CN116804287B - Method for preparing palladium diselenide monocrystal by adopting oscillation temperature and application - Google Patents
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- 230000010355 oscillation Effects 0.000 title claims abstract description 57
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 23
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 23
- XIMIGUBYDJDCKI-UHFFFAOYSA-N diselenium Chemical compound [Se]=[Se] XIMIGUBYDJDCKI-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 239000013078 crystal Substances 0.000 claims abstract description 95
- 238000007789 sealing Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 230000000052 comparative effect Effects 0.000 description 14
- 239000011669 selenium Substances 0.000 description 13
- 239000010453 quartz Substances 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 238000010586 diagram Methods 0.000 description 10
- 239000010410 layer Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 8
- 238000003786 synthesis reaction Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 230000008859 change Effects 0.000 description 6
- 230000005669 field effect Effects 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000000399 optical microscopy Methods 0.000 description 5
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 4
- 238000001237 Raman spectrum Methods 0.000 description 4
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002524 electron diffraction data Methods 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
The invention discloses a method for preparing palladium diselenide monocrystal by adopting oscillation temperature and application thereof, wherein the method comprises the following steps: tabletting Pd and Se mixture, and vacuum-maintaining at 1×10 ‑3 5×10 ‑4 Sealing in Pa environment, reacting at 850-1100 deg.C to obtain polycrystal PdSe 2 The method comprises the steps of carrying out a first treatment on the surface of the Polycrystalline PdSe 2 Mixing with Se, tabletting, and vacuum-maintaining at 1×10 ‑3 5×10 ‑4 Sealing in Pa environment, and oscillating at 750 850 deg.C high temperature region and 600 700 deg.C low temperature region to obtain PdSe 2 A single crystal; the oscillating temperature refers to that the high temperature area and the low temperature area oscillate with the same oscillating temperature amplitude and oscillating time period. The invention solves the problem of PdSe in the prior art 2 The single crystal block has the technical problems of slow growth rate, long total time and small size of the single crystal.
Description
Technical Field
The invention relates to a method for preparing a palladium diselenide monocrystal, in particular to a method for preparing a palladium diselenide monocrystal by adopting oscillation temperature and application thereof.
Background
Palladium diselenide (PdSe) 2 ) Is a layered two-dimensional material similar to graphene. Researchers in 2017 found that palladium diselenide (PdSe) 2 ) The band gap of the represented noble metal two-dimensional material varies greatly with the layer number, such as PdSe decreases with the layer number 2 The band gap increases from 0.06eV (bulk) to 1.3eV (monolayer), correspondingly covering the visible to mid-infrared band, and it is very stable in air, thus pdSe 2 The noble metal two-dimensional material is an excellent infrared material, and PdSe 2 Great attention is being paid to field effect transistor and photodetector applications.
Preparation of PdSe 2 The common method for monocrystal is chemical vapor phase transmission mode, and the prior art is as follows:
xiao et al 2017 (JAmChemSoc.2017Oct11; 139 (40): 14090-14097) discloses a chemical vapor transport process for preparing PdSe 2 The method for monocrystal comprises the following specific steps: pdSe can be grown by self-help solvent method 2 Single crystal block, wherein the atomic ratio of Pd and Se powder is 1:6, mixing, vacuum sealing in quartz tube with sealing vacuum degree of 10 -6 Torr, then placing in a single temperature zone tube furnace, slowly heating the furnace body to 850 deg.C, holding for 50 hr, slowly cooling to 450 deg.C at a rate of 3 deg.C/hr, and obtaining small-sized PdSe 2 Monocrystalline bulk material. The single crystal obtained by the growth of the technical proposal has smaller size and is not suitable for commercial application.
