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Article(id=1319726209496363470, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1319726164160139662, articleNumber=null, orderNo=null, doi=10.14062/j.issn.0454-5648.20250057, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1737388800000, receivedDateStr=2025-01-21, revisedDate=1738857600000, revisedDateStr=2025-02-07, acceptedDate=null, acceptedDateStr=null, onlineDate=1792576847670, onlineDateStr=2026-10-21, pubDate=1752940800000, pubDateStr=2025-07-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1792576847670, onlineIssueDateStr=2026-10-21, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1792576847670, creator=13701087609, updateTime=1792576847670, updator=13701087609, issue=Issue{id=1319726164160139662, tenantId=1146029695717560320, journalId=1263187385517883426, year='2025', volume='53', issue='7', pageStart='1777', pageEnd='2078', issueExtLink='null', onlineDate='null', pubDate='1752940800000', pubDateStr='2025-07-20', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1792576836862, creator='13701087609', updateTime=1792577335628, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1319728256174117458, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1319726164160139662, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1319728256174117459, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1319726164160139662, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=1993, endPage=2000, ext={EN=ArticleExt(id=1319726209701884367, articleId=1319726209496363470, tenantId=1146029695717560320, journalId=1263187385517883426, language=EN, title=High-Quality Heavy Sn-Doped ZnGa2O4 Single Crystal, columnId=1319726165087077079, journalTitle=Journal of the Chinese Ceramic Society, columnName=Research Article, runingTitle=null, highlight=null, articleAbstract=
Introduction

Ultra-wide bandgap (UWBG) semiconductor materials have attracted extensive attention in the fields of optoelectronics, sensing systems, and high-power devices due to their high critical electric field, high-temperature resistance, and excellent photoelectric properties. In this paper, high-quality Sn4+-doped ZnGa2O4 crystals with a volume of approximately 10 cm3 were successfully obtained by the VGF method. The crystal structure of the grown Sn4+∶ ZnGa2O4 crystals was detected by single crystal X-ray diffraction (XRD), and their crystal quality was studied by high-resolution X-ray diffraction (HRXRD). In addition, the optical and electrical properties of the grown Sn4+∶ ZnGa2O4 crystals were investigated by UV-Vis spectroscopy, XPS, and Hall measurements. The results show that the optical properties are affected by the Sn4+ concentration, and it is demonstrated for the first time that the electrical properties of ZnGa2O4 single crystals can be controlled by the concentration of doped Sn4+. The carrier concentration of the grown Sn4+-doped ZnGa2O4 single crystal at room temperature is higher than that of previously studied ZnGa2O4 single crystals (1.39 × 1019 cm-3) and Sn4+-doped β-Ga2O3 (3 × 1018 - 3 ×1019 cm-3). The improved photoelectric properties of ZnGa2O4 crystals after Sn4+ doping are expected to find applications in high-power devices and optoelectronic devices.

Methods

ZnGa2O4 bulk single crystals doped with Sn4+ were grown by the VGF method. High-purity (99.999%) Ga2O3, ZnO and SnO2 powders were used as starting materials. The three powders were mixed for 80 h at a speed of 40 revolutions per minute, and then the mixed powders were cold-pressed into blocks at a pressure of 2000 bar and calcined in air at 600 ℃ in an alumina crucible for 16 h. Subsequently, ZnGa2O4 bulk single crystals doped with Sn4+ were grown in a crucible with an inner diameter of 60 mm and a height of 60 mm. The furnace was heated to 1900 ℃ at a rate of 250 ℃/h in an atmosphere of argon and 12% oxygen, and maintained at this temperature for about 2 h. Then the furnace was cooled slowly at a rate of 2-3 ℃ per minute. Sn4+ doped ZnGa2O4 bulk single crystals were obtained.

