CN103343315A - Bismuth-ferrite-doped semiconductor film material and preparation method thereof - Google Patents

Bismuth-ferrite-doped semiconductor film material and preparation method thereof Download PDF

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CN103343315A
CN103343315A CN2013102239296A CN201310223929A CN103343315A CN 103343315 A CN103343315 A CN 103343315A CN 2013102239296 A CN2013102239296 A CN 2013102239296A CN 201310223929 A CN201310223929 A CN 201310223929A CN 103343315 A CN103343315 A CN 103343315A
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骆溁
陈江鹏
马赫
袁国亮
刘治国
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Nanjing University of Science and Technology
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Abstract

The invention discloses a bismuth-ferrite-doped semiconductor film material and a preparation method thereof. The film material is a n type semiconductor with a molecular formula of BiFe1-xAxO3, wherein x is 0.0005-0.5, A is one or two of Nb and Mn, the thickness of the film material is 15-500 nm, the resistivity is 8.6*10<-5> - 3*10<-3> omega*cm, and the n type carrier concentration is 1.4*10<19>-1.6*10<22> cm<-3>. By adjusting the doping amount, the semiconductor performances comprising the resistivity, the n type carrier concentration and the like are accurately regulated and controlled, and therefore the bismuth-ferrite-doped semiconductor film material possesses tremendous practical application value in the fields of electronic components, photoelectric detectors, solar energy cells and the like.

Description

A kind of doped bismuth ferrite semiconductor film material and preparation method thereof
Technical field
The invention belongs to the semiconductor film material field, relate to a kind of doped bismuth ferrite semiconductor film material and preparation method thereof.
Background technology
Ferroelectric material refers to have the material of spontaneous polarization when being lower than Curie temperature, its spontaneous polarization direction can redirect under the extra electric field greater than ferroelectric coercive field.It is isolator under the ferroelectric material normal temperature.
Resistivity is between good conductor and isolator and have the material of negative temperature coefficient of resistance to be called semi-conductor, semi-conductive application is very extensive, mainly be the components and parts of making specific function, as field-effect transistor, diode, rectifier, vibrator and various photoelectric detector, microwave device, solar cell etc.
Doping in the semi-conductor term refers to control the quantity of special impurities atom, thereby on purpose increases the concentration in electronics or hole.Can forever change the electroconductibility of material by mixing, thereby to be semi-conductor can make the great reason that various devices obtain widespread uses for this.
Through suitable doping, ferroelectric insulator can become n type or p-type semi-conductor.
Have the minority Chinese patent to introduce the integrated and compatible of ferroelectric material and semiconducter substrate, perhaps part involves the semiconducting behavior in other material.For example, Chinese patent CN101315881A makes heterojunction with ferroelectric material Lithium niobium trioxide and III hi-nitride semiconductor material, prepared the Ferro-Electric Semiconductor laminated film based on " Lithium niobium trioxide/III group-III nitride ", prepare concrete device by semiconductor device technology, it just is combined into heterojunction with ferroelectric material and another kind of semiconductor material.The patent of introducing the preparation of Ferro-Electric Semiconductor material and various application thereof is also few.Chinese patent CN1276439A has introduced a kind of method for preparing the Nb-doped barium titanate film, has prepared the different barium titanate films of mixing content of niobium, the ferroelectric thin-flim materials that obtains having metalline.Chinese patent CN102157682A is at Pb (Zr xTi 1-x) O 3, Ba (Sr xTi 1-x) O 3, Bi 1-xA xFe 1-yB yO 3In mix Cr, Mn, Co, one or more trivalent transition metal ions of Ni and Cu utilize iron electric polarization to regulate and control its semiconducting behavior.
Summary of the invention
The purpose of this invention is to provide ferrous acid bismuth semiconductor film material of a kind of regulation and control resistivity of mixing and preparation method thereof.Utilize the change of doping, the resistivity of accuracy controlling bismuth ferrite thin film makes it controllably to be changed to the n N-type semiconductorN by isolator.
The technical scheme that realizes the object of the invention is: a kind of doped bismuth ferrite semiconductor film material, its thin-film material are the n N-type semiconductorN, and molecular formula is BiFe 1-xA xO 3, wherein x is 0.0005-0.5, A is one or both in Nb or the Mn element.
