CN101864556A - High dielectric coefficient titanium-aluminum oxide film and preparation method and application thereof - Google Patents

High dielectric coefficient titanium-aluminum oxide film and preparation method and application thereof Download PDF

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CN101864556A
CN101864556A CN 201010172490 CN201010172490A CN101864556A CN 101864556 A CN101864556 A CN 101864556A CN 201010172490 CN201010172490 CN 201010172490 CN 201010172490 A CN201010172490 A CN 201010172490A CN 101864556 A CN101864556 A CN 101864556A
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film
tio
preparation
aluminum oxide
ceramic target
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殷江
周越
汤振杰
夏奕东
刘治国
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Nanjing University
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Abstract

The invention relates to a high dielectric coefficient titanium-aluminum oxide film. The chemical formula of the film is (TiO2)x(Al2O3)1-x, wherein x is more than or equal to 0.2 and is less than or equal to 0.5. The preparation method is characterized in that: a pulse laser deposition technology is utilized, a (TiO2)x(Al2O3)1-x ceramic target material is utilized to prepare the film under high-vacuum low-oxygen partial pressure: the (TiO2)x(Al2O3)1-x ceramic target material is firstly prepared, then the (TiO2)x(Al2O3)1-x ceramic target material is arranged on a target platform of a pulse laser deposition system, a silicone substrate material is arranged on a substrate platform, and both the target platform and the substrate platform are arranged inside a growth chamber; pulse laser beam is focused on the (TiO2)x(Al2O3)1-x ceramic target material through a focus lens, the ceramic target material is stripped by the pulse laser, and the produced laser ion body is deposited on the silicone substrate to obtain the titanium-aluminum oxide film; and the laser bean plasma is ensured to be uniformly deposited on the substrate. The high dielectric coefficient titanium-aluminum oxide film can be used for preparing non-volatile memory part with small size, high density and stable performance.

Description

A kind of high dielectric coefficient titanium-aluminum oxide film and preparation method and application thereof
Technical field
The invention belongs to the microelectronic material field, but be specifically related to be applied to (the TiO based on the non-volatile trapped-charge memory of high density of nanocrystalline fast reading and writing 2) x(Al 2O 3) 1-xFilm and preparation method thereof
Background technology
The storage system that current computer uses comprises volatile memory and nonvolatile memory.The former is multiplex in the internal storage of computer system, when not having power supply to support, and can not save data.And the latter is not when having power supply to support, can the original data of complete preservation, preserve so be widely used in the data of electronic system, as computer, digital equipment, industrial control equipment etc.The nonvolatile memory magnetic medium memory of current use because magnetic head and recording medium machinery will take place relatively move in the read-write process, thereby can't be realized fast reading and writing.Electronics memory technologies such as Flash need not mechanical part, but owing to adopt thicker tunnel layer, cause it that shortcomings such as operating voltage height, read or write speed be relatively slow are arranged.The ferroelectric memory of studying in addition in addition (FeRAM), based on the M-RAM of spin-electronic material etc., they also use as yet in a large number because of some weakness separately.
The electric charge capture memory technology was proposed by people such as A.R.Wegener as far back as 1967, but was subjected to the restriction of material and device fabrication level, and its performance is difficult to and floating-gate memory contends with, so this technology only is applied at some special dimensions.SNOS/MONOS (the P/E voltage of 14-18V) before and after the electric charge capture memory technology has experienced from the early stage MNOS seventies in last century (the P/E voltage of 25-30V) to the eighties to the early-stage development course of the SONOS (the P/E voltage of 5-12V) of the nineties, has entered into and has adopted the conceptual phase of high k material as tunnel layer, accumulation layer, blocking layer more at present.Along with the improvement and the memory cell size of material properties such as accumulation layer enters nanoscale, the advantage of CTM is obvious day by day, has received extensive attention, and will become the mainstream development direction of 32nm with the non-volatile memory technology of lower node CMOS compatible front-end process.
