2.1Chemicals
Sodium borohydride (NaBH4,99%),tellurium powder(-200 mesh,99.8%),cadmium chloride hemi(pentahydrate)(CdCl2,99+%),thiourea(97%),and 3-mercaptopropionic acid (MPA,99%) were purchased from Aldrich.All chemical were
used without additional purification.Distilled water was used
throughout.
2.1Chemicals
硼氢化钠（硼氢化钠， 99 ％ ） ，碲粉（ -200目， 99.8 ％ ） ，氯化镉半（五） （镉， 99 + ％ ） ，硫脲（ 97 ％ ） ，和3 -巯基丙酸（MPA， 99 ％ ）均购自Aldrich.所有化学品被用来无需额外提纯.各方面使用蒸馏水
2.2Preparation of Te source NaHTe
A modified literature method was adopted.Briefly,50.8 mg(0.4mmol) of tellurium powder and 37.8 mg(1 mmol) of NaBH4 were loaded in a 25 ml two-necked flask and air in the system was pumped off and replaced with N2.Then reaction mixture was heated at 80℃ for 30 min under N2 flow to get a deep red clear solution. The NaHTe solution obtained was stored for further use at room temperature, still under the protection of N2.
2.2Te源的预处理
采用一种改进的理论方法。简单的讲，50.8毫克（ 0.4mmol ）碲粉和37.8毫克（ 1mmol）的硼氢化钠被装在一个25毫升双口瓶，抽空空气，用氮气保护。然后反应混合物被加热到80 ℃ ， 30分钟下N2气氛中得到深红色透明的溶液。该得NaHTe溶液储存在室温下，仍保护下氮气以用于进一步使用。
2.3Synthesis of CdTe cores
The
synthetic procedure was according to the literature method with
minor modification. Typically,0.2 mmol of Cd solution, and 0.4 mmol
of MPA solution were mixed in a 40 ml solution and the pH of the
solution was adjusted to 10.0 by solution was palced in a
three-necked flask and was deaerated. Under stirring,2.0 ml of
freshly prepared NaHTe solution(0.01M) was added through a syringe
into the Cd precursor solution at room temperature .So the ratio of
Cd :MPA:Te in the reaction solution was 1:2:0.2.Then the reaction
mixture was heated to reflux temperature 100℃ under N2 protection.
Aliquots of the sample were taken at different time intervals and
used to record their UV-vis and PL spectra.When the PL peak reached
about 520 nm(CdTe samples with particle diameters of about 2.7 nm
were formed ;usually it took about 10 min), the heated source was
removed to stop the reaction, and the mixture was cooled to room
temperature
合成的程序是根据文献的方法稍作修改。通常情况下， 0.2浓度的镉溶液，和0.4浓度的MPA的混合溶液中40ml溶液和pH值的溶液是调整，以10.0的溶液放置在是在三口瓶中，并除去溶液中的气体.在室温搅拌下，2.0毫升新鲜准备NaHTe溶液（ 0.01M ）增加通过注射到Cd前体的溶液。所以反应溶液中镉：MPA：碲的摩尔比是1:2:0.2 。然后反应混合物被加热到回流温度100 ℃下氮气保护。等分试样的样品采取了在不同的时间间隔和用来记录其紫外可见和PL峰值.当PL峰值达到约520纳米（碲化镉样品粒径约为2.7 nm的形成;通常花了约10分钟） ，加热源被删除停止反应，混合物被冷却到室温。
2.4Growth of the CdTe/CdS core/shell shtructure
The obtained CdTe NCs reaction solution was divided equally in two 50 ml three-neck flask .To one flask,0.08 mmol of thiourea solution (thiourea : Cd=4:1) was added for the growth of CdTe/CdS core/shell nanocrystals; to the other one, an equal volume of distilled water was added to serve as the control experiment. Then, the pH value of the reaction systems were heated to the boiling point 100℃ under N2 protection. Timing started when the temperature reached 100℃.Aliquots of the sample were taken at different time intervals and used to record their UV-vis and PL spectra.
The above
approach is readily extended to a gram-scale production and the
period for a production cycle can usually be finished in less than
4 h. In a large-scale synthesis, all procedures are identical to
those used in the small-scale synthesis expect for the amount of
reagents used.