Described semiconductor film material thickness is 15-500nm, and resistivity is 8.6 * 10 -5-3 * 10 -3Ω cm, n type carrier concentration is 1.4 * 10 19-1.6 * 10 22Cm -3
A kind of preparation method of doped bismuth ferrite semiconductor film material may further comprise the steps:
(1) BiFe 1-xA xO 3The preparation of target: with Bi 2O 3, Fe 2O 3With the oxide compound of A correspondence be raw material, press each element chemistry metering of compound than weighing oxide compound, wherein, x is 0.0005-0.5 in the compound, A is one or both in Nb or the Mn element, and the oxide compound that weighs up is put into ball grinder, ball milling behind the adding alcohol, the process furnace sintering is put in the material oven dry that ball milling is good behind the compression molding;
(2) BiFe 1-xA xO 3The preparation of film: adopt physical vaporous deposition, the target in substrate and the step 1 is fit in the growth chamber, vacuumize, after oxygen is pressed in adjusting underlayer temperature and the growth chamber, earlier pre-sputter, deposit film again;
(3) 10 -5-10 5Pa oxygen is depressed annealing.
Ratio of grinding media to material described in the step (1) is 3:1, and the described ball milling time is 6-10 hour, and described sintering temperature is 800-900 ℃, and sintering time is 0.5-2 hour.
Physical vaporous deposition described in the step (2) is pulsed laser deposition, laser molecular beam epitaxy method or magnetron sputtering method.
Substrate described in the step (2) is SrTiO 3, DyScO 3, LaAlO 3Perhaps NdGaO 3, underlayer temperature is 300-700 ℃, and oxygen is pressed and is 0.1-100Pa in the growth chamber, and pre-sputtering time is 3-15 minute.
In described pulsed laser deposition and the laser molecular beam epitaxy method, energy of lasers is 30-300mJ, and frequency is at 1-10Hz.
In the described magnetron sputtering method, sputtering power is 100-1500W.
Annealing temperature described in the step (3) is 300-700 ℃, and annealing time is 10-200 minute.
The present invention successfully adopts the mode of doping, carries out effective regulation and control of ferrous acid bismuth resistivity, obtains its semiconducting behavior.This is different from existing some patent need be with a kind of ferroelectric material and the integrated method of another kind of semiconductor material.Ferrous acid bismuth semiconductor film material provided by the invention, increased the selection degree of freedom of semiconductor applications designs greatly, its semiconducting behavior parameter can realize that scope is big, can change by doping and come accuracy controlling, the ferrous acid bismuth semiconductor film of all size can be provided as required, can be used for fields such as electronic devices and components, photodetector and solar cell.
Description of drawings
Fig. 1 is for being grown in SrTiO 3BiFe on the substrate 0.9995Nb 0.0005O 3The macroscopic cross section structural representation of film.
Fig. 2 is for being grown in SrTiO 3BiFe on the substrate 0.9995Nb 0.0005O 3The X ray diffracting spectrum of film.
Fig. 3 is for being grown in SrTiO 3BiFe on the substrate 0.8Nb 0.2O 3The X ray diffracting spectrum of film.
Fig. 4 is for being grown in SrTiO 3BiFe on the substrate 0.5Nb 0.5O 3The X ray diffracting spectrum of film.
Fig. 5 is for being grown in SrTiO 3BiFe on the substrate 0.9995Mn 0.0005O 3The X ray diffracting spectrum of film.
Fig. 6 is for being grown in SrTiO 3BiFe on the substrate 0.7Mn 0.3O 3The X ray diffracting spectrum of film.
Fig. 7 is for being grown in SrTiO 3BiFe on the substrate 0.5Mn 0.5O 3The X ray diffracting spectrum of film.
Fig. 8 is for being grown in SrTiO 3BiFe on the substrate 0.6Nb 0.2Mn 0.2O 3The X ray diffracting spectrum of film.
