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Article(id=1325123182000222512, tenantId=1146029695717560320, journalId=1255847867265597444, issueId=1325123175192855060, articleNumber=null, orderNo=null, doi=10.11858/gywlxb.20261106, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1779811200000, receivedDateStr=2026-05-27, revisedDate=1782403200000, revisedDateStr=2026-06-26, acceptedDate=null, acceptedDateStr=null, onlineDate=1793863586187, onlineDateStr=2026-11-05, pubDate=1788537600000, pubDateStr=2026-09-05, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1793863586187, onlineIssueDateStr=2026-11-05, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1793863586187, creator=13701087609, updateTime=1793863586187, updator=13701087609, issue=Issue{id=1325123175192855060, tenantId=1146029695717560320, journalId=1255847867265597444, year='2026', volume='40', issue='9', pageStart='090101-1', pageEnd='090114-12', issueExtLink='null', onlineDate='null', pubDate='1788537600000', pubDateStr='2026-09-05', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=1, specialIssue=0, createTime=1793863584564, creator='13701087609', updateTime=1793864402827, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1325126607446356730, tenantId=1146029695717560320, journalId=1255847867265597444, issueId=1325123175192855060, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1325126607450551035, tenantId=1146029695717560320, journalId=1255847867265597444, issueId=1325123175192855060, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=090110-1, endPage=090110-12, ext={EN=ArticleExt(id=1325123182407070001, articleId=1325123182000222512, tenantId=1146029695717560320, journalId=1255847867265597444, language=EN, title=Nitrogen Aggregation Induced by High-Pressure High-Temperature Pretreatment and Its Effect on the Apparent Charge-State Ratio of NV Centers in Diamond, columnId=1325123176816050710, journalTitle=Chinese Journal of High Pressure Physics, columnName=Carbon under High Pressure, runingTitle=null, highlight=null, articleAbstract=

Formation of nitrogen-vacancy (NV) centers and their apparent charge-state response in high-pressure high-temperature (HPHT) type-Ⅰb diamond were investigated. Effects of the initial substitutional nitrogen content (C-center nitrogen), electron irradiation, vacuum annealing, and HPHT pretreatment on the photoluminescence (PL) behavior of NV centers were compared. Two groups of HPHT diamond single crystals with different C-center nitrogen contents were subjected to electron irradiation, vacuum annealing (600−1000 ℃), and HPHT pretreatment (5 GPa, 1100−1900 ℃). Fourier-transform infrared spectroscopy (FTIR), Raman spectroscopy, and photoluminescence spectroscopy were employed to analyze nitrogen aggregation, lattice state, and NV-related photoluminescence responses. The results show that high-nitrogen samples exhibit more pronounced NV-related emission, whereas irradiation-induced vacancies in the low-nitrogen samples tend to remain as GR1 centers. As the vacuum annealing temperature increases, the overall emission intensities of NV0 and NV− increase, while the apparent photoluminescence response of NV− relative to NV0 generally decreases. HPHT pretreatment does not directly generate a large number of NV centers but promotes nitrogen aggregation and modifies the apparent NV−/NV0 charge-state ratio during subsequent irradiation and annealing. These results indicate that HPHT pretreatment can serve as a preceding processing parameter for regulating the initial defect state before irradiation and the subsequent apparent charge-state ratio of NV centers.

, authors=Weijian LI, Ning CHEN, Hongwei WANG, Hao WANG, Shixiu ZHAO, Yilong PAN, authorsList=Weijian LI, Ning CHEN, Hongwei WANG, Hao WANG, Shixiu ZHAO, Yilong PAN, authorCompany=null, correspAuthors=Yilong PAN, authorNote=null, correspAuthorsNote=null, copyrightStatement=Copyright © 2026 Chinese Journal of High Pressure Physics. All rights reserved., copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, fund=null), CN=ArticleExt(id=1325123185624101184, articleId=1325123182000222512, tenantId=1146029695717560320, journalId=1255847867265597444, language=CN, title=高温高压预处理诱导的氮聚集及其对金刚石NV色心表观电荷态比的影响, columnId=1325123177629745688, journalTitle=高压物理学报, columnName=高压下的碳材料, runingTitle=null, highlight=null, articleAbstract=

针对高温高压（high-pressure high-temperature, HPHT）法合成的Ⅰb型金刚石中氮空位（nitrogen vacancy，NV）色心形成及电荷态调控问题，比较了初始替位氮含量（C心氮）、电子辐照、真空退火和HPHT预处理对NV色心发光行为的影响。选取2组不同C心氮含量的HPHT金刚石单晶样品，通过电子辐照、600～1000 ℃真空退火以及5 GPa、1100～1900 ℃的HPHT预处理，结合红外吸收光谱、Raman光谱和光致发光光谱分析氮聚集、晶格状态及NV色心发光响应。结果表明：高氮样品更易形成明显的NV相关发光，低氮样品中辐照空位更易以GR1色心形式保留；随着真空退火温度升高，中性态NV0和负电态NV−发光整体增强，但NV−相对于NV0的表观发光响应整体下降。HPHT预处理本身未直接生成大量NV色心，但可促进氮聚集，并改变后续辐照和退火过程中NV−/NV0的表观电荷态比。结果表明，HPHT预处理可作为调控辐照前缺陷初态及后续NV色心电荷态比的前置工艺。

, authors=李玮健, 陈宁, 王宏伟, 王浩, 赵仕修, 潘益龙, authorsList=李玮健, 陈宁, 王宏伟, 王浩, 赵仕修, 潘益龙, authorCompany=null, correspAuthors=潘益龙, authorNote=