2019 Zhou et al discloses a method for preparing PdSe 2 The method for single crystal (ACSnano, 2019,13 (2): 2511-2519) comprises the following specific steps: pdSe can be grown by self-help solvent method 2 Single crystal block, high purity Pd (granule) and Se powder in atomic ratio of 1:2, placing in quartz tube, vacuum degree of 10 -3 Sealing the tube under Pa, slowly heating to 800 ℃ and maintaining for 5 hours, then heating to 1050 ℃ within 2 hours and maintaining for 20 hours, and obtaining the polycrystalline PdSe 2 Material, and then polycrystalline PdSe 2 Mixing the material and Se powder according to an atomic ratio of 1:4, placing the mixture into a quartz tube for vacuum sealing, slowly heating to 850 ℃, keeping for 70 hours, slowly cooling to 450 ℃ at a cooling rate of 2 ℃/h, and finally stopping heating and naturally cooling to room temperature. The preparation period of the technical scheme is about 15 days, and the single crystal size is small. Thus, pdSe in the prior art 2 The single crystal bulk not only has a slow growth rate and a long total time, but also has a small size.
Disclosure of Invention
The invention aims to provide a method for preparing palladium diselenide monocrystal by adopting oscillation temperature and application thereof, which solves the problem of PdSe in the prior art 2 The single crystal block has the technical problems of slow growth rate, long total time and small size of the single crystal.
In order to achieve the above object, the present invention provides a method for producing a palladium diselenide single crystal using an oscillation temperature, the method comprising:
(1) Tabletting Pd and Se mixture, and vacuum-maintaining at 1×10 -3 5×10 -4 Sealing in Pa environment, reacting at 850-1100 deg.C to obtain polycrystal PdSe 2 ；
(2) The polycrystal PdSe obtained in the step (1) is processed 2 Mixing with Se, tabletting, and vacuum-maintaining at 1×10 -3 5×10 -4 Sealing in Pa environment, and oscillating at 750 850 deg.C high temperature region and 600 700 deg.C low temperature region to obtain PdSe 2 A single crystal;
the oscillating temperature refers to that the high temperature area and the low temperature area oscillate with the same oscillating temperature amplitude and oscillating time period.
Preferably, in step (1), the mass ratio of Pd and Se is 1:2; the Pd is in the state of particles or powder; the Se is in a powder state.
More preferably, when the Pd is in a particulate state, the Se powder is mixed with the Pd particles after being individually tabletted; when Pd is in powder state, the particle size of Pd is less than or equal to 75 mu m, and the Pd powder and Se powder are mixed and then tabletted.
Preferably, in step (1), the reaction time of 850 ℃ 1100 ℃ is 24-32 h.
Preferably, in step (2), the polycrystalline PdSe 2 The mass ratio to Se is 1:0.5. In step (2), if the polycrystalline PdSe 2 Too large a difference in the amount ratio of substances to Se has a large influence because too much Se is added as a transfer agent, which suppresses the growth of single crystals, and too little transfer agent affects the transfer efficiency.
Preferably, in step (2), the high temperature zone is 800 ℃ and the low temperature zone is 650 ℃. In the step (2), the temperature of the high temperature area and the low temperature area are required to be correspondingly adjusted due to the difference of the heating conditions and the heat dissipation conditions of the used furnace bodies. If the furnace cavity is bigger, the heat conduction efficiency is lower, the heat dissipation is bigger, the temperature of each part needs to be correspondingly increased, otherwise, the temperature of each part needs to be reduced.
Preferably, in step (2), the oscillation temperature amplitude is 1 ℃ to 10 ℃.
Preferably, in step (2), the oscillation time period is 12-24 hours.
Preferably, in step (2), the total time of the oscillation temperature growth is 79 days.
The invention also provides a PdSe prepared by the method 2 And (3) single crystals.
Preferably, the PdSe 2 The size of the single crystal was 4 mm.
The invention also provides a PdSe as described 2 Use of single crystals in nanoelectronic devices.
The invention discloses a method for preparing palladium diselenide monocrystal by adopting oscillation temperature and application thereof, which solves the problem of PdSe in the prior art 2 The single crystal has the technical problems of slow growth rate, longer total time and smaller size, and has the following advantages:
1. the invention adopts the PdSe with the oscillation temperature amplitude of 1 ℃ and the oscillation time period of 12 to 24 hours and the total growth time of 79 days 2 The size of the single crystal was 4 mm.