4碲化镉/硫化镉核/壳结构的生长
获得新生的碲化镉反应的溶液是均分在两个50毫升三口瓶。一个瓶， 0.08mmol的硫脲溶液（硫脲：镉= 4:1 ）是为增长的CdTe / CdS的核/壳纳米晶;其他的，等体积的蒸馏水作为对照试验. 然后 pH值的反应系统，加热到沸点100 ℃下氮气保护。定时开始当温度达到100 ℃ 。等分试样的样品已采取在不同时间间隔，用来记录其紫外可见光谱和光致发光。
上述办法很容易扩展到克级规模生产，不到4小时的生产周期通常可以完成大规模合成，所有的程序都是相同的用于小规模的综合预计的数额试剂。
Sodium borohydride (NaBH4,99%),tellurium powder(-200 mesh,99.8%),cadmium chloride hemi(pentahydrate)(CdCl2,99+%),thiourea(97%),and 3-mercaptopropionic acid (MPA,99%) were purchased from
2.1Chemicals
硼氢化钠（硼氢化钠， 99 ％ ） ，碲粉（ -200目， 99.8 ％ ） ，氯化镉半（五） （镉， 99 + ％ ） ，硫脲（ 97 ％ ） ，和3 -巯基丙酸（MPA， 99 ％ ）均购自Aldrich.所有化学品被用来无需额外提纯.各方面使用蒸馏水
2.2Preparation of Te source NaHTe
A modified literature method was adopted.Briefly,50.8 mg(0.4mmol) of tellurium powder and 37.8 mg(1 mmol) of NaBH4 were loaded in a 25 ml two-necked flask and air in the system was pumped off and replaced with N2.Then reaction mixture was heated at 80℃ for 30 min under N2 flow to get a deep red clear solution. The NaHTe solution obtained was stored for further use at room temperature, still under the protection of N2.
2.2Te源的预处理
采用一种改进的理论方法。简单的讲，50.8毫克（ 0.4mmol ）碲粉和37.8毫克（ 1mmol）的硼氢化钠被装在一个25毫升双口瓶，抽空空气，用氮气保护。然后反应混合物被加热到80 ℃ ， 30分钟下N2气氛中得到深红色透明的溶液。该得NaHTe溶液储存在室温下，仍保护下氮气以用于进一步使用。
2.3Synthesis of CdTe cores
合成的程序是根据文献的方法稍作修改。通常情况下， 0.2浓度的镉溶液，和0.4浓度的MPA的混合溶液中40ml溶液和pH值的溶液是调整，以10.0的溶液放置在是在三口瓶中，并除去溶液中的气体.在室温搅拌下，2.0毫升新鲜准备NaHTe溶液（ 0.01M ）增加通过注射到Cd前体的溶液。所以反应溶液中镉：MPA：碲的摩尔比是1:2:0.2 。然后反应混合物被加热到回流温度100 ℃下氮气保护。等分试样的样品采取了在不同的时间间隔和用来记录其紫外可见和PL峰值.当PL峰值达到约520纳米（碲化镉样品粒径约为2.7 nm的形成;通常花了约10分钟） ，加热源被删除停止反应，混合物被冷却到室温。
2.4Growth of the CdTe/CdS core/shell shtructure
The obtained CdTe NCs reaction solution was divided equally in two 50 ml three-neck flask .To one flask,0.08 mmol of thiourea solution (thiourea : Cd=4:1) was added for the growth of CdTe/CdS core/shell nanocrystals; to the other one, an equal volume of distilled water was added to serve as the control experiment. Then, the pH value of the reaction systems were heated to the boiling point 100℃ under N2 protection. Timing started when the temperature reached 100℃.Aliquots of the sample were taken at different time intervals and used to record their UV-vis and PL spectra.
4碲化镉/硫化镉核/壳结构的生长
获得新生的碲化镉反应的溶液是均分在两个50毫升三口瓶。一个瓶， 0.08mmol的硫脲溶液（硫脲：镉= 4:1 ）是为增长的CdTe / CdS的核/壳纳米晶;其他的，等体积的蒸馏水作为对照试验. 然后 pH值的反应系统，加热到沸点100 ℃下氮气保护。定时开始当温度达到100 ℃ 。等分试样的样品已采取在不同时间间隔，用来记录其紫外可见光谱和光致发光。
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