Embodiment
Example 1:
Choose x=0.0005, the thick BiFe of preparation 15nm 0.9995Nb 0.0005O 3Film:
(1) preparation BiFe 0.9995Nb 0.0005O 3Target.The Bi of the corresponding proportioning of weighing 2O 3, Fe 2O 3, Nb 2O 5, put into ball grinder, according to the ratio of grinding media to material of total mass ratio 3:1, add the ball milling pearl, add alcohol then, ball milling 6 hours.The material oven dry that ball milling is good, compression molding is put into the process furnace sintering.800 ℃ of sintering temperatures, sintering time 0.5 hour.
(2) adopt pulsed laser deposition to prepare film.With (001) orientation SrTiO 3As substrate, growing epitaxial BiFe 0.9995Nb 0.0005O 3Film.Substrate and target are fit in the growth chamber, utilize mechanical pump and molecular pump to be pumped into the 0.0001Pa vacuum subsequently, pre-sputter is after 3 minutes, and BiFe grows 0.9995Nb 0.0005O 3Layer, 300 ℃ of underlayer temperatures, air pressure 0.1Pa, laser energy 30mJ, frequency 1Hz.Thin film deposition finishes the back 10 -5Pa oxygen is pressed, and anneals 10 minutes down for 300 ℃.Treat to take out after temperature drops to room temperature, take out film, cover mask plate and put into growth chamber again, growth Pt top electrode.Wherein, underlayer temperature is room temperature, laser energy 300mJ, vacuum pressure 10 -5Pa, frequency 1Hz.Film macroscopic cross section structural representation as shown in Figure 1.
(3) to prepared BiFe 0.9995Nb 0.0005O 3Film carries out the X-ray diffraction test.X ray diffracting spectrum as shown in Figure 2, at SrTiO 3The BiFe that grows on the substrate 0.9995Nb 0.0005O 3The epitaxial film lattice match is good, no dephasign.
(4) adopt the Hall effect instrument to test the electric property of prepared film.Resistivity 3 * 10 -3Ω cm, n type carrier concentration 1.4 * 10 19Cm -3
Example 2:
Choose x=0.2, the thick BiFe of preparation 200nm 0.8Nb 0.2O 3Film:
(1) preparation BiFe 0.8Nb 0.2O 3Target.The Bi of the corresponding proportioning of weighing 2O 3, Fe 2O 3, Nb 2O 5, put into ball grinder, according to the ratio of grinding media to material of total mass ratio 3:1, add the ball milling pearl, add alcohol then, ball milling 8 hours.The material oven dry that ball milling is good, compression molding is put into the process furnace sintering.850 ℃ of sintering temperatures, sintering time 1 hour.
(2) adopt pulsed laser deposition to prepare film.With (001) orientation SrTiO 3As substrate, growing epitaxial BiFe 0.8Nb 0.2O 3Film.Substrate and target are fit in the growth chamber, utilize mechanical pump and molecular pump to be pumped into 10 subsequently -4Pa vacuum, pre-sputter are after 10 minutes, and BiFe grows 0.8Nb 0.2O 3Layer, 500 ℃ of underlayer temperatures, air pressure 10Pa, laser energy 100mJ, frequency 5Hz.Thin film deposition finishes the back presses at 1000Pa oxygen, anneals 100 minutes down for 500 ℃.Treat to take out after temperature drops to room temperature, take out film, cover mask plate and put into growth chamber again, growth Pt top electrode.Wherein, underlayer temperature is room temperature, laser energy 300mJ, vacuum pressure 10 -5Pa, frequency 1Hz.
(3) to prepared BiFe 0.8Nb 0.2O 3Film carries out the X-ray diffraction test.X ray diffracting spectrum as shown in Figure 3, at SrTiO 3The BiFe that grows on the substrate 0.8Nb 0.2O 3The epitaxial film lattice match is good, no dephasign.
(4) adopt the Hall effect instrument to test the electric property of prepared film.Resistivity 1.1 * 10 -4Ω cm, n type carrier concentration 6.2 * 10 21Cm -3
Example 3:
Choose x=0.5, the thick BiFe of preparation 500nm 0.5Nb 0.5O 3Film:
(1) preparation BiFe 0.5Nb 0.5O 3Target.The Bi of the corresponding proportioning of weighing 2O 3, Fe 2O 3, Nb 2O 5, put into ball grinder, according to the ratio of grinding media to material of total mass ratio 3:1, add the ball milling pearl, add alcohol then, ball milling 10 hours.The material oven dry that ball milling is good, compression molding is put into the process furnace sintering.900 ℃ of sintering temperatures, sintering time 2 hours.
