CN104862664A - Preparation method of ultrathin graphical aluminium oxide film - Google Patents
Preparation method of ultrathin graphical aluminium oxide film Download PDFInfo
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Abstract
The invention discloses a preparation method of an ultrathin graphical aluminium oxide film specially applied to the atomic layer chemical vapor deposition technology. Used raw materials comprise trimethylaluminum, inert gas, ozone and a flaky substrate. The preparation method of the ultrathin graphical aluminium oxide film comprises steps as follows: the substrate is fixed on a special sample tray with a magnetic clamping method, the upper surface of the substrate is covered with a metal mask with required graphs, and the ultrathin graphical aluminium oxide film is prepared with the atomic layer chemical vapor deposition technology. With the adoption of the method, the ultrathin aluminium oxide film can be prevented from being polluted by impurity ions, graph edges are clear, no lateral intrusion phenomenon exists, the film cannot be damaged easily, and the process is simple.
Description
Technical field
The present invention relates to a kind of preparation method of patterned alumina ultrathin film, specifically a kind of preparation method being specifically designed to the patterned alumina ultrathin film of atomic layer chemical vapor deposition technology.
Technical background
As everyone knows, aluminum oxide (Al
2o
3) film has very excellent physicals and chemical property, as physical strength and hardness high, Heat stability is good, thermal conductivity is high, radioresistance injury reinforcing ability is strong, alkali resistant iontophoretic injection ability is strong, broad stopband, transparent in very wide wavelength region, insulativity is splendid, at machinery, many fields such as optics and microelectronics have a wide range of applications, at microelectronic, along with the integrated level of si-substrate integrated circuit improves constantly, as field effect transistor gate material earth silicon material because of under nanoscale tunnelling current cannot ignore, more and more be not suitable as insulating material.Aluminum oxide film, as the equivalent material of silicon-dioxide, causes the interest of researchist.Atomic layer chemical vapor deposition technology, owing to having the advantages such as film growth thickness controllable precise, step coverage be splendid, is particularly suitable for the growth of ultrathin film, more and more wider in microelectronic application.The photopermeability of aluminum oxide film Yin Qigao, can also be used for the light collection layer of solar cell.
Alumina ultrathin film is applied to the occasions such as unicircuit, sensor, MEMS (micro electro mechanical system), solar cell, alumina ultrathin film is all needed to be made into specific figure, and at microelectronics technology, by film material graphics, the technical scheme of usual employing is increasing method or subtraction, increasing method utilizes mask plate to form specific figure when film growth for adopting mask plate to carry out film growth, and subtraction, for etch film, can be divided into Physical etching/chemical method to etch further.
According to Physical etching, its etching depth is often difficult to control, and especially for nano level ultrathin film, the problem of overetch is more serious, can damage the substrate material of film lower floor, and its processing parameter is extremely difficult to be controlled; According to chemical etching, there is the problem of above-mentioned overetch equally, and, film also simultaneously can because of the employing of etching agent pollute by foreign ion; In addition, no matter be Physical etching or chemical method etching, all need the mask layer of the patterned etch resistant of well in advance before etching, manage to remove this one deck after etching technics completes again, this also makes the technique of etching method very complicated.
Therefore, adopting increasing method to carry out the growing patterned of film is good selection.
For pulsed laser deposition, chemical Vapor deposition process, magnetron sputtering method, vacuum vapour deposition etc., conventional mask plate method can be used for preparing patterned oxide aluminium film, has had the utilization of a large amount of maturations.But, when required aluminum oxide film film thickness reduces to the magnitude of several nanometer and requires that precise thickness control, step coverage are outstanding, these methods aforementioned turn turtle, and atomic layer chemical vapor deposition ultrathin alumina film becomes most suitable selection.
