CN115180636A - Method for improving visible light absorption range of CuSCN - Google Patents
Method for improving visible light absorption range of CuSCN Download PDFInfo
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- CN115180636A CN115180636A CN202210986264.3A CN202210986264A CN115180636A CN 115180636 A CN115180636 A CN 115180636A CN 202210986264 A CN202210986264 A CN 202210986264A CN 115180636 A CN115180636 A CN 115180636A
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- pressure
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- cuscn
- visible light
- light absorption
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- PDZKZMQQDCHTNF-UHFFFAOYSA-M copper(1+);thiocyanate Chemical compound [Cu+].[S-]C#N PDZKZMQQDCHTNF-UHFFFAOYSA-M 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000031700 light absorption Effects 0.000 title claims abstract description 15
- 238000010521 absorption reaction Methods 0.000 claims abstract description 12
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 7
- 239000010432 diamond Substances 0.000 claims abstract description 7
- 238000011049 filling Methods 0.000 claims abstract description 5
- 238000004528 spin coating Methods 0.000 claims abstract description 4
- 238000007790 scraping Methods 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 8
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 238000007373 indentation Methods 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- 239000004005 microsphere Substances 0.000 claims description 3
- 239000010979 ruby Substances 0.000 claims description 3
- 229910001750 ruby Inorganic materials 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000032900 absorption of visible light Effects 0.000 claims description 2
- 230000005540 biological transmission Effects 0.000 claims description 2
- 238000005553 drilling Methods 0.000 claims description 2
- 239000003921 oil Substances 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 239000008204 material by function Substances 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 10
- 239000011521 glass Substances 0.000 description 5
- 239000010409 thin film Substances 0.000 description 4
- 238000001237 Raman spectrum Methods 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000005280 amorphization Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- LJSQFQKUNVCTIA-UHFFFAOYSA-N diethyl sulfide Chemical compound CCSCC LJSQFQKUNVCTIA-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000005525 hole transport Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 238000000584 ultraviolet--visible--near infrared spectrum Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C3/00—Cyanogen; Compounds thereof
- C01C3/20—Thiocyanic acid; Salts thereof
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/003—Light absorbing elements
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
Abstract
The invention discloses a method for improving the visible light absorption range of CuSCN, belonging to the technical field of high-pressure preparation of functional materials. Preparing a beta-CuSCN film by adopting a spin coating method of solution treatment, scraping a sample by utilizing a sharp needle, filling the sample into a sample cavity of a diamond anvil cell press, continuously pressurizing the sample to 9.3GPa, keeping for 24 hours, and slowly releasing pressure to normal pressure to obtain the sample with the absorption edge of 427nm and good visible light absorption property. The method increases the absorption range of the CuSCN film to visible light by approximately 62nm, is simple, convenient to operate and good in repeatability, and has important application value and scientific significance for a high-efficiency light pressure sensor under pressure and a photovoltaic device with adjustable pressure of a visible light area.
Description
Technical Field
The invention belongs to the technical field of high-pressure preparation of functional materials. In particular to a novel method for improving the visible light absorption of beta-CuSCN by high-pressure treatment by utilizing a diamond anvil cell high-pressure technology.
Background
Cuprous thiocyanate (CuSCN) as an excellent p-type wide bandgap (3.4 eV) transparent semiconductor material has the advantages of high light transmittance, good stability, high conductivity and the like, so that CuSCN as a hole transport material has wide application prospects on photoelectronic devices. Optically, in an ultraviolet visible near infrared spectrum, the CuSCN film is almost transparent, the absorption range of light is an ultraviolet region, no obvious absorption peak exists in the visible region, and the power conversion efficiency of the CuSCN photovoltaic device is severely limited by an overlarge band gap. Although the power conversion efficiency has increased slightly over the past few years with continued advances in thin film technology, the inherent disadvantages of this material are difficult to overcome using conventional, complex and costly chemical methods. Therefore, in the current research stage, the optimization of the band gap has become a core problem for improving the performance of the CuSCN optoelectronic device.
