CN103196773B - Device for online measuring stoichiometric proportions and ingredient masses of PLD (Pulsed Laser deposition) film - Google Patents
Device for online measuring stoichiometric proportions and ingredient masses of PLD (Pulsed Laser deposition) film Download PDFInfo
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Abstract
The invention relates to the field of pulsed laser deposition film coating and discloses a device for online measuring stoichiometric proportions and ingredient masses of a PLD (Pulsed Laser deposition) film. The device comprises a pulsed laser deposition (PLD) film coating system, a laser induced breakdown spectrometry (LIBS) measuring system and a quartz crystal microbalance (QCM) measuring system. The device disclosed by the invention can be used for online measuring the stoichiometric proportions and ingredient masses of the pulsed laser deposition film in situ on the basis of the pulsed laser deposition film coating technology, the laser induced breakdown spectrometry technology and the quartz crystal microbalance technology, no interference is generated on the film coating process, the construction of the device is simple, and the device is easy to operate; and the device is suitable to be applied in the field of pulsed laser deposition film coating.
Description
Technical field
The present invention relates to pulsed laser deposition plated film field, particularly the device of a kind of on-line measurement PLD film stoichiometry when each composition quality.
Background technology
Pulsed laser deposition (PLD) prepares film, project on target after the normally a branch of pulse laser focusing of its process, the high-energy-density of laser will make on target by the moment ablation of the component material of irradiation zone, normal direction preferentially along target is transmitted by ablation thing subsequently, forms plasma plume at target material surface.Ablation thing in space basad direction transports, and in substrate surface cohesion, forming core, growth, finally obtain required film.In whole growth course, usually can be filled with certain gas of certain pressure intensity in cavity, such as generally be filled with a certain amount of oxygen during deposition oxide.Duration in each stage of PLD process from psec to microsecond not etc.One of main advantage of PLD is the stoichiometric proportion of film and the basically identical of target material.But, have many factors can have impact to the stoichiometric proportion of film, such as: environmental gas kind, pressure, pulsed laser energy, target material surface condition and ablation characteristics etc.These make target become more complicated to the transfer of the stoichiometric proportion of film, can not ensure that film grows according to stoichiometric proportion.
Therefore determine that film stoichiometry comparison forms high-quality thin film, significant.We adopt Laser-induced Breakdown Spectroscopy means to measure thin film composition stoichiometric proportion, measure the total deposition of film and thickness by QCM (Quartz Crystal Microbalance), the result of the two are combined, obtain the content of various composition in film.
Laser-induced Breakdown Spectroscopy (Laser-induced breakdown spectroscopy, LIBS) can be used to carry out quantitative and qualitative analysis ultimate analysis to the sample of non-principal component, can be used for measuring the chemical composition that laser ablation produces material.When high energy pulse laser beam focus is at target material surface, extremely preheating target one fritter volume, causes producing transient state plasma by above irradiation zone.The light that plasma plume sends and light intensity depend on the element kind and content thereof that are sputtered out, and the spectrum launched with spectrometer analysis, can obtain qualitative or quantitative analysis result.LIBS original position can analyze multiple element simultaneously, measures real-time, obtain the number percent of their content to sputtered material (namely by the material of film forming) out.
Multiple method is had to LIBS data analysis.Wherein freely determine calibration method not need to draw calibration curve by carrying out experiment measuring to standard model, but directly calculate the concentration analyzing component according to the relative intensity of the spectral line obtained.Advantage: without the need to calibrating thing, program simplification, cost is lower; Full elements are contained; Really realize remote online real-time analysis.Shortcoming: do not consider self absorption effect, has impact to measurement result; Need analyze all spectral lines, workload is relatively large.
QCM (Quartz Crystal Microbalance) (Quartz Crystal Microbalance, QCM or QMB) is inverting element with quartz crystal, utilizes two effects of quartz crystal, i.e. piezoelectric effect and mass loading effect.By the change detecting quartz crystal natural frequency, realize the monitoring to film thickness and deposition rate, measuring accuracy can Da Nake magnitude.QCM has that structure is simple, cost is low, resolution is high, highly sensitive, specificity good, can the advantage such as real time on-line monitoring, be widely used in the every field such as physics, biology, chemistry, medical science.QCM has the locus and temporal resolution well determined for the growth of monitoring film.The valuable data that it can provide material to obtain and lose in low heat flux zones.