(2) adopt pulsed laser deposition to prepare film.With (001) orientation SrTiO 3As substrate, growing epitaxial BiFe 0.5Nb 0.5O 3Film.Substrate and target are fit in the growth chamber, utilize mechanical pump and molecular pump to be evacuated subsequently, pre-sputter is after 15 minutes, and BiFe grows 0.5Nb 0.5O 3Layer, 700 ℃ of underlayer temperatures, oxygen is pressed 100Pa, laser energy 300mJ, frequency 10Hz.The growth finish after 10 5Pa oxygen is pressed, and anneals 200 minutes down for 700 ℃.When waiting to be cooled to room temperature, take out film, cover mask plate, put into growth chamber, temperature is raised to 200 ℃, regulate the oxygen pressure and be 13Pa, laser energy 200mJ, frequency 3Hz, growth ITO electrode.
(3) to prepared BiFe 0.5Nb 0.5O 3Film carries out the X-ray diffraction test.X ray diffracting spectrum as shown in Figure 4, at SrTiO 3The BiFe that grows on the substrate 0.5Nb 0.5O 3The epitaxial film lattice match is good, no dephasign.
(4) adopt the Hall effect instrument to test the electric property of prepared film.Resistivity 8.6 * 10 -5Ω cm, n type carrier concentration 1.4 * 10 22Cm -3
Example 4:
Choose x=0.0005, the thick BiFe of preparation 15nm 0.9995Mn 0.0005O 3Film:
(1) preparation BiFe 0.9995Mn 0.0005O 3Target.The Bi of the corresponding proportioning of weighing 2O 3, Fe 2O 3, Mn 2O 5, put into ball grinder, according to the ratio of grinding media to material of total mass ratio 3:1, add the ball milling pearl, add alcohol then, ball milling 6 hours.The material oven dry that ball milling is good, compression molding is put into the process furnace sintering.800 ℃ of sintering temperatures, sintering time 0.5 hour.
(2) prepare BiFe with magnetron sputtering method 0.9995Mn 0.0005O 3Film.With (001) orientation SrTiO 3As substrate, growing epitaxial BiFe 0.9995Mn 0.0005O 3Film.Substrate and target are fit in the growth chamber, utilize mechanical pump and molecular pump to be pumped into the 0.0001Pa vacuum subsequently, pre-sputter is after 3 minutes, and BiFe grows 0.9995Mn 0.0005O 3Layer, 300 ℃ of underlayer temperatures, oxygen is pressed 0.1Pa, and sputtering power is 100W.Thin film deposition finishes the back at 300 ℃, and 1000Pa oxygen is depressed annealing 10 minutes, takes out after waiting to drop to room temperature, takes out film, cover mask plate and put into growth chamber again, growth Pt top electrode, wherein, underlayer temperature is room temperature, and sputtering power is 500W, vacuum pressure 0.0001Pa.
(3) to prepared BiFe 0.9995Mn 0.0005O 3Film carries out the X-ray diffraction test.X ray diffracting spectrum as shown in Figure 5, at SrTiO 3The BiFe that grows on the substrate 0.9995Mn 0.0005O 3The epitaxial film lattice match is good, no dephasign.
(4) adopt the Hall effect instrument to test the electric property of prepared film.Resistivity 2.8 * 10 -3Ω cm, n type carrier concentration 1.5 * 10 19Cm -3
Example 5:
Choose x=0.3, the thick BiFe of preparation 300nm 0.7Mn 0.3O 3Film:
(1) preparation BiFe 0.7Mn 0.3O 3Target.The Bi of the corresponding proportioning of weighing 2O 3, Fe 2O 3, Mn 2O 5, put into ball grinder, according to the ratio of grinding media to material of total mass ratio 3:1, add the ball milling pearl, add alcohol then, ball milling 8 hours.The material oven dry that ball milling is good, compression molding is put into the process furnace sintering.850 ℃ of sintering temperatures, sintering time 1 hour.