2. The palladium diselenide monocrystal block prepared by the method has the advantages of large size, high yield, high growth speed, short total growth time, simple and feasible preparation method and wide application prospect.
Drawings
FIG. 1 shows preparation of PdSe according to example 1 of the present invention 2 A flow chart of a single crystal;
FIG. 2 is a schematic diagram of chemical vapor transport according to example 1 of the present invention;
FIG. 3 is a graph showing the oscillation temperature of example 1 of the present invention;
FIG. 4 is a diagram showing the crystal structure of example 1 and comparative example 1 according to the present invention;
FIG. 5 is a graph showing the comparison of the crystal sizes and the numbers of crystals produced in example 1 of the present invention and comparative example 1;
FIG. 6 shows a crystal PdSe prepared in example 25 of the present invention 2 A physical diagram;
FIG. 7 shows PdSe prepared in example 1 of the present invention 2 High resolution TEM images and electron diffraction patterns of single crystals;
FIG. 8 shows PdSe prepared in example 1 of the present invention 2 An optical microscopy image and a raman spectrum image;
FIG. 9 shows PdSe prepared in example 1 of the present invention 2 Device optical microscopy, IV curve, and field effect curve.
Detailed Description
The following description of the embodiments of the present invention will be made in detail, with clarity, intact, and detailed descriptions of the embodiments of the present invention, it being apparent that the described embodiments are only some, but not all, embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A method for preparing palladium diselenide monocrystal by using oscillation temperature is shown in FIG. 1, and is that in embodiment 1 of the invention, pdSe is prepared by using oscillation temperature 2 A flow chart of a single crystal, the method comprising:
(1) Mixing palladium powder and selenium powder with the mass ratio of 1:2, tabletting, placing into quartz tube, and vacuumizingUp to 5X 10 -4 Pa, sealing the tube by flame of oxyhydrogen machine, setting 1100 ℃ in a tube furnace for reaction for 24h to obtain polycrystal PdSe 2 A material;
(2) Mixing selenium powder with the mass ratio of 0.5:1 and PdSe prepared in the step (1) 2 Mixing polycrystalline materials, grinding, tabletting, placing into quartz tube, and vacuumizing to 5×10 -4 Pa tube sealing, setting a high temperature region 800 ℃, a low temperature region 650 ℃, simultaneously carrying out oscillation temperature to grow single crystals, wherein the oscillation temperature amplitude of the high temperature region and the low temperature region is 10 ℃ during the oscillation temperature, namely the change range of the high temperature region is 790 810 ℃, the change range of the low temperature region is 640 660 ℃, the oscillation time period is 24 hours, namely the repeated oscillation is carried out with 24 hours as one period, the total growth time is 8 days, and finally the PdSe can be obtained in the low temperature region of the quartz tube 2 And (3) single crystals.
As shown in FIG. 2, the chemical vapor deposition of PdSe according to example 1 of the present invention 2 Schematic representation of single crystal. As can be seen from FIG. 2, the raw materials required for growing single crystals are pressed into sheets and placed in a quartz tube, the quartz tube is sealed by oxyhydrogen flame after being pumped into high vacuum, and then placed in a tube furnace with a double temperature zone for growing, the raw materials are placed in a high temperature zone, and after the raw materials are melted at high temperature, the transfer agent Se carries PdSe 2 The molecules reach a low temperature region, and after recrystallization in the low temperature region, pdSe can be obtained 2 Single crystal bulk.
As shown in FIG. 3, a specific oscillation temperature diagram of example 1 of the present invention is shown, wherein the abscissa is time and the ordinate is temperature. As can be seen from fig. 3, the amplitude of the oscillation temperature is 10 ℃ and the oscillation time period is 24 hours, and the temperature of the high temperature region is raised from 800 ℃ to 810 ℃ and then lowered to 790 ℃ and then raised to 800 ℃ in one oscillation period; meanwhile, the temperature of the low temperature region is increased from 650 ℃ to 660 ℃ and then is reduced to 640 ℃ and then is increased to 650 ℃, and the heating rate and the cooling rate of the high temperature region and the low temperature region are 10 ℃/6h.
