阅读说明：本技术 一种Cs2SnI6粉末及其制备方法 (A kind of Cs2SnI6Powder and preparation method thereof ) 是由 王科范 肖乃瑞 柳朵朵 邱雅丽 汤叶华 于 2019-07-18 设计创作，主要内容包括：本发明属于太阳能电池材料技术领域,具体涉及一种无机钙钛矿半导体Cs_2SnI_6粉末及其制备方法。所述制备方法包括以下步骤：1)将CsI粉末与SnI_2或SnI_4粉末混合,得混合物A；2)向混合物A内加入溶剂,在室温下搅拌至反应完全,得粗产物；3)将粗产物经过滤、干燥,即得高纯的Cs_2SnI_6晶态粉末。本发明提供了一种新的、简单的制备方法来生产Cs_2SnI_6粉末,在特定摩尔比和在特定的溶剂中,将CsI和SnI_2(或SnI_4)粉末在室温下充分搅拌后即可获得高纯的Cs_2SnI_6晶态粉末。(The invention belongs to solar cell material technical fields, and in particular to a kind of inorganic perovskite semiconductor Cs 2 SnI 6 Powder and preparation method thereof.The preparation method comprises the following steps: 1) by CsI powder and SnI 2 Or SnI 4 Powder mixing, obtains mixture A；2) solvent is added into mixture A, is stirred at room temperature to fully reacting, obtains crude product；3) crude product filtered, dried to get high-purity Cs 2 SnI 6 Crystalline, powder.The present invention provides a kind of new, simple preparation methods to produce Cs 2 SnI 6 Powder, in specific molar ratio and in specific solvent, by CsI and SnI 2 (or SnI 4 ) powder can be obtained high-purity Cs after being sufficiently stirred at room temperature 2 SnI 6 Crystalline, powder.)

1. a kind of Cs₂SnI₆The preparation method of powder, which comprises the following steps:

1) by CsI powder and SnI₂Or SnI₄Powder mixing, obtains mixture A；

2) solvent is added into mixture A, is stirred at room temperature to fully reacting, obtains crude product；

3) crude product is filtered, dry to get.

2. Cs according to claim 1₂SnI₆The preparation method of powder, which is characterized in that CsI and SnI in step 1)₂Rub You are than being 1:1, CsI and SnI₄Molar ratio be 3:2 or 2:1.

3. Cs according to claim 1₂SnI₆The preparation method of powder, which is characterized in that solvent described in step 2 is anhydrous Ethyl alcohol or acetonitrile, the ratio between volume and the mole of mixture A of solvent are (1-1.4) ml:1mmol.

4. Cs according to claim 1₂SnI₆The preparation method of powder, which is characterized in that CsI, SnI in step 1)₂And SnI₄ Purity be all larger than 99.9%.

5. Cs according to claim 1₂SnI₆The preparation method of powder, which is characterized in that dehydrated alcohol and acetonitrile in step 2 Purity be all larger than 99.5%.

6. Cs according to claim 1₂SnI₆The preparation method of powder, which is characterized in that the mixing speed in step 2 is 400-1000 r/min。

7. the Cs that any the method for claim 1-6 is prepared₂SnI₆Powder.

8. Cs described in claim 7₂SnI₆Application of the powder in solar cell material.

Technical field

The invention belongs to solar cell material technical fields, and in particular to a kind of inorganic perovskite semiconductor Cs₂SnI₆Powder End and preparation method thereof.

Background technique

Nearly ten years, it is very big to cause people for the application of hybrid inorganic-organic perovskite compound in solar cells Interest, this is mainly due to the raisings of its energy conversion efficiency it is rapid, manufacturing process is simple, low in cost the advantages that.Calcium titanium The improved efficiency of mine solar cell is very rapid, and from 2009 to 2019 year, the energy conversion efficiency of perovskite solar cell is Through having reached 24.2% from 3.8%.However, the stability of hybrid inorganic-organic perovskite solar battery is still bad, mainly Due to the degradation and volatilization of contained organic group, its large-scale business application is hindered.

On the other hand, due to full-inorganic perovskite compound such as CsPbI₃Or CsSnI₃With better heat/wet stability, Therefore it has been to be concerned by more and more people.Up to the present, CsPbI₃Perovskite solar battery in nitrogen glove box 15.7% high efficiency is reached.However, being used as α-phase CsPbI of the light absorbing layer of solar battery₃It can only be in > 300 °C of It is thermodynamically stable, and it includes toxic elements Pb.B-γ-CsSnI₃The efficiency of perovskite solar battery only has 4.81%, and Sn^{2 +}Ion is unstable in air, is easy to be oxidized by oxygen into Sn⁴⁺。

Cs₂SnI₆It is a kind of inorganic perovskite variant material, studies less, the high oxidation state (Sn with tin⁴⁺), thus have There is stronger oxidation resistance.In addition, its direct band gap is about 1.3 ~ 1.62 eV, theoretically its S-Q transformation efficiency is reachable 30-33%.This excellent performance makes Cs₂SnI₆Probably become a kind of promising solar cell material.Currently, pure Cs₂SnI₆As the light absorbing layer of solar battery, 0.96% efficiency can get；Work as Cs₂SnI₆Part is by Br^-Substitution is formed Cs₂SnI₄Br₂When, its transfer efficiency is up to 2.1%.Therefore Cs₂SnI₆Solar battery still has very big improved efficiency space.