李玮健（1996－），男，硕士研究生，主要从事金刚石高温高压合成及改性研究. E-mail：

, correspAuthorsNote=
潘益龙（1988－），男，博士，研究员，主要从事大腔体压机实验技术、功能材料设计与合成研究. E-mail：
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李玮健（1996－），男，硕士研究生，主要从事金刚石高温高压合成及改性研究. E-mail：

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李玮健（1996－），男，硕士研究生，主要从事金刚石高温高压合成及改性研究. E-mail：

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SampleTa/℃ $ {\sigma }_{\text{h}} $/GPa $ {R}_{i} $SampleTa/℃ $ {\sigma }_{\text{h}} $/GPa $ {R}_{i} $
A0−0.2912.31B0−0.2830.17
A10.1014.36B10.0850.76
A6006000.93157.57B6006000.4052.21
A7007000.61114.53B7007000.5501.66
A8008000.4513.35B8008000.6170.89
A9009000.4490.71B9009000.4160.06
A100010000.3530.33B100010000.4180.03
), ArticleFig(id=1325123191244468603, tenantId=1146029695717560320, journalId=1255847867265597444, articleId=1325123182000222512, language=CN, label=表1, caption=

辐照-真空退火样品的残余应力及表观电荷态比

, figureFileSmall=null, figureFileBig=null, tableContent=
SampleTa/℃ $ {\sigma }_{\text{h}} $/GPa $ {R}_{i} $SampleTa/℃ $ {\sigma }_{\text{h}} $/GPa $ {R}_{i} $
A0−0.2912.31B0−0.2830.17
A10.1014.36B10.0850.76
A6006000.93157.57B6006000.4052.21
A7007000.61114.53B7007000.5501.66
A8008000.4513.35B8008000.6170.89
A9009000.4490.71B9009000.4160.06
A100010000.3530.33B100010000.4180.03
), ArticleFig(id=1325123191319966076, tenantId=1146029695717560320, journalId=1255847867265597444, articleId=1325123182000222512, language=EN, label=Table 2, caption=Residual stress and apparent charge-state ratio of samples treated by HPHT pretreatment, electron irradiation and vacuum annealing, figureFileSmall=null, figureFileBig=null, tableContent=
SampleTp/℃Ta/℃ $ {\sigma }_{\text{h}} $/GPa $ {R}_{i} $SampleTp/℃Ta/℃ $ {\sigma }_{\text{h}} $/GPa $ {R}_{i} $
A8008000.4513.35AVA60019006000.3553.39
APA110011008000.9640.47AVA70019007000.3831.15
APA130013008000.6060.51AVA80019008000.3102.58
APA150015008000.4160.85AVA90019009000.3700.44
APA170017008000.4701.45AVA1000190010000.3890.58
), ArticleFig(id=1325123191391269245, tenantId=1146029695717560320, journalId=1255847867265597444, articleId=1325123182000222512, language=CN, label=表2, caption=

HPHT预处理-辐照-真空退火样品的残余应力及表观电荷态比

, figureFileSmall=null, figureFileBig=null, tableContent=
SampleTp/℃Ta/℃ $ {\sigma }_{\text{h}} $/GPa $ {R}_{i} $SampleTp/℃Ta/℃ $ {\sigma }_{\text{h}} $/GPa $ {R}_{i} $
A8008000.4513.35AVA60019006000.3553.39
APA110011008000.9640.47AVA70019007000.3831.15
APA130013008000.6060.51AVA80019008000.3102.58
APA150015008000.4160.85AVA90019009000.3700.44
APA170017008000.4701.45AVA1000190010000.3890.58
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李玮健 , 陈宁 , 王宏伟 , 王浩 , 赵仕修 , 潘益龙
高压物理学报 | 高压下的碳材料 2026,40(9): 090110-1-090110-12
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高压物理学报 |高压下的碳材料 2026 , 40 (9) : 090110-1 -090110-12
高温高压预处理诱导的氮聚集及其对金刚石NV色心表观电荷态比的影响
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李玮健（1996－），男，硕士研究生，主要从事金刚石高温高压合成及改性研究. E-mail：

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李玮健（1996－），男，硕士研究生，主要从事金刚石高温高压合成及改性研究. E-mail：

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李玮健 , 陈宁, 王宏伟, 王浩, 赵仕修, 潘益龙
作者信息
  • 宁波大学物理科学与技术学院高压物理科学研究院, 浙江 宁波　315211
通讯作者:
潘益龙（1988－），男，博士，研究员，主要从事大腔体压机实验技术、功能材料设计与合成研究. E-mail：
作者简介:

李玮健（1996－），男，硕士研究生，主要从事金刚石高温高压合成及改性研究. E-mail：

Nitrogen Aggregation Induced by High-Pressure High-Temperature Pretreatment and Its Effect on the Apparent Charge-State Ratio of NV Centers in Diamond
Weijian LI , Ning CHEN, Hongwei WANG, Hao WANG, Shixiu ZHAO, Yilong PAN
Affiliations
  • Institute of High Pressure Physics, School of Physical Science and Technology, Ningbo University, Ningbo 315211, Zhejiang, China
出版时间: 2026-09-05 doi: 10.11858/gywlxb.20261106
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针对高温高压（high-pressure high-temperature, HPHT）法合成的Ⅰb型金刚石中氮空位（nitrogen vacancy，NV）色心形成及电荷态调控问题，比较了初始替位氮含量（C心氮）、电子辐照、真空退火和HPHT预处理对NV色心发光行为的影响。选取2组不同C心氮含量的HPHT金刚石单晶样品，通过电子辐照、600～1000 ℃真空退火以及5 GPa、1100～1900 ℃的HPHT预处理，结合红外吸收光谱、Raman光谱和光致发光光谱分析氮聚集、晶格状态及NV色心发光响应。结果表明：高氮样品更易形成明显的NV相关发光，低氮样品中辐照空位更易以GR1色心形式保留；随着真空退火温度升高，中性态NV0和负电态NV−发光整体增强，但NV−相对于NV0的表观发光响应整体下降。HPHT预处理本身未直接生成大量NV色心，但可促进氮聚集，并改变后续辐照和退火过程中NV−/NV0的表观电荷态比。结果表明，HPHT预处理可作为调控辐照前缺陷初态及后续NV色心电荷态比的前置工艺。

