CN104911714B - A kind of method that high hydrostatic pressure grows organic-inorganic composite semiconductor crystal - Google Patents
A kind of method that high hydrostatic pressure grows organic-inorganic composite semiconductor crystal Download PDFInfo
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Abstract
The present invention relates to a kind of method that high hydrostatic pressure grows organic-inorganic composite semiconductor crystal, including step are as follows：Organic-inorganic composite semiconductor powder is well mixed with a small amount of solvent, then sealing is placed under high hydrostatic pressure, is heated to 60~350 DEG C of constant temperature and carries out crystal growth in 6~720 hours, obtain organic-inorganic composite semiconductor crystal.On the one hand the method for the present invention can suppress the decomposition of organic-inorganic composite semiconductor by introducing high hydrostatic pressure, isotropic, without residual stress a environment on the other hand can be provided for crystal growth, and drive particle to be combined with each other and grow；Meanwhile, by adding a small amount of solvent in composite semiconductor, promote transporting and dissolving-recrystallization process for material molecule, it is easier to grow high-quality, large-sized organic-inorganic composite semiconductor crystal.
Description
Technical field
The present invention relates to a kind of method that high hydrostatic pressure grows Organic-inorganic composite semiconductor crystal, belong to semiconductor material
Material and device fabrication techniques field.
Background technology
With developing rapidly for present information and energy technology, the requirement to semi-conducting material is more and more harsher.For example, removing
It is required that material has outside high photoelectric transformation efficiency and carrier mobility, require that material has a high stabilization toward contact
Property, many combination properties such as wide scope Modulatory character of good machinability, low cost and structure and performance.From mesh
Preceding situation is seen, to fully meet these requirements, and single organic and inorganic materials all seem helpless.Naturally enough, people
It can attempt organic material and inorganic material being combined, by component regulation and control and structure and interphase match, by the advantage knot of the two
The Organic-inorganic composite semi-conducting material with excellent comprehensive performance is prepared altogether.In fact, by regulating and controlling organic and nothing
The structure of machine component and composite semiconductor, composite semiconductor can have structure diversity, the easy processing of organic material simultaneously
Property, the high carrier mobility of high efficiency and inorganic material, band gap adjustability, high mechanical strength, various dielectric property
Etc..And the collaboration optimization function of two kinds of components, abundant structure type and significant new property can be produced again and new existing
As providing the material of high-quality for new generation high-performance, inexpensive composite semiconductor photoelectric functional device.But, organic-nothing
Machine composite semiconductor is easily decomposed and lacks suitable solvent when heated so that growing mixed semiconductor crystal and prepare film
Extreme difficulties are run into during device.Therefore, develop new method growth Organic-inorganic composite semiconductor crystal, be the energy and information
Technology provides the composite semiconductor material with excellent comprehensive performance, is the work with important actual application value.
Generally when growing organic and inorganic semiconductor crystal, the main method used can be divided into melting-recrystallization,
The major class of dissolution-recrystallization two, this two classes method requires that material either with very high heat endurance or can be dissolved in conjunction
In suitable solvent.But, for Organic-inorganic composite semi-conducting material, because their heat endurance is poor, and
It is difficult to suitable solvent is found, therefore above-mentioned two classes method is met when for growing Organic-inorganic composite semiconductor crystalline material
Very big difficulty is arrived.In order to grow Organic-inorganic composite semiconductor crystal, it is necessary to solve two crucial problems：One is to prevent to have
The decomposition of machine-inorganic composite semiconductor material, two, which are to provide condition, promotes composite semiconductor constantly to grow up.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of high hydrostatic pressure growth Organic-inorganic composite semiconductor crystal
Method, this method suppresses the decomposition of Organic-inorganic composite semi-conducting material by applying high pressure, and drives particle mutually to tie
Close and grow；Meanwhile, add a small amount of solvent and isotropic fluid-like state growing environment be provided, reduce and even eliminate residual stress,
Improve the crystalline quality of Organic-inorganic composite semiconductor crystal.
Technical scheme is as follows：
A kind of method that high hydrostatic pressure grows Organic-inorganic composite semiconductor crystal, including step are as follows：
(1) Organic-inorganic composite Semiconductor Powder and solvent are pressed into mass volume ratio 1：The ratio mixing of (1~2000) is equal
It is even, obtain mixture, unit：Gram/microlitre,
(2) mixture sealing made from step (1) is placed under high hydrostatic pressure, described high hydrostatic pressure pressure is：20~
600MPa, pressurize is heated to 60~350 DEG C of constant temperature and carries out crystal growth in 6~720 hours, natural after crystal growing process terminates
Room temperature is cooled to, recovers normal pressure, produces Organic-inorganic composite semiconductor crystal.
