CN103668108A - Atomic layer deposition method of oxide medium - Google Patents
Atomic layer deposition method of oxide medium Download PDFInfo
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- CN103668108A CN103668108A CN201310667554.2A CN201310667554A CN103668108A CN 103668108 A CN103668108 A CN 103668108A CN 201310667554 A CN201310667554 A CN 201310667554A CN 103668108 A CN103668108 A CN 103668108A
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- atomic layer
- layer deposition
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Abstract
The invention discloses an atomic layer deposition method of an oxide medium. The method is used for preparation of the oxide medium by using an atomic layer deposition system, and comprises the following steps: 1, setting growth parameters of the atomic layer deposition system; 2, leading in a metal precursor source pulse to a reaction cavity of the atomic layer deposition system, and then cleaning by using high-purity nitrogen to remove a reaction by-product and residual metal precursor source; 3, leading in a water pulse to the reaction cavity of the atomic layer deposition system, and then cleaning by using high-purity nitrogen to remove the reaction by-product and residual water; 4, leading in an in-situ treatment gas pulse to the reaction cavity of the atomic layer deposition system, and then cleaning by using the high-purity nitrogen to remove the reaction by-product and residual in-situ treatment gas; 5, repeatedly carrying out the steps 2, 3 and 4 orderly, so as to obtain an oxide medium film with a high dielectric constant. The atomic layer deposition method of the oxide medium disclosed by the invention can be applied to growth of a gate medium employing a complementary metal-oxide-semiconductor transistor (CMOS) technology.
Description
Technical field
The present invention relates to the preparation method of oxide dielectric, relate in particular to a kind of Atomic layer deposition method of medium of oxides, belong to semi-conductor integrated technology field.
Background technology
Semiconductor technology, as core and the basis of information industry, is the important symbol of weighing a national science technical progress and overall national strength.In in the past more than 40 year, silica-based integrated technology is followed Moore's Law and is improved working speed, the increase integrated level of device and reduced costs by the characteristic dimension of reduction of device, and the characteristic dimension of silicon base CMOS device narrows down to nanoscale by micro-meter scale.Yet when the grid length of MOS device narrows down to below 90 nanometers, traditional silicon base CMOS integrated technology starts to face the double challenge from physics and technical elements.Silicon-dioxide can not meet current semiconducter device to dielectric requirement, and high dielectric constant oxide has obtained increasing application in CMOS integrated technology as gate dielectric material.
Adopting high mobility channel material to substitute traditional silicon material will be the important development direction of semi-conductor integrated technology in " rear mole of epoch ", wherein germanium and III-V group iii v compound semiconductor material are most possibly realized large-scale application, and the high dielectric constant oxide that searching is applicable to germanium and III-V group iii v compound semiconductor material also becomes in the recent period study hotspot both at home and abroad.
The method of ald has that homogeneity is high, surface coverage good, from the accurate advantage such as controlled of limiting surface absorption reaction and the speed of growth, be applied in the process of growth of current C MOS technology gate medium.Method based on ald, the deposition method of the medium of oxides of exploitation high-performance high-k has important application prospect.
Summary of the invention
(1) technical problem that will solve
Main purpose of the present invention is to provide a kind of Atomic layer deposition method of medium of oxides, to optimize the growth conditions of ald of the medium of oxides of high-k.
(2) technical scheme
For achieving the above object, the invention provides a kind of Atomic layer deposition method of medium of oxides, the method is to utilize atomic layer deposition system to carry out the preparation of medium of oxides, comprising:
Step 1: set atomic layer deposition system growth parameter(s);
Step 2: pass into the pulse of metal precursor source in atomic layer deposition system reaction cavity, and then clean with high pure nitrogen, wash out byproduct of reaction and residual metal precursor source;
Step 3: pass into Aquapulse in atomic layer deposition system reaction cavity, and then clean with high pure nitrogen, wash out byproduct of reaction and residual water;
Step 4: pass into in-situ treatment gas pulses in atomic layer deposition system reaction cavity, and then clean with high pure nitrogen, wash out byproduct of reaction and residual in-situ treatment gas;
Step 5: repeat successively step 2, step 3 and step 4, obtain the medium of oxides film of high-k.
In such scheme, in described step 1, the reaction chamber temperature of described atomic layer deposition system is 20 degrees Celsius-500 degrees Celsius, and reaction chamber pressure is 0.5 millibar-10 millibars.
