氮化硼的半导体特性和紫外光电探测器的基础研究
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摘要
氮化硼（BN）材料具有立方氮化硼（cBN）、六方氮化硼（hBN）、三方氮化硼（rBN）、纤维锌矿结构氮化硼（wBN）四种晶体结构，其中cBN和hBN因其宽的禁带宽度、优异的物化性质和半导体性质备受研究者们的关注。它们在微电子及光电子器件等方面具有广泛的应用前景。目前研究的重点主要是制备高质量的BN单晶及薄膜材料，器件方面的研究较少，特别是对BN深紫外光电探测器的研究还处于起步阶段。本文主要对cBN的表面极性、掺杂特性、金半接触特性、BN薄膜的制备和性质、以及BN紫外光电探测器的设计和模拟等进行了一系列基础研究，取得的主要研究结果如下：
（1）cBN单晶表面极性研究
根据所用cBN单晶样品具有颜色分区的特性，发现了一种利用显微镜观察即可区分cBN晶体{111}B面和{111}N面的方法。{111}N面的生长扇区聚集很多缺陷和杂质，成为色心，呈现琥珀色，而{111}B生长扇区的缺陷和杂质很少，因而是无色透明的。与{111}B面相比，{111}N面具有更快的腐蚀速度和更大的表面漏电流，其Raman光谱也因为杂质和缺陷的扰动而表现出无序活性的Raman散射（disorder-activated Raman scattering，DARS）现象。研究结果均表明{111}B面具有更好的晶体完整性和化学稳定性。
（2）cBN晶体的掺杂研究
采用高温热扩散工艺对cBN晶体进行了Si掺杂研究。典型的掺杂温度为850—950℃，掺杂时间为4—5h。XPS谱分析表明晶体表层的Si含量可达2.7%以上。Si主要占据B位，成为替位式施主杂质。测量了掺杂后的cBN样品的杂质激活能，激活能普遍大于0.4eV，因而Si杂质室温下很难电离，掺杂后的cBN样品依然具有较高的电阻率，其I-V特性曲线符合空间电荷限制电流模型。可以通过控制掺杂时间和掺杂温度来控制杂质的浓度和电离能。掺杂时间越长、掺杂温度越高，杂质电离能越低。
（3）cBN晶体的金半接触特性研究
采用真空蒸镀的方法在cBN样品上制作了Au、Al电极，采用磁控溅射方法在cBN样品上制作了Cr、Ti等电极，研究了这些金属电极以及金浆、银浆与cBN样品的接触类型。结果表明Au、金浆和银浆可与cBN晶体形成欧姆接触，而Al、Cr、Ti与cBN单晶的接触为肖特基接触。对Cr/Au金属电极分别在450℃、900℃退火20分钟，金属与cBN单晶间的接触质量得到了改善。
（4）BN薄膜制备及表征
采用射频磁控溅射方法，在N型Si衬底和石英玻璃衬底上制备了BN薄膜，采用FTIR、UV-Via谱等对薄膜进行了表征。FTIR谱结果表明在Ar/N2=4:1时，BN薄膜生长速率最快；Ar/N2=1:1时，得到了六方相含量为80%以上的薄膜，此薄膜的光学带隙为5.8eV，185nm处吸收系数为40000cm-1。但是此BN薄膜不稳定，暴露在潮湿的空气中最终会转化为硼酸晶体，导致薄膜碎裂和脱落。为了得到稳定的宽带隙薄膜，在BN薄膜生长过程中引入了Fe元素，制备出Fe-B-N-O薄膜，XPS结果表明薄膜主要包含Fe-N-O、B-N-O和Fe-O等化学键。在溅射功率150W、衬底温度300℃、溅射时间120min，纯氩气条件下得到的Fe-B-N-O薄膜在可见光区具有良好的透光性，光学带隙为5.32eV，185nm处吸收系数达到100000cm-1，并且与N型Si衬底形成的异质结构具有良好的整流特性，整流比达到103量级。Fe-B-N-O薄膜结构稳定，与衬底结合稳固，在紫外光区有很强的的吸收，适用于紫外光电探测器的制作。
（5）cBN紫外光电探测器的设计与模拟研究
建立了cBN材料的参数库及器件模拟的物理模型，研究了掺杂浓度、电极结构对cBN紫外光电探测器性能的影响。模拟结果显示在外加电压小于5V的较低电压下，材料掺杂浓度为1013cm-3的器件有较高的光响应；而电压大于5V时，掺杂浓度为1014cm-3器件的光响应率更高。电极宽度3μm、电极间距为10μm的器件具有低的暗电流和高的光、暗电流比。对于电极宽度和电极间距相等的器件，随着电极尺寸的增加光电流的变化不大，而暗电流在迅速降低。
利用蒸镀、溅射和光刻技术分别制备了两种具有MSM交叉指状电极结构的cBN紫外探测器原型器件，一种是以Au为电极，为光电导器件，另一种以Cr为电极，为光伏型器件。以30W氘灯为光源，测量了两种cBN探测器件的紫外光电响应，前者的光电流与暗电流比为2~3，而后者的光电流与暗电流比值达到56，与模拟结果一致。由于cBN单晶含有较多缺陷和深能级杂质，cBN单晶紫外探测器的性能有待进一步改善。
Boron nitride is a poly-phase system of different stacking/layered structure:hexagonal boron nitride (hBN)，cubic boron nitride (cBN)，wurtzitic boron nitride(wBN) and rhombohedral boron nitride (rBN). cBN and hBN attracted researcher’sattention because of their excellent physicochemical properties, semiconductorproperties and wide bandgap. They have broad potential applications in the fields ofmicroelectronic and optoelectronic devices. At present, the major research is focusedon the preparation of high quality BN single crystals and thin films. Less attention ispaid to devices, especially to the BN based deep ultraviolet (UV) photodetectors. Inthis dissertation, primary studies on the surface polarity, doping, metal-semiconductorcontact of cBN, preparation and property of BN thin films, and design and simulationof BN based UV photodetectors, etc. were carried out. The main research results arelisted as follow:
(1) The studies of the surface polarity of cBN single crystals. According tothe truth that cBN crystal samples have obvious color zoning, a simple method ofdistinguishing {111}B and {111}N faces by microscopy was found. The defectsand impurities incorporate in {111}N sectors serving as the amber color centers,while very little defects and impurities exist in {111}B sectors, so {111}B sectorsare colorless. Compared with {111}B faces,{111}N faces have faster etch rateand larger surface leakage current, and the disorder-activated Raman scatteringhappens in {111}N faces because of the high density of defects and impurities. Allresults indicate that {111}B faces have better crystalline and chemical stability.
(2) The studies of doping cBN crystals. Si was doped into cBN crystals bythermal diffusion at high temperature. The typical doping temperature is850~950℃，and the doping time is about4~5hours. XPS analysis indicated that the content of Siimpurity at the surface layer of cBN samples was more than2.7%. Si mainly occupiedB lattices and became substitutional donor impurities. The measured activation energyof doped cBN samples were larger than0.4eV, so it was difficult for Si impurities tobe ionized at room temperature, and the doped cBN samples still had very high resistivity and the mechanism of space charge limited current. The activation energyand density of Si impurity can be controlled by the doping time and temperature. Thelonger the doping time is, or the higher the doping temperature is, the lower theactivation energy becomes.
(3) The studies of metal-semiconductor contact of cBN crystals. Au and Alelectrodes were evaporated on the cBN samples in vacuum. Cr and Ti electrodes weredeposited on the cBN samples by RF magnetron sputtering. The contact properties ofthese metal electrodes, as well as Au pastes and Ag pastes, with cBN samples wereinvestigated. The results revealed that Al, Cr, Ti can formed Schottky contacts withcBN crystals, and Au, Au paste or Ag paste were able to form the ohmic contacts withcBN. After vacuum annealing at450℃and900℃for20minutes respectively, thecontact quality of Cr/Au with cBN was improved.