金刚石  /  氮空位色心  /  电子辐照  /  真空退火  /  高温高压

Formation of nitrogen-vacancy (NV) centers and their apparent charge-state response in high-pressure high-temperature (HPHT) type-Ⅰb diamond were investigated. Effects of the initial substitutional nitrogen content (C-center nitrogen), electron irradiation, vacuum annealing, and HPHT pretreatment on the photoluminescence (PL) behavior of NV centers were compared. Two groups of HPHT diamond single crystals with different C-center nitrogen contents were subjected to electron irradiation, vacuum annealing (600−1000 ℃), and HPHT pretreatment (5 GPa, 1100−1900 ℃). Fourier-transform infrared spectroscopy (FTIR), Raman spectroscopy, and photoluminescence spectroscopy were employed to analyze nitrogen aggregation, lattice state, and NV-related photoluminescence responses. The results show that high-nitrogen samples exhibit more pronounced NV-related emission, whereas irradiation-induced vacancies in the low-nitrogen samples tend to remain as GR1 centers. As the vacuum annealing temperature increases, the overall emission intensities of NV0 and NV− increase, while the apparent photoluminescence response of NV− relative to NV0 generally decreases. HPHT pretreatment does not directly generate a large number of NV centers but promotes nitrogen aggregation and modifies the apparent NV−/NV0 charge-state ratio during subsequent irradiation and annealing. These results indicate that HPHT pretreatment can serve as a preceding processing parameter for regulating the initial defect state before irradiation and the subsequent apparent charge-state ratio of NV centers.

