CN101260515B - Device and method for real time monitoring metal source beam flow change in active gas environment - Google Patents
Device and method for real time monitoring metal source beam flow change in active gas environment Download PDFInfo
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- CN101260515B CN101260515B CN2008101042699A CN200810104269A CN101260515B CN 101260515 B CN101260515 B CN 101260515B CN 2008101042699 A CN2008101042699 A CN 2008101042699A CN 200810104269 A CN200810104269 A CN 200810104269A CN 101260515 B CN101260515 B CN 101260515B
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Abstract
The invention discloses a device for the real-time monitoring of the change of metal source beam current in the film growing process under the environment of active gas and a method thereof. The device comprises a vacuum gauge, a vacuum gauge power supply, a digital voltage detecting instrument and a computer control system. The method comprises the following steps that: active gas with constant flow rate is conducted to a film growing chamber; the digital voltage detecting instrument is utilized to measure a vacuum gauge electrical signal value corresponding to background air pressure; a metal source is heated to the temperature needed for film growing and stabilized for 10 to 30 minutes; through precisely detecting the changing value of the electrical signal, the change of the metal source beam current is detected. The method and the device are utilized to master the tiny change of the metal source beam flow rate at any time in the film growing process and achieve the aim of precisely controlling the flow rate through temperature regulation, thereby realizing the high-quality growing of the film in the active gas and having good repeatability.
Description
Technical field
The present invention relates to a kind of thin film growth process apparatus and method of monitoring metal source beam flow variation in real time that are used for, belong to technical field of vacuum plating.
Background technology
The important component part that the accurate control growing technology of film is the contemporary high-tech art is being brought into play important role in improving film and device performance.In multiple film preparing technology, the molecular beam epitaxy technique that the 60 to 70's of last century grows up is because clean environment, the accurate control of epitaxy layer thickness and the characteristics such as control with a wide range of precise of doping content of its ultrahigh vacuum, obtained application more and more widely at industrial circles such as semiconductors, from the preparation of simple substance membrane, progressively develop into the preparation of alloy firm and compound film.A nearest important development is that molecular beam epitaxy technique is used to prepare third generation semiconductor material with wide forbidden band such as nitride, oxide, be characterized in adopting active gases to provide source metal as nitrogen or oxygen source and traditional diffusion furnace, as adopt oxygen plasma or ozone as oxygen source, utilize metallic zinc as zinc source developing zinc oxide monocrystal thin films (Z.X.Mei, et al, Appl.Phys.Lett.86,112111 (2005)); And for example adopt the plasma of nitrogen or ammonia as nitrogenous source, utilize the gallium stove that gallium source growing gallium nitride single crystal film (L.He, et al, Appl.Phys.Lett.88,071901 (2006) are provided; A.Salvador, et al, Appl.Phys.Lett.69 2692, (1996)).As everyone knows, in the molecular beam epitaxy technique, accurate control to line is the basis that the realization film is accurately controlled growth, metal source beam flow in traditional molecular beam epitaxy technique is that the temperature by accurate control diffusion furnace realizes, in the growing film process, keep the temperature-resistant of diffusion furnace, then the metal line just can keep stable.And when films such as growth ZnO, GaN, source metal is exposed under the environment of active gases, the source metal surface that is in heated condition can react with background gas and generate wrappage, influence the evaporation of source metal gradually, thereby metal source beam flow is changed, and this variation can have a strong impact on growth for Thin Film speed and quality.Therefore, how under active gases, to monitor the key issue that metal source beam flow becomes films such as present growth ZnO, GaN in real time.
The present invention is directed to this problem, thereby utilize the reaction of active gases and metal line to cause air pressure in the growth room this rule that changes, develop a kind of technology that can monitor the variation of metal source beam flow trace in real time, thereby solved the difficulty in the film growth control under active gases such as oxide, nitride, realized the preparation of high-quality thin film.
Summary of the invention:
The object of the present invention is to provide a kind of apparatus and method that metal source beam flow changes that are used for monitoring in real time in the active gas environment molecular beam epitaxial growth thin-film process.Utilize this apparatus and method, can in experimentation, constantly grasp the small variation of metal beam flow, and can reach the purpose of accurate Control Flow, and have good repeatability by adjustment.