Summary of the invention
The object of the present invention is to provide a kind of high dielectric coefficient titanium-aluminum oxide film and preparation method, and the application in non-volatile trapped-charge memory memory cell.
A kind of high dielectric coefficient titanium-aluminum oxide film, the chemical formula that it is characterized in that this film is (TiO 2) x(Al 2O 3) 1-x, 0.2≤x≤0.5 wherein, this film at room temperature is amorphous state, through high-temperature quick thermal annealing, film portion crystallization TiAl 2O 5Nanocrystalline.
Film utilizes pulsed laser deposition technique, uses (TiO 2) x(Al 2O 3) 1-xCeramic target prepares under the high vacuum low oxygen partial pressure, and its preparation process is as follows:
A, (TiO 2) x(Al 2O 3) 1-xThe preparation of ceramic target: with pure TiO 2, Al 2O 3Powder through the abundant ball milling of ball mill, is pressed into disk to mixed-powder after evenly mixing again, and sintering in chamber type electric resistance furnace obtains (TiO 2) x(Al 2O 3) 1-xCeramic target;
The selection of B, backing material and processing: select P type Si (100) as substrate, at first P type Si (100) is put into the absolute ethyl alcohol ultrasonic cleaning, erode the lip-deep SiO of Si with hydrofluoric acid solution then 2, use at last deionized water rinsing, taking-up is dried rear for subsequent use;
C, with (TiO 2) x(Al 2O 3) 1-xCeramic target is placed on the target platform of impulse laser deposition system, and silicon substrate material is put on the substrate table, and target platform and substrate table all are placed in the growth room;
D, vacuum in the growth room is extracted into 1.0 * 10 with mechanical pump -1Pa starts molecular pump then, and growth room's internal pressure is continued to be extracted into 1.0 * 10 -5Pa;
E, usefulness resistance furnace heated substrate platform make the Si substrate material be heated to design temperature 300-500 ℃;
F, starting impulse laser instrument make pulse laser beam by condenser lens laser beam be focused on (TiO 2) x(Al 2O 3) 1-xOn the ceramic target, utilize pulse laser stripped ceramic target, the lasing ion body of generation is deposited on the silicon substrate material and makes titanium-aluminum oxide film; In the film-forming process, motor is housed all under target platform and the substrate table, with constant 30-90 rev/min speed rotation, guarantees laser beam plasma uniform deposition on substrate, thereby make the film of even thickness.
TiO in the steps A 2, Al 2O 3Powder is with mol ratio x: 1-x evenly mixes, and ball milling 12-24 hour, under 13-15Mpa pressure, be cold-pressed into then diameter 22mm, thickness is the disk of 4mm, at last at 1200-1500 ℃ of sintering 6-8 hour.
P type Si (100) resistivity is 2-10 Ω cm among the step B -1, P type Si (100) ultrasonic cleaning in dehydrated alcohol was cleaned after 3-5 minute, used 1: 20 hydrofluoric acid solution of mol ratio to erode the SiO on Si surface again 2, use deionized water rinsing at last.
Molecular laser described in the step F is the KrF excimer laser, wavelength 248nm, and pulsewidth degree 30ns, single pulse energy 300mJ, energy density is 2.0J/cm 3
The application of described high dielectric coefficient titanium-aluminum oxide film in the non-volatile trapped-charge memory memory cell of preparation.