(4) The preparation and characterization of BN films. BN films weredeposited on the substrates of N-type Si and quartz glass by using RF magnetronsputtering, and were characterized by FTIR, UV-Via spectra etc. FTIR resultsrevealed that the fastest growth rate of BN films obtained when Ar:N2was4:1. WhenAr:N2was1:1, the BN films including more than80%hBN phase were attained. Theoptical bandgap of this film was about5.8eV, and the absorption factor was40000cm-1at185nm. However, this BN film was unstable and could become intoboric acid in moist air, which will make the films break and separate from thesubstrate. In order to obtain the stable film with wide bandgap, Fe was added in thegrowth process of BN films, and FeBNO films were achieved. XPS results showedthat the FeBNO films mainly included Fe-N-O, B-N-O, and Fe-O etc. chemical bonds.The FeBNO films were deposited for120minutes with the sputtering power of150W,the substrate temperature of300℃in pure argon atmosphere. The FeBNO films weretransparent for the visible light, and the optical bandgap and the absorption factors ofthe films were5.32eV and100000cm-1at185nm respectively. Moreover, theheterojunction between the FeBNO films and N-type Si substrate had goodrectification characteristics, the rectification ratio reached103. The FeBNO films arevery stable, tightly bond with the substrate, and have very strong absorption in UVregion, therefore, they are suitable to manufacture the UV photodetectors.
(5) The design and simulation of cBN UV photodetectors. A parameter libraryof cBN single crystal and a model of a cBN MSM UV photodetector are established with the simulation package Atlas. The simulation results showed that under less than5V voltage, the UV detector with doping concentration of1013cm-3had highresponsibility. When the voltage was greater than5V, the photodetector with dopingconcentration of1014cm-3have higher responsibility. The device with3μm electrodewidth and10μm electrode spacing had the lowest dark current and the highest ratioof photocurrent to dark current. As for the devices with the same electrode width andspacing, the dark current reduced rapidly with the increase of the size of electrodes,but the photocurrent was almost the constant.
Two kinds of MSM cBN UV photodetectors with interdigitated finger electrodeswere fabricated by evaporation, sputtered and lithography. One was thephotoconductive device with Au electrodes, and the other was photovoltaic devicewith Cr electrodes. The dark currents and UV photoresponses of the two devices weremeasured. The ratio of photocurrent to dark current the former was only2-3, as forthe latter, the ratio reached56, which was in accordance with the simulation. Becauseof the bad quality of cBN crystals, the performances of cBN UV photodetectors needto be improved further.
（1）cBN单晶表面极性研究
根据所用cBN单晶样品具有颜色分区的特性，发现了一种利用显微镜观察即可区分cBN晶体{111}B面和{111}N面的方法。{111}N面的生长扇区聚集很多缺陷和杂质，成为色心，呈现琥珀色，而{111}B生长扇区的缺陷和杂质很少，因而是无色透明的。与{111}B面相比，{111}N面具有更快的腐蚀速度和更大的表面漏电流，其Raman光谱也因为杂质和缺陷的扰动而表现出无序活性的Raman散射（disorder-activated Raman scattering，DARS）现象。研究结果均表明{111}B面具有更好的晶体完整性和化学稳定性。