But, according to mask plate mechanical grip method and the conventional atomic layer chemical vapor deposition technique (H of routine
2o and TMA ALT pulse) just complete the graphical of film when deposited aluminum oxide thin film, also there is very large problem: during due to atomic layer chemical vapor deposition ultrathin alumina film, always very little gap is there is between mask plate and substrate material, deionized water steam as oxygen source extremely easily invades gap, even if seem very smooth, the mask plate good with substrate attaching also cannot play the effect stopping that deionized water steam invades at all, find in actual deposition technique to adopt this method cannot complete the graphical of film at all, a few indifference of aluminum oxide ultrathin membrane obtained when the aluminum oxide ultrathin membrane obtained and non-mask plate, in addition, conventional mask plate is when being placed on substrate, with magnetron sputtering method, pulsed laser deposition, Vacuum Coating method, the thin film deposition processes such as molecular beam epitaxy are different, in atomic layer chemical vapor deposition technique, due to carrier gas, the pulse feature impact air-flow periodically effect of precursor gas, the mask plate fixation method of prior art causes damage and pollutes always to clean substrate surface, also make the edge blurry of figure unclear, mechanical clamping also causes at loading, cause major injury can to during sampling the film of very thin (thickness below several nanometer).
Above-mentioned factor makes the ultrathin film preparing patterned aluminium oxide nano level thickness, all the time be a technical barrier being difficult to overcome, simple technical problem is seemed in micron order, submicron order, deep-submicron technique epoch, in the photoelectric elements epoch, become particularly difficulty, prior art cannot adapt to new technique.Before making the present invention, not yet there is the preparation method that technique is simple, efficiency is high, exempt to pollute, be specifically designed to the patterned alumina ultrathin film of atomic layer chemical vapor deposition technology, need the technology of preparing of the new patterned alumina ultrathin film of exploitation badly.
Summary of the invention
The object of the invention is to provide a kind of preparation method being specifically designed to the patterned alumina ultrathin film of atomic layer chemical vapor deposition technology for the deficiencies in the prior art.
For achieving the above object, the present invention realizes by the following technical solutions:
A kind of preparation method being specifically designed to the patterned alumina ultrathin film of atomic layer chemical vapor deposition technology, the raw material used comprises: aluminium source, rare gas element, oxygen source and sheet-like substrates, and the preparation method of described patterned alumina ultrathin film comprises the following steps successively:
(1) substrate prepares: by substrate with after organic solvent cleaning, dry up with rare gas element, described organic solvent is dehydrated alcohol or acetone;
(2) fixed sample: the substrate of the cleaning obtained in step (1) is positioned in the shallow slot of sample tray, the preprepared metal mask version with required figure on substrate top surface covers, then be placed in metal mask version by annular permanent magnnet or ring electromagnet, the center of circle of annular permanent magnnet or ring electromagnet and the center superposition of shallow slot;
(3) sample introduction: the vacuum reaction chamber sending into atomic layer chemical vapor deposition system, vacuumizes and make the vacuum tightness of vacuum reaction chamber reach 1 ~ 5hpa;
(4) atomic layer chemical vapor deposition of patterned alumina ultrathin film: after oxygen and rare gas element mix according to certain volume ratio, by ozonizer generates ozone gas; Pass into rare gas element in depositing system, make in reaction chamber and intermediate space air pressure remains on 1 ~ 5hpa and 6 ~ 15hpa respectively; Each growth circulation is made up of following four gas pulses:
A, trimethyl aluminium pulse 0.1 second, use rare gas element to be transported to reaction chamber as carrier gas, carrier gas flux is 100-400sccm;
B, rare gas element rinse cavity 2 ~ 30 seconds, and flow is 100-400sccm;
C, ozone purge 3 seconds, ozone flow is 100-400sccm, and use rare gas element to be transported to reaction chamber as carrier gas, carrier gas flux is 100-400sccm;
D, rare gas element rinse cavity 6 seconds, and flow is 100-400sccm;
Utilize from limiting surface adsorption effect, obtained alumina ultrathin film;
When adopting ring electromagnet stationary substrate and metal mask plate, electronic switch closes, is powered to ring electromagnet by 3V ~ 12V output end of pressure-stabilizing of host power supply;
(5) sample: close atomic layer chemical vapor deposition system, when adopting ring electromagnet stationary substrate and metal mask plate, electronic switch disconnects, and takes out patterned alumina ultrathin film sample.