In such scheme, in described step 2, described metal precursor source is trimethyl aluminium (Al (CH
3)
3), four (ethylmethylamino) hafnium (Hf[N (CH
3) (C
2h
5)]
4), four (diethylamino) hafnium (Hf[N (CH
3)
2]
4), four (diethylamino) hafnium (Hf[N (C
2h
5)
2]
4), four trimethyl carbinol hafnium (Hf[O-C (CH
3)
3]
4), three (N, N '-di-isopropyl-amd) yttrium (Y (
ipr
2amd)
3), three (N, N '-di-isopropyl carbonamidine) lanthanum (La (
ipr
2fmd)
3) and glucinum methide (Be (CH
3)
2), titanium tetrachloride (TiCl
4), zinc ethyl ((C
2h
5)
2zn) one or more in.
In such scheme, in described step 2, the temperature in described metal precursor source is 15 degrees Celsius-300 degrees Celsius, the burst length in described metallic precursor source be 1 millisecond-60 seconds, the purity of described high pure nitrogen be 99.999% and more than, the flow of described high pure nitrogen is 10sccm-1000sccm, the scavenging period of described high pure nitrogen be 10 milliseconds-120 seconds.
In such scheme, in described step 3, the burst length of described Aquapulse be 1 millisecond-60 seconds; The purity of described high pure nitrogen be 99.999% and more than, the flow of described high pure nitrogen is 10sccm-1000sccm, the scavenging period of described high pure nitrogen be 10 milliseconds-120 seconds.
In such scheme, in described step 4, the flow of described in-situ treatment gas between 0sccm-1000sccm, the burst length of described in-situ treatment gas pulses be 1 millisecond-10 minutes.
In such scheme, in described step 4, the flow of described high pure nitrogen is 10sccm-1000sccm, the scavenging period of described high pure nitrogen be 10 milliseconds-120 seconds.
In such scheme, in described step 4, described in-situ treatment gas is one or more mixed gass in oxygen, nitrogen, ammonia, hydrogen, laughing gas.
In such scheme, in described step 5, described medium of oxides is one or more combinations of aluminium sesquioxide, hafnium oxide, lanthanum sesquioxide, yttrium oxide, beryllium oxide, titanium dioxide, zinc oxide.
(3) beneficial effect
The Atomic layer deposition method of medium of oxides provided by the present invention, can be applicable to the preparation of silica-based, germanium base and compound semiconductor base MOS device gate medium.This Atomic layer deposition method increases to three kinds of reaction precursor body sources by two kinds of reaction precursor body sources in conventional atomic layer deposition method, water is cooked precursor source and has been guaranteed that reaction carbon foreign matter content in low-temperature epitaxy and reaction product is low, in-situ treatment gas pulses passes in reaction cavity after Aquapulse completes can effectively reduce the defects such as oxygen room in medium of oxides, and can fill the room causing because of steric effect, thereby improve the electrology characteristic of medium of oxides, reduce gate medium electric leakage and improve gate dielectric breakdown voltage.These characteristics show that the present invention possesses wide application prospect and market outlook in rear mole of epoch CMOS integrated technology gate medium deposition.
Accompanying drawing explanation
Fig. 1 is the method flow diagram according to the ald of the aluminium sesquioxide of the embodiment of the present invention.
Embodiment
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.
The present invention is to provide a kind of Atomic layer deposition method of medium of oxides, the method is to utilize atomic layer deposition system to carry out the preparation of medium of oxides, comprises the following steps:
Step 1: set atomic layer deposition system growth parameter(s); Wherein, the reaction chamber temperature of atomic layer deposition system is 20 degrees Celsius-500 degrees Celsius, and reaction chamber pressure is 0.5 millibar-10 millibars.