diamond  /  nitrogen-vacancy (NV) center  /  electron irradiation  /  vacuum annealing  /  high-pressure high-temperature
李玮健, 陈宁, 王宏伟, 王浩, 赵仕修, 潘益龙. 高温高压预处理诱导的氮聚集及其对金刚石NV色心表观电荷态比的影响. 高压物理学报, 2026 , 40 (9) : 090110-1 -090110-12 . DOI: 10.11858/gywlxb.20261106
Weijian LI, Ning CHEN, Hongwei WANG, Hao WANG, Shixiu ZHAO, Yilong PAN. Nitrogen Aggregation Induced by High-Pressure High-Temperature Pretreatment and Its Effect on the Apparent Charge-State Ratio of NV Centers in Diamond[J]. Chinese Journal of High Pressure Physics, 2026 , 40 (9) : 090110-1 -090110-12 . DOI: 10.11858/gywlxb.20261106
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氮空位（nitrogen vacancy，NV）色心是金刚石中典型的量子功能缺陷，由孤立替位氮原子与相邻碳空位组成，主要包括中性态NV0和负电态NV−两种电荷态[1–3]。金刚石晶格中单个氮原子替代碳原子形成的孤立替位氮通常称为C心氮，2个相邻替位氮原子形成的双原子聚集氮则称为A心氮。C心氮既可作为形成NV色心的直接氮源，也可作为深能级电子供体影响NV−相关发光。由于NV−色心具有可光学读出的自旋三重态以及较好的室温稳定性[2, 4–5]，在量子传感、磁场探测、单光子器件等领域具有重要的应用价值[6–10]，因此，实现NV色心的高效形成，并进一步调控NV−/NV0相对发光响应，是金刚石功能化处理中的重要问题。
对含氮金刚石而言，电子辐照结合退火处理是制备NV色心的常用路线。电子辐照可在金刚石晶格中引入空位，随后通过退火激活空位迁移，使其与C心氮复合形成NV色心[11–15]。辐照剂量主要决定空位引入数量，退火温度则影响空位迁移、缺陷复合和NV色心的形成效率[13]。对于高温高压（high-pressure high-temperature, HPHT）法合成的Ⅰb型金刚石，由于其中通常含有一定浓度的C心氮，因此，该路线具有较好的体相NV色心制备可行性[11–12]。然而，单纯改变辐照剂量和真空退火温度，将主要调控空位的产生与迁移过程，对辐照前已经存在的氮聚集状态、局域应力环境和复杂缺陷背景的调控有限。
实际上，NV色心的形成并不只由空位数量决定。初始C心氮含量决定可参与NV形成的氮源数量，同时C心氮也可作为电子供体影响NV−的稳定性。另一方面，C心氮在高温条件下可能向A心氮等氮聚集态转化，复杂缺陷和局域应力也会影响空位俘获、非辐射复合和电荷补偿过程[16–21]。因此，如果能够在电子辐照前预先调控氮相关缺陷状态和局域晶格环境，就有可能改变后续辐照和真空退火过程中空位的竞争复合路径及NV−/NV0相对响应。HPHT预处理正是这样一种前置调控手段，它可以在金刚石稳定区内通过高温与压力的共同作用，调节氮聚集、缺陷重排和局域应力状态，而不必先引入大量辐照损伤。
基于此，本研究选取2组不同初始C心氮原子分数（NC0）的HPHT合成的金刚石单晶（样品A：NC0=4.4×10−5；样品B：NC0=0.7×10−5）作为研究对象：首先，比较其在相同电子辐照剂量和600～1000 ℃真空退火条件下的NV色心形成规律，明确初始C心氮含量对GR1、NV0和NV−竞争形成路径的影响；然后，选取NV相关发光更明显的高氮样品A，引入5 GPa、1100～1900 ℃的HPHT预处理，考察其对辐照前氮相关缺陷状态、局域应力环境以及后续辐照和退火处理后NV表观电荷态比的影响；最后，通过傅里叶变换红外（Fourier transform infrared, FTIR）光谱、Raman光谱和光致发光（photoluminescence, PL）光谱对样品进行综合表征，为构建面向不同目标NV色心状态的综合调控提供实验依据。
1 实　验
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金刚石的合成及HPHT预处理均在国产SPD-6×2700型六面顶压机上进行。金刚石单晶样品在5 GPa、1300 ℃条件下合成，以Fe-Ni合金为触媒，石墨片为碳源，通过调节Ti-Cu除氮剂添加量获得2种不同氮含量样品。根据红外光谱中1130 cm−1处C心氮相关吸收峰的估算，样品A和样品B的初始C心氮原子分数分别约为4.4×10−5和0.7×10−5[16]。计算前，先对FTIR光谱进行基线校正，利用2030～2160 cm−1区间的金刚石双声子吸收作为内标，以减小样品厚度和测试条件差异的影响。C心氮原子分数的计算公式为
$ \mu (1\,130\;{\text{cm}}^{-1})=(A(1\,290\;{\text{cm}}^{-1})-A(1\,370\;{\text{cm}}^{-1}))/0.31 $
$ \mu (2\,120\;{\text{cm}}^{-1})=\frac{40A(2\,030\;{\text{cm}}^{-1})+90A(2\,160\;{\text{cm}}^{-1})}{130}-A(2\,120\;{\text{cm}}^{-1}) $
$ {N}_{1\,130}= 1.375\times {10}^{-4} \mu (1\,130\;{\text{cm}}^{-1})/\mu (2\,120\;{\text{cm}}^{-1})$
式中：$ A $为对应波数处的吸收强度，$ \mu $为经内标法校正后的吸收系数，N1130为由1130 cm−1吸收峰计算得到的C心氮原子分数。根据该方法计算可得，样品A和样品B的初始C心氮原子分数分别约为4.4×10−5和0.7×10−5，说明2类样品在初始替位氮含量上存在明显差异。