The device (being called for short metal line monitoring device) that is used for the real-time monitoring of molecular beam epitaxial growth process metal source beam flow under the active gases provided by the invention comprises vacuum gauge, vacuum gauge power supply, digital voltage detection table, computer control system; Described vacuum gauge is connected by vacuum flange with thin film growth chamber, is used for obtaining the electric signal of thin film growth chamber gas pressure intensity value; Described vacuum gauge power supply links to each other with vacuum gauge, and vacuum gauge is powered; Described digital voltage detects table (abbreviation voltage table), links to each other with vacuum gauge by the vacuum gauge power supply, is used for the voltage of the electric signal that high Precision Detection obtained by vacuum gauge; Described computer control system and digital voltage detect epiphase and connect, and are used for the electric signal that the digital voltage detector obtains is handled.
Further, described active gases can with monitored source metal generation chemical reaction.
Further, described active gases is oxygen or ozone or oxygen plasma, and described monitored source metal is zinc or magnesium.
Further, the range of described digital voltage detection table is at least 0～2mV, and figure place showing is at least 4.
The method that is used for the real-time monitoring of molecular beam epitaxial growth thin-film process metal source beam flow under the active gases provided by the invention is achieved by the following technical solution:
1) at the indoor feeding active gases of film growth, utilize the metal source beam flow monitoring device measure active gases background gas pressure value the magnitude of voltage V of corresponding electric signal
0
2) heating of metal source makes it be warmed up to the required temperature of film growth, and after stablizing 10～30 minutes, utilize above-mentioned metal source beam flow monitoring device once more MEASUREMENTS OF THIN growth room internal gas pressure value the magnitude of voltage V of corresponding electric signal
1
3) with step 2) in the preceding magnitude of voltage V of intensification that write down in the magnitude of voltage that obtains and the step 1)
0It is poor to do, and obtains difference V
0-V
1=Δ V, the film growth room pressure that is source metal intensification front and back changes pairing voltage difference, and the result of gained is exactly the data of sign metal source beam flow under this temperature;
4) when the air pressure in the thin film growth chamber changes, adjust the source oven temperature degree of source metal, make electric signal voltage difference equal difference DELTA V corresponding to line.
Further, the active gases in the described step 1) refers to the gas that can react with monitored source metal, and during as the line of monitoring metallic zinc, magnesium, oxygen, ozone and oxygen plasma etc. are active gases.
Further, the background gas pressure value in the described step 1) is 10
-5～10
-2Pa.
Further, internal gas pressure changing value in growth room's is evaporated to growth chamber owing to metallic atom and reacts with active gases and causes in the described step 3) from diffusion furnace, the metallic atom line is big more, many more with the active gases reaction, then the air pressure change value is just big more, therefore, this changing value has reflected the size of metal line.
When needing to adjust metal source beam flow in the experiment, the source stove is heated up or cooling, and observe the registration changing value of voltage table in the metal line monitoring device.The size of voltage change indicates the size that line changes.
The principle that said method can be measured the metal source beam flow variation mainly is that metallic atom and the active gases molecule that has utilized the heating source stove to evaporate reacts, thereby reduced the air pressure in the vacuum chamber, further utilize high accuracy number voltage detecting table that the subtle change of air pressure is accurately measured, thereby realize the real-time monitoring that the minute metallic line changes.In logical active gases, the heating of source metal also can impact the air pressure in the vacuum chamber, but because in ultra-high vacuum environment, the free path of molecule is length (10 extremely
-6Molecule mean free path approximately is 5000m under the Pa), and hold the mouth of pot and misalignment vacuum gauge (or the line rule) filament of source metal, it is also insensitive to make that vacuum gauge (or line rule) detects the metal line, the actual detection value is the contribution that arrives the metallic atom of rule filament after the vacuum chamber inwall repeatedly reflects, so detected value and actual value differ far away.For 10
-8～10
-7The background vacuum of Pa, the heating of metal source to the experiment in temperature after, vacuum is 10
-6About Pa, and in the growth course of metal oxide, nitride, the pressure of active gases often will reach 10
-3Pa, and be full of whole vacuum system with the form of gas.When source fender plate is not opened, after source metal is heated, metallic atom is evaporated from crucible, can be stopped by baffle plate, and, in this process, fully react generation solid-state oxide or nitride with active gases in indoor repeatedly reflection, and finally be adsorbed on the wall of chamber, make room pressure descend.As seen, the metallic atom that evaporate this moment has had sufficient contribution to atmospheric pressure value, and we just can pass through the heating of metal source, and the changing value of observed and recorded room pressure obtains the data that are closely related with the metal beam rheologyization.