Cs₂SnI₆Film can pass through vacuum heat deposition, electrospray, spray coating method, aerosol assistant chemical vapor deposition The methods of (AACVD) preparation.Cs₂SnI₆Powder can also be synthesized by vitreosil pipe solid-phase sintering by chemical solution Preparation.Cs₂SnI₆The synthesis of powder has important application value, because of Cs₂SnI₆Powder can be directly as vacuum heat deposition Evaporation source, be also soluble in organic solution for film spin coating.However, synthesizing Cs at present₂SnI₆The method of powder is still It is more complicated and expensive.Cs₂SnI₆The vacuum-sintering synthesis of powder needs high vacuum, high temperature and longer process time, its change It is still more complicated to learn the relatively cheap and time saving but current synthetic route of synthetic method.

Therefore, it is badly in need of a kind of method that synthetic route is simple, at low cost to produce high-purity Cs₂SnI₆Crystalline, powder.

Summary of the invention

In order to overcome the problems of the prior art, the present invention provides a kind of simple inorganic perovskite semiconductor Cs₂SnI₆ The preparation method of powder, this method is by the CsI and SnI of specific molar ratio₂(or SnI₄) powder is dissolved in specific solvent and carries out Reaction, can be obtained high-purity Cs after being sufficiently stirred at room temperature₂SnI₆Crystalline, powder.

The present invention also provides the inorganic perovskite semiconductor Cs obtained using above-mentioned preparation method₂SnI₆Powder.

To achieve the above object, technical scheme is as follows:

A kind of inorganic perovskite semiconductor Cs₂SnI₆The preparation method of powder, comprising the following steps:

1) by CsI powder and SnI₂Or SnI₄Powder mixing, obtains mixture A；

2) solvent is added into mixture A, is stirred at room temperature to fully reacting, obtains crude product；

3) crude product filtered, dried to get high-purity Cs₂SnI₆Crystalline, powder.

Preferably, CsI and SnI in step 1)₂Molar ratio be 1:1, CsI and SnI₄Molar ratio be 3:2 or 2:1.

Preferably, solvent described in step 2 is dehydrated alcohol or acetonitrile, the mole of the volume of solvent and mixture A it Than for (1-1.4) ml:1mmol, i.e. the volume of acetonitrile or dehydrated alcohol and CsI and SnI₂Or CsI and SnI₄The sum of mole Than.

Preferably, CsI, SnI in step 1)₂And SnI₄Purity be all larger than 99.9%.

Preferably, the purity of step 2 dehydrated alcohol and acetonitrile is all larger than 99.5%.

Preferably, the mixing speed in step 2 is 400-1000 r/min.

Preferably, rate of drying can be accelerated when step 3) is dry using the method for heating, heating temperature is 40-60 °C.

Specifically, room temperature, that is, temperature is 25 ± 5 °C.

The Cs being prepared using the above method₂SnI₆Powder.

The Cs₂SnI₆Application of the powder in solar cell material.

Compared to the prior art, the beneficial effects of the present invention are:

1. the present invention is in the CsI and SnI of specific molar ratio₂(or SnI₄) powder is dissolved in suitable specific solvent (anhydrous second Alcohol or acetonitrile) it is inner, it can be obtained high-purity Cs after being sufficiently stirred at room temperature₂SnI₆Crystalline, powder；

2. the present invention prepares Cs using one-step method₂SnI₆, preparation method is simple, quick, and process conditions are easily realized, is convenient for industry Change.

Detailed description of the invention

Fig. 1 is the Cs prepared using the method for embodiment 1-6₂SnI₆The XRD diagram of powder；

Fig. 2 is the high-purity Cs prepared using the method for embodiment 1-2₂SnI₆The SEM of crystalline, powder schemes；

Fig. 3 is the high-purity Cs prepared using the method for embodiment 3-4₂SnI₆The SEM of crystalline, powder schemes；

Fig. 4 is the Cs prepared using the method for embodiment 1-4₂SnI₆The light absorption spectrogram of powder.

Specific embodiment

Below with reference to embodiment and attached drawing, invention is further explained, but is not limitation of the present invention.This Preparation of the invention before being reacted: whipping process uses magnetic agitation, and the vial for having magnet rotor is successively existed It is cleaned by ultrasonic in acetonitrile, acetone, isopropanol, deionized water and ethanol solution, it is 10 minutes ultrasonic respectively every time, after wash clean It is used after drying.