将合成后的样品先经热稀硝酸处理，去除外围的合金触媒，再置于硫酸与硝酸混合溶液中煮沸，去除表面残留的石墨与金属杂质。将初始样品分别记为A0和B0。电子辐照采用10 MeV高能电子束，剂量为5×1017 e−/cm2。辐照过程中，将样品置于冷水中，以降低局部过热和开裂风险。真空退火在管式炉中进行，升温速率为10 ℃/min，保温1 h后随炉冷却至室温。
本研究设计2类实验。第1类采用电子辐照结合真空退火的常规后处理工艺，用于比较初始C心氮含量对NV色心形成的影响。对样品A和样品B进行相同剂量的电子辐照，将未退火处理的样品分别记为A1和B1，随后在600、700、800、900和1000 ℃下真空退火1 h，将所得样品分别记为A600～A1000和B600～B1000。
第2类采用HPHT预处理结合电子辐照与真空退火后处理工艺，用于考察HPHT预处理对后续NV色心形成和表观电荷态比的前置调控作用。由于低氮样品B的NV相关发光较弱，难以清晰分辨HPHT预处理对电荷态分布的影响，因此，该部分选取高氮样品A作为研究对象。经第1组实验，固定后续真空退火温度为800 ℃，改变HPHT预处理温度。首先，将样品在5 GPa、1100～1900 ℃下保温1 h，温度间隔200 ℃；随后，进行相同剂量的电子辐照，并统一在800 ℃下真空退火1 h，将样品记为APA1100～APA1900。第2组实验固定HPHT预处理条件为5 GPa、1900 ℃下保温1 h，随后经相同剂量的电子辐照，再分别在600～1000 ℃下真空退火1 h，将样品记为AVA600～AVA1000。其中，APA1900与AVA800对应相同的实验条件，为同一样品，为便于2组实验序列比较，予以重复列出。
采用光学显微镜观察样品形貌和宏观颜色变化；采用FTIR光谱分析HPHT预处理前后氮相关缺陷状态；采用Raman光谱分析样品的一阶金刚石特征峰位和半高全宽（full width at half maximum, FWHM），用于表征残余应力与晶格有序程度，在Raman测试中，每个样品选取多个无明显裂纹、包裹体和非边缘位置进行重复采集，并对1332 cm−1附近的金刚石一阶Raman峰进行Gaussian拟合；采用PL光谱表征NV0、NV−及GR1等缺陷相关发光特征，PL测试采用532 nm激光激发，所有样品均在相同的激光功率、积分时间和光路条件下采集。考虑到测试波长范围较宽，采用分段扫描方式获取PL谱，并在相邻波段保留约25%的重合区域用于拟合拼接。因此，在650～750 nm区间，部分样品可能出现局部强度抖动，该抖动主要源于分段采集和拼接处理，并不代表声子边带发生异常变化。Raman和PL测试前均以单晶硅片进行仪器标定，并采用高品质金刚石标准样品校验测试精度，以保证不同样品间测试结果的可比性。
2 结果与讨论
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2.1 初始氮含量对辐照和真空退火后宏观颜色变化的影响
为比较不同初始C心氮含量样品在相同辐照和真空退火后处理工艺下色心形成行为的变化，首先对高氮A组（NC0=4.4×10−5）和低氮B组（NC0=0.7×10−5）样品进行了光学显微观察。图1显示了初始样品A0和B0、相同剂量电子辐照后未退火高氮和低氮样品A1和B1、600～1000 ℃真空退火后的样品A600～A1000和B600～B1000的光学照片。
由图1可见，2种样品整体均呈较规则的六-八面体形貌，说明电子辐照和后续真空退火未造成样品宏观形貌的明显破坏。初始状态下，高氮样品A0呈金黄色，低氮样品B0呈灰白色，反映两者的初始氮杂质背景存在明显差异。经相同剂量电子辐照后，样品 A1由金黄色转为黄绿色，样品B1由灰白色转为蓝色，表明电子辐照引起了样品光学吸收特征的明显变化，其中样品B1与文献[14]报道的电子辐照后GR1色心相关颜色变化相似，结合741 nm附近出现的GR1特征峰，说明在低氮样品中，辐照引入的空位较难及时与C心氮复合形成NV色心，因而更容易以GR1相关形式保留。相比之下，样品A1的黄绿色可理解为初始黄色与辐照缺陷相关色调叠加的结果。
经600～1000 ℃真空退火后，A、B两组样品的颜色均发生进一步变化。样品A600和A700仍保持较弱的黄绿色调，800 ℃及以上退火后逐渐转为带橙色调的紫色；B组样品表现出类似的变化趋势，但整体颜色变化较浅。该现象说明，真空退火能够促进辐照空位迁移并诱导NV色心进一步转化，而初始C心氮含量会影响最终形成的色心种类和相对浓度。高氮样品中，可参与NV色心形成的氮源更充足，因此，后续退火更容易形成明显的NV相关色心；低氮样品中，C心氮不足，空位更容易以GR1或其他空位相关缺陷形式保留。
需要强调的是，光学颜色是多种吸收中心与发光中心共同作用的宏观结果，只能作为色心演化的直观辅助证据，不能单独用于判定具体缺陷类型。NV0、NV−和GR1等缺陷归属及其相对变化仍需结合PL光谱进一步确认。
2.2 电子辐照结合真空退火的后处理过程中的应力状态与NV色心发光演化
为进一步分析辐照和真空退火过程中样品晶格状态及缺陷发光的变化，对A、B两组样品进行了Raman和PL光谱测试。Raman光谱主要用于分析金刚石主体晶格的一阶特征峰位和FWHM变化，从而判断辐照和退火引起的局域应力及晶格无序程度；PL光谱则用于识别NV0、NV−和GR1等缺陷相关发光特征。
图2为样品A和样品 B在辐照和真空退火后的Raman光谱。理想无应力金刚石的一阶Raman特征峰位于1332.00 cm−1，对应sp3碳骨架的声子振动[22]。金刚石的Raman峰相较于无应力峰位的偏移可用于估算样品内部的残余应力，其近似关系[23]可写为
$ {\sigma }_{\text{h}}=(\gamma {-\gamma }_{0})/2.88 $
式中：$ {\sigma }_{\text{h}} $为内部的残余应力，单位为GPa；$ \gamma $为实验样品的一阶Raman特征峰的峰位，单位为cm−1；$ {\gamma }_{0} $为无应力金刚石的一阶Raman特征峰的峰位，取1332.00 cm−1；计算结果为正值代表压应力，负值代表拉应力。需要指出的是，Raman峰位除受残余应力影响外，还可能受到局域缺陷浓度、晶体形貌、晶体厚度等因素影响。特别是当不同样品间峰位变化较小时，其差异可能接近仪器分辨率和拟合误差范围。因此，本研究计算的残余应力主要用于辅助比较不同处理条件下Raman峰位和晶格状态的相对变化趋势，而不作为高精度绝对应力结果。为比较2种电荷态的相对强度，对575和637 nm处零声子线进行局部基线扣除和峰拟合，并定义NV色心的表观电荷态比Ri为