Use high-dielectric coefficient (TiO 2) x(Al 2O 3) 1-xThe method of film preparation nonvolatile memory memory elements, its preparation process is as follows:
A, with Al 2O 3Powder evenly mixes, and ball milling 12-24 hour, under 13-15Mpa pressure, be cold-pressed into then diameter 22mm, thickness is the disk of 4mm, at 1200-1500 ℃ of sintering 6-8 hour, obtains Al at last 2O 3Ceramic target;
The basic configuration of B, memory elements is three-decker, is about to one deck (TiO 2) x(Al 2O 3) 1-xThe film charge storage layer is clipped in amorphous Al 2O 3Film tunnel layer and amorphous Al 2O 3Be built into a miniature three-decker between the thin-film barrier layer, a Here it is memory cell is as a button capacitor;
C, this three-decker preparation are on the backing material silicon chip;
D, backing material top deposited amorphous Al 2O 3Film is as tunnel layer, and its thickness is 1nm to 4nm;
E, in amorphous Al 2O 3Film tunnel layer top deposit thickness is that 3nm is to (the TiO of 7nm 2) x(Al 2O 3) 1-xFilm is as accumulation layer;
F, at (TiO 2) x(Al 2O 3) 1-xFilm charge storage layer top deposit thickness is that 8nm is to the amorphous Al of 15nm 2O 3Film is as the barrier layer;
G, with this three-decker at 700-1000 ℃ of N 2Middle rapid thermal annealing 2-5min.Make the accumulation layer partially crystallizable separate out TiAl 2O 5Nanocrystalline.Al 2O 3Film tunnel layer and barrier layer keep amorphous;
H, in amorphous Al 2O 3Film barrier layer top covering diameter is the metal mask of 0.1mm, the platinum electrode of deposition 80 to 200nm.
Use this high-dielectric coefficient (TiO 2) x(Al 2O 3) 1-xThe performance test of film preparation nonvolatile memory memory cell:
The instrument that the memory cell that makes is carried out performance test is the accurate electric impedance analyzer of Agilent HP4294A.Main test component " is wiped " and " writing " afterwards variation of flat-band voltage, and the ability that keeps this variation.
Use the non-volatile electric charge capture memory cell of this film preparation to have following beneficial effect:
A, Fig. 3 have at length shown based on nanocrystalline high-dielectric coefficient (TiO 2) x(Al 2O 3) 1-x(wherein x=0.4) film memory cell electric capacity is to the response of voltage, thereby and the flat-band voltage that can therefrom obtain this memory cell change the ability of extrapolating its stored charge.As can be seen from the figure: write and the process of clashing be respectively voltage from 6V scan-6V and voltage scans 6V from-6V, writes and clashes process flat-band voltage difference and be worth approximately and be 2.3V, is about 1*10 through calculating its stored charge ability 13/ cm 2The test result explanation is based on nanocrystalline high-dielectric coefficient (TiO 2) x(Al 2O 3) 1-xThe film memory cell has significant stored charge ability, and this is very beneficial for reading of memory elements.
Under B, the normal temperature, apply the recession of 15V voltage at the electrode of this memory cell and remove, this moment this memory cell store electrons, flat-band voltage moves toward positive direction, measure this memory cell flat-band voltage over time this moment, Measuring Time continues 10 4Second; Electrode at this memory cell after measure finishing applies-recession of 15V voltage removes, this moment this memory cell storage oxygen room, flat-band voltage moves toward negative direction, measure this memory cell flat-band voltage over time this moment, Measuring Time continues 10 4Second.Fig. 4 has at length shown high-dielectric coefficient (TiO 2) x(Al 2O 3) 1-x(wherein x=0.4) film memory cell " wipe " and " writing " after flat-band voltage trend over time.Flat-band voltage becomes linear dependence substantially with the logarithm of time, because we can predict its long variation tendency, we can be to 10 from figure 8(～10 years) charge loss is about 18% after second.Under 80 ℃ of high temperature, repeat said process, we can see 10 from figure 8(～10 years) charge loss is about 33% after second.Illustrate that memory device has good retention.
Description of drawings
Fig. 1 is that the present invention prepares high-dielectric coefficient (TiO 2) x(Al 2O 3) 1-xThe structural representation of the pld (pulsed laser deposition) growing system of film,
Reference numeral: 1-substrate material; The 2-KrF excimer laser; The 3-condenser lens; 4-Al 2O 3(TiO 2) x(Al 2O 3) 1-xCeramic target; 5-target platform; The 6-growth room; The interface valve of 7-mechanical pump and molecular pump; The 8-substrate table.