Described aluminium source is trimethyl aluminium, and described oxygen source is oxygen.Described rare gas element is nitrogen or argon gas.The purity of rare gas element and oxygen is all not less than 99.999%.
Described sheet-like substrates be silicon chip, nickel acid lanthanum sheet, oxidation indium sheet, oxidation magnesium sheet, tinsel, gan sheet, nitrogenize titanium sheet, nitrogenize aluminium flake, quartz plate, sapphire sheet one of them.
Described sample tray is circular, the size of pallet and the size of reaction chamber adapt, pallet material is iron content, nickel or cobalt wherein one or more soft magnetic metal alloy, pallet circumference is provided with the flange higher than holding tray surface 0.2 ~ 1mm, this flange is also provided with two symmetrical breach, gap width is 1 ~ 2mm, cut height and flange height keep identical, be 0.2 ~ 1mm, the setting of described breach, most important for the homogeneity of film growth, controllability, purity and the speed of growth; Be provided with circle or square shallow slot that one or more degree of depth is 0.2 ~ 1mm in holding tray surface, the setting of described shallow slot be in order to avoid in thin film growth process backing sheet blow away by air-flow; The circumferential edges of pallet is provided with two through holes, a pair positive and negative power-line terminal is equipped with respectively in two through holes, insulation layer is filled with between power-line terminal and pallet, pallet is furnished with annular permanent magnnet or ring electromagnet, and between ring electromagnet with described positive and negative power-line terminal, flexible electrical is connected; The internal diameter of annular permanent magnnet or ring electromagnet is greater than the graphics field of metal mask plate, and external diameter and the shallow slot internal diameter of annular permanent magnnet or ring electromagnet adapt.
When the temperature of reaction of reaction chamber adopts annular permanent magnnet or ring electromagnet lower than when 100 DEG C, when the temperature of reaction of reaction chamber adopts electro-magnet higher than when 100 DEG C.
The bracket for accommodating sample tray of atomic layer chemical vapor deposition system is provided with a pair elastic sheet metal matched with the positive and negative power-line terminal of a pair on described pallet, is electrically connected between described a pair elastic sheet metal and 3V ~ 12V output end of pressure-stabilizing of the host power supply of atomic layer chemical vapor deposition equipment by electronic switch;
Preferably, 3V ~ 12V output end of pressure-stabilizing of the host power supply of described atomic layer chemical vapor deposition equipment is that direct current exports, and described electronic switch is power-type MOSFET, and this electronic switch is controlled to open or disconnect by the operating system of main frame; Or
Preferably, 3V ~ 12V output end of pressure-stabilizing of the host power supply of described atomic layer chemical vapor deposition equipment exports for exchanging, and described electronic switch is thyratron transistor, and this electronic switch is controlled to open or disconnect by the operating system of main frame;
In step (2), the substrate of the cleaning obtained in step (1) is positioned in the shallow slot of sample tray, the preprepared metal mask version with required figure on substrate top surface covers, then annular permanent magnnet or ring electromagnet are placed in metal mask version, the center of circle of annular permanent magnnet or ring electromagnet and the center superposition of shallow slot;
In step (4), when adopting ring electromagnet stationary substrate and metal mask plate, electronic switch closes, is powered to annular permanent magnnet by 3V ~ 12V output end of pressure-stabilizing of host power supply; Further, this voltage stabilizing exports has a starting stage, and in the described starting stage, voltage exports and is increased to a stationary value gradually by zero voltage, by this flexible loading technique, can avoid the damage that conventional mask plate chucking method is brought to substrate and film.
In step (5), when adopting ring electromagnet stationary substrate and metal mask plate, electronic switch disconnects.