$ {R}_{i}={A}_{637}/{A}_{575} $
式中：A637和A575分别为637 nm处NV−零声子线（zero-phonon line，ZPL）和575 nm处NV0零声子线的拟合积分面积。Ri用于表征同一测试条件下NV−相对于NV0的表观发光强度比，并不直接等同于NV−/NV0的绝对浓度比。为避免PL强度受样品尺寸、局部吸收和采集位置的影响，采用归一化峰面积变化来比较同一样品系列内的变化趋势。除此之外，NV0和NV−电荷态分布还可能受到光致电离、采集效率、探测器响应、样品吸收背景和局域缺陷环境等因素影响。所以，Ri不能直接用于确定NV−/NV0的绝对浓度比，也不能独立证明NV−的稳定性发生变化。本研究中所有PL光谱均在相同激发波长、激光功率、积分时间、光路条件和拟合方法下获得，故Ri可作为同一批样品在不同处理条件下表观发光响应变化的半定量比较参数，但相关讨论仍需结合NV0、NV−和GR1的特征峰、FTIR及Raman结果进行综合判断。表1给出了A、B两组样品在不同处理条件下的残余应力σh和表观电荷态比$ {R}_{i} $，其中Ta为退火处理温度。
由表1可见，初始样品A0和B0的Raman峰相对于无应力金刚石发生红移，表现为轻微拉应力。经电子辐照后，样品A1和样品B1由初始拉应力转变为压应力，说明高能电子束在金刚石晶格中引入空位、间隙原子及其复合缺陷[24]，改变了局域应力状态。进一步真空退火后，样品A600～A1000的残余压应力随退火温度升高而整体降低，表明退火促进部分辐照缺陷复合和湮灭，使晶格应力得到一定释放。相比之下，样品B600～B1000的残余应力变化不呈单调趋势，说明在低氮样品中，由于可捕获空位形成NV色心的C心氮较少，残余空位、间隙碳及其他复合缺陷对Raman峰位的影响更为复杂。Raman峰的FWHM可反映局域晶格无序程度。电子辐照后样品A和样品B的FWHM均增大，说明空位和间隙原子的引入增加了晶格无序。随着退火温度升高，FWHM呈先增大后减小的变化趋势，表明中低温退火阶段缺陷迁移和局域重排可能增强局部无序，而较高温度退火有利于部分辐照缺陷进一步复合、湮灭和晶格恢复。
图3为A、B两组样品在不同处理条件下的PL光谱。初始样品A0和B0的PL谱主要表现为572.5 nm附近的金刚石一阶Raman散射峰，未见明显的NV0或NV−特征峰，说明初始样品中可检测的NV色心发光较弱。电子辐照后，样品A1在575和637 nm附近出现新峰，分别对应NV0和NV−色心的零声子线，650～750 nm范围内的宽包络峰主要与NV0和NV−声子边带叠加有关[25]。在相同的测试条件下，样品A1中637 nm处NV−的零声子线强于575 nm处NV0的零声子线，说明高氮样品A中较高的C心氮浓度不仅提供NV色心形成所需的氮源，也为NV−稳定提供了相对充分的局域电子供给环境。相比之下，样品 B1经电子辐照后未观察到明显的575和637 nm峰，但在741 nm附近出现GR1色心特征峰，与图1中样品B1辐照后呈蓝色的现象一致。这说明相同剂量的电子辐照已在样品B中有效引入空位，在后续退火过程中，空位获得迁移能力，若附近存在可利用的C心氮，部分空位可被氮俘获并形成NV色心。因此，GR1和NV并非彼此排斥且不可转化的独立终产物，而是空位在不同处理阶段和局域氮环境下的不同存在形式。低氮样品B中可俘获空位的C心氮较少，因而辐照后更多空位暂时以GR1相关的形式保留。高氮样品A中的空位更容易与氮结合并形成NV色心。该结果说明，初始C心氮含量会影响辐照空位在GR1保留、NV形成及其他缺陷俘获路径之间的分配与后续转化。
A、B两组样品中与NV0和NV−色心相关的PL信号经局部基线扣除和峰拟合后，NV0和NV−的零声子线积分面积随退火温度的升高而整体增加，说明退火能够激活空位迁移并促进NV色心形成。由图3和表1可知，样品A在辐照后及真空退火过程中均表现出强于样品B的NV相关发光，说明较高C心氮含量有利于空位与氮复合形成NV色心。样品A600的Ri较高，主要是由于575 nm处的NV0峰相对较弱，使$ {A}_{637}/{A}_{575} $被放大，因此，该数值不能解释为样品A600具有异常高的NV−绝对比例，也不能用于判断其NV−稳定性，该数值可作为相对趋势参考，而不宜理解为绝对电荷态比例。随着退火温度的升高，样品A和样品B的NV0和NV−发光整体增强，但Ri整体下降，说明较高真空退火温度虽然促进NV总发光增强，却降低了NV−相对于NV0的表观发光响应。这可能与高温退火促进更多空位与C心氮复合、消耗有效孤立氮施主，并改变局域电荷补偿环境有关。对于低氮样品B，NV相关发光总体较弱，尤其900和1000 ℃退火后NV−的相对强度较低，说明当C心氮源和电子供给能力不足时，即使空位获得迁移能力，NV−的稳定形成仍受到限制。
综上，电子辐照结合真空退火能够有效诱导金刚石中NV色心形成，但该路线主要调控空位的引入、迁移和复合过程。初始C心氮含量则决定可参与NV色心形成的氮源及局域电子供给能力。仅通过提高真空退火温度，可以增强NV的总发光响应，但不能同步提高NV−相对于NV0的表观发光强度。若要进一步调控NV色心的电荷态分布，仅依赖辐照和真空退火是不够的，还需要在辐照前调节样品的氮相关缺陷状态和局域缺陷背景。
2.3 HPHT预处理对辐照前缺陷初态及后续NV色心形成的调控
2.2节结果表明，电子辐照和真空退火可以有效诱导金刚石NV色心形成，但该过程主要通过调控空位引入和空位迁移实现。对于给定初始氮含量的样品，单纯提高真空退火温度虽然能增强NV0和NV−发光峰，但Ri未同步提高，反而在较高退火温度时下降，说明常规的后处理方式难以同时实现NV总发光增强和NV−相对发光响应提升。其原因在于，NV色心的形成和电荷态分布不仅受空位迁移控制，还取决于辐照前样品中C心氮、氮聚集态、复杂缺陷与局域应力环境共同决定的初始缺陷状态。
引入HPHT预处理的目的是在电子辐照前调控高氮样品A中的氮相关缺陷状态和局域晶格环境，从而改变后续空位俘获、缺陷复合和电荷补偿过程。由于低氮样品B中NV相关发光较弱，难以清晰分辨HPHT预处理对NV表观电荷态比的影响，以下将选取高氮样品A作为研究对象。将样品A在5 GPa、1100～1900 ℃下保温1 h，温度间隔200 ℃，得到的样品记为AP1100～AP1900。