(2) prepare BiFe with magnetron sputtering method 0.7Mn 0.3O 3Film.With (001) orientation SrTiO 3As substrate, growing epitaxial BiFe 0.7Mn 0.3O 3Film.Substrate and target are fit in the growth chamber, utilize mechanical pump and molecular pump to be pumped into the 0.0001Pa vacuum subsequently, pre-sputter is after 10 minutes, and BiFe grows 0.7Mn 0.3O 3Layer, 500 ℃ of underlayer temperatures, oxygen is pressed 26Pa, and sputtering power is 500W.Deposition finishes the back at 400 ℃, and 2000Pa oxygen is depressed annealing 80 minutes, takes out after waiting to drop to room temperature, takes out film, and cover mask plate and put into growth chamber again, growth Pt top electrode, wherein, underlayer temperature is room temperature, sputtering power is 500W, vacuum pressure 0.0001Pa.
(3) to prepared BiFe 0.7Mn 0.3O 3Film carries out the X-ray diffraction test.X ray diffracting spectrum as shown in Figure 6, at SrTiO 3The BiFe that grows on the substrate 0.7Mn 0.3O 3The epitaxial film lattice match is good, no dephasign.
(4) adopt the Hall effect instrument to test the electric property of prepared film.Resistivity 1.2 * 10 -4Ω cm, n type carrier concentration 5.7 * 10 21Cm -3
Example 6:
Choose x=0.5, the thick BiFe of preparation 500nm 0.5Mn 0.5O 3Film:
(1) preparation BiFe 0. 5Mn 0. 5O 3Target.The Bi of the corresponding proportioning of weighing 2O 3, Fe 2O 3, Mn 2O 5, put into ball grinder, according to the ratio of grinding media to material of total mass ratio 3:1, add the ball milling pearl, add alcohol then, ball milling 10 hours.The material oven dry that ball milling is good, compression molding is put into the process furnace sintering.900 ℃ of sintering temperatures, sintering time 2 hours.
(2) prepare BiFe with magnetron sputtering method 0.5Mn 0.5O 3Film.With (001) orientation SrTiO 3As substrate, growing epitaxial BiFe 0.5Mn 0.5O 3Film.Substrate and target are fit in the growth chamber, utilize mechanical pump and molecular pump to be pumped into the 0.0001Pa vacuum subsequently, pre-sputter is after 15 minutes, and BiFe grows 0.5Mn 0.5O 3Layer, 700 ℃ of underlayer temperatures, oxygen is pressed 100Pa, and sputtering power is 500W.Deposition finishes the back at 700 ℃, and 1000Pa oxygen is depressed annealing 200 minutes, takes out after waiting to drop to room temperature, takes out film, and cover mask plate and put into growth chamber again, growth Pt top electrode, wherein, underlayer temperature is room temperature, sputtering power is 500W, vacuum pressure 10 5Pa.
(3) to prepared BiFe 0.5Mn 0.5O 3Film carries out the X-ray diffraction test.X ray diffracting spectrum as shown in Figure 7, at SrTiO 3The BiFe that grows on the substrate 0.5Mn 0.5O 3The epitaxial film lattice match is good, no dephasign.
(4) adopt the Hall effect instrument to test the electric property of prepared film.Resistivity 9 * 10 -5Ω cm, n type carrier concentration 1.6 * 10 22Cm -3
Example 7:
Choose x=0.2, the thick BiFe of preparation 400nm 0.6Nb 0.2Mn 0.2O 3Film:
(1) preparation BiFe 0.6Nb 0.2Mn 0.2O 3Target.The Bi of the corresponding proportioning of weighing 2O 3, Fe 2O 3, Nb 2O 5, Mn 2O 5, put into ball grinder, according to the ratio of grinding media to material of total mass ratio 3:1, add the ball milling pearl, add alcohol then, ball milling 7 hours.The material oven dry that ball milling is good, compression molding is put into the process furnace sintering.830 ℃ of sintering temperatures, sintering time 0.8 hour.