Utilize from limiting surface adsorption effect, repetition above-mentioned steps a, b, c, d several times obtain alumina ultrathin film, the number of times repeated is by expecting that the film thickness obtained determines: cycles=thickness/GPC, here cycles represents the number of times of repetition, thickness represents the film thickness of expecting and obtaining, GPC is film growth rates, i.e. the thickness of every secondary growth;
Thickness and the atomic layer chemical vapor deposition cycle index of alumina ultrathin film are linear.When cycle index is 250 time, the film thickness obtained is 35.33 nanometers; When cycle index is 500 time, the film thickness obtained about 70 nanometer.
Above-mentioned reaction carries out in the vacuum reaction chamber of sealing.This preparation method realizes based on atomic layer chemical vapor deposition system.The method is adapted to various atomic layer chemical vapor deposition system.
The vaccum-pumping equipment that the method adopts is without oil type vacuum mechanical pump.
Compared with prior art, the present invention has following beneficial effect:
What the present invention prepared is a kind of patterned alumina ultrathin film, relative to the aluminum oxide film that other atomic layer chemical vapor deposition techniques obtain, excellent insulation performance, film surface densification are smooth except possessing equally for this material, growth thickness accurate controlled, step coverage is splendid, with except the advantage such as silicon-based semiconductor process compatible, also possesses following features: alumina ultrathin film pollutes from foreign ion, pattern edge is clear, without side direction penetration phenomenon, film does not subject to damage, and technique simply, easily controls.
Accompanying drawing explanation
Fig. 1: sample tray schematic diagram, does not mark annular permanent magnnet or ring electromagnet in figure;
Fig. 2: the ultrathin alumina film of a kind of dot pattern adopting the inventive method to make.
Embodiment
Embodiment 1
The preparation method of patterned alumina ultrathin film comprises the following steps successively:
(1) substrate prepares: after silicon chip substrate washes of absolute alcohol, dry up with nitrogen;
(2) fixed sample: the substrate of the cleaning obtained in step (1) is positioned in the shallow slot of sample tray, the preprepared metal mask version with required figure on substrate top surface covers, then annular permanent magnnet is placed in metal mask version, the center of circle of annular permanent magnnet and the center superposition of shallow slot;
(3) sample introduction: the vacuum reaction chamber sending into atomic layer chemical vapor deposition system, vacuumizes and make the vacuum tightness of vacuum reaction chamber reach 1 ~ 5hpa;
(4) atomic layer chemical vapor deposition of patterned alumina ultrathin film: the temperature of reaction of reaction chamber keeps at room temperature, carrying out refrigeration to the source bottle that trimethyl aluminium is housed makes its temperature remain on 15 ~ 20 DEG C, oxygen and nitrogen according to 95: 5 ~ 90: 10 volume ratio mix after, by ozonizer generates ozone gas; Pass into nitrogen in depositing system, make in reaction chamber and intermediate space air pressure remains on 1 ~ 5hpa and 6 ~ 15hpa respectively; Each growth circulation is made up of following four gas pulses:
A, trimethyl aluminium pulse 0.1 second, use nitrogen to be transported to reaction chamber as carrier gas, carrier gas flux is 200sccm;
B, nitrogen wash cavity 2 ~ 30 seconds, flow is 200sccm;
C, ozone purge 3 seconds, ozone flow is 200 ~ 300sccm, and use nitrogen to be transported to reaction chamber as carrier gas, carrier gas flux is 200sccm;
D, nitrogen wash cavity 6 seconds, flow is 200sccm;
Utilize from limiting surface adsorption effect, obtained alumina ultrathin film;
(5) sample: close atomic layer chemical vapor deposition system, take out patterned alumina ultrathin film sample.