（2）cBN晶体的掺杂研究
采用高温热扩散工艺对cBN晶体进行了Si掺杂研究。典型的掺杂温度为850—950℃，掺杂时间为4—5h。XPS谱分析表明晶体表层的Si含量可达2.7%以上。Si主要占据B位，成为替位式施主杂质。测量了掺杂后的cBN样品的杂质激活能，激活能普遍大于0.4eV，因而Si杂质室温下很难电离，掺杂后的cBN样品依然具有较高的电阻率，其I-V特性曲线符合空间电荷限制电流模型。可以通过控制掺杂时间和掺杂温度来控制杂质的浓度和电离能。掺杂时间越长、掺杂温度越高，杂质电离能越低。
（3）cBN晶体的金半接触特性研究
采用真空蒸镀的方法在cBN样品上制作了Au、Al电极，采用磁控溅射方法在cBN样品上制作了Cr、Ti等电极，研究了这些金属电极以及金浆、银浆与cBN样品的接触类型。结果表明Au、金浆和银浆可与cBN晶体形成欧姆接触，而Al、Cr、Ti与cBN单晶的接触为肖特基接触。对Cr/Au金属电极分别在450℃、900℃退火20分钟，金属与cBN单晶间的接触质量得到了改善。
（4）BN薄膜制备及表征
采用射频磁控溅射方法，在N型Si衬底和石英玻璃衬底上制备了BN薄膜，采用FTIR、UV-Via谱等对薄膜进行了表征。FTIR谱结果表明在Ar/N2=4:1时，BN薄膜生长速率最快；Ar/N2=1:1时，得到了六方相含量为80%以上的薄膜，此薄膜的光学带隙为5.8eV，185nm处吸收系数为40000cm-1。但是此BN薄膜不稳定，暴露在潮湿的空气中最终会转化为硼酸晶体，导致薄膜碎裂和脱落。为了得到稳定的宽带隙薄膜，在BN薄膜生长过程中引入了Fe元素，制备出Fe-B-N-O薄膜，XPS结果表明薄膜主要包含Fe-N-O、B-N-O和Fe-O等化学键。在溅射功率150W、衬底温度300℃、溅射时间120min，纯氩气条件下得到的Fe-B-N-O薄膜在可见光区具有良好的透光性，光学带隙为5.32eV，185nm处吸收系数达到100000cm-1，并且与N型Si衬底形成的异质结构具有良好的整流特性，整流比达到103量级。Fe-B-N-O薄膜结构稳定，与衬底结合稳固，在紫外光区有很强的的吸收，适用于紫外光电探测器的制作。
（5）cBN紫外光电探测器的设计与模拟研究
建立了cBN材料的参数库及器件模拟的物理模型，研究了掺杂浓度、电极结构对cBN紫外光电探测器性能的影响。模拟结果显示在外加电压小于5V的较低电压下，材料掺杂浓度为1013cm-3的器件有较高的光响应；而电压大于5V时，掺杂浓度为1014cm-3器件的光响应率更高。电极宽度3μm、电极间距为10μm的器件具有低的暗电流和高的光、暗电流比。对于电极宽度和电极间距相等的器件，随着电极尺寸的增加光电流的变化不大，而暗电流在迅速降低。
利用蒸镀、溅射和光刻技术分别制备了两种具有MSM交叉指状电极结构的cBN紫外探测器原型器件，一种是以Au为电极，为光电导器件，另一种以Cr为电极，为光伏型器件。以30W氘灯为光源，测量了两种cBN探测器件的紫外光电响应，前者的光电流与暗电流比为2~3，而后者的光电流与暗电流比值达到56，与模拟结果一致。由于cBN单晶含有较多缺陷和深能级杂质，cBN单晶紫外探测器的性能有待进一步改善。
Boron nitride is a poly-phase system of different stacking/layered structure:hexagonal boron nitride (hBN)，cubic boron nitride (cBN)，wurtzitic boron nitride(wBN) and rhombohedral boron nitride (rBN). cBN and hBN attracted researcher’sattention because of their excellent physicochemical properties, semiconductorproperties and wide bandgap. They have broad potential applications in the fields ofmicroelectronic and optoelectronic devices. At present, the major research is focusedon the preparation of high quality BN single crystals and thin films. Less attention ispaid to devices, especially to the BN based deep ultraviolet (UV) photodetectors. Inthis dissertation, primary studies on the surface polarity, doping, metal-semiconductorcontact of cBN, preparation and property of BN thin films, and design and simulationof BN based UV photodetectors, etc. were carried out. The main research results arelisted as follow:
(1) The studies of the surface polarity of cBN single crystals. According tothe truth that cBN crystal samples have obvious color zoning, a simple method ofdistinguishing {111}B and {111}N faces by microscopy was found. The defectsand impurities incorporate in {111}N sectors serving as the amber color centers,while very little defects and impurities exist in {111}B sectors, so {111}B sectorsare colorless. Compared with {111}B faces,{111}N faces have faster etch rateand larger surface leakage current, and the disorder-activated Raman scatteringhappens in {111}N faces because of the high density of defects and impurities. Allresults indicate that {111}B faces have better crystalline and chemical stability.
