CN104120404A - Ultra-thin silicon oxide film material and manufacturing method thereof - Google Patents
Ultra-thin silicon oxide film material and manufacturing method thereof Download PDFInfo
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- CN104120404A CN104120404A CN201410354061.8A CN201410354061A CN104120404A CN 104120404 A CN104120404 A CN 104120404A CN 201410354061 A CN201410354061 A CN 201410354061A CN 104120404 A CN104120404 A CN 104120404A
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Abstract
The invention provides an ultra-thin silicon oxide film material and a manufacturing method of the ultra-thin silicon oxide film material. According to the method, a substrate is arranged in a high-density plasma enhanced chemical gas phase deposition equipment cavity, O2 gas and SiH4 gas are led into the cavity to be used as reaction gas, argon is led into the cavity to be used as a carrier and protection gas, gas phase deposition is carried out, and the ultra-thin silicon oxide film material is obtained; the working temperature of the high-density plasma enhanced chemical gas phase deposition equipment cavity is controlled to 200 DEG C to 260 DEG C, the working pressure is one Pa to three Pa, and the power of the cavity is 120 W to 200 W; the gas phase deposition time is 10 s to 20 s; the volume ratio of the SiH4 gas to the O2 gas is 8 to 12, and the volume ratio of the argon to the SiH4 gas is 2 to 5. According to the method, the thickness of the silicon oxide film material manufactured on the silicon substrate of four inches is 5.23 nm to 5.33 nm, and the inhomogeneity of the film is lower than 1.0 percent.
Description
Technical field
The invention belongs to optics, semi-conductor and technical field of microelectronic devices; be specifically related to a kind of ultra-thin silicon oxide film material; described mould material has good homogeneity; thickness is 5.23-5.33nm; it has good insulativity, stability and mechanical characteristics; can be used as insulation layer, protective membrane or blooming, be widely used in the fields such as semi-conductor, microwave, photoelectron and optics.
Background technology
Film is a kind of special physical form, because it is small-sized on this specific direction of thickness, the amount that just microcosmic can be surveyed, and on thickness direction due to surface, interface existence, material continuity is interrupted, make thus thin-film material produce the special performance different from bulk material.
Optical thin film is to consist of thin layered medium, propagates a class optical medium material of light beam by interface, is widely used in optics and photoelectron technology field, manufactures various opticinstruments.Optical film technique has formed rounded system at theory, design, calculating and process aspect, the function film of some new microstructures is continually developed out, the appearance in succession of these function films, is penetrated in each emerging field of scientific study optical film technique widely.Silicon oxide film is a kind of important Fine Ceramic Thim Films material, has good insulating property, optical property, inactivating performance, stability and mechanical property, in fields such as microelectronics, photoelectricity and material surface modifyings, has a wide range of applications.
Along with the application of film is more and more extensive, the technology of preparing of film also becomes the important means in high-tech product processing technology gradually.The preparation method of film is a lot, as vapor growth method, liquid-phase growth method (or gas, liquid epitaxial method), oxidation style, diffusion and coating method, electrochemical plating etc., and can be divided into several method in each film-forming method.Plasma activated chemical vapour deposition (PECVD) method is because its handiness, depositing temperature are low, and reproducible feature, provides the possibility of preparing various films in different matrix, becomes and prepares one of the most frequently used method of silicon oxide film.
The homogeneity of ultrathin membrane is key issue and the challenge that first needs solution in film preparation process.The ununiformity of film thickness, has reflected the situation that the film thickness that deposits on substrate to be plated changes according to the variation of substrate present position in vacuum chamber.Membrane thickness unevenness comprises two aspects: 1. in same group is coated with process, the film in substrates of different position deposition has approximate film thickness distribution; 2. the film thickness error that the every film obtaining is only deposited within the specific limits distributes.1. the aspect of membrane thickness unevenness has guaranteed the plated film efficiency of industrialization, and 2. aspect has guaranteed each end properties.Therefore, membrane thickness unevenness is to weigh an important indicator of film coating apparatus performance and film quality, directly has influence on reliability, the stability of plated film device, and the consistence of product.Yield rate impact on device production such as optics, photoelectricity is very large.
Therefore, a kind of ultra-thin silicon oxide film material with excellent homogeneity need to be sought in this area.