Embodiment 2
The preparation method of patterned alumina ultrathin film comprises the following steps successively:
(1) substrate prepares: by quartz plate substrate with after acetone cleaning, dry up with argon gas;
(2) fixed sample: the substrate of the cleaning obtained in step (1) is positioned in the shallow slot of sample tray, the preprepared metal mask version with required figure on substrate top surface covers, then ring electromagnet is placed in metal mask version, the center of circle of ring electromagnet and the center superposition of shallow slot;
(3) sample introduction: the vacuum reaction chamber sending into atomic layer chemical vapor deposition system, vacuumizes and make the vacuum tightness of vacuum reaction chamber reach 1 ~ 5hpa;
(4) atomic layer chemical vapor deposition of patterned alumina ultrathin film: electronic switch closes, is powered to ring electromagnet by 3V ~ 12V voltage stabilizing ac output end of host power supply; At the temperature of reaction of reaction chamber remains on 100 DEG C, refrigeration is carried out to the source bottle that trimethyl aluminium is housed and makes its temperature remain on 15 ~ 20 DEG C, oxygen and argon gas according to 95: 5 ~ 90: 10 volume ratio mix after, by ozonizer generates ozone gas; Pass into argon gas in depositing system, make in reaction chamber and intermediate space air pressure remains on 1 ~ 5hpa and 6 ~ 15hpa respectively; Each growth circulation is made up of following four gas pulses:
A, trimethyl aluminium pulse 0.1 second, use argon gas to be transported to reaction chamber as carrier gas, carrier gas flux is 200sccm;
B, argon cleaning cavity 2 ~ 30 seconds, flow is 200sccm;
C, ozone purge 3 seconds, ozone flow is 100 ~ 300sccm, and use argon gas to be transported to reaction chamber as carrier gas, carrier gas flux is 200sccm;
D, argon cleaning cavity 6 seconds, flow is 200sccm;
Utilize from limiting surface adsorption effect, obtained alumina ultrathin film;
(5) sample: close atomic layer chemical vapor deposition system, electronic switch disconnects, and takes out patterned alumina ultrathin film sample.
Embodiment 3
The preparation method of patterned alumina ultrathin film comprises the following steps successively:
(1) substrate prepares: by silicon chip substrate with after acetone cleaning, dry up with nitrogen;
(2) fixed sample: the substrate of the cleaning obtained in step (1) is positioned in the shallow slot of sample tray, the preprepared metal mask version with required figure on substrate top surface covers, then ring electromagnet is placed in metal mask version, the center of circle of annular permanent magnnet and the center superposition of shallow slot;
(3) sample introduction: the vacuum reaction chamber sending into atomic layer chemical vapor deposition system, vacuumizes and make the vacuum tightness of vacuum reaction chamber reach 1 ~ 5hpa;
(4) atomic layer chemical vapor deposition of patterned alumina ultrathin film: electronic switch closes, is powered to ring electromagnet by 3V ~ 12V voltage stabilizing ac output end of host power supply; At the temperature of reaction of reaction chamber remains on 350 DEG C, refrigeration is carried out to the source bottle that trimethyl aluminium is housed and makes its temperature remain on 15 ~ 20 DEG C, oxygen and nitrogen according to 95: 5 ~ 90: 10 volume ratio mix after, by ozonizer generates ozone gas; Pass into nitrogen in depositing system, make in reaction chamber and intermediate space air pressure remains on 1 ~ 5hpa and 6 ~ 15hpa respectively; Each growth circulation is made up of following four gas pulses:
A, trimethyl aluminium pulse 0.1 second, use nitrogen to be transported to reaction chamber as carrier gas, carrier gas flux is 200sccm;
B, nitrogen wash cavity 2 ~ 30 seconds, flow is 200sccm;
C, ozone purge 3 seconds, ozone flow is 200 ~ 300sccm, and use nitrogen to be transported to reaction chamber as carrier gas, carrier gas flux is 200sccm;
D, nitrogen wash cavity 6 seconds, flow is 200sccm;
Utilize from limiting surface adsorption effect, obtained alumina ultrathin film;
(5) sample: close atomic layer chemical vapor deposition system, take out patterned alumina ultrathin film sample.