Comparative example 1
A method for producing a palladium diselenide single crystal was substantially the same as in example 1, except that:
in the step (2), in the double-temperature zone tube furnace, the high temperature zone reaches 800 ℃, and the low temperature zone reachesHeating to 650deg.C, maintaining the temperature of the high temperature region and the low temperature region, growing at constant temperature gradient for 12 days to obtain PdSe in the low temperature region of quartz tube 2 And (3) single crystals.
Example 2
A method for producing a palladium diselenide single crystal using an oscillation temperature was substantially the same as in example 1, except that:
in the step (1), setting 850 ℃ in a tube furnace for reaction for 24 hours to obtain polycrystalline PdSe 2 A material.
Example 3
A method for producing a palladium diselenide single crystal using an oscillation temperature was substantially the same as in example 1, except that:
in the step (1), the vacuum in the quartz tube is changed to 1×10 -3 Pa。
Example 4
A method for producing a palladium diselenide single crystal using an oscillation temperature was substantially the same as in example 1, except that:
in the step (2), the oscillation temperature amplitude of the high temperature region and the low temperature region is 1 ℃ during the oscillation temperature, namely the change range of the high temperature region is 799 801 ℃, the change range of the low temperature region is 649 651 ℃, the oscillation time period is 12 hours, namely the repeated oscillation is carried out with 12 hours as one period, the total growth time is 8 days, and finally the PdSe can be obtained in the low temperature region of the quartz tube 2 And (3) single crystals.
Example 5
A method for producing a palladium diselenide single crystal using an oscillation temperature was substantially the same as in example 1, except that:
in the step (2), the oscillation time period is changed to 12 hours, namely, the oscillation is repeated by taking 12 hours as one period, the total growth time is 8 days, and finally, the PdSe can be obtained in the low-temperature area of the quartz tube 2 And (3) single crystals.
Experimental example 1 PdSe prepared in example 1 and comparative example 1, example 25 2 Single crystal comparison
1. Analysis of Single Crystal real objects prepared in example 1 and comparative example 1 respectively
As shown in FIG. 4, the crystal PdSe prepared in example 1 and comparative example 1 of the present invention 2 A physical diagram in which the single crystal above is the single crystal prepared in comparative example 1; the lower single crystal was the single crystal prepared in example 1. As can be seen from FIG. 4, the number of single crystals produced by 12-day growth in comparative example 1 is significantly smaller than that of PdSe produced by 7-day growth in example 1 2 The number of single crystals and the size of the single crystal obtained in example 1 were large, and thus, the single crystal prepared in example 1 using the oscillation temperature effectively improved the yield of the single crystal.
2. The single crystals prepared in example 1 and comparative example 1 were further analyzed for size and number
As shown in FIG. 5, the crystals PdSe prepared in example 1 and comparative example 1 of the present invention 2 A comparison of size, number, wherein the abscissa is the size of single crystals and the ordinate is the number of single crystals; the left side is the result of analysis of the single crystal of comparative example 1, and the right side is the result of analysis of the single crystal of example 1. As can be seen from FIG. 5, the single crystal prepared by 12 days of growth in comparative example 1 had a size of 2.3 mm and a number of pieces of 2; whereas example 1 produced single crystals with a size of 4.6 mm and a number of pieces of about 20 pieces by 7 days of growth.
As can be seen from a comprehensive analysis of FIGS. 4 to 5, comparative example 1 illustrates the synthesis of PdSe 2 The single crystal had an optimum synthesis temperature, and was analyzed to be about 720℃and compared with comparative example 1, example 1 uses an oscillation temperature to prepare a single crystal PdSe 2 Is larger in size and single crystal PdSe 2 The growth rate of (2) is faster and the total growth time is shorter.
3. Example 1 and example 25 PdSe prepared 2 Single crystal comparison
As shown in FIG. 6, the crystal PdSe prepared in example 25 of the present invention 2 A physical diagram, wherein (a) is the crystal PdSe prepared in example 2 of the present invention 2 A physical diagram; (b) Crystalline PdSe prepared for example 3 of the present invention 2 A physical diagram; (c) The crystal PdSe prepared in example 4 of the present invention 2 A physical diagram; (d) The crystal PdSe prepared in example 5 of the present invention 2 And (5) a physical diagram.