Summary of the invention
In order to overcome the larger defect of silicon oxide ultrathin film ununiformity in prior art, one of object of the present invention is to provide a kind of ultra-thin silicon oxide film material, and the thickness of described ultra-thin silicon oxide film material is 5.23-5.33nm; And within the scope of four inches of substrates, film ununiformity is lower than 1.0%;
Wherein, the method for calculation of described ununiformity are: within the scope of inch substrate of film ununiformity=(maximum value-minimum value)/(mean value * 2) * 100%, four, the difference of surveying is counted and is no less than 17.
Wherein, described maximum value is the maximum value of silicon oxide film testing of materials dot thickness; Minimum value is the minimum value of silicon oxide film testing of materials dot thickness; Mean value is the mean value of silicon oxide film testing of materials dot thickness, and calculation formula is: mean value=test point thickness sum/number of checkpoints.
Preferably, the component of described ultra-thin silicon oxide film material is SiO
x, 1≤x≤2 wherein.
The film ununiformity of ultra-thin silicon oxide film material provided by the invention is lower than 1.0%.
Two of object of the present invention has been to provide the preparation method of the described ultra-thin silicon oxide film material of one of a kind of object, and described method is:
Substrate is placed in to high-density plasma reinforced chemical vapor deposition apparatus cavity, passes into O
2gas and SiH
4gas, as reactant gases, passes into argon gas as carrier and shielding gas, carries out vapour deposition, obtains ultra-thin silicon oxide film material;
Wherein, the working temperature of controlling high-density plasma reinforced chemical vapor deposition apparatus cavity is 200～260 ℃, and operating pressure is 1～3Pa, and power is 120～200W;
Wherein, the time of described vapour deposition is 10～20s; Described SiH
4gas and O
2the volume ratio of gas is 8～12, argon gas and SiH
4the volume ratio of gas is 3～6.
For adopting high-density plasma reinforced chemical vapor deposition apparatus, prepare the method for ultra-thin silicon oxide film material, operational condition is more, comprise temperature, pressure, power, time, pass into gas ratio etc., and there is each other close mutual relationship, it not unitary variant independently, therefore how finding a suitable operational condition, is that tool acquires a certain degree of difficulty for those skilled in the art.
Adopt high-density plasma reinforced chemical vapor deposition apparatus to prepare in the operational condition of ultra-thin silicon oxide film material, by the working temperature of high-density plasma reinforced chemical vapor deposition apparatus cavity is arranged on to 200～260 ℃, operating pressure is arranged on 1～3Pa, and power setting is 120～200W; And the time of controlling vapour deposition is 10～20s; The SiH that control passes into
4gas and O
2the volume ratio of gas is 8～12, controls the argon gas and the SiH that pass into
4the volume ratio of gas is 3～6, and having realized and having controlled thickness is that the ultra-thin silicon oxide film material film ununiformity of 5nm left and right is lower than 1.0% object.
Employing high-density plasma reinforced chemical vapor deposition apparatus of the present invention is prepared in the operational condition of ultra-thin silicon oxide film material, the numerical value limiting comprises any numerical value in described scope, for example, the working temperature of high-density plasma reinforced chemical vapor deposition apparatus cavity can be 200 ℃, 217 ℃, 228 ℃, 259 ℃ etc., operating pressure can be 1.2Pa, 1.8Pa, 2.0Pa, 2.3Pa, 2.7Pa, 2.9Pa etc., power can be 120W, 159W, 163W, 175W, 187W, 193W, 198W etc., the time of vapour deposition can be 11s, 13s, 15s, 18s, 20s etc., the SiH passing into
4gas and O
2the volume ratio of gas can be 8.4,10,11.8,12 etc.
Substrate of the present invention is any a kind in P type doped monocrystalline silicon, N-type doped monocrystalline silicon or metal; Or on above-mentioned substrate, prepare the uniform metal of one deck or nonmetal film as the substrate of this experiment.
Preferably, described P type doped monocrystalline silicon or N-type doped single crystal silicon substrate carry out following pre-treatment: with using washed with de-ionized water after HF acid soak, then dry;
Preferably, the mass concentration of described HF acid is 2～10%, such as 3%, 5%, 7%, 8.3%, 9% etc., and more preferably 5%.
Preferably, the described time by HF acid soak is 0.5～10min, such as 1min, 1.4min, 3min, 5min, 7min, 8.4min, 9min, etc., 3min more preferably.