Pressure is an effective and simple tool to change the atomic arrangement, and can greatly change the electronic structure and physical properties of a material without changing the chemical composition. The invention provides a novel method for reducing the CuSCN band gap value and improving the visible light absorption range by using a high-voltage means. Provides a new idea for the material to have wider application prospect in optoelectronic devices.
Disclosure of Invention
The invention aims to overcome the defects in the background art and provide a novel method for improving the visible light absorption range of CuSCN by using a high-voltage means.
The technical scheme of the invention can be described as follows:
a method for improving the visible light absorption range of CuSCN comprises the following steps:
1): preparing a beta-CuSCN film by adopting a spin-coating method of solution treatment to obtain a sample required by high-pressure operation;
2): scraping a sample from the beta-CuSCN film obtained in the step 1) by using a sharp needle, filling the sample into a sample cavity of a diamond anvil cell press, continuously pressurizing the sample to 9.3GPa, keeping the pressure for 24 hours, and slowly releasing the pressure to normal pressure to obtain the sample with the absorption edge of 427nm and good visible light absorption property.
Further, the specific operation of step 2) is: prepressing a T301 steel sheet by using a 300-micron diamond anvil cell press, wherein the thickness of an indentation is 40-60 microns, and drilling a hole with the diameter of 100-120 microns in the center of the indentation; filling a beta-CuSCN film initial material into holes of a steel sheet, adding silicon oil as a pressure transmission medium, adding ruby microspheres as a pressure mark (detecting the pressure in a pressure chamber), sealing a press, pressurizing, keeping for 24 hours after the pressure is increased to 9.3GPa, slowly releasing the pressure to normal pressure, and red-shifting the absorption edge of a CuSCN sample from initial 362nm to 427nm, thereby greatly increasing the absorption of visible light.
Further, the step 2) of slowly releasing the pressure to the normal pressure refers to releasing the pressure to the normal pressure at a rate of 2-3 GPa/h.
Has the beneficial effects that:
1. the method is simple and convenient to operate.
2. The method of the invention can increase the visible light absorption range of the CuSCN film to be close to 62nm.
3. The method has good repeatability, and has important application value and scientific significance for high-efficiency light pressure sensors under pressure and photovoltaic devices with adjustable pressure in a visible light area.
Drawings
FIG. 1 is a Raman spectrum of a beta-CuSCN thin film prepared by a spin coating method in example 2.
FIG. 2 is the UV-Vis absorption spectrum of the starting material of the sample of example 3 at a pressure of 0 GPa.
FIG. 3 is the UV-visible absorption spectrum obtained for the sample of example 4 at a pressure of 9.3 GPa.
FIG. 4 is a UV-visible absorption spectrum obtained from the pressure relief to 0GPa at a pressure of 9.3GPa for the sample of example 5.
FIG. 5 is the UV-visible absorption spectrum obtained for the sample of example 6 at a pressure of 12.7 GPa.
FIG. 6 is a Raman spectrum obtained from the sample of example 6 at a pressure of 12.7 GPa.
Detailed Description
The invention will be further illustrated with reference to specific examples.
Example 1:
first, the slides were placed in a custom glass wash rack and the loaded glass wash rack was placed in a beaker. And sequentially adding water, deionized water, isopropanol, deionized water and absolute ethyl alcohol dropwise added with the liquid detergent into the beaker, ultrasonically cleaning for 30 minutes respectively, then placing the glass cleaning frame in a vacuum drying oven, and drying for 12 hours at 80 ℃ for later use.