In the growth course of reality, have many factor affecting and the control of temperature metal source beam flow, this traditional just line control method is difficult to the problem that solves by simple means.Such as, continuous consumption along with source metal, line under the uniform temp also changes thereupon, like this, the parameter of sign metal line has been not only the temperature of source metal stove, though classic method can be by carrying out the line test so that the corresponding relation of temperature and line is calibrated to all source metal of using before each experiment, this will waste the time and improve experimental cost for experiment increases complicated step.Different with classic method, the present invention has overcome because line and shortcoming inequality under the uniform temp that the consumption of source metal brings, by the air pressure change amount that is caused before and after the observed and recorded lifting source metal temperature, the fine setting temperature, and make atmospheric pressure value be stabilized in needed value, reaching the purpose of accurate control line, and this method simple and fast.
In addition, in the growth of each oxide, all can cause to a certain degree oxidation to the source metal surface in the vacuum chamber.The saturated vapour pressure of these oxides is very low, although be extremely thin one deck, also can hinder the evaporation of metallic atom, influences the metal line under the uniform temp greatly.Do not handle and the line test if source metal is degassed before the experiment,, under this temperature, may only evaporate the metallic atom of minute quantity so, can't reach the experiment effect of expection still with the temperature control metal source beam flow of experience.The film of other kinds of preparation more or less all exists similar situation under active gases, has caused harm to repeating to prepare high-quality thin film.And the present invention has conveniently solved this problem efficiently, has improved the evaporation efficiency of source metal.
In addition, monitoring when the present invention also is fit to two kinds of metal source beam flows, this growth to alloy firm is very useful.The monitoring of two kinds of metal source beam flows can be achieved by the following scheme:
1) at the indoor feeding active gases of film growth, utilize metal line monitoring device record active gases background gas pressure value the magnitude of voltage V of corresponding electric signal
0
2) heating first source metal makes it be warmed up to the required temperature of film growth, and after stablizing 10～30 minutes; Utilize metal line monitoring device MEASUREMENTS OF THIN growth room internal gas pressure value the magnitude of voltage V of corresponding electric signal
1
3) with step 2) the middle magnitude of voltage V that obtains
1With the magnitude of voltage V before the intensification of being write down in the step 1)
0It is poor to do, and obtains difference V
0-V
1=Δ V
1, the film growth room pressure that is first source metal intensification front and back changes pairing voltage difference, and the result of gained is exactly the data of sign first metal source beam flow under this temperature;
4) temperature with first source metal keeps constant, heats second source metal, and it is temperature required that it is warmed up to, and stablized 10～30 minutes;
5) utilize metal line monitoring device MEASUREMENTS OF THIN growth room internal gas pressure value the magnitude of voltage V of corresponding electric signal
2, and with V
2With the magnitude of voltage V before the intensification of being write down in the step 3)
1It is poor to do, and obtains the second difference V
2-V
1=Δ V
2, the film growth room pressure that is second source metal intensification front and back changes pairing voltage difference, and the result of gained is exactly the data of sign second metal source beam flow under this temperature.
When needing to change the line of first source metal (or second source metal) in the growth course, regulate the temperature of first source metal (or second source metal) and keep stable, after 10～30 minutes, utilize metal line monitoring device to measure the variation of the magnitude of voltage of the caused vacuum gauge electric signal of air pressure change, judge whether the metal line reaches predetermined value.
By with top same step, the present invention is applicable to the monitoring of metal source beam flow more than three kinds or three kinds in the molecular beam epitaxial growth of alloy material under the active gases.