Step 2: pass into the pulse of metal precursor source in atomic layer deposition system reaction cavity, and then clean with high pure nitrogen, wash out byproduct of reaction and residual metal precursor source;
Wherein, described metal precursor source is trimethyl aluminium (Al (CH
3)
3), four (ethylmethylamino) hafnium (Hf[N (CH
3) (C
2h
5)]
4), four (diethylamino) hafnium (Hf[N (CH
3)
2]
4), four (diethylamino) hafnium (Hf[N (C
2h
5)
2]
4), four trimethyl carbinol hafnium (Hf[O-C (CH
3)
3]
4), three (N, N '-di-isopropyl-amd) yttrium (Y (
ipr
2amd)
3), three (N, N '-di-isopropyl carbonamidine) lanthanum (La (
ipr
2fmd)
3) and glucinum methide (Be (CH
3)
2), titanium tetrachloride (TiCl
4), zinc ethyl ((C
2h
5)
2zn) one or more in.The temperature in described metal precursor source is 15 degrees Celsius-300 degrees Celsius, the burst length in described metallic precursor source be 1 millisecond-60 seconds, the purity of described high pure nitrogen be 99.999% and more than, the flow of described high pure nitrogen is 10sccm-1000sccm, the scavenging period of described high pure nitrogen be 10 milliseconds-120 seconds.
Step 3: pass into Aquapulse in atomic layer deposition system reaction cavity, and then clean with high pure nitrogen, wash out byproduct of reaction and residual water;
Wherein, the burst length of described Aquapulse be 1 millisecond-60 seconds; The purity of described high pure nitrogen be 99.999% and more than, the flow of described high pure nitrogen is 10sccm-1000sccm, the scavenging period of described high pure nitrogen be 10 milliseconds-120 seconds.
Step 4: pass into in-situ treatment gas pulses in atomic layer deposition system reaction cavity, and then clean with high pure nitrogen, wash out byproduct of reaction and residual in-situ treatment gas;
Wherein, the flow of described in-situ treatment gas between 0sccm-1000sccm, the burst length of described in-situ treatment gas pulses be 1 millisecond-10 minutes.The flow of described high pure nitrogen is 10sccm-1000sccm, the scavenging period of described high pure nitrogen be 10 milliseconds-120 seconds.Described in-situ treatment gas is one or more mixed gass in oxygen, nitrogen, ammonia, hydrogen, laughing gas.
Step 5: repeat successively step 2, step 3 and step 4, obtain the medium of oxides film of high-k; Wherein, described medium of oxides is one or more combinations of aluminium sesquioxide, hafnium oxide, lanthanum sesquioxide, yttrium oxide, beryllium oxide, titanium dioxide, zinc oxide.
Following examples specifically describe a kind of medium of oxides aluminium sesquioxide (Al provided by the present invention
2o
3) Atomic layer deposition method.
As shown in Figure 1, Fig. 1 is that the method comprises the steps: according to the method flow diagram of the ald of the aluminium sesquioxide of the embodiment of the present invention
Step 101: as shown in Figure 1, atomic layer deposition system parameter setting, reaction chamber temperature is 250 degrees Celsius, reaction chamber pressure is 1.5 millibars;
Step 102: pass into metal precursor source Al (CH in atomic layer deposition system reaction cavity
3)
3pulse, Al (CH
3)
3the temperature in source is 20 degrees Celsius, and the burst length is 100 milliseconds, and then with high pure nitrogen, cleans, and the purity of high pure nitrogen is 99.999%, and the flow of high pure nitrogen is 300sccm, and scavenging period is 3 seconds.
Step 103: pass into Aquapulse in atomic layer deposition system reaction cavity, the temperature at water source is 20 degrees Celsius, and the burst length is 100 milliseconds, and then with high pure nitrogen, clean, the purity of high pure nitrogen is 99.999%, and the flow of high pure nitrogen is 300sccm, and scavenging period is 3 seconds.
Step 104: pass into pulse of oxygen in atomic layer deposition system reaction cavity, pulse of oxygen is that purity is 99.9999%, the flow 500sccm of oxygen, 5 seconds burst lengths of oxygen, and then with high pure nitrogen, clean, the purity of high pure nitrogen is 99.999%, and the flow of high pure nitrogen is 300sccm, and scavenging period is 4 seconds.
Step 102, step 103 and step 104 form a growth cycle of aluminium sesquioxide, and the thickness of each growth cycle is 0.1 nanometer, and repeating step 102, step 103 and step 104 circulate 100 times successively, the thick aluminium sesquioxide film of growth 10nm.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (9)
1. an Atomic layer deposition method for medium of oxides, is characterized in that, the method is to utilize atomic layer deposition system to carry out the preparation of medium of oxides, comprising:
Step 1: set atomic layer deposition system growth parameter(s);
Step 2: pass into the pulse of metal precursor source in atomic layer deposition system reaction cavity, and then clean with high pure nitrogen, wash out byproduct of reaction and residual metal precursor source;
Step 3: pass into Aquapulse in atomic layer deposition system reaction cavity, and then clean with high pure nitrogen, wash out byproduct of reaction and residual water;
Step 4: pass into in-situ treatment gas pulses in atomic layer deposition system reaction cavity, and then clean with high pure nitrogen, wash out byproduct of reaction and residual in-situ treatment gas;
Step 5: repeat successively step 2, step 3 and step 4, obtain the medium of oxides film of high-k.