Results and discussion

XRD analysis indicates that the Sn4+-doped ZnGa2O4 crystal maintains a pure spinel phase without any impurity phases, and the lattice constant slightly increases due to the introduction of Sn4+. The high-resolution X-ray diffraction (HRXRD) results show that the full width at half maximum (FWHM) of the rocking curve of the crystal is only 82 arcsec, indicating excellent crystal quality. X-ray photoelectron spectroscopy (XPS) analysis confirms that Sn4+ mainly enters the octahedral sites of the lattice by replacing Ga3+. X-ray fluorescence spectroscopy (XRF) analysis indicates that Sn4+ is successfully doped into the crystal, but the actual doping concentration is lower than the theoretical value due to the volatility of SnO2. Optical performance tests show that Sn4+ doping slightly reduces the optical band gap of ZnGa2O4 crystals and increases the absorption in the near-infrared band, which is related to the increase in carrier concentration. Hall measurement results show that Sn4+ doping significantly increases the carrier concentration of the crystal (up to 3.32×1019 cm-3) and reduces the resistivity (0.006 Ω·cm), outperforming undoped ZnGa2O4 and Sn4+-doped β-Ga2O3 crystals.

Conclusions

In this study, high-quality Sn4+-doped ZnGa2O4 single crystals with a volume of 10 cm3 were successfully grown by the vertical gradient freezing (VGF) method. The obtained Sn4+-doped ZnGa2O4 crystals showed no significant shift in diffraction peaks and a full width at half maximum (FWHM) of the rocking curve as low as 82 arc seconds, confirming the extremely high quality of the single crystals. X-ray fluorescence spectroscopy (XRF) and X-ray photoelectron spectroscopy (XPS) analyses respectively confirmed the contents of Zn, Ga, O, and Sn elements, as well as the fact that Sn4+ were mainly incorporated into the ZnGa2O4 crystal by replacing Ga3+ at octahedral sites in the spinel structure. With the increase of Sn4+ doping concentration, the optical band gap of ZnGa2O4 crystals decreased to 4.58 eV and 4.56 eV, respectively. The introduction of Sn4+ did not cause significant changes in the cutoff absorption edge at about 275 nm, but increased absorption in the near-infrared wavelength range, which was related to the increase in carrier concentration. Hall measurements verified the effect of Sn4+ doping on the electrical properties of ZnGa2O4 single crystals. The results indicated that the introduction of Sn4+ significantly increased the carrier concentration of ZnGa2O4 crystals (2.65×1019-3.32×1019 cm-3) and decreased the resistivity (0.006-0.008 Ω·cm). These properties were superior to undoped ZnGa2O4 single crystals and Sn4+-doped β-Ga2O3 single crystals. Overall, the Sn4+-doped ZnGa2O4 crystals grown in this study demonstrated significant application potential in power devices and solar-blind detection, and are expected to play a key role in the development of future high-power and high-frequency electronic and optoelectronic devices.

, authors=Zhengyuan LI, Huihui LI, Kun ZHANG, Qiang YIN, Pei WANG, Jin ZHANG, Zhitai JIA, Wenxiang MU, authorsList=Zhengyuan LI, Huihui LI, Kun ZHANG, Qiang YIN, Pei WANG, Jin ZHANG, Zhitai JIA, Wenxiang MU, authorCompany=null, correspAuthors=Zhitai JIA, Wenxiang MU, authorNote=

LI Zhengyuan (1998-), male, Doctoral candidate. E-mail:

, correspAuthorsNote=
JIA Zhitai (1981-), male, Ph.D., Professor. E-mail: ;
MU Wenxiang (1989-), male, Ph.D., Associate Professor.
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超宽禁带（UWBG）半导体材料具有高临界电场、耐高温、光电特性优异，因可在高功率器件、电力电子、光电子应用等领域发挥重要作用而备受关注。采用垂直梯度凝固（VGF）法成功生长出体积约10 cm3的高质量Sn4+掺杂ZnGa2O4单晶。通过X射线衍射（XRD）、X射线光电子能谱、霍尔测试和紫外-可见光谱对晶体结构、电学性能和光学性能进行了系统研究。XRD结果表明，Sn4+掺杂ZnGa2O4晶体为纯尖晶石相无杂质相，摇摆曲线半高宽（FWHM）仅为82″。所获得的不同Sn4+掺杂浓度的ZnGa2O4单晶的光学带隙分别为4.58 eV和4.56 eV，均在约275 nm处有明显的吸收截止边。霍尔测试的结果显示，随着Sn4+掺杂浓度的升高，晶体的电导率增加，最高载流子浓度可达3.32×1019 cm-3，电子迁移率为30 cm2·V-1·s-1，电阻率为0.006 Ω·cm。载流子浓度明显高于之前研究的未掺杂的ZnGa2O4单晶。本工作为ZnGa2O4材料的掺杂改性提供了重要的理论和实验依据。锡掺杂到ZnGa2O4晶体中后，光电性能改善，有望在高功率器件和光电器件领域获得应用。

, authors=李政沅, 李慧慧, 张坤, 尹强, 王佩, 张晋, 贾志泰, 穆文祥, authorsList=李政沅, 李慧慧, 张坤, 尹强, 王佩, 张晋, 贾志泰, 穆文祥, authorCompany=null, correspAuthors=贾志泰, 穆文祥, authorNote=

李政沅（1998—），男，博士研究生。

, correspAuthorsNote=
贾志泰（1981—），男，博士，教授；
穆文祥（1989—），男，博士，副教授。
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高质量重锡掺杂ZnGa2O4单晶
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李政沅 , 李慧慧 , 张坤 , 尹强 , 王佩 , 张晋 , 贾志泰 , 穆文祥
硅酸盐学报 | 研究论文 2025,53(7): 1993-2000
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硅酸盐学报 |研究论文 2025 , 53 (7) : 1993 -2000
高质量重锡掺杂ZnGa2O4单晶
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李政沅 , 李慧慧, 张坤, 尹强, 王佩, 张晋, 贾志泰 , 穆文祥
作者信息
  • 山东大学晶体材料国家重点实验室，新一代半导体材料研究院晶体材料研究所，济南 250100
通讯作者:
贾志泰（1981—），男，博士，教授；
穆文祥（1989—），男，博士，副教授。
作者简介:

李政沅（1998—），男，博士研究生。

High-Quality Heavy Sn-Doped ZnGa2O4 Single Crystal
Zhengyuan LI , Huihui LI, Kun ZHANG, Qiang YIN, Pei WANG, Jin ZHANG, Zhitai JIA , Wenxiang MU
Affiliations
  • State Key Laboratory of Crystal Materials, Institute of Novel Semiconductors, Institute of Crystal Materials, Shandong University, Jinan 250100, China
    • Corresponding Author:
    JIA Zhitai (1981-), male, Ph.D., Professor. E-mail: ;
    MU Wenxiang (1989-), male, Ph.D., Associate Professor.

    LI Zhengyuan (1998-), male, Doctoral candidate. E-mail:

出版时间: 2025-07-20 doi: 10.14062/j.issn.0454-5648.20250057
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摘要
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超宽禁带（UWBG）半导体材料具有高临界电场、耐高温、光电特性优异，因可在高功率器件、电力电子、光电子应用等领域发挥重要作用而备受关注。采用垂直梯度凝固（VGF）法成功生长出体积约10 cm3的高质量Sn4+掺杂ZnGa2O4单晶。通过X射线衍射（XRD）、X射线光电子能谱、霍尔测试和紫外-可见光谱对晶体结构、电学性能和光学性能进行了系统研究。XRD结果表明，Sn4+掺杂ZnGa2O4晶体为纯尖晶石相无杂质相，摇摆曲线半高宽（FWHM）仅为82″。所获得的不同Sn4+掺杂浓度的ZnGa2O4单晶的光学带隙分别为4.58 eV和4.56 eV，均在约275 nm处有明显的吸收截止边。霍尔测试的结果显示，随着Sn4+掺杂浓度的升高，晶体的电导率增加，最高载流子浓度可达3.32×1019 cm-3，电子迁移率为30 cm2·V-1·s-1，电阻率为0.006 Ω·cm。载流子浓度明显高于之前研究的未掺杂的ZnGa2O4单晶。本工作为ZnGa2O4材料的掺杂改性提供了重要的理论和实验依据。锡掺杂到ZnGa2O4晶体中后，光电性能改善，有望在高功率器件和光电器件领域获得应用。