(2) adopt pulsed laser deposition to prepare film, with (001) orientation SrTiO 3As substrate, growing epitaxial BiFe 0.6Nb 0.2Mn 0.2O 3Film.Substrate and target are fit in the growth chamber, utilize mechanical pump and molecular pump to be evacuated subsequently, pre-sputter is after 5 minutes, and BiFe grows 0.6Nb 0.2Mn 0.2O 3Layer, 670 ℃ of underlayer temperatures, oxygen is pressed 13Pa, laser energy 70mJ, frequency 3Hz.Press at 1000Pa oxygen after growth is finished, annealed 30 minutes down for 650 ℃.When waiting to be cooled to room temperature, take out film, cover mask plate, put into growth chamber, temperature is raised to 200 ℃, regulate the oxygen pressure and be 13Pa, laser energy 200mJ, frequency 3Hz, growth ITO top electrode.
(3) to prepared BiFe 0.6Nb 0.2Mn 0.2O 3Film carries out the X-ray diffraction test.X ray diffracting spectrum as shown in Figure 8, at SrTiO 3The BiFe that grows on the substrate 0.6Nb 0.2Mn 0.2O 3The epitaxial film lattice match is good, no dephasign.
(4) adopt the Hall effect instrument to test the electric property of prepared film.Resistivity 9.8 * 10 -5Ω cm, n type carrier concentration 1.2 * 10 22Cm -3

Claims (9)

1. a doped bismuth ferrite semiconductor film material is characterized in that described thin-film material is the n N-type semiconductorN, and molecular formula is BiFe 1-xA xO 3, wherein x is 0.0005-0.5, A is one or both in Nb or the Mn element.
2. doped bismuth ferrite semiconductor film material according to claim 1 is characterized in that described semiconductor film material thickness is 15-500nm, and resistivity is 8.6 * 10 -5-3 * 10 -3Ω cm, n type carrier concentration is 1.4 * 10 19-1.6 * 10 22Cm -3
3. the preparation method of a doped bismuth ferrite semiconductor film material is characterized in that may further comprise the steps:
(1) BiFe 1-xA xO 3The preparation of target: with Bi 2O 3, Fe 2O 3With the oxide compound of A correspondence be raw material, press each element chemistry metering of compound than weighing oxide compound, wherein, x is 0.0005-0.5 in the compound, A is one or both in Nb or the Mn element, and the oxide compound that weighs up is put into ball grinder, ball milling behind the adding alcohol, the process furnace sintering is put in the material oven dry that ball milling is good behind the compression molding;
(2) BiFe 1-xA xO 3The preparation of film: adopt physical vaporous deposition, the target in substrate and the step 1 is fit in the growth chamber, vacuumize, after oxygen is pressed in adjusting underlayer temperature and the growth chamber, earlier pre-sputter, deposit film again;
(3) 10 -5-10 5Pa oxygen is depressed annealing.
4. the preparation method of doped bismuth ferrite semiconductor film material according to claim 3, it is characterized in that the ratio of grinding media to material described in the step 1 is 3:1, the described ball milling time is 6-10 hour, and described sintering temperature is 800-900 ℃, and sintering time is 0.5-2 hour.
5. the preparation method of doped bismuth ferrite semiconductor film material according to claim 3 is characterized in that the substrate described in the step 2 is SrTiO 3, DyScO 3, LaAlO 3Or NdGaO 3, underlayer temperature is 300-700 ℃, and oxygen is pressed and is 0.1-100Pa in the growth chamber, and pre-sputtering time is 3-15 minute.
6. the preparation method of doped bismuth ferrite semiconductor film material according to claim 3 is characterized in that the physical vaporous deposition described in the step 2 is pulsed laser deposition, laser molecular beam epitaxy method or magnetron sputtering method.
7. the preparation method of doped bismuth ferrite semiconductor film material according to claim 6 is characterized in that energy of lasers is 30-300mJ in described pulsed laser deposition and the laser molecular beam epitaxy method, and frequency is at 1-10Hz.
8. the preparation method of doped bismuth ferrite semiconductor film material according to claim 6 is characterized in that in the described magnetron sputtering method, and sputtering power is 100-1500W.
9. the preparation method of doped bismuth ferrite semiconductor film material according to claim 3 is characterized in that the annealing temperature described in the step 3 is 300-700 ℃, and annealing time is 10-200 minute.
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