Preferably, described metal substrate is carried out following pre-treatment: with acetone and the ultrasonic cleaning respectively of isopropyl alkyd, then dry; Described ultrasonic time is preferably 5min.
As most preferably, in the preparation method of ultra-thin silicon oxide film material of the present invention, the working temperature of controlling high-density plasma reinforced chemical vapor deposition apparatus cavity is 230 ℃, and operating pressure is 2Pa, and power is 171W; The time of described vapour deposition is 10～20min; Described SiH
4gas and O
2the volume ratio of gas is 10, argon gas and SiH
4the volume ratio of gas is 3.0.
As optimal technical scheme, the thickness having good uniformity of the present invention comprises the steps: at the ultra-thin silicon oxide film material preparation method of 5nm left and right
(1) substrate is placed in to high-density plasma reinforced chemical vapor deposition apparatus cavity, vacuumizing and making back end vacuum tightness is 1 * 10
-4～1 * 10
-6pa, heated substrate to 200～260 ℃;
(2) by 1:(8～12) volume ratio pass into O
2gas and SiH
4as reactant gases, pass into argon gas as carrier gas and shielding gas, adjustment operating air pressure is 1～3Pa, power is 120～200W, carries out chemical vapour deposition 10～20s;
(3) under the atmosphere of protective gas, be down to room temperature, obtain the ultra-thin silicon oxide film material described in claim 1 or 2.
Preferably, step 3) described protective gas is rare gas element; The preferred argon gas of described rare gas element.
Three of object of the present invention has been to provide the purposes of the described ultra-thin silicon oxide film material of one of object, and described ultra-thin silicon oxide film material, as insulation layer, protective membrane or blooming, is applied to the fields such as semi-conductor, microwave, photoelectron and optics.
Compared with prior art, the present invention has following beneficial effect:
(1) thickness of ultra-thin silicon oxide film material provided by the invention is in about 5nm, and has good homogeneity, and within the scope of four inches of substrates, film ununiformity is lower than 1.0%; The homogeneity of the ultra-thin silicon oxide film material that its more existing magnetron sputtering method and electron beam evaporation plating method obtain is significantly improved;
(2) substrate that the present invention uses adopts on P (or N) type doped monocrystalline silicon, metal or above-mentioned substrate prepares layer of metal or nonmetal film, can have excellent homogeneity in differing materials interface preparation, thickness is the ultra-thin silicon oxide film material of 5nm left and right;
(3) the silicide film material preparation process with excellent homogeneity hundred nanometers provided by the invention is simple, has great application potential.
Accompanying drawing explanation
Fig. 1 is the distribution plan of the embodiment of the present invention 1 performance characterization test point thickness.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment helps to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment 1
A ultra-thin silicon oxide film material, prepares by the following method:
(1) with P type (100) doped monocrystalline silicon of polishing, do substrate, and carry out following pre-treatment: first described substrate is used to the HF acid soak 3min of 5wt%, then used washed with de-ionized water, its surface of final drying;
(2) pretreated substrate step (1) being obtained is put into high-density plasma reinforced chemical vapor deposition apparatus cavity, and Bing Jiang sediment chamber vacuumizes, and makes back end vacuum tightness 1 * 10
-5pa left and right, and heated substrate to 230 ℃;
(3) with purity, be all greater than 99.99% SiH
4gas, O
2gas and Ar
2gas is source of the gas; Wherein, SiH
4gas, O
2gas is reactant gases, Ar
2gas is carrier gas and protection gas, the Ar of supply
2gas, O
2gas and SiH
4airshed is respectively: 400sccm, 12.9sccm, 129.8sccm; The operating air pressure of controlling sediment chamber is 2Pa, and power is 171W, carries out chemical vapour deposition 13s;
(4) at Ar
2under gas atmosphere, be cooled to room temperature, acquisition has good uniformity, and thickness is the SiO of 5.2nm left and right
2mould material;
Performance characterization:
By the SiO obtaining
2mould material carries out spectroscopic ellipsometers (unit type is SE 850) test, test condition is: room temperature, the scanning of 200～930nm wavelength region, choose 17 test point, described 17 test point be distributed as 1 central point, 8 circumferential point that radius is r, 8 circumferential point that radius is 2r, described circumferential point is uniformly distributed on the circumference of place, and wherein, the value of r is less than 1/4 long (schematic diagram that Fig. 1 is test point) of minor face of substrate; Test result as shown in Figure 1; By calculating its homogeneity, be 0.76%.