2. the Atomic layer deposition method of medium of oxides according to claim 1, is characterized in that, in described step 1, the reaction chamber temperature of described atomic layer deposition system is 20 degrees Celsius-500 degrees Celsius, and reaction chamber pressure is 0.5 millibar-10 millibars.
3. the Atomic layer deposition method of medium of oxides according to claim 1, is characterized in that, in described step 2, described metal precursor source is trimethyl aluminium (Al (CH
3)
3), four (ethylmethylamino) hafnium (Hf[N (CH
3) (C
2h
5)]
4), four (diethylamino) hafnium (Hf[N (CH
3)
2]
4), four (diethylamino) hafnium (Hf[N (C
2h
5)
2]
4), four trimethyl carbinol hafnium (Hf[O-C (CH
3)
3]
4), three (N, N '-di-isopropyl-amd) yttrium (Y (
ipr
2amd)
3), three (N, N '-di-isopropyl carbonamidine) lanthanum (La (
ipr
2fmd)
3) and glucinum methide (Be (CH
3)
2), titanium tetrachloride (TiCl
4), zinc ethyl ((C
2h
5)
2zn) one or more in.
4. the Atomic layer deposition method of medium of oxides according to claim 1, it is characterized in that, in described step 2, the temperature in described metal precursor source is 15 degrees Celsius-300 degrees Celsius, the burst length in described metallic precursor source be 1 millisecond-60 seconds, the purity of described high pure nitrogen be 99.999% and more than, the flow of described high pure nitrogen is 10sccm-1000sccm, the scavenging period of described high pure nitrogen be 10 milliseconds-120 seconds.
5. the preparation method of high dielectric constant oxide according to claim 1, is characterized in that, in described step 3, the burst length of described Aquapulse be 1 millisecond-60 seconds; The purity of described high pure nitrogen be 99.999% and more than, the flow of described high pure nitrogen is 10sccm-1000sccm, the scavenging period of described high pure nitrogen be 10 milliseconds-120 seconds.
6. the Atomic layer deposition method of medium of oxides according to claim 1, it is characterized in that, in described step 4, the flow of described in-situ treatment gas between 0sccm-1000sccm, the burst length of described in-situ treatment gas pulses be 1 millisecond-10 minutes.
7. the Atomic layer deposition method of medium of oxides according to claim 1, is characterized in that, in described step 4, the flow of described high pure nitrogen is 10sccm-1000sccm, the scavenging period of described high pure nitrogen be 10 milliseconds-120 seconds.
8. the Atomic layer deposition method of medium of oxides according to claim 1, is characterized in that, in described step 4, described in-situ treatment gas is one or more mixed gass in oxygen, nitrogen, ammonia, hydrogen, laughing gas.
9. the Atomic layer deposition method of medium of oxides according to claim 1, it is characterized in that, in described step 5, described medium of oxides is one or more combinations of aluminium sesquioxide, hafnium oxide, lanthanum sesquioxide, yttrium oxide, beryllium oxide, titanium dioxide, zinc oxide.
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Cited By (6)
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| CN106756878A (en) * | 2016-12-29 | 2017-05-31 | 中国科学院微电子研究所 | A kind of Atomic layer deposition method of medium of oxides |
| CN107190362A (en) * | 2017-07-17 | 2017-09-22 | 宁波工程学院 | A kind of high-purity ZnO/BiVO4The preparation method of heterogeneous micro belt |
| CN107516692A (en) * | 2016-06-15 | 2017-12-26 | 常州天合光能有限公司 | The method and solar cell of deposit dielectrics film on a silicon substrate |
| 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 |
| CN112746265A (en) * | 2020-12-29 | 2021-05-04 | 兰州空间技术物理研究所 | Method for preparing coating on inner surface of spray pipe |
| TWI744313B (en) * | 2016-04-14 | 2021-11-01 | 日商Ｗａｃｏｍ研究所股份有限公司 | Manufacturing method of HfN film and HfN film |
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Application publication date: 20140326 |