Example 2:
first, 0.05mg of beta-CuSCN powder is weighed into 1mL of ethyl sulfide solvent, sealed and stirred vigorously at room temperature for 120 minutes, and then the undissolved sample is removed by ultrasound and filtration. In order to obtain a CuSCN film with uniform thickness and suitable for a high-pressure experiment, 200uL of CuSCN solution is transferred by a liquid transfer gun and dripped on a glass slide rotating at the speed of 1000 revolutions per minute within 20 seconds, and the glass slide is rotated for 60 seconds; then, the obtained CuSCN thin film is annealed for about 8 hours at 80 ℃ in a nitrogen atmosphere to obtain the CuSCN thin film. The above procedure was repeated 10 times to obtain a film of sufficient thickness to obtain the desired β -CuSCN film for the high pressure experiment. The Raman spectrum of the β -CuSCN film prepared in this example is shown in FIG. 1.
Example 3:
a T301 steel sheet (about 0.25mm multiplied by 10 mm) is pre-pressed by an anvil press by a diamond with an anvil surface of 300 mu m, the indentation thickness is 40-60 mu m, and a hole with the diameter of 100-120 mu m is drilled at the center of the indentation and is used as a sample cavity filled with the original material. The sample beta-CuSCN film prepared in example 2 was scraped with a sharp needle and filled into a hole (sample cavity) of a steel sheet, silicone oil was dropped as a pressure medium, and ruby microspheres were added as a pressure mark (pressure in the pressure cavity was detected) to encapsulate a press machine, and a pressing operation was performed. When the pressure of the beta-CuSCN starting material in the sample chamber is 0GPa, the absorption edge of the packed starting material is 362nm, see fig. 2.
Example 4:
the press, sample chamber and pressure medium were the same as in example 3. The sample cavity pressure was raised to 9.3GPa and the absorption edge of the sample red-shifted to 461nm, see fig. 3.
Example 5:
the press, sample chamber and pressure medium were the same as in example 3. After the pressure of the sample cavity is increased to 9.3GPa, the pressure is maintained for 24 hours, then the pressure is slowly released to 0GPa at the average speed of 2-3 GPa/h, the absorption edge of the sample is 427nm, and the good visible light absorption property is maintained, as shown in figure 4.
Example 6:
the press, sample chamber and pressure medium were the same as in example 3. The sample cavity pressure was raised to 12.7GPa and the absorption edge red-shifted to 499nm, see fig. 5. However, cuSCN begins to undergo amorphization according to raman spectroscopy, and the CuSCN structure is no longer maintained, see fig. 6.
In summary, it can be found from the above example results that the increase of the visible light absorption of the β -CuSCN can be achieved by applying a suitable pressure. The method is simple to operate, and has important application value and scientific significance for high-efficiency optical pressure sensors under pressure and photovoltaic devices with adjustable pressure in visible light regions.
Claims (3)
1. A method for improving the visible light absorption range of CuSCN comprises the following steps:
1): preparing a beta-CuSCN film by adopting a spin-coating method of solution treatment to obtain a sample required by high-pressure operation;
2): scraping a sample from the beta-CuSCN film obtained in the step 1) by using a sharp needle, filling the sample into a sample cavity of a diamond anvil cell press, continuously pressurizing the sample to 9.3GPa, keeping the pressure for 24 hours, and slowly releasing the pressure to normal pressure to obtain the sample with the absorption edge of 427nm and good visible light absorption property.
2. The method for improving the visible light absorption range of CuSCN according to claim 1, wherein the specific operations of step 2) are as follows: prepressing a T301 steel sheet by using a 300-micron diamond anvil cell press, wherein the thickness of an indentation is 40-60 microns, and drilling a hole with the diameter of 100-120 microns in the center of the indentation; filling an initial material of a beta-CuSCN film into holes of a steel sheet, adding silicon oil as a pressure transmission medium, adding ruby microspheres as a pressure mark, sealing a press, pressurizing, keeping for 24 hours after the pressure is increased to 9.3GPa, slowly releasing the pressure to normal pressure, and red-shifting the absorption edge of a CuSCN sample from initial 362nm to 427nm, thereby greatly increasing the absorption of visible light.