Fig. 2: based on nanocrystalline high-dielectric coefficient (TiO 2) x(Al 2O 3) 1-xThe non-volatile trapped-charge memory memory cell structural representation of film preparation,
Reference numeral: 9-silicon substrate; 10-Al 2O 3Film is as tunnel layer; 11-(TiO 2) x(Al 2O 3) 1-xFilm is as charge storage layer; 12-Al 2O 3As barrier layer; 13-platinum (Pt) electrode; The 14-bottom electrode.
Fig. 3: based on nanocrystalline high-dielectric coefficient (TiO 2) x(Al 2O 3) 1-x(wherein x=0.4) thin-film memory memory cell electric capacity is to voltage response curves figure.
Fig. 4: based on nanocrystalline high-dielectric coefficient (TiO 2) x(Al 2O 3) 1-x(wherein x=0.4) thin-film memory memory cell writes and clashes over time curve map of rear flat-band voltage.
Embodiment
Embodiment 1.Al 2O 3The thin film technology method, its preparation process is as follows:
A, Al 2O 3The preparation of ceramic target: Al 2O 3After the powder mill is even, powder is pressed into disk, sintering in chamber type electric resistance furnace obtains Al 2O 3Ceramic target;
The selection of B, backing material and processing: select P type Si (100) as substrate, at first P type Si (100) is put into the absolute ethyl alcohol ultrasonic cleaning, erode the lip-deep SiO of Si with hydrofluoric acid solution then 2, use at last deionized water rinsing, taking-up is dried rear for subsequent use;
C, with Al 2O 3Ceramic target is placed on the target platform of impulse laser deposition system, and silicon substrate material is put on the substrate table, and target platform and substrate table all are placed in the growth room;
D, vacuum in the growth room is extracted into 1.0 * 10 with mechanical pump -1Pa starts molecular pump then, and growth room's internal pressure is continued to be extracted into 1.0 * 10 -5Below the Pa;
E, usefulness resistance furnace heated substrate platform make the Si substrate material be heated to design temperature 300-500 ℃;
F, starting impulse laser instrument make pulse laser beam by condenser lens laser beam be focused on Al 2O 3On the ceramic target, utilize pulse laser stripped ceramic target, the lasing ion body of generation is deposited on the silicon substrate material and makes titanium-aluminum oxide film; In the film-forming process, motor is housed all under target platform and the substrate table, with constant 30-90 rev/min speed rotation, guarantees laser beam plasma uniform deposition on substrate, thereby make the film of even thickness.
Embodiment 2. high-dielectric coefficient (TiO 2) x(Al 2O 3) 1-xThe thin film technology method, its preparation process is as follows:
A, (TiO 2) x(Al 2O 3) 1-xThe preparation of ceramic target: with pure TiO 2, Al 2O 3Powder through the abundant ball milling of ball mill, is pressed into disk to mixed-powder after evenly mixing again, and sintering in chamber type electric resistance furnace obtains (TiO 2) x(Al 2O 3) 1-xCeramic target; X=0.4 wherein;
The selection of B, backing material and processing: select P type Si (100) as substrate, at first P type Si (100) is put into the absolute ethyl alcohol ultrasonic cleaning, erode the lip-deep SiO of Si with hydrofluoric acid solution then 2, use at last deionized water rinsing, taking-up is dried rear for subsequent use;
C, with (TiO 2) x(Al 2O 3) 1-xCeramic target is placed on the target platform of impulse laser deposition system, and silicon substrate material is put on the substrate table, and target platform and substrate table all are placed in the growth room;
D, vacuum in the growth room is extracted into 1.0 * 10 with mechanical pump -1Pa starts molecular pump then, and growth room's internal pressure is continued to be extracted into 1.0 * 10 -5Below the Pa;
E, usefulness resistance furnace heated substrate platform make the Si substrate material be heated to design temperature 300-500 ℃;
F, starting impulse laser instrument make pulse laser beam by condenser lens laser beam be focused on (TiO 2) x(A1 2O 3) 1-xOn the ceramic target, utilize pulse laser stripped ceramic target, the lasing ion body of generation is deposited on the silicon substrate material and makes titanium-aluminum oxide film; In the film-forming process, motor is housed all under target platform and the substrate table, with constant 30-90 rev/min speed rotation, guarantees laser beam plasma uniform deposition on substrate, thereby make the film of even thickness.