Currently preferred, described Organic-inorganic composite semi-conducting material is substitution bipyridyl-iodine complex, substitution
Bipyridyl-metal halide complex, organic amine-metal halide complex or acridine-metal halide complex.
It is further preferred that described substitution bipyridyl-iodine complex is dibutyl bipyridyl-I2Complex, it is described
Substitution bipyridyl-metal halide complex is picoline-stannic chloride, dibutyl bipyridyl-iodate lead source or two fourths
Base bipyridyl-stannic iodide complex, described organic amine-metal halide complex is chloroaniline-iodate lead source, bromobenzene
Amine-iodate lead source or bromaniline-chlorination lead source, described acridine-metal halide complex are acridine-cadmium iodide
Complex.
Currently preferred, the solvent is alcohols, amine, sulfoxide type, ketone, esters, aromatic hydrocarbon or alkane.
It is further preferred that alcohols is methanol or ethanol, amine is dimethylformamide (DMF), and sulfoxide type is dimethyl
Sulfoxide (DMSO), ketone is acetone, and esters are ethyl acetate or butyl acetate, and aromatic hydrocarbon is ortho-xylene, and alkane is n-hexane.
Currently preferred, in step (2), the pressure of high hydrostatic pressure is：120~600MPa, it is further preferably, high quiet
The pressure of pressure is：250~360MPa.
Currently preferred, in step (2), heating-up temperature is：100~300 DEG C, constant temperature time：48~600h, further
It is preferred that, heating-up temperature is：150~240 DEG C, constant temperature time：100~200h.
It is currently preferred, a kind of method that high hydrostatic pressure grows Organic-inorganic composite semiconductor crystal, including step is such as
Under：
(1) Organic-inorganic composite Semiconductor Powder and solvent are pressed into mass volume ratio 1：The ratio mixing of (1~2000) is equal
It is even, obtain mixture, unit：Gram/microlitre,
(2) mixture made from step (1) is wrapped up with fexible film, sealed, is subsequently placed in autoclave, filled
Liquid transmission medium, applies pressure, and pressure is：20~600MPa, 60~350 DEG C of constant temperature 6~720 are heated to by autoclave
Hour, after crystal growing process terminates, room temperature is naturally cooled to, recovers normal pressure, produces Organic-inorganic composite semiconductor crystal.
Currently preferred, fexible film is plastic sheeting, rubber film, polytetrafluoroethylene film or gold in step (2)
Belong to paper tinsel.
It is currently preferred, in step (2) liquid transmission medium be silicone oil, esters, alcohols, benzene, substituted benzene, amide-type or
Alkane.
The Organic-inorganic composite semiconductor crystal of above method growth is used for composite semiconductor microelectronic switch, photophore
In the development of the photoelectric functional device such as part and photovoltaic device.
Beneficial effects of the present invention：
On the one hand the method for the present invention can suppress the decomposition of Organic-inorganic composite semiconductor by introducing high hydrostatic pressure,
On the other hand isotropic, without residual stress a environment can be provided for crystal growth, and drives particle to be combined with each other
And growth；Meanwhile, by adding a small amount of solvent in composite semiconductor, promote transporting and dissolve-repreparation mistake for material molecule
Journey, it is easier to grow high-quality, large-sized Organic-inorganic composite semiconductor crystal.
Brief description of the drawings
Fig. 1 is the dibutyl bipyridyl-I in embodiment 12Complex, the Organic-inorganic composite semiconductor crystal prepared
X-ray diffraction spectrogram.
Fig. 2 is the dibutyl bipyridyl-I in embodiment 122Complex, the Organic-inorganic composite semiconductor crystal prepared
X-ray diffraction spectrogram.
Fig. 3 is the dibutyl bipyridyl-I in embodiment 12Complex, the Organic-inorganic composite semiconductor crystal prepared
Infrared absorpting light spectra.
Fig. 4 is the dibutyl bipyridyl-I in embodiment 12The TG-DTA curve of complex at ambient pressure.
Fig. 5 is the dibutyl bipyridyl-I in embodiment 12Complex, the Organic-inorganic composite semiconductor crystal prepared
SEM shape appearance figures, wherein, (a) is dibutyl bipyridyl-I2Coordinate the SEM shape appearance figures of raw material, (b) is the organic and inorganic prepared
The SEM shape appearance figures of compound semiconductor crystal.