Embodiment 2
A ultra-thin silicon oxide film material, prepares by the following method:
(1) at intrinsic (100) doped monocrystalline silicon sheet of polishing, do substrate, and carry out following pre-treatment: first described substrate is used to the HF acid soak 3min of 5wt%, then used washed with de-ionized water, its surface of final drying;
(2) pretreated substrate step (1) being obtained is put into high-density plasma reinforced chemical vapor deposition apparatus cavity, and Bing Jiang sediment chamber vacuumizes, and makes back end vacuum tightness 1 * 10
-5pa left and right, and heated substrate to 50 ℃;
(3) with purity, be all greater than 99.99% SiH
4gas, O
2gas and Ar
2gas is source of the gas; Wherein, SiH
4gas, O
2gas is reactant gases, Ar
2gas is carrier gas and protection gas, the Ar of supply
2gas, O
2gas and SiH
4airshed is respectively: 350sccm, 12.9sccm, 149.8sccm; The operating air pressure of controlling sediment chamber is 2Pa, and power is 126W, carries out chemical vapour deposition 15s;
(4) at Ar
2under gas atmosphere, be cooled to room temperature, obtain and to have good uniformity, thickness be 5.5nm left and right Si
3o
4mould material;
By the Si obtaining
3o
4mould material carries out spectroscopic ellipsometers (unit type is SE 850) test, and testing method is identical with the performance characterization method of embodiment 1; Crossing and calculating its homogeneity is 0.82%.
Embodiment 3
A ultra-thin silicon oxide film material, prepares by the following method:
(1) with the sapphire of polishing, do substrate, and carry out following pre-treatment: first by acetone and each ultrasonic 5min of Virahol for described substrate, then use washed with de-ionized water, its surface of final drying;
(2) pretreated substrate step (1) being obtained is put into high-density plasma reinforced chemical vapor deposition apparatus cavity, and Bing Jiang sediment chamber vacuumizes, and makes back end vacuum tightness 1 * 10
-6pa left and right, and heated substrate to 260 ℃;
(3) with purity, be all greater than 99.99% SiH
4gas, O
2gas and Ar
2gas is source of the gas; Wherein, SiH
4gas, O
2gas is reactant gases, Ar
2gas is carrier gas and protection gas, the Ar of supply
2gas, O
2gas and SiH
4airshed is respectively: 455sccm, 15.8sccm, 129.8sccm; The operating air pressure of controlling sediment chamber is 2.5Pa, and power is 155W, carries out chemical vapour deposition 18s;
(4) at Ar
2under gas atmosphere, be cooled to room temperature, obtain and to have good uniformity, thickness be 6.0nm left and right SiO film;
The SiO mould material of acquisition is carried out to spectroscopic ellipsometers (unit type is SE 850) test, and testing method is identical with the performance characterization method of embodiment 1; By calculating its homogeneity, be 0.88%.
Applicant's statement, the present invention illustrates detailed method of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed method, does not mean that the present invention must rely on above-mentioned detailed method and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to the selection of the interpolation of the equivalence replacement of each raw material of product of the present invention and ancillary component, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (10)
1. a ultra-thin silicon oxide film material, is characterized in that, the thickness of described ultra-thin silicon oxide film material is 5.23-5.33nm; And within the scope of four inches of substrates, film ununiformity is lower than 1.0%;
Wherein, described inhomogeneity method of calculation are: within the scope of inch substrate of film ununiformity=(maximum value-minimum value)/(mean value * 2) * 100%, four, the difference of surveying is counted and is no less than 17.
2. ultra-thin silicon oxide film material as claimed in claim 1, is characterized in that, the component of described ultra-thin silicon oxide film material is SiO
x, 1≤x≤2 wherein.