Embodiment 3. uses high-dielectric coefficient (TiO 2) x(Al 2O 3) 1-xThe preparation method of the non-volatile trapped-charge memory memory cell of film, concrete preparation process is as follows:
A, backing material top deposited amorphous Al 2O 3Film is as tunnel layer, and its thickness is 1nm to 4nm
B, in amorphous Al 2O 3Film tunnel layer top deposit thickness is that 3nm is to (the TiO of 7nm 2) x(Al 2O 3) 1-xFilm is as accumulation layer, wherein x=0.4;
C, at (TiO 2) x(Al 2O 3) 1-xFilm charge storage layer top deposit thickness is that 8nm is to the amorphous Al of 15nm 2O 3Film is as the barrier layer;
D, with this three-decker at 700-1000 ℃ of N 2Middle rapid thermal annealing 2-5min.Make the accumulation layer partially crystallizable separate out TiAl 2O 5Nanocrystalline.Al 2O 3Film tunnel layer and barrier layer keep amorphous;
E, in amorphous Al 2O 3Film barrier layer top covering diameter is the metal mask of 0.1mm, the platinum electrode of deposition 80 to 200nm.
The chemical formula of film of the present invention is (TiO 2) x(Al 2O 3) 1-x, the scope of 0.2≤x≤0.5 and x=0.4 have performance to there is no big difference with respect to film.

Claims (6)

1. high dielectric coefficient titanium-aluminum oxide film, the chemical formula that it is characterized in that this film is (TiO 2) x(Al 2O 3) 1-x, 0.2≤x≤0.5 wherein, this film at room temperature is amorphous state, through 700-1000 ℃ of high-temperature quick thermal annealing, film portion crystallization TiAl 2O 5Nanocrystalline.
2. the preparation method of the described a kind of high dielectric coefficient titanium-aluminum oxide film of claim 1 is characterized in that using pulsed laser deposition technique, uses (TiO 2) x(Al 2O 3) 1-xCeramic target prepares under the high vacuum low oxygen partial pressure, and its preparation process is as follows:
A, (TiO 2) x(Al 2O 3) 1-xThe preparation of ceramic target: with pure TiO 2, Al 2O 3Powder through the abundant ball milling of ball mill, is pressed into disk to mixed-powder after evenly mixing again, and sintering in chamber type electric resistance furnace obtains (TiO 2) x(Al 2O 3) 1-xCeramic target;
The selection of B, backing material and processing: select P type Si (100) as substrate, at first P type Si (100) is put into the absolute ethyl alcohol ultrasonic cleaning, erode the lip-deep SiO of Si with hydrofluoric acid solution then 2, use at last deionized water rinsing, taking-up is dried rear for subsequent use;
C, with (TiO 2) x(Al 2O 3) 1-xCeramic target is placed on the target platform of impulse laser deposition system, and silicon substrate material is put on the substrate table, and target platform and substrate table all are placed in the growth room;
D, growth room's internal pressure is continued to be extracted into 1.0 * 10 -5Below the Pa;
E, usefulness resistance furnace heated substrate platform make the Si substrate material be heated to design temperature 300-500 ℃;
F, starting impulse laser instrument make pulse laser beam by condenser lens laser beam be focused on (TiO 2) x(Al 2O 3) 1-xOn the ceramic target, utilize pulse laser stripped ceramic target, the lasing ion body of generation is deposited on the silicon substrate material and makes titanium-aluminum oxide film; In the film-forming process, motor is housed all under target platform and the substrate table, with constant 30-90 rev/min speed rotation, guarantees laser beam plasma uniform deposition on substrate, thereby make the film of even thickness.