图4为样品A经不同温度HPHT预处理后、电子辐照前的FTIR光谱。其中，1130和1344 cm−1附近的吸收峰通常与C心氮相关，1280 cm−1附近的吸收峰则与A心氮相关。随着HPHT预处理温度由1100 ℃升高至1900 ℃，1280 cm−1附近的吸收峰逐渐增强，说明较高的HPHT预处理温度可能促进了部分C心氮向A心氮转化。该结果表明，HPHT预处理确实在电子辐照前改变了样品的氮相关缺陷状态。需要指出的是，氮聚集对后续NV色心形成具有双重影响。一方面，C心氮是形成NV色心的直接氮源，也是稳定NV−色心的重要电子供体；若部分孤立氮转化为A心氮，可能减少后续与空位复合形成NV的有效氮源，并降低局域电子供给能力。另一方面，HPHT处理也可能促进部分复杂缺陷重排、局域应力释放和非辐射复合中心减少，从而改变后续空位迁移和电荷补偿环境。因此，HPHT预处理对最终NV发光强度和$ {R}_{i} $的影响不能仅由1280 cm−1峰增强单独判断，经合理推测，可理解为氮聚集、缺陷重构与局域电荷环境共同作用的结果。
此外，对这些辐照前样品进行了Raman和PL测试，用于判断是否破坏了金刚石主体晶格或直接生成NV色心。图5(a)的Raman结果显示，各样品均保持清晰尖锐的金刚石一阶 Raman峰，未观察到明显石墨化或非晶碳相关特征，说明5 GPa、1100～1900 ℃的HPHT预处理未造成金刚石主体晶格明显劣化。各样品的Raman峰位集中在1331 cm−1附近，不同预处理温度之间的峰位差异较小，表明HPHT预处理未引起可由Raman明确分辨的系统性残余应力变化。在较高的预处理温度下，FWHM有所降低，表明HPHT处理可降低局域无序或应变不均。图5(b)的PL结果显示，辐照前各样品主要表现为572.5 nm附近的金刚石一阶Raman散射峰，未观察到明显的575 nm NV0和637 nm NV−的零声子线，也未见明显的741 nm的GR1色心信号。这表明HPHT预处理本身并未直接产生大量NV色心或辐照型空位缺陷。因此，后续辐照和真空退火后NV发光和Ri的差异主要应归因于HPHT预处理改变了辐照前氮相关缺陷状态、局域应力和缺陷背景，从而影响电子辐照后空位的复合路径和电荷补偿环境。
为进一步研究HPHT预处理对NV形成的影响，设计了2组复合处理实验。第1组固定电子辐照剂量和后续真空退火条件，改变HPHT预处理温度。样品A先在5 GPa、1100～1900 ℃下退火1 h，随后进行电子辐照，并统一在800 ℃下真空退火1 h，得到样品APA1100～APA1900，以未经HPHT预处理但经相同电子辐照和800 ℃真空退火的样品A800作为对照。该实验用于比较不同HPHT处理温度对后续NV色心形成和$ {R}_{i} $的影响。
第2类固定HPHT预处理条件为5 GPa、1900 ℃、1 h，随后进行相同剂量的电子辐照，并改变后续真空退火温度为600～1000 ℃，得到样品AVA600～AVA1000。该实验用于区分HPHT预处理和后续真空退火在NV色心形成过程中的不同作用。APA1900与AVA800对应相同的处理条件，即1900 ℃的HPHT预处理、电子辐照、800 ℃真空退火，为同一样品数据。
图6显示了2组实验后样品的光学照片。对于样品APA1100～APA1900，随着HPHT预处理温度升高，经后续处理后样品色调发生变化，说明HPHT预处理会影响后续色心形成的宏观光学表现。对于样品AVA600～AVA1000，在固定1900 ℃的HPHT预处理后，样品色调随真空退火温度升高而逐渐加深，800 ℃以上更明显，与前述样品A、B中空位迁移和NV相关色心形成在中高温退火区增强的趋势一致。颜色变化仅反映可见光吸收和发光中心的综合结果，具体的NV0、NV−及GR1演化仍需结合PL光谱分析。
本实验中各样品峰位集中在1332.89～1334.78 cm−1区间，并随处理条件发生偏移。根据拉曼频移与应力之间的近似线性关系，1～2 cm−1的峰位变化可对应亚吉帕量级的应力调制，说明不同热处理过程已明显改变晶体内部的应力分布与缺陷环境，结果见表2，其中Tp为HPHT预处理温度。
图7显示了复合处理后样品的Raman谱和PL谱，表2列出了对应的残余应力$ {\sigma }_{\text{h}} $和$ {R}_{i} $。对于样品APA1100～APA1900，Ri随着HPHT预处理温度由1100 ℃升高至1900 ℃而逐步增加，说明较高的预处理温度有利于增强NV−相对于NV0的表观发光响应。结合红外光谱可知，该过程伴随氮聚集态增强；结合Raman结果可知，样品主体晶格未发生明显劣化。因此，Ri的变化更可能与HPHT诱导的氮状态演化、复杂缺陷重排和局域电荷补偿条件变化有关。然而，与未经过HPHT预处理但经相同电子辐照和800 ℃真空退火的样品A800相比，样品APA1100～APA1700的Ri均明显降低，样品APA1900的Ri虽明显提升，但仍低于样品A800。这说明HPHT预处理提供的是一个独立于电子辐照和真空退火之外的前置调控维度，而不是简单提高NV−相对比例的通用方法。其作用结果取决于氮聚集、有效C心氮供体、复杂缺陷俘获与后续退火条件之间的共同作用。
在样品AVA600～AVA1000中，900～1000℃退火样品的$ {R}_{i} $明显低于600～800 ℃退火样品，说明在HPHT预处理下，较高的真空退火温度不利于维持NV−相对发光响应。这一现象与样品A、B在常规后处理方式下得到的趋势一致，说明真空退火主要调控空位迁移和后续电荷再分配；当退火温度过高时，更多空位参与复合，C心氮施主环境和局域电荷补偿状态随之改变，NV0的相对贡献增强，从而导致Ri降低。
从能级结构角度看，NV电荷态转化可能是局域费米能级与缺陷能级之间相互作用的结果。C心氮可作为施主提供电子，有利于NV−稳定；当体系中有效施主浓度较高且深能级陷阱较少时，NV色心更容易获得电子并以NV−形式存在[25–27]。相反，若C心氮被聚集消耗，电子可能被其他深能级缺陷俘获，或局域电荷补偿环境发生变化，NV−的稳定性可能下降并表现为NV0的相对贡献增强。因此，Ri的变化不应简单地理解为NV−绝对浓度的变化，而应理解为同一测试条件下NV−相对于NV0的表观发光响应变化。