Description of drawings
Fig. 1 monitors the device synoptic diagram that metal source beam flow changes in real time in the active gas environment;
Fig. 2 is the real-time observation interface of metal source beam flow;
Fig. 3 monitors the block diagram that metal source beam flow changes in real time in active gas environment;
Fig. 4 is that aerating oxygen is stablized rear backdrop air pressure detection curve in the embodiment of the invention 1;
Fig. 5 determines background relative barometric pressure figure in the embodiment of the invention 1;
Fig. 6 is the line detection curve of Zn temperature-rise period in the embodiment of the invention 1;
Fig. 7 is the line detection curve when the Zn temperature arrives maximum in the embodiment of the invention 1;
Fig. 8 is the line detection curve after the Zn cooling in the embodiment of the invention 1.
Embodiment
The present invention is described in detail below in conjunction with embodiment, but can not be interpreted as limiting the scope of the invention.
Monitor the device synoptic diagram that metal source beam flow changes in the thin film growth chamber in a kind of active gas environment of the present invention as shown in Figure 1 in real time.This device comprises: vacuum gauge 1, vacuum gauge power supply 2, digital voltage detect table 3, computer control system 4, wherein vacuum gauge 1 with contain active other thin film growth chamber and be connected by vacuum flange, be used for obtaining the electric signal of thin film growth chamber gas pressure intensity value; Vacuum gauge power supply 2 links to each other with vacuum gauge 1, is used for providing power supply to vacuum gauge; Digital voltage detects table 3 (abbreviation voltage table) and links to each other with vacuum gauge 1 by vacuum gauge power supply 2, is used for the magnitude of voltage of the electric signal that high Precision Detection obtained by vacuum gauge; Computer control system 4 detects table 3 with digital voltage and links to each other, and is used for the electric signal that digital voltage detection table obtains is handled.The real-time observation interface of metal line as shown in Figure 2 comprises two parts content, i.e. the metal line Monitoring and Controlling interface of the Pressure monitoring of left part control interface and right side part.The interface, left side comprise be positioned at below " air pressure detect control " shift knob, middle " relative barometric pressure " display window and " relative barometric pressure " display box of left part; If click " air pressure detects control " shift knob, computer system promptly begins to gather the electric signal of the indoor background relative barometric pressure of film growth correspondence, and the form with figure line shows in " relative barometric pressure " display window of centre, and " relative barometric pressure " display box of on the left side shows the electric signal numerical value V of film growth room pressure correspondence in real time simultaneously
1The interface, right side then comprises " beam monitoring control " shift knob, " record background relative barometric pressure " OK button, " background relative barometric pressure " display box, " metal beam rheologyization " display box and middle " metal line " display window.When background gas pressure is stablized, click right side " record background relative barometric pressure " button, computer system will collect the electric signal numerical value V of the indoor background relative barometric pressure of film growth this moment correspondence automatically
0, and in " background relative barometric pressure " display box, show.If begin heating of metal source stove this moment, the film growth room pressure reduces, and the electric signal of its real-time air pressure correspondence is V
1(i.e. numerical value in the display box of top, left side), computer real-time writes down this numerical value, and with V
1With V
0Difference (Δ V=V
0-V
1) be presented in " metal beam rheologyization " display box, the form with figure line shows in " metal line " display window simultaneously.
During embodiment 1 developing ZnO monocrystal film to the monitoring method of Zn line
Utilize as shown in Figure 1 metal line monitoring device and the real-time observation interface of metal line as shown in Figure 2, and according to the block diagram that changes of monitoring metal source beam flow in real time in the active gas environment of the present invention as shown in Figure 3, developing ZnO monocrystal film.At first, the vacuum gauge power supply is powered to vacuum gauge, and obtain the electric signal of the indoor reflection atmospheric pressure value of film growth by vacuum gauge, this electric signal is separated by the vacuum gauge power supply, and detects the table high Precision Detection by digital voltage; Computer control system and digital voltage detect epiphase and connect, and analyze, control the voltage detecting data, realize the detection of halved tie rheologyization.Its concrete monitoring method of Zn line when developing ZnO monocrystal film is as follows:
1) opens the oxygen quality flow control meter (Mass FlowController) that links to each other with thin film growth chamber,, carry out the oxygen discharge, in thin film growth chamber, obtain oxygen plasma with the oxygen flow of 2.20sccm and 250 watts radio-frequency power; Radio-frequency power is transferred to 340 watts, keep constant, thereby obtain stable background active gases pressure.