氧化锌镓  /  垂直梯度凝固法  /  锡掺杂  /  电学性能  /  超宽禁带半导体
Introduction

Ultra-wide bandgap (UWBG) semiconductor materials have attracted extensive attention in the fields of optoelectronics, sensing systems, and high-power devices due to their high critical electric field, high-temperature resistance, and excellent photoelectric properties. In this paper, high-quality Sn4+-doped ZnGa2O4 crystals with a volume of approximately 10 cm3 were successfully obtained by the VGF method. The crystal structure of the grown Sn4+∶ ZnGa2O4 crystals was detected by single crystal X-ray diffraction (XRD), and their crystal quality was studied by high-resolution X-ray diffraction (HRXRD). In addition, the optical and electrical properties of the grown Sn4+∶ ZnGa2O4 crystals were investigated by UV-Vis spectroscopy, XPS, and Hall measurements. The results show that the optical properties are affected by the Sn4+ concentration, and it is demonstrated for the first time that the electrical properties of ZnGa2O4 single crystals can be controlled by the concentration of doped Sn4+. The carrier concentration of the grown Sn4+-doped ZnGa2O4 single crystal at room temperature is higher than that of previously studied ZnGa2O4 single crystals (1.39 × 1019 cm-3) and Sn4+-doped β-Ga2O3 (3 × 1018 - 3 ×1019 cm-3). The improved photoelectric properties of ZnGa2O4 crystals after Sn4+ doping are expected to find applications in high-power devices and optoelectronic devices.

Methods

ZnGa2O4 bulk single crystals doped with Sn4+ were grown by the VGF method. High-purity (99.999%) Ga2O3, ZnO and SnO2 powders were used as starting materials. The three powders were mixed for 80 h at a speed of 40 revolutions per minute, and then the mixed powders were cold-pressed into blocks at a pressure of 2000 bar and calcined in air at 600 ℃ in an alumina crucible for 16 h. Subsequently, ZnGa2O4 bulk single crystals doped with Sn4+ were grown in a crucible with an inner diameter of 60 mm and a height of 60 mm. The furnace was heated to 1900 ℃ at a rate of 250 ℃/h in an atmosphere of argon and 12% oxygen, and maintained at this temperature for about 2 h. Then the furnace was cooled slowly at a rate of 2-3 ℃ per minute. Sn4+ doped ZnGa2O4 bulk single crystals were obtained.

Results and discussion

XRD analysis indicates that the Sn4+-doped ZnGa2O4 crystal maintains a pure spinel phase without any impurity phases, and the lattice constant slightly increases due to the introduction of Sn4+. The high-resolution X-ray diffraction (HRXRD) results show that the full width at half maximum (FWHM) of the rocking curve of the crystal is only 82 arcsec, indicating excellent crystal quality. X-ray photoelectron spectroscopy (XPS) analysis confirms that Sn4+ mainly enters the octahedral sites of the lattice by replacing Ga3+. X-ray fluorescence spectroscopy (XRF) analysis indicates that Sn4+ is successfully doped into the crystal, but the actual doping concentration is lower than the theoretical value due to the volatility of SnO2. Optical performance tests show that Sn4+ doping slightly reduces the optical band gap of ZnGa2O4 crystals and increases the absorption in the near-infrared band, which is related to the increase in carrier concentration. Hall measurement results show that Sn4+ doping significantly increases the carrier concentration of the crystal (up to 3.32×1019 cm-3) and reduces the resistivity (0.006 Ω·cm), outperforming undoped ZnGa2O4 and Sn4+-doped β-Ga2O3 crystals.