As is known from FIG. 6 (a), example 2 also produced a larger amount of large-size PdSe 2 The comparison of the single crystal size of about 20 pieces with example 1, which is about 4-6 mm, shows that the reaction temperature in step (1) is higher than that in step (2)PdSe 2 The effect of single crystals is not great.
As is known from FIG. 6 (b), example 3 also produced relatively large-sized PdSe 2 The comparison of the single crystal size of about 20 pieces with example 1 shows that the vacuum degree of the tube sealing in the step (1) is compared with that in the step (2) PdSe 2 The growth of single crystals is not greatly affected.
As is known from FIG. 6 (c), example 4 also produced relatively large-sized PdSe 2 The single crystal size was between 4 and 8mm, and about 15 pieces, compared with example 1, showed that the oscillation temperature amplitude in step (2) was compared with PdSe 2 The single crystal synthesis has obvious influence, compared with the example 1, the example 4 reduces the oscillation temperature amplitude, the oscillation time period is kept unchanged, the single crystal size is obviously increased, the total quantity is reduced, the total growth range is reduced, the optimal synthesis temperature stays at a single position for a long time after the temperature gradient changes slowly, and the oscillation temperature ensures the gaseous PdSe 2 Better fluidity of molecules, and increases the capture of gaseous PdSe by single crystals in a low temperature region 2 Probability of molecule, pdSe 2 The single crystal size can be grown larger; since the range of movement of the optimum synthesis temperature is reduced, both the total number of single crystals and the total range are reduced. Thus, example 4 shows that the oscillation temperature amplitude and oscillation time period need to be optimized to achieve a dynamic balance between optimum synthesis temperature shift range and single crystal capture molecule probability, thereby achieving a balance of maximum yield and maximum size single crystal.
As is known from FIG. 6 (d), example 5 also produced relatively large-sized PdSe 2 The single crystal size was between 4 and 6mm, and about 10 pieces, compared with example 1, showed that the oscillation time period of step (2) was compared with that of PdSe 2 Compared with the embodiment 1, the embodiment 5 keeps the oscillation temperature amplitude unchanged, reduces the oscillation time period, has no obvious change of the single crystal size, greatly reduces the total number and the total growth range; after the oscillation time period of example 5 was reduced, the oscillation temperature change rate was accelerated, and the gaseous PdSe was increased 2 The mobility of the molecules is not effective in increasing the size of the single crystal, and the total growth range is relatively largeThe reduction is a great indication of a reduced range of optimum synthesis temperature movement. Thus, example 5 also shows that the oscillation temperature amplitude and oscillation time period need to be optimized to achieve a dynamic balance between optimum synthesis temperature shift range and single crystal capture molecule probability, thereby achieving a balance of maximum yield and maximum size single crystal.
Experimental example 2 PdSe prepared in example 1 2 High resolution TEM images and electron diffraction patterns of single crystals
For the PdSe prepared in example 1 of the present invention 2 The single crystals were subjected to transmission electron microscopy analysis, respectively.
As shown in FIG. 7, pdSe prepared in example 1 of the present invention 2 A high-resolution TEM image and an electron diffraction image of a single crystal, wherein (a) is the crystal PdSe obtained in example 1 of the present invention 2 A high resolution TEM image of (a); (b) The crystal PdSe prepared in example 1 of the present invention 2 Is known from FIG. 7 to be PdSe 2 。
Experimental example 3 PdSe of example 1 2 Single crystal prepared few and thick layers of PdSe 2 Optical microscopy and raman spectra of the films.
For the PdSe prepared in example 1 of the present invention 2 Mechanically stripping the single crystal to obtain a small layer and a thick layer of PdSe 2 The film was subjected to raman spectroscopy.