Embodiment 4
The preparation method of patterned alumina ultrathin film comprises the following steps successively:
(1) substrate prepares: by silicon chip substrate with after raw spirit cleaning, dry up with nitrogen;
(2) fixed sample: the substrate of the cleaning obtained in step (1) is positioned in the shallow slot of sample tray, the preprepared metal mask version with required figure on substrate top surface covers, then ring electromagnet is placed in metal mask version, the center of circle of annular permanent magnnet and the center superposition of shallow slot;
(3) sample introduction: the vacuum reaction chamber sending into atomic layer chemical vapor deposition system, vacuumizes and make the vacuum tightness of vacuum reaction chamber reach 1 ~ 5hpa;
(4) atomic layer chemical vapor deposition of patterned alumina ultrathin film: electronic switch closes, is powered to ring electromagnet by 3V ~ 12V voltage stabilizing ac output end of host power supply; At the temperature of reaction of reaction chamber remains on 180 DEG C, refrigeration is carried out to the source bottle that trimethyl aluminium is housed and makes its temperature remain on 18 ~ 20 DEG C, oxygen and nitrogen according to 90: 10 volume ratio mix after, by ozonizer generates ozone gas; Pass into nitrogen in depositing system, make in reaction chamber and intermediate space air pressure remains on 1 ~ 5hpa and 6 ~ 15hpa respectively; Each growth circulation is made up of following four gas pulses:
A, trimethyl aluminium pulse 0.1 second, use nitrogen to be transported to reaction chamber as carrier gas, carrier gas flux is 200sccm;
B, nitrogen wash cavity 2 ~ 30 seconds, flow is 220sccm;
C, ozone purge 3 seconds, ozone flow is 250 ~ 300sccm, and use nitrogen to be transported to reaction chamber as carrier gas, carrier gas flux is 220sccm;
D, nitrogen wash cavity 6 seconds, flow is 220sccm;
Utilize from limiting surface adsorption effect, obtained alumina ultrathin film;
(5) sample: close atomic layer chemical vapor deposition system, take out patterned alumina ultrathin film sample.
Embodiment 5
The preparation method of patterned alumina ultrathin film comprises the following steps successively:
(1) substrate prepares: after silicon chip substrate washes of absolute alcohol, dry up with nitrogen;
(2) fixed sample: the substrate of the cleaning obtained in step (1) is positioned in the shallow slot of sample tray, the preprepared metal mask version with required figure on substrate top surface covers, then annular permanent magnnet is placed in metal mask version, the center of circle of annular permanent magnnet and the center superposition of shallow slot;
(3) sample introduction: the vacuum reaction chamber sending into atomic layer chemical vapor deposition system, vacuumizes and make the vacuum tightness of vacuum reaction chamber reach 1 ~ 5hpa;
(4) atomic layer chemical vapor deposition of patterned alumina ultrathin film: at the temperature of reaction of reaction chamber remains on 50 DEG C, carrying out refrigeration to the source bottle that trimethyl aluminium is housed makes its temperature remain on 15 ~ 20 DEG C, oxygen and nitrogen according to 95: 5 ~ 90: 10 volume ratio mix after, by ozonizer generates ozone gas; Pass into nitrogen in depositing system, make in reaction chamber and intermediate space air pressure remains on 1 ~ 5hpa and 6 ~ 15hpa respectively; Each growth circulation is made up of following four gas pulses:
A, trimethyl aluminium pulse 0.1 second, use nitrogen to be transported to reaction chamber as carrier gas, carrier gas flux is 200sccm;
B, nitrogen wash cavity 2 ~ 30 seconds, flow is 200sccm;
C, ozone purge 3 seconds, ozone flow is 200 ~ 300sccm, and use nitrogen to be transported to reaction chamber as carrier gas, carrier gas flux is 200sccm;
D, nitrogen wash cavity 6 seconds, flow is 200sccm;
Utilize from limiting surface adsorption effect, obtained alumina ultrathin film;
(5) sample: close atomic layer chemical vapor deposition system, take out patterned alumina ultrathin film sample.