3. preparation method according to claim 2 is characterized in that TiO in steps A 2, Al 2O 3Powder is with mol ratio x: 1-x evenly mixes, and ball milling 12-24 hour, under 13-15Mpa pressure, be cold-pressed into then diameter 22mm, thickness is the disk of 4mm, at last at 1200-1500 ℃ of sintering 6-8 hour.
4. the preparation method of a kind of high dielectric coefficient titanium-aluminum oxide film according to claim 2 is characterized in that P type Si (100) resistivity is 2-10 Ω cm among the step B -1, P type Si (100) ultrasonic cleaning in dehydrated alcohol was cleaned after 3-5 minute, used 1: 20 hydrofluoric acid solution of mol ratio to erode the SiO on Si surface again 2, use deionized water rinsing at last.
5. preparation method according to claim 2 is characterized in that at the molecular laser described in the step F be the KrF excimer laser, wavelength 248nm, and pulsewidth degree 30ns, single pulse energy 300mJ, energy density is 2.0J/cm 3
6. the application of the described high dielectric coefficient titanium-aluminum oxide film of claim 1 in preparation nonvolatile memory memory cell; Described nonvolatile memory memory cell is with one deck (TiO 2) x(Al 2O 3) 1-xThe film charge storage layer is clipped in amorphous Al 2O 3Film tunnel layer and amorphous Al 2O 3Be built into a miniature three-decker between the thin-film barrier layer.
CN 201010172490 2010-05-14 2010-05-14 High dielectric coefficient titanium-aluminum oxide film and preparation method and application thereof Pending CN101864556A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102208346A (en) * 2011-04-22 2011-10-05 南京大学 Nonvolatile charge capture type storage device, preparation method thereof and application
CN105206615A (en) * 2015-09-28 2015-12-30 南京大学 High-dielectric-coefficient composite oxide charge storage medium thin film and application
CN105463373A (en) * 2015-12-31 2016-04-06 陕西师范大学 Preparation method of n type copper oxide thin film
CN111636051A (en) * 2020-05-18 2020-09-08 广西大学 Device of amorphous InGaN/Si heterojunction solar cell and preparation method thereof

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CN1450600A (en) * 2002-04-10 2003-10-22 台湾积体电路制造股份有限公司 Method for mfg of double grid structure
CN1862827A (en) * 2006-01-25 2006-11-15 南京大学 High-dielectric coefficient grid dielectric material titanium aluminate film and preparing method thereof

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US6514826B1 (en) * 1999-12-22 2003-02-04 Hyundai Electronics Industries Co., Ltd. Method of forming a gate electrode in a semiconductor device
CN1309419A (en) * 2000-02-14 2001-08-22 国际商业机器公司 Semiconductor field effect metal oxide transistor with minimum covered capacitance
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102208346A (en) * 2011-04-22 2011-10-05 南京大学 Nonvolatile charge capture type storage device, preparation method thereof and application
CN102208346B (en) * 2011-04-22 2013-08-28 南京大学 Nonvolatile charge capture type storage device, preparation method thereof and application
CN105206615A (en) * 2015-09-28 2015-12-30 南京大学 High-dielectric-coefficient composite oxide charge storage medium thin film and application
CN105463373A (en) * 2015-12-31 2016-04-06 陕西师范大学 Preparation method of n type copper oxide thin film
CN111636051A (en) * 2020-05-18 2020-09-08 广西大学 Device of amorphous InGaN/Si heterojunction solar cell and preparation method thereof

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Application publication date: 20101020