier device.
具体实施方式 Detailed ways
以下结合实施例对本发明作进一步的说明。The present invention will be further described below in conjunction with embodiment.
实施例一Embodiment one
A)阳极氧化法制备TiO2纳米管阵列A) Preparation of TiO2 nanotube arrays by anodic oxidation
将铂片作为阴极、钛片(1cm宽×3cm长)作为阳极，将钛片沿长边方向2cm(露1cm钛片在液面上以留作电极)浸入在0.25％wt(即重量百分比为0.25％)氟化铵的乙二醇溶液中进行阳极氧化，电压为55v，氧化时间13小时，即在钛片表面生长出TiO2纳米管阵列。Platinum sheet is used as cathode, titanium sheet (1cm wide * 3cm long) is used as anode, titanium sheet is immersed in 0.25%wt (that is, weight percentage is 0.25%) ammonium fluoride in ethylene glycol solution for anodic oxidation, the voltage is 55v, and the oxidation time is 13 hours, that is, TiO2 nanotube arrays grow on the surface of the titanium sheet.
B)水热合成CuS/TiO2纳米管阵列复合材料B) Hydrothermal synthesis of CuS/TiO nanotube array composites
将A步骤生长有TiO2纳米管阵列的钛片放入装有氯化铜和硫代硫酸钠的混合溶液中，混合溶液的氯化铜和硫代硫酸钠的摩尔浓度相同，浓度均为0.005mol/L；用高压釜封好后，放入炉中加温，时间为17小时，温度为100℃。Put the titanium sheet with TiO2 nanotube array grown in step A into the mixed solution containing copper chloride and sodium thiosulfate, the molar concentration of copper chloride and sodium thiosulfate in the mixed solution is the same, the concentration is 0.005 mol/L; After sealing with an autoclave, put it into a furnace to heat for 17 hours at a temperature of 100°C.
C)制作条形铝电极C) Making strip aluminum electrodes
在CuS/TiO2纳米管阵列复合材料表面蒸镀铝电极，铝电极垂直于钛片的长边，蒸镀时真空度为5-10-4pa，铝电极的厚度为100nm，宽度为3mm，长度即钛片的宽度10mm，铝电极之间间隔2mm。以铝电极为正极，裸露的钛基底为负极，整个体系即构成具有大击穿电压的半导体整流器件。Evaporate aluminum electrodes on the surface of the CuS/ TiO2 nanotube array composite material. The aluminum electrodes are perpendicular to the long side of the titanium sheet. The vacuum degree during evaporation is 5-10-4 Pa. The thickness of the aluminum electrodes is 100nm and the width is 3mm. The length, that is, the width of the titanium sheet is 10mm, and the interval between the aluminum electrodes is 2mm. With the aluminum electrode as the positive electrode and the exposed titanium substrate as the negative electrode, the whole system constitutes a semiconductor rectifier device with a large breakdown voltage.
从图1可以看出CuS/TiO2纳米管阵列复合材料保持了原有的管状结构，纳米管管壁被一层纳米颗粒包覆，纳米颗粒的尺寸在20nm左右，管壁厚度增加为150nm，管内径(d2)减小到90nm，外径(D2)约为370nm。如图2所示为复合产物经超声剥离后的剖面图，从图中可以看出纳米颗粒对管口及距管口200-600nm范围内的管外壁形成了包覆，管口处纳米粒子对管壁包覆程度最大，远离管口的距离越远，管外壁的包覆程度越低，基本只有单层纳米粒子的吸附，同时从破损的纳米管可以看出管内壁未见纳米粒子填充。从图2可见超声后部分TiO2纳米管裸露出了管口，表面光滑，其管壁厚度为15-20nm，内径(d1)约为160nm，外径(D1)约为200nm；因此可以从几何关系推断CuS纳米颗粒在管口内外壁包覆的厚度，沿管内壁包覆的厚度为(d1-d2)/2，即35nm左右，沿管外壁包覆的厚度为(D2-D1)/2，即85nm左右，两者之和加上TiO2纳米管自身的管壁厚度(20nm)为140nm，与直接测量的复合后管口处管壁的厚度150nm接近。通过扫描只能大致判断出纳米管口内外壁的包覆情况，而不能得出沿纳米管口向外纳米粒子的包覆厚度。如图3所示的TEM图可见纳米管口处有明显的纳米粒子包覆，沿管口处向外的包覆厚度约为45nm，同时可以看出管内部及远离管口的管外壁没有纳米粒子存在，与从扫描图得出的结论一致。It can be seen from Figure 1 that the CuS/TiO 2 nanotube array composite maintains the original tubular structure, and the nanotube wall is covered by a layer of nanoparticles. The size of the nanoparticles is about 20nm, and the thickness of the tube wall increases to 150nm. The inner diameter (d2) of the tube is reduced to 90nm and the outer diameter (D2) is about 370nm. As shown in Figure 2, it is a cross-sectional view of the composite product after ultrasonic peeling. From the figure, it can be seen that the nanoparticles have formed a coating on the outer wall of the pipe mouth and the pipe mouth in the