As shown in FIG. 8, pdSe prepared in example 1 of the present invention 2 Wherein (a) is the few-layer PdSe of example 1 of the present invention 2 Is a photo-image of the image; (b) Example 1 of the invention few layer PdSe 2 Raman spectrum of the optical photograph of (2), raman shift in cm on the abscissa -1 The ordinate is intensity; (c) For example 1 of the invention, thick layer PdSe 2 Is a photo-image of the image; (d) For example 1 of the invention, thick layer PdSe 2 Raman spectrum of (2), raman shift in cm on the abscissa -1 The ordinate is intensity. The Raman spectral peak positions of FIGS. 8 (b) and 8 (d) show that example 1 of the present invention was prepared as PdSe 2 And (3) single crystals.
Experimental example 4PdSe 2 Optical microscopy, IV curve and field effect deviceField effect curve
PdSe prepared from inventive example 1 2 PdSe prepared by preparing metal electrode from single crystal through mechanical stripping and micro-nano processing 2 Field effect device for preparing PdSe 2 The device was subjected to optical microscopy and electrical analysis, respectively.
As shown in FIG. 9, pdSe prepared in example 1 of the present invention 2 Device optical microscopy, IV and field effect curves, wherein (a) is PdSe prepared in example 1 of the present invention 2 An optical photograph of the device; (b) PdSe prepared for example 1 of the present invention 2 IV graph of device, abscissa V bg (V) ordinate I ds (nA); (c) PdSe prepared for example 1 of the present invention 2 Field effect plot of the device. As is known from FIG. 9 (c), pdSe is obtained 2 The film has better bipolar property and higher electron and hole mobility.
While the present invention has been described in detail through the foregoing description of the preferred embodiment, it should be understood that the foregoing description is not to be considered as limiting the invention. Many modifications and substitutions of the invention will now become apparent to those skilled in the art upon reading the foregoing. Accordingly, the scope of the invention should be limited only by the attached claims.
Claims (2)
1. A method for preparing a palladium diselenide single crystal using an oscillation temperature, the method comprising:
(1) Tabletting Pd and Se mixture, and vacuum-maintaining at 1×10 -3 ～5×10 -4 Sealing in Pa environment, reacting at 1100 deg.C to obtain polycrystal PdSe 2 ；
The mass ratio of Pd to Se is 1:2;
(2) The polycrystal PdSe obtained in the step (1) is processed 2 Mixing with Se, tabletting, and vacuum-maintaining at 1×10 -3 ～5×10 -4 Sealing in Pa environment, and oscillating at high temperature of 790-810 deg.C and low temperature of 640-660 deg.C to obtain PdSe 2 A single crystal;
the oscillation temperature refers to oscillation of the high-temperature area and the low-temperature area with the same oscillation temperature amplitude and oscillation time period;
the temperature of the high temperature region is 800 ℃, the temperature of the low temperature region is 650 ℃, the oscillation temperature amplitudes of the high temperature region and the low temperature region are 10 ℃, namely the variation range of the high temperature region is 790-810 ℃, and the variation range of the low temperature region is 640-660 ℃;
the oscillation time period is 24 hours;
the polycrystalline PdSe 2 The mass ratio to Se is 1:0.5.
2. The method according to claim 1, wherein in step (2), the total time of the oscillation temperature growth is 7 to 9 days.
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| CN102779597A (en) * | 2011-05-10 | 2012-11-14 | 江苏新澳电力技术有限公司 | Composite housed lightning arrester with disconnector |
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| Palladium Diselenide Long-Wavelength Infrared Photodetector with High Sensitivity and Stability;Mingsheng Long et al.;《ACS NANO》;第2511-0219 * |
| PdSe2: Pentagonal Two-Dimensional Layers with High Air Stability for Electronics;Kai Xiao et al.;《JACS》;14090-04097 * |
| 基于界面效应调控的新型二维光电器件研究;谢柳;《中国博士学位论文全文数据库 工程科技Ⅰ辑》;参见第56页最后1段、第57页第4段、图3.19c * |
| 谢柳.基于界面效应调控的新型二维光电器件研究.《中国博士学位论文全文数据库 工程科技Ⅰ辑》.2021,参见第56页最后1段、第57页第4段、图3.19c. * |
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