3. The method according to claim 1, wherein the slow pressure relief to normal pressure in step 2) is at a rate of 2-3 GPa/h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210986264.3A CN115180636B (en) | 2022-07-22 | 2022-07-22 | Method for improving visible light absorption range of CuSCN |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202210986264.3A CN115180636B (en) | 2022-07-22 | 2022-07-22 | Method for improving visible light absorption range of CuSCN |
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| CN115180636A true CN115180636A (en) | 2022-10-14 |
| CN115180636B CN115180636B (en) | 2023-06-06 |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1329316C (en) * | 1985-03-08 | 1994-05-10 | Gerhard Meyer | Process for the preparation of aqueous ammonium thiocyanate |
| JP2002246623A (en) * | 2001-02-20 | 2002-08-30 | Sharp Corp | Dye-sensitized solar cell and method of manufacturing it |
| CN102199088A (en) * | 2011-03-30 | 2011-09-28 | 武汉工程大学 | Synthesis process of alkyl carbonate |
| US20110245074A1 (en) * | 2008-11-10 | 2011-10-06 | Wilson Smith | Photocatalytic structures, methods of making photocatalytic structures, and methods of photocatalysis |
| CN107039554A (en) * | 2016-12-28 | 2017-08-11 | 成都中建材光电材料有限公司 | A kind of cadmium telluride diaphragm solar battery and preparation method |
| CN109225298A (en) * | 2018-09-29 | 2019-01-18 | 台州学院 | A kind of MnISCN nanocomposite and its preparation method and application with high visible-light activity |
| CN109860401A (en) * | 2019-04-09 | 2019-06-07 | 湖南师范大学 | A kind of perovskite thin film solar battery and preparation method thereof using cuprous rhodanide as hole transmission layer |
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| CN114371197A (en) * | 2021-05-12 | 2022-04-19 | 湖北大学 | Visible light absorption type hydrogen sensor based on zinc oxide film |
-
2022
- 2022-07-22 CN CN202210986264.3A patent/CN115180636B/en active Active
Patent Citations (9)
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|---|---|---|---|---|
| CA1329316C (en) * | 1985-03-08 | 1994-05-10 | Gerhard Meyer | Process for the preparation of aqueous ammonium thiocyanate |
| JP2002246623A (en) * | 2001-02-20 | 2002-08-30 | Sharp Corp | Dye-sensitized solar cell and method of manufacturing it |
| US20110245074A1 (en) * | 2008-11-10 | 2011-10-06 | Wilson Smith | Photocatalytic structures, methods of making photocatalytic structures, and methods of photocatalysis |
| CN102199088A (en) * | 2011-03-30 | 2011-09-28 | 武汉工程大学 | Synthesis process of alkyl carbonate |
| CN107039554A (en) * | 2016-12-28 | 2017-08-11 | 成都中建材光电材料有限公司 | A kind of cadmium telluride diaphragm solar battery and preparation method |
| CN109225298A (en) * | 2018-09-29 | 2019-01-18 | 台州学院 | A kind of MnISCN nanocomposite and its preparation method and application with high visible-light activity |
| CN109860401A (en) * | 2019-04-09 | 2019-06-07 | 湖南师范大学 | A kind of perovskite thin film solar battery and preparation method thereof using cuprous rhodanide as hole transmission layer |
| KR20220037609A (en) * | 2020-09-18 | 2022-03-25 | 성균관대학교산학협력단 | Quantum dots solar cell having excellent photo-stability and preparing method of the same |
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| Title |
|---|
| ALDAKOV, D ET AL: "Properties of electrodeposited CuSCN 2D layers and nanowires influenced by their mixed domain structure", 《JOURNAL OF PHYSICAL CHEMISTRY C》 * |
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Application publication date: 20221014 Assignee: Zhangjiakou Yuanqing Environmental Testing Service Co.,Ltd. Assignor: HEBEI NORTH University Contract record no.: X2023980052751 Denomination of invention: A method to improve the visible light absorption range of CuSCN Granted publication date: 20230606 License type: Common License Record date: 20231215 |
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