range of 200-600nm away from the pipe mouth. The degree of coating of the tube wall is the largest, and the farther away from the nozzle, the lower the coating degree of the outer wall of the tube. Basically, only a single layer of nanoparticles is adsorbed. At the same time, it can be seen from the damaged nanotubes that the inner wall of the tube is not filled with nanoparticles. It can be seen from Fig. 2 that part of the TiO 2 nanotube has exposed the mouth of the tube after the ultrasonic wave, the surface is smooth, the thickness of the tube wall is 15-20nm, the inner diameter (d 1 ) is about 160nm, and the outer diameter (D 1 ) is about 200nm; therefore, it can be The thickness of the coating of CuS nanoparticles on the inner and outer walls of the tube mouth is inferred from the geometric relationship. The thickness of the coating along the inner wall of the tube is (d 1 -d 2 )/2, which is about 35nm, and the thickness of the coating along the outer wall of the tube is (D 2 - D 1 )/2, which is about 85nm, the sum of the two plus the wall thickness (20nm) of the TiO 2 nanotube itself is 140nm, which is close to the 150nm thickness of the tube wall at the mouth of the composite tube after direct measurement. The coating of the inner and outer walls of the nanotube mouth can only be roughly judged by scanning, but the coating thickness of the nanoparticles along the nanotube mouth outward can not be obtained. The TEM image shown in Figure 3 shows that there are obvious coatings of nanoparticles at the mouth of the nanotube, and the thickness of the coating along the mouth of the tube is about 45nm. Particles are present, consistent with conclusions drawn from the scans.
如图4所示的X射线衍射谱表明除了Ti基底和锐钛矿型TiO2的衍射峰外，其余衍射峰与CuS(JCPDS No.06-0464)对应，说明覆盖在TiO2纳米管管壁上是CuS纳米粒子[9]，两者结合形成了CuS/TiO2纳米管复合材料。The X-ray diffraction spectrum shown in Figure 4 shows that except for the diffraction peaks of the Ti substrate and anatase TiO 2 , the rest of the diffraction peaks correspond to CuS (JCPDS No.06-0464), indicating that the TiO 2 nanotube wall is covered Above are CuS nanoparticles [9] , and the combination of the two forms CuS/TiO 2 nanotube composites.
图5所示Ti/CuS/TiO2纳米管阵列复合材料/Al半导体整流器件的I-V曲线图，由图可见其正向导通电压约为3.5V，反向击穿电压高于15V，说明CuS/TiO2之间的界面电场较强。The IV curve diagram of Ti/CuS/ TiO2 nanotube array composite material/Al semiconductor rectifier device shown in Figure 5, it can be seen from the figure that its forward conduction voltage is about 3.5V, and its reverse breakdown voltage is higher than 15V, indicating that CuS/ The interfacial electric field between TiO2 is stronger.
图6所示改变CuCl2浓度后得到的器件的整流曲线，同样可见明显的整流效应，反向电压仍然很大。As shown in Figure 6, the rectification curve of the device obtained after changing the concentration of CuCl 2 can also be seen to have an obvious rectification effect, and the reverse voltage is still very large.
采用本发明的基本方法，在实际实施中，工艺条件还可作一些变化，比如混合溶液的氯化铜和硫代硫酸钠的摩尔浓度相同，浓度均为0.005-0.02mol/L的范围内，均能获得良好的效果。Adopt basic method of the present invention, in actual implementation, technological condition also can make some changes, the molar concentration of the cupric chloride such as mixed solution and sodium thiosulfate is identical, and concentration is in the scope of 0.005-0.02mol/L, Good results can be obtained.
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