2.4 机制讨论
综合上述结果，HPHT预处理、电子辐照和真空退火分别对应NV色心制备过程中不同的调控环节。电子辐照主要提供空位来源，真空退火主要激活空位迁移并促进空位与氮相关缺陷复合，而HPHT预处理则在辐照前改变样品中的氮相关缺陷状态、局域应力和缺陷背景。
对于未经HPHT预处理的样品A、B，初始C心氮含量决定了空位复合路径和局域电子供给能力。高氮样品A中，C心氮含量较高，辐照产生的空位更容易与氮相关缺陷复合并形成NV色心，同时较充足的电子供体环境有利于NV−相关发光。低氮样品B中，可参与NV形成的C心氮数量较少，辐照后更多空位以GR1相关的形式保留，即使后续真空退火激活空位迁移，其NV相关发光和$ {R}_{i} $仍受到限制。该结果说明，初始氮含量不仅决定NV色心形成效率，也会影响辐照空位在GR1保留、NV0/NV−形成以及其他缺陷俘获路径之间的分配与转化。
对于HPHT预处理样品，FTIR光谱结果表明，较高的预处理温度会促进A心氮相关吸收增强，说明部分孤立C心氮向A心氮转化。该过程可能减少后续形成NV色心所需的孤立氮源和电子供体，不利于NV−稳定。这可以解释APA系列样品的Ri整体低于未预处理样品A800。值得注意的是，在APA系列样品中，Ri随预处理温度升高而逐步增加，说明氮聚集并非决定Ri的唯一因素。空位俘获路径、复杂缺陷分布及局域供体/受体空间关系等也可能随HPHT条件发生变化，但现有实验尚不能确定各因素的具体贡献。同时，HPHT处理也可能改变复杂缺陷、局域应力和深能级陷阱分布，使电子辐照后空位俘获和电荷补偿过程发生变化。因此，HPHT预处理对NV色心形成的作用具有双重性：一方面调节氮聚集状态，另一方面可能改变缺陷背景和局域电荷环境。最终Ri是上述因素共同作用的结果。
对于后续真空退火温度，其主要作用是调控空位迁移和缺陷复合。中等温度退火可促进空位与C心氮复合，增强NV相关发光；但过高的退火温度可能使更多C心氮参与复合或电离过程，改变局域施主有效性和电荷补偿状态，从而增强NV0的相对贡献并降低Ri。因此，对于以NV−为主要目标的量子传感和磁场测量等应用，工艺优化不应单纯追求更高退火温度或更强总PL发光，而应在NV总发光强度、NV−相对响应、GR1残留和晶格缺陷背景之间取得平衡。
由此可以建立HPHT金刚石NV色心的工艺调控图谱：HPHT预处理温度主要调控辐照前氮聚集状态和缺陷背景；电子辐照剂量决定空位引入数量；真空退火温度决定空位迁移和后续电荷再分配。对于发光增强或颜色中心调控等应用，可适当提高真空退火温度，以促进NV色心总量增加；对于量子传感和磁场测量等更依赖NV−色心的应用，应避免过高真空退火温度导致Ri下降，并通过合适的HPHT预处理调节缺陷背景和局域电荷补偿环境。该认识为后续通过HPHT预处理构建不同目标NV色心状态提供了实验依据。
需要强调的是，本研究主要基于室温PL峰面积比、Raman参数和FTIR光谱讨论NV色心表观电荷态变化及局域缺陷演化。关于施主电离、深能级陷阱和费米能级移动的解释仍属于基于光谱趋势的合理推测。同时，基于本研究现有的测试手段尚不能定量区分氮聚集、复杂缺陷重构和局域电荷环境变化的相对贡献。在缺少各类缺陷浓度和转化速率参数的情况下，建立定量动力学模型可能引入较强的假设。因此，本研究将相关讨论限定为基于现有光谱结果的可能物理图像。后续可结合电子顺磁共振、低温PL和红外定量分析，进一步区分C心氮、A心氮、空位相关缺陷及NV电荷态的演化过程，从而更准确地建立HPHT预处理、电子辐照和真空退火之间的缺陷分配与转化关系。
3 结　论
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本工作研究了初始C心氮含量、电子辐照、真空退火及HPHT预处理对金刚石NV色心形成行为和表观电荷态比的影响。结果表明，高氮样品更易形成明显的NV0和NV−相关发光，而低氮样品中辐照空位更容易以GR1色心形式保留，说明初始C心氮含量不仅影响NV色心的形成效率，也会改变空位在GR1、NV0与NV−之间的竞争转化路径。真空退火能够激活空位迁移并增强NV相关发光，但随着退火温度升高，Ri整体下降，表明较高的真空退火温度虽然有利于提高NV的总发光响应，却不利于维持NV−相对于NV0的表观发光优势。因此，真空退火温度需要在促进空位迁移与维持NV−电荷态稳定之间取得平衡。HPHT预处理能够在电子辐照前改变样品的氮相关缺陷状态和局域缺陷背景。较高的HPHT预处理温度促进氮聚集，且Ri随预处理温度升高而增加，说明HPHT预处理可作为调控后续NV表观电荷态比的前置工艺参数。总体而言，HPHT预处理、电子辐照和真空退火分别调控辐照前缺陷初态、空位引入和空位迁移过程，研究结果为金刚石中NV色心的可控制备提供了新的工艺调控思路。

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2026年第40卷第9期
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doi: 10.11858/gywlxb.20261106
  • 接收时间：2026-05-27
  • 首发时间：2026-11-05
  • 出版时间：2026-09-05
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  • 收稿日期：2026-05-27
  • 修回日期：2026-06-26
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    宁波大学物理科学与技术学院高压物理科学研究院, 浙江 宁波　315211

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潘益龙（1988－），男，博士，研究员，主要从事大腔体压机实验技术、功能材料设计与合成研究. E-mail：
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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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