3. a preparation method for ultra-thin silicon oxide film material as claimed in claim 1 or 2, is characterized in that, described method is:
Substrate is placed in to high-density plasma reinforced chemical vapor deposition apparatus cavity, passes into O
2gas and SiH
4gas, as reactant gases, passes into argon gas as carrier and shielding gas, carries out vapour deposition, obtains ultra-thin silicon oxide film material;
Wherein, the working temperature of controlling high-density plasma reinforced chemical vapor deposition apparatus cavity is 200～260 ℃, and operating pressure is 1～3Pa, and power is 100～200W;
Wherein, the time of described vapour deposition is 10～20s; Described SiH
4gas and O
2the volume ratio of gas is 8～12, argon gas and SiH
4the volume ratio of gas is 3～6.
4. the preparation method of ultra-thin silicon oxide film material as claimed in claim 3, is characterized in that, described substrate is P type doped monocrystalline silicon, N-type doped monocrystalline silicon or metal any a kind; Or on above-mentioned substrate, prepare the uniform metal of one deck or nonmetal film as the substrate of this experiment.
5. the preparation method of ultra-thin silicon oxide film material as claimed in claim 4, is characterized in that, described P type doped monocrystalline silicon, N-type doped monocrystalline silicon carry out following pre-treatment: with using washed with de-ionized water after HF acid soak, then dry;
Preferably, the mass concentration of described HF acid is 2～10%, more preferably 5%;
Preferably, the described time by HF acid soak is 0.5～10min, more preferably 3min.
6. the preparation method of ultra-thin silicon oxide film material as claimed in claim 4, is characterized in that, described metal substrate is carried out following pre-treatment: with acetone and the ultrasonic cleaning respectively of isopropyl alkyd, then dry; Described ultrasonic time is preferably 5min.
7. the preparation method of the ultra-thin silicon oxide film material as described in one of claim 3～6, is characterized in that step 2) purity of described silane, argon gas and ammonia is all greater than 99.99%, and wherein silane is the gas that 95% argon gas mixes; In the preparation method of described ultra-thin silicon oxide film material, the working temperature of controlling high-density plasma reinforced chemical vapor deposition apparatus cavity is 230 ℃, and operating pressure is 2Pa, and power is 171W; The time of described vapour deposition is 10～20s; Described SiH
4gas and O
2the volume ratio of gas is 10, described argon gas and SiH
4the volume ratio of gas is 3.0.
8. the preparation method of the ultra-thin silicon oxide film material as described in one of claim 3～7, is characterized in that, described method comprises the steps:
(1) substrate is placed in to high-density plasma reinforced chemical vapor deposition apparatus cavity, vacuumizing and making back end vacuum tightness is 1 * 10
-4～1 * 10
-6pa, heated substrate to 200～260 ℃;
(2) by 1:(8～12) volume ratio pass into O
2gas and SiH
4as reactant gases, pass into argon gas as carrier gas and shielding gas, adjustment operating air pressure is 1～3Pa, power is 120～200W, carries out chemical vapour deposition 10～20s;
(3) under the atmosphere of protective gas, be down to room temperature, obtain the ultra-thin silicon oxide film material described in claim 1 or 2.
9. the preparation method of the ultra-thin silicon oxide film material as described in one of claim 3～8, is characterized in that step 3) described protective gas is rare gas element; The preferred argon gas of described rare gas element.
10. a purposes for ultra-thin silicon oxide film material as claimed in claim 1 or 2, is characterized in that, described ultra-thin silicon oxide film material, as insulation layer, protective membrane or blooming, is applied to the fields such as semi-conductor, microwave, photoelectron and optics.
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Cited By (5)
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| CN109923239A (en) * | 2016-09-30 | 2019-06-21 | 沙特基础工业全球技术公司 | Method for the coating of thermoplastic material plasma |
| CN111893461A (en) * | 2020-07-06 | 2020-11-06 | 山东大学 | Growth method of silicon oxide-like flexible film |
| CN112779519A (en) * | 2019-11-11 | 2021-05-11 | 夏泰鑫半导体(青岛)有限公司 | Low-dielectric-constant silicon oxide film layer, preparation method thereof and semiconductor component |
| CN115196639A (en) * | 2022-05-13 | 2022-10-18 | 常州工学院 | Two-dimensional ultrathin silica compound and preparation method thereof |
| CN116641035A (en) * | 2023-07-26 | 2023-08-25 | 南京诺源医疗器械有限公司 | Film coating method for laparoscopic optical piece |
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| CN109923239A (en) * | 2016-09-30 | 2019-06-21 | 沙特基础工业全球技术公司 | Method for the coating of thermoplastic material plasma |
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Application publication date: 20141029 |