Embodiment
The technology of the present invention is described further with reference to embodiment and accompanying drawing.
The raw material dibutyl bipyridyl-I used in embodiment2Complex, acridine-iodate cadmium complex, chloroaniline-iodate
Lead source, bromaniline-iodate lead source, dibutyl bipyridyl-iodate lead source, dibutyl bipyridyl-stannic iodide are matched somebody with somebody
Compound, picoline-stannic chloride, bromaniline-chlorination lead source, market are bought, and can be also made by prior art.
Picoline-stannic chloride is made by prior art, referring to Crystal structure of bis (4-
methylpyridinium)hexachlorotin(IV),(C6H8N)2SnCl6,Z.Kristallogr.NCS 2009,224
(1),79-80.
Chlorobenzene ammonium-lead iodide (bromaniline-lead iodide, bromaniline-lead chloride) is made by prior art, referring to Crystal
Structure of bis (4-chloroanilinium) tetra iodoplumbate (II), (ClC6H4NH3) 2PbI4,
Z.Kristallogr.NCS 2004,219,457-458
Dibutyl bipyridyl-I2, (dibutyl bipyridyl-lead iodide, dibutyl bipyridyl stannic iodide) presses prior art system
, referring to：The research of organic-inorganic composite based on 4,4'- bipyridyls, Zhao Dan, 2012-05-24, master.
Acridine-cadmium iodide source is made by prior art, referring to the knot of corrdination type organic/inorganic composite semiconductor material
Structure and property research, Wang Wei, Tsing-Hua University, 2009-04-01, doctor.
Embodiment 1：
A kind of method that high hydrostatic pressure grows Organic-inorganic composite semiconductor crystal, including step are as follows：
(1) by 0.1g dibutyl bipyridyls-I2Coordinate powder to be well mixed with 0.5 microlitre of ethanol, obtain mixture,
(2) mixture made from step (1) is wrapped up with polytetrafluoroethylene film, sealed, the sample of good seal is placed in
In autoclave, sealed after filling silicon oil, apply 250MPa pressure, autoclave is heated to 200 DEG C of constant temperature 48 hours
Growth crystal is carried out, after crystal growing process terminates, room temperature is naturally cooled to, recovers normal pressure, produce dibutyl bipyridyl-I2Match somebody with somebody
Solvate crystal.
Dibutyl bipyridyl-I made from the present embodiment2The XRD of complex crystal is as shown in figure 1, infrared absorpting light spectra
As shown in Figure 3.
By the raw material dibutyl bipyridyl-I in embodiment 12Coordinate powder under the atmosphere that nitrogen is protected, with 10 DEG C/
Min heating rate, thermogravimetric differential thermal under normal pressure is carried out in the range of -800 DEG C of room temperature and is tested, test effect is as shown in Figure 4.By
Fig. 4 is understood, below 200 DEG C, and thermogravimetric curve keeps level substantially, there is an endothermic peak appearance, two fourths while starting weightless
Base bipyridyl-I2There is obvious decomposing phenomenon in complex.
Dibutyl bipyridyl-I obtained by the present embodiment2Complex crystal SEM photograph joins pyrrole as shown in figure 5, figure a is dibutyl
Pyridine-I2Complex morphology microstructure, complex is in granular form, and particle size is at 2 μm or so, and figure b is dibutyl bipyridyl-I2Coordinate
Thing crystal, particle be combined with each other crystal boundary disappearance, and crystal structure size significantly increases.
Embodiment 2:Preparation method is same as Example 1, except that：The addition of ethanol is 20 microlitres.
Embodiment 3:Preparation method is same as Example 1, except that：The addition of ethanol increases to 80 microlitres.
Embodiment 4:Preparation method is same as Example 1, except that：The addition of ethanol becomes 200 microlitres.
Embodiment 5:Preparation method is same as Example 1, except that：The pressure for applying high hydrostatic pressure is 120MPa.
Embodiment 6:Preparation method is same as Example 1, except that：The pressure for applying high hydrostatic pressure is 320MPa.
Embodiment 7:Preparation method is same as Example 1, except that：The pressure for applying high hydrostatic pressure is 600MPa.
Embodiment 8:Preparation method is same as Example 1, except that：Change polytetrafluoroethylene film into plastics thin
Film.
Embodiment 9:Preparation method is same as Example 1, except that：Change polytetrafluoroethylene film into gold thin film.
Embodiment 10:Preparation method is same as Example 1, except that：Heating-up temperature is 60 DEG C.
Embodiment 11:Preparation method is same as Example 1, except that：Heating-up temperature is 150 DEG C.