(2) The studies of doping cBN crystals. Si was doped into cBN crystals bythermal diffusion at high temperature. The typical doping temperature is850~950℃，and the doping time is about4~5hours. XPS analysis indicated that the content of Siimpurity at the surface layer of cBN samples was more than2.7%. Si mainly occupiedB lattices and became substitutional donor impurities. The measured activation energyof doped cBN samples were larger than0.4eV, so it was difficult for Si impurities tobe ionized at room temperature, and the doped cBN samples still had very high resistivity and the mechanism of space charge limited current. The activation energyand density of Si impurity can be controlled by the doping time and temperature. Thelonger the doping time is, or the higher the doping temperature is, the lower theactivation energy becomes.
(3) The studies of metal-semiconductor contact of cBN crystals. Au and Alelectrodes were evaporated on the cBN samples in vacuum. Cr and Ti electrodes weredeposited on the cBN samples by RF magnetron sputtering. The contact properties ofthese metal electrodes, as well as Au pastes and Ag pastes, with cBN samples wereinvestigated. The results revealed that Al, Cr, Ti can formed Schottky contacts withcBN crystals, and Au, Au paste or Ag paste were able to form the ohmic contacts withcBN. After vacuum annealing at450℃and900℃for20minutes respectively, thecontact quality of Cr/Au with cBN was improved.
(4) The preparation and characterization of BN films. BN films weredeposited on the substrates of N-type Si and quartz glass by using RF magnetronsputtering, and were characterized by FTIR, UV-Via spectra etc. FTIR resultsrevealed that the fastest growth rate of BN films obtained when Ar:N2was4:1. WhenAr:N2was1:1, the BN films including more than80%hBN phase were attained. Theoptical bandgap of this film was about5.8eV, and the absorption factor was40000cm-1at185nm. However, this BN film was unstable and could become intoboric acid in moist air, which will make the films break and separate from thesubstrate. In order to obtain the stable film with wide bandgap, Fe was added in thegrowth process of BN films, and FeBNO films were achieved. XPS results showedthat the FeBNO films mainly included Fe-N-O, B-N-O, and Fe-O etc. chemical bonds.The FeBNO films were deposited for120minutes with the sputtering power of150W,the substrate temperature of300℃in pure argon atmosphere. The FeBNO films weretransparent for the visible light, and the optical bandgap and the absorption factors ofthe films were5.32eV and100000cm-1at185nm respectively. Moreover, theheterojunction between the FeBNO films and N-type Si substrate had goodrectification characteristics, the rectification ratio reached103. The FeBNO films arevery stable, tightly bond with the substrate, and have very strong absorption in UVregion, therefore, they are suitable to manufacture the UV photodetectors.
(5) The design and simulation of cBN UV photodetectors. A parameter libraryof cBN single crystal and a model of a cBN MSM UV photodetector are established with the simulation package Atlas. The simulation results showed that under less than5V voltage, the UV detector with doping concentration of1013cm-3had highresponsibility. When the voltage was greater than5V, the photodetector with dopingconcentration of1014cm-3have higher responsibility. The device with3μm electrodewidth and10μm electrode spacing had the lowest dark current and the highest ratioof photocurrent to dark current. As for the devices with the same electrode width andspacing, the dark current reduced rapidly with the increase of the size of electrodes,but the photocurrent was almost the constant.
Two kinds of MSM cBN UV photodetectors with interdigitated finger electrodeswere fabricated by evaporation, sputtered and lithography. One was thephotoconductive device with Au electrodes, and the other was photovoltaic devicewith Cr electrodes. The dark currents and UV photoresponses of the two devices weremeasured. The ratio of photocurrent to dark current the former was only2-3, as forthe latter, the ratio reached56, which was in accordance with the simulation. Becauseof the bad quality of cBN crystals, the performances of cBN UV photodetectors needto be improved further.
引文
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