Claims (6)
1. one kind is specifically designed to the preparation method of the patterned alumina ultrathin film of timesharing pulse gas pouring-in atomic layer chemical vapor deposition technology, the raw material used comprises: aluminium source, rare gas element, oxygen source and sheet-like substrates, described aluminium source is trimethyl aluminium, and described oxygen source is oxygen; The purity of rare gas element and oxygen is all not less than 99.999%, described sheet-like substrates be silicon chip, nickel acid lanthanum sheet, oxidation indium sheet, oxidation magnesium sheet, tinsel, gan sheet, nitrogenize titanium sheet, nitrogenize aluminium flake, quartz plate, sapphire sheet one of them; The preparation method of described patterned alumina ultrathin film comprises the following steps successively:
(1) substrate prepares: by substrate with after organic solvent cleaning, dry up with rare gas element, described organic solvent is dehydrated alcohol or acetone;
(2) fixed sample: the substrate of the cleaning obtained in step (1) and metal mask version are fixed on sample tray;
(3) sample introduction: the vacuum reaction chamber sending into atomic layer chemical vapor deposition system, vacuumizes and make the vacuum tightness of vacuum reaction chamber reach 1 ~ 5hpa;
(4) atomic layer chemical vapor deposition of patterned alumina ultrathin film;
(5) sample: close atomic layer chemical vapor deposition system, take out patterned alumina ultrathin film sample;
It is characterized in that:
Described sample tray is circular, the size of pallet and the size of reaction chamber adapt, pallet material is iron content, nickel or cobalt wherein one or more soft magnetic metal alloy, and pallet circumference is provided with the flange higher than holding tray surface 0.2 ~ 1mm, this flange is also provided with two symmetrical breach, gap width is 1 ~ 2mm, cut height and flange height keep identical, be 0.2 ~ 1mm, circle or square shallow slot that one or more degree of depth is 0.2 ~ 1mm is provided with in holding tray surface, the circumferential edges of pallet is provided with two through holes, be equipped with one respectively in two through holes to align, negative supply terminal stud, insulation layer is filled with between power-line terminal and pallet, pallet is furnished with annular permanent magnnet or ring electromagnet, described ring electromagnet and just described, between negative supply terminal stud, flexible electrical connects, the internal diameter of described annular permanent magnnet or ring electromagnet is greater than the graphics field of metal mask plate, and external diameter and the shallow slot internal diameter of annular permanent magnnet or ring electromagnet adapt,
When the temperature of reaction of reaction chamber adopts annular permanent magnnet or ring electromagnet lower than when 100 DEG C, when the temperature of reaction of reaction chamber adopts electro-magnet higher than when 100 DEG C;
The bracket for accommodating sample tray of atomic layer chemical vapor deposition system is provided with a pair elastic sheet metal matched with the positive and negative power-line terminal of a pair on described pallet, is electrically connected between described a pair elastic sheet metal and 3V ~ 12V output end of pressure-stabilizing of the host power supply of atomic layer chemical vapor deposition equipment by electronic switch;
3V ~ 12V output end of pressure-stabilizing of the host power supply of described atomic layer chemical vapor deposition equipment is that direct current exports, and described electronic switch is power-type MOSFET, and this electronic switch is controlled to open or disconnect by the operating system of main frame; Or
3V ~ 12V output end of pressure-stabilizing of the host power supply of described atomic layer chemical vapor deposition equipment exports for exchanging, and described electronic switch is thyratron transistor, and this electronic switch is controlled to open or disconnect by the operating system of main frame;
In step (2), the substrate of the cleaning obtained in step (1) is positioned in the shallow slot of sample tray, the preprepared metal mask version with required figure on substrate top surface covers, then annular permanent magnnet or ring electromagnet are placed in metal mask version, the center of circle of annular permanent magnnet or ring electromagnet and the center superposition of shallow slot;