2) open the real-time observation interface of computer control system, click " air pressure detects control " shift knob, it is the value of electrical signals that the interval scan vacuum gauge records that computer system begins with 1 second, this value is corresponding to the vacuum film growth room pressure, and be presented in the display box of left side top (as accompanying drawing 4) with the numerical value form, be 0.3078;
3) after the wait stable gas pressure, the hit OK button is to obtain the value of electrical signals V that current air pressure is background
0, this value no longer changes, and is presented in the background relative barometric pressure display box, and numerical value degree of accuracy is wherein adjusted to five position effective digitals, is 0.30737 (as accompanying drawing 5);
4) Zn source stove begins to heat up, and clicks and then click " beam monitoring control " shift knob, and computer system begins the line variation of Zn is detected.As shown in Figure 6, instantaneous relative value of electrical signals V
1Be 0.29724, with background relative barometric pressure V
0It is poor to do, and obtains
Δ V=0.30737-0.29724 ≈ 0.01014, this value is this line changing value preceding with respect to intensification of Zn constantly, is presented in the metal beam rheology display box;
5) Zn source stove be warming up to 320 ℃ stable after, air pressure begins to stablize, the Zn line tends towards stability, expression Δ V=0.01387 (as accompanying drawing 7) can begin the growth of ZnO film;
6) behind the growth ending, Zn source stove begins cooling, pressure rises, and the Zn line descends, and last Δ V is tending towards 0 (as accompanying drawing 8).
In above-mentioned growth course,,, thereby reduced air pressure with oxygen reaction because the rising of Zn source oven temperature degree makes the Zn atom be evaporated out.The corresponding electric signal difference of 320 ℃ Zn source temperature is 0.01387, so just, can estimate the line of Zn 320 ℃ the time according to the film thickness that grows, when the Zn solid particles surface oxidized, or remaining Zn source is seldom the time, the variation that causes Δ V just can in time be adjusted the source oven temperature degree less than 0.01387 o'clock, made the electric signal difference DELTA V of reflection line equal 0.01387 at last, thereby obtained and the identical Zn line of experiment last time, guaranteed the repeatedly repeatability of experiment.
During embodiment 2 growth MgZnO monocrystal thin films to the monitoring method of Zn, Mg line
It is identical with embodiment 1 that line detects principle, as follows to the concrete monitoring method of Zn, Mg line:
1) opens the oxygen quality flow control meter (Mass FlowController) that links to each other with thin film growth chamber,, carry out the oxygen discharge, in thin film growth chamber, obtain oxygen plasma with the oxygen flow of 2.20sccm and 250 watts radio-frequency power; Radio-frequency power is transferred to 340 watts, and oxygen flow is elevated to 2.60sccm and keeps constant, thereby obtains stable background active gases pressure.
2) computer system begin with 1 second be the value of electrical signals that the interval scan vacuum gauge records, this is worth corresponding to the vacuum film growth room pressure, electric signal corresponding after the stable gas pressure is 0.35206, this value is V
0
3) Zn source stove begins to heat up and is stabilized in 325 ℃ of the required temperature of film growth, corresponding value of electrical signals V at this moment
1Be 0.32954, with background relative barometric pressure (V
0) do poorly, obtain Δ V
1=V
0-V
1=0.35206-0.32954=0.02252, this value is this line changing value preceding with respect to intensification of Zn constantly;
4) Mg source stove begins to heat up and is stabilized in 375 ℃ of the required temperature of film growth, corresponding value of electrical signals V at this moment
2Be 0.32276, with the background relative barometric pressure (V of this moment
1) do poorly, obtain Δ V
2=V
1-V
2=0.32954-0.322796=0.00158, this value is this line changing value preceding with respect to intensification of Mg constantly.
5) can begin growing film this moment, behind the growth ending Zn, Mg source stove be lowered the temperature.