Embodiment 12:Preparation method is same as Example 1, except that：Heating-up temperature is 240 DEG C.
Embodiment 13:Preparation method is same as Example 1, except that：Heating-up temperature is 350 DEG C.
Embodiment 14:Preparation method is same as Example 1, except that：Crystal constant temperature growth time is 6 hours.
Embodiment 15:Preparation method is same as Example 1, except that：Crystal constant temperature growth time is 200 hours.
Embodiment 16:Preparation method is same as Example 1, except that：Crystal constant temperature growth time is 720 hours.
Embodiment 17:Preparation method is same as Example 1, except that：Change etoh solvent into ortho-xylene, neighbour two
The addition of toluene is 20 microlitres.
Embodiment 18:Preparation method is same as Example 1, except that：Change etoh solvent into dimethyl sulfoxide (DMSO)
(DMSO), the addition of dimethyl sulfoxide (DMSO) (DMSO) is 20 microlitres.
Embodiment 19:Preparation method is same as Example 1, except that：Change etoh solvent into methanol, methanol adds
Dosage is 8 microlitres.
Embodiment 20:Preparation method is same as Example 1, except that：The addition of ethanol is changed into 20 microlitres, liquid
Transmission medium changes ethyl acetate into by silicone oil.
Embodiment 21:Preparation method is same as Example 1, except that：Ethanol addition increases to 50 microlitres, liquid
Transmission medium changes butyl acetate into by silicone oil.
Embodiment 22:Preparation method is same as Example 1, except that：The addition of ethanol increases to 20 microlitres, biography
Pressure medium silicone oil is replaced by DMF.
Embodiment 23:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is dibutyl bipyridyl-I3Complex, etoh solvent changes acetone into, and addition is 10 microlitres.
Embodiment 24:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is dibutyl bipyridyl-I3Complex, the addition of ethanol is 80 microlitres.
Embodiment 25:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is dibutyl bipyridyl-I3Complex, the addition of ethanol is 200 microlitres.
Embodiment 26:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is acridine-iodate cadmium complex.
Embodiment 27:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is acridine-iodate cadmium complex, and the addition of ethanol is 20 microlitres, and the pressure for applying high hydrostatic pressure is 120MPa.
Embodiment 28:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is acridine-iodate cadmium complex, and ethanol addition is 50 microlitres, and the pressure for applying high hydrostatic pressure is 320MPa.
Embodiment 29:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is acridine-iodate cadmium complex, and the pressure for applying high hydrostatic pressure is 600MPa.
Embodiment 30:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is parachloroanilinum-iodate lead source.
Embodiment 31:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is parachloroanilinum-iodate lead source, and the addition of ethanol is 20 microlitres, and it is thin that polytetrafluoroethylene film changes plastics into
Film.
Embodiment 32:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is parachloroanilinum-iodate lead source, and the addition of ethanol is 120 microlitres, and polytetrafluoroethylene film changes gold thin film into.
Embodiment 33:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is para-bromoaniline-iodate lead source, and ethanol addition is 130 microlitres, and heating-up temperature is 60 DEG C.
Embodiment 34:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is para-bromoaniline-iodate lead source, and etoh solvent changes methanol into, and the addition of methanol is 80 microlitres, heating-up temperature
For 150 DEG C.
Embodiment 35:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is para-bromoaniline-iodate lead source, and etoh solvent changes methanol into, and the addition of methanol is 20 microlitres, heating-up temperature
For 240 DEG C.
Embodiment 36:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is dibutyl bipyridyl-iodate lead source, and etoh solvent addition is 60 microlitres, and crystal constant temperature growth time is 6
Hour.
Embodiment 37:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is dibutyl bipyridyl-iodate lead source, and etoh solvent is replaced by dimethylformamide (DMF), dimethyl formyl
The addition of amine (DMF) is 10 microlitres, and crystal constant temperature growth time is 200 hours.
Embodiment 38:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is dibutyl bipyridyl-iodate lead source, and crystal constant temperature growth time is 720 hours.
Embodiment 39:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is dibutyl bipyridyl-stannic iodide complex, and ethanol changes ortho-xylene into, and the addition of ortho-xylene is 20 microlitres.
Embodiment 40:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is dibutyl bipyridyl-stannic iodide complex, and ethanol changes dimethyl sulfoxide (DMSO) (DMSO) into, dimethyl sulfoxide (DMSO) (DMSO)
Addition is 6 microlitres.
Embodiment 41:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is dibutyl bipyridyl-stannic iodide complex, and ethanol changes methanol into, and the addition of methanol is 90 microlitres.