In step (4), when adopting ring electromagnet stationary substrate and metal mask plate, electronic switch closes, is powered to annular permanent magnnet by 3V ~ 12V output end of pressure-stabilizing of host power supply; Further, this voltage stabilizing exports has a starting stage, and in the described starting stage, above-mentioned voltage stabilizing output voltage is increased to a stationary value gradually by zero voltage;
The concrete steps of the atomic layer chemical vapor deposition of patterned alumina ultrathin film are as follows: carry out refrigeration to the source bottle that trimethyl aluminium is housed and make its temperature remain on 15 ~ 20 DEG C, oxygen and rare gas element according to 95: 5 ~ 90: 10 volume ratio mix after, by ozonizer generates ozone gas; Pass into rare gas element in depositing system, make in reaction chamber and intermediate space air pressure remains on 1 ~ 5hpa and 6 ~ 15hpa respectively; Each growth circulation is made up of following four gas pulses:
A, trimethyl aluminium pulse 0.1 second, use rare gas element to be transported to reaction chamber as carrier gas, carrier gas flux is 100-400sccm;
B, rare gas element rinse cavity 2 ~ 30 seconds, and flow is 100-400sccm;
C, ozone purge 3 seconds, ozone flow is 100-400sccm, and use rare gas element to be transported to reaction chamber as carrier gas, carrier gas flux is 100-400sccm;
D, rare gas element rinse cavity 6 seconds, and flow is 100-400sccm;
Utilize from limiting surface adsorption effect, repetition above-mentioned steps a, b, c, d several times obtain alumina ultrathin film, the number of times repeated is by expecting that the film thickness obtained determines: cycles=thickness/GPC, here cycles represents the number of times of repetition, thickness represents the film thickness of expecting and obtaining, GPC is film growth rates, i.e. the thickness of every secondary growth;
In step (5), when adopting ring electromagnet stationary substrate and metal mask plate, electronic switch disconnects.
2. be specifically designed to a preparation method for the patterned alumina ultrathin film of timesharing pulse gas pouring-in atomic layer chemical vapor deposition technology as claimed in claim 1, it is characterized in that: described rare gas element is nitrogen or argon gas.
3. be specifically designed to a preparation method for the patterned alumina ultrathin film of timesharing pulse gas pouring-in atomic layer chemical vapor deposition technology as claimed in claim 1 or 2, it is characterized in that: the substrate temperature be fixed on the sample tray of vacuum reaction chamber remains between room temperature to 400 DEG C.
4. the preparation method being specifically designed to the patterned alumina ultrathin film of timesharing pulse gas pouring-in atomic layer chemical vapor deposition technology as described in claim 1 or 2 or 3, is characterized in that: thickness and the atomic layer chemical vapor deposition cycle index of alumina ultrathin film are linear.
5. the preparation method being specifically designed to the patterned alumina ultrathin film of timesharing pulse gas pouring-in atomic layer chemical vapor deposition technology as claimed in claim 1 or 2 or 3 or 4, is characterized in that: the method is adapted to various atomic layer chemical vapor deposition system.
6. the preparation method being specifically designed to the patterned alumina ultrathin film of timesharing pulse gas pouring-in atomic layer chemical vapor deposition technology as described in claim 1 or 2 or 3 or 4 or 5, is characterized in that: the vaccum-pumping equipment that the method adopts is without oil type vacuum mechanical pump.
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| CN110042365A (en) * | 2019-03-04 | 2019-07-23 | 中国科学院物理研究所 | A kind of Atomic layer deposition method in two-dimensional material surface growth aluminium oxide |
| CN112481602A (en) * | 2019-09-11 | 2021-03-12 | 艾特材料有限公司 | Method and equipment for depositing metal oxide film on ceramic backboard |
| CN113005432A (en) * | 2021-02-18 | 2021-06-22 | 西安交通大学 | Method for depositing ZnO functional layer in patterned mode, strain sensor and preparation method of strain sensor |
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| CN112481602B (en) * | 2019-09-11 | 2023-12-15 | 艾特材料有限公司 | Method and equipment for depositing metal oxide film on ceramic backboard |
| CN113005432A (en) * | 2021-02-18 | 2021-06-22 | 西安交通大学 | Method for depositing ZnO functional layer in patterned mode, strain sensor and preparation method of strain sensor |
| CN113005432B (en) * | 2021-02-18 | 2022-05-20 | 西安交通大学 | Method for depositing ZnO functional layer in patterned mode, strain sensor and preparation method of strain sensor |
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