In above-mentioned growth course, after Zn source oven temperature degree (325 ℃) is enough stable, background gas pressure no longer changes, make the Mg atom be evaporated out the line that the air pressure that reduces with oxygen reaction can indicate Mg, if the air pressure in the thin film growth chamber changes at this moment, adjust the source oven temperature degree of Mg, make electric signal voltage difference equal the second difference DELTA V corresponding to Mg source line
2
Claims (7)
1. the device that changes of monitoring metal source beam flow in real time in the thin film growth process in the active gas environment, it is characterized in that this device comprises: vacuum gauge, vacuum gauge power supply, digital voltage detect table, computer control system; Described active gases can with monitored source metal generation chemical reaction; Vacuum gauge is connected with the thin film growth chamber that contains active gases, is used for obtaining the electric signal of thin film growth chamber gas pressure intensity value; The vacuum gauge power supply links to each other with vacuum gauge, is used for providing power supply to vacuum gauge; Digital voltage detects table and links to each other with vacuum gauge by the vacuum gauge power supply, is used to detect the voltage of the electric signal that is obtained by vacuum gauge; Computer control system and digital voltage detect epiphase and connect, and are used for the electric signal that the digital voltage detector obtains is handled, shown.
2. device as claimed in claim 1 is characterized in that, described active gases is oxygen or ozone or oxygen plasma, and described monitored source metal is zinc or magnesium.
3. device as claimed in claim 1 is characterized in that, the range of described digital voltage detection table is at least 0～2mV, and figure place showing is at least 4.
4. the method that changes of monitoring metal source beam flow in real time in the active gas environment is characterized in that: described active gases can with monitored source metal generation chemical reaction, said method comprising the steps of:
1) at the indoor feeding active gases of film growth, utilize as in the claim 1 to 5 as described in each measurement device active gases background gas pressure value the magnitude of voltage V of corresponding electric signal
0
2) heating of metal source makes it be warmed up to the required temperature of film growth, and after stablizing 10～30 minutes, utilize as in the claim 1 to 5 as described in each device once more MEASUREMENTS OF THIN growth room internal gas pressure value the magnitude of voltage V of corresponding electric signal
1
3) with step 2) in the preceding magnitude of voltage V of intensification that write down in the magnitude of voltage that obtains and the step 1)
0It is poor to do, and obtains difference V
0-V
1=Δ V, the film growth room pressure that is source metal intensification front and back changes pairing voltage difference, and difference DELTA V is exactly the data of sign metal source beam flow under this temperature;
4) when the air pressure in the thin film growth chamber changes, adjust the source oven temperature degree of source metal, make electric signal voltage difference equal difference DELTA V corresponding to line.
5. method as claimed in claim 4, wherein the background gas pressure value described in the step 1) is 10
-5～10
-2Pa.
6. method as claimed in claim 4, wherein the film growth room pressure changing value described in the step 3) is evaporated to the growth room owing to metallic atom and reacts with active gases and causes from diffusion furnace, and this changing value has reflected the size of metal line.
7. monitor the method that two kinds of metal source beam flows change in real time in an active gas environment, it is characterized in that, may further comprise the steps:
1) at the indoor feeding active gases of film growth, utilize each described device in 1 to 5 record active gases background gas pressure value the magnitude of voltage V of corresponding electric signal
0
2) heating first source metal makes it be warmed up to the required temperature of film growth, and after stablizing 10～30 minutes, utilize metal line monitoring device MEASUREMENTS OF THIN growth room internal gas pressure value the magnitude of voltage V of corresponding electric signal
1
3) with step 2) the middle magnitude of voltage V that obtains
1With the magnitude of voltage V before the intensification of being write down in the step 1)
0It is poor to do, and obtains the first difference V
0-V
1=Δ V
1, the film growth room pressure that is first source metal intensification front and back changes pairing voltage difference, the first difference DELTA V
1The data that indicate first metal source beam flow under this temperature exactly;
4) the first source metal temperature is kept constant, heat second source metal, it is temperature required that it is warmed up to, and stablized 10～30 minutes;
5) utilize each described measurement device film growth room pressure value in 1 to 5 the magnitude of voltage V of corresponding electric signal
2, and with V
2With the magnitude of voltage V before the intensification of being write down in the step 3)
1It is poor to do, and obtains the second difference V
1-V
2=Δ V
2, the film growth room pressure that is second source metal intensification front and back changes pairing voltage difference, the second difference DELTA V
2The data that indicate second metal source beam flow under this temperature exactly;
6) when the air pressure in the thin film growth chamber changes, adjust the source oven temperature degree of second source metal, make electric signal voltage difference equal the second difference DELTA V corresponding to second metal source beam flow
2
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