Embodiment 42:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is picoline-stannic chloride complex.
Embodiment 43:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is picoline-stannic chloride complex, and transmission medium changes ethyl acetate into by silicone oil.
Embodiment 44:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is picoline-stannic chloride complex, and transmission medium changes n-hexane into by silicone oil.
Embodiment 45:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is picoline-stannic chloride complex, and transmission medium changes benzene into by silicone oil.
Embodiment 46:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is para-bromoaniline-chlorination lead source.
Embodiment 47:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is para-bromoaniline-chlorination lead source, and the pressure for applying high hydrostatic pressure is 120MPa.
Embodiment 48:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is para-bromoaniline-chlorination lead source, and polytetrafluoroethylene film changes plastic sheeting into.
Embodiment 49:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is para-bromoaniline-chlorination lead source, and polytetrafluoroethylene film changes silicon rubber film into, and heating-up temperature is 60 DEG C.
Embodiment 50:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is para-bromoaniline-chlorination lead source, and crystal constant temperature growth time is 200 hours.
Embodiment 51:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is para-bromoaniline-chlorination lead source, and etoh solvent changes ortho-xylene into.
Embodiment 52:Preparation method is same as Example 1, except that：Organic-inorganic composite is partly led in step (1)
Body powder is para-bromoaniline-chlorination lead source, and transmission medium silicone oil changes dimethylbenzene into.
Claims (7)
1. a kind of method that high hydrostatic pressure grows Organic-inorganic composite semiconductor crystal, including step are as follows：
（1）Organic-inorganic composite Semiconductor Powder and solvent are pressed into mass volume ratio 1：（1~2000）Ratio be well mixed, obtain
Mixture, unit：Gram/microlitre, described Organic-inorganic composite semi-conducting material is substitution bipyridyl-iodine complex, substitution connection
Pyridine-metal halide complex, organic amine-metal halide complex or acridine-metal halide complex；The solvent
For alcohols, amine, sulfoxide type, ketone, esters, aromatic hydrocarbon or alkane；
（2）By step（1）Obtained mixture sealing is placed under high hydrostatic pressure, and described high hydrostatic pressure pressure is：120~
600MPa, pressurize is heated to 100 ~ 300 DEG C of constant temperature and carries out crystal growth in 48 ~ 600h hours, after crystal growing process terminates, from
Room temperature is so cooled to, recovers normal pressure, produces Organic-inorganic composite semiconductor crystal.
2. the method that high hydrostatic pressure according to claim 1 grows Organic-inorganic composite semiconductor crystal, its feature exists
In alcohols is methanol or ethanol, and amine is dimethylformamide（DMF）, sulfoxide type is dimethyl sulfoxide (DMSO)（DMSO）, ketone is third
Ketone, esters are ethyl acetate or butyl acetate, and aromatic hydrocarbon is ortho-xylene, and alkane is n-hexane.
3. the method that high hydrostatic pressure according to claim 1 grows Organic-inorganic composite semiconductor crystal, its feature exists
In step（2）In, the pressure of the high hydrostatic pressure is：250~360MPa.
4. the method that high hydrostatic pressure according to claim 1 grows Organic-inorganic composite semiconductor crystal, its feature exists
In step（2）In, heating-up temperature is：150 ~ 240 DEG C, constant temperature time：100~200h.
5. the method that high hydrostatic pressure according to claim 1 grows Organic-inorganic composite semiconductor crystal, including step is such as
Under：
（1）Organic-inorganic composite Semiconductor Powder and solvent are pressed into mass volume ratio 1：（1~2000）Ratio be well mixed, obtain
Mixture, unit：Gram/microlitre,
（2）By step（1）Obtained mixture is wrapped up with fexible film, sealed, and is subsequently placed in autoclave, filling liquid
Transmission medium, applies pressure, and pressure is：20 ~ 600MPa, 60 ~ 350 DEG C of constant temperature is heated to 6 ~ 720 hours by autoclave, brilliant
After body growth course terminates, room temperature is naturally cooled to, recovers normal pressure, produces Organic-inorganic composite semiconductor crystal.
6. the method that high hydrostatic pressure according to claim 5 grows Organic-inorganic composite semiconductor crystal, its feature exists
In step（2）Middle fexible film is plastic sheeting, rubber film or metal foil.
7. the method that high hydrostatic pressure according to claim 5 grows Organic-inorganic composite semiconductor crystal, its feature exists
In step（2）Middle liquid transmission medium is silicone oil, esters, alcohols, benzene, substituted benzene, amide-type or alkane.
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