Conclusions

In this study, high-quality Sn4+-doped ZnGa2O4 single crystals with a volume of 10 cm3 were successfully grown by the vertical gradient freezing (VGF) method. The obtained Sn4+-doped ZnGa2O4 crystals showed no significant shift in diffraction peaks and a full width at half maximum (FWHM) of the rocking curve as low as 82 arc seconds, confirming the extremely high quality of the single crystals. X-ray fluorescence spectroscopy (XRF) and X-ray photoelectron spectroscopy (XPS) analyses respectively confirmed the contents of Zn, Ga, O, and Sn elements, as well as the fact that Sn4+ were mainly incorporated into the ZnGa2O4 crystal by replacing Ga3+ at octahedral sites in the spinel structure. With the increase of Sn4+ doping concentration, the optical band gap of ZnGa2O4 crystals decreased to 4.58 eV and 4.56 eV, respectively. The introduction of Sn4+ did not cause significant changes in the cutoff absorption edge at about 275 nm, but increased absorption in the near-infrared wavelength range, which was related to the increase in carrier concentration. Hall measurements verified the effect of Sn4+ doping on the electrical properties of ZnGa2O4 single crystals. The results indicated that the introduction of Sn4+ significantly increased the carrier concentration of ZnGa2O4 crystals (2.65×1019-3.32×1019 cm-3) and decreased the resistivity (0.006-0.008 Ω·cm). These properties were superior to undoped ZnGa2O4 single crystals and Sn4+-doped β-Ga2O3 single crystals. Overall, the Sn4+-doped ZnGa2O4 crystals grown in this study demonstrated significant application potential in power devices and solar-blind detection, and are expected to play a key role in the development of future high-power and high-frequency electronic and optoelectronic devices.

zinc gallium oxide  /  vertical gradient freeze method  /  stannum-doped  /  electrical property  /  ultra-wide bandgap semiconductors
李政沅, 李慧慧, 张坤, 尹强, 王佩, 张晋, 贾志泰, 穆文祥. 高质量重锡掺杂ZnGa2O4单晶. 硅酸盐学报, 2025 , 53 (7) : 1993 -2000 . DOI: 10.14062/j.issn.0454-5648.20250057
Zhengyuan LI, Huihui LI, Kun ZHANG, Qiang YIN, Pei WANG, Jin ZHANG, Zhitai JIA, Wenxiang MU. High-Quality Heavy Sn-Doped ZnGa2O4 Single Crystal[J]. Journal of the Chinese Ceramic Society, 2025 , 53 (7) : 1993 -2000 . DOI: 10.14062/j.issn.0454-5648.20250057
基金
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  • 国家重点研发计划(2024YFA1208800)
  • 国家自然科学基金（NSFC）(U23A20358)
  • 山东省自然科学基金(ZR2023ZD05和2022TSGC2120)
  • 深圳市基础研究计划(GJHZ20220913142605011)
  • 小米基金会/小米青年人才计划
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doi: 10.14062/j.issn.0454-5648.20250057
  • 接收时间：2025-01-21
  • 首发时间：2026-10-21
  • 出版时间：2025-07-20
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  • 收稿日期：2025-01-21
  • 修回日期：2025-02-07
基金
国家重点研发计划(2024YFA1208800)
国家自然科学基金（NSFC）(U23A20358)
山东省自然科学基金(ZR2023ZD05和2022TSGC2120)
深圳市基础研究计划(GJHZ20220913142605011)
小米基金会/小米青年人才计划
作者信息
    山东大学晶体材料国家重点实验室，新一代半导体材料研究院晶体材料研究所，济南 250100

通讯作者:

贾志泰（1981—），男，博士，教授；
穆文祥（1989—），男，博士，副教授。
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https://castjournals.cast.org.cn/joweb/gsyxb/CN/10.14062/j.issn.0454-5648.20250057
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鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
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