Summary of the invention
The object of the invention is: in order to solve technical matters of the prior art, the device of a kind of on-line measurement PLD film stoichiometry when each composition quality is provided, the present invention is based on pulsed laser deposition coating technique, LIBS, QCM (Quartz Crystal Microbalance) survey thickness technology, energy real-time in-situ on-line measurement pulsed laser deposition plated film film stoichiometry when each composition quality, and interference can not be had to coating process, and build simple, be easy to operation.
For achieving the above object, the technical solution used in the present invention is: the device providing a kind of on-line measurement PLD film stoichiometry when each composition quality, comprising: pulsed deposition coating system (PLD), Laser-induced Breakdown Spectroscopy (LIBS) measuring system, QCM (Quartz Crystal Microbalance) (QCM) measuring system, data analysis system.
Described pulsed laser deposition plated film (PLD) system is used for the film in substrate deposition specific function, comprising: vacuum chamber 1, pulsed laser 4, rotatable target platform 6, target 7, rotatable base station 8, substrate 9, first condenser lens 10; Described vacuum chamber 1 outer wall is provided with vacuum pump group 11, vacuum gauge 14, air intake opening 16, first quartz window 12, for the formation of the environmental gas condition needed for plated film; Described target 7, substrate 9 are placed in rotatable target platform 6 in vacuum chamber 1, rotatable base station 8 respectively; It is interior and corresponding with the first quartz window 12 of vacuum chamber 1 that described first condenser lens 10 is placed on vacuum chamber 1; It is outside that described pulsed laser 4 is positioned at vacuum chamber 1.
Pulsed laser 4 sends pulse laser, enters vacuum chamber 1 through the first quartz window 12, focuses on target 7 surface, as the energy source of ablation sputtering target material through the first condenser lens 10; The substrate 9 that rotatable base station 8 is placed, as the substrate of growing film; The target 9 that rotatable target platform 8 is placed, as the source of film substrate.
Described Laser-induced Breakdown Spectroscopy (LIBS) measuring system for the formation of and store the LIBS spectrum of laser splash target plasma plume, comprising: fiber spectrometer 2, second condenser lens 19, optical fiber 15; It is interior and corresponding with the second quartz window 20 of vacuum chamber 1 that described second condenser lens 19 is placed on vacuum chamber 1; Described fiber spectrometer 2 gathers LIBS spectrum by optical fiber 13.
Pulsed laser is sent out 4 and is gone out pulse laser, enters vacuum chamber 1 through the first quartz window 12, focuses on target material surface through the first condenser lens 10, forms plasma plume; Second condenser lens 19 focuses on optical fiber 15 receiving surface for the light sent by plasma plume 13; Optical fiber 15 is for transmitting LIBS spectrum; Fiber spectrometer 2 is for gathering LIBS spectrum.
Described QCM (Quartz Crystal Microbalance) (QCM) measuring system, for measuring film thickness information, comprising: quartz crystal film thickness monitor 3, oscillator 5, quartz crystal sensor 17, quartz crystal 21; Described quartz crystal 21 to be fixed on quartz crystal sensor 17 and to be placed in vacuum chamber 1; Described quartz crystal sensor 17, oscillator 5, quartz crystal film thickness monitor 3 are connected by BNC cable successively.
Quartz crystal 21 is for deposit film, and quartz crystal sensor 17 gives the electric current of quartz crystal 21 for transmission oscillator 5, make quartz crystal 21 vibration at high speed, and the electric signal transmission produced by quartz crystal 21 is to oscillator 5; Electronic signal is delivered to quartz crystal film thickness monitor 3 by oscillator 5; Quartz crystal film thickness monitor 3 is for controlling quartz crystal sensor 17 and recording the change of thickness; High temperature, high heat load all can reduce the performance of quartz crystal 21, in order to keep the life-span of quartz crystal 21, when not needing to measure, the baffle plate of quartz crystal sensor 9 should be closed, and quartz crystal 21 is become certain distance with detected materials.
Described data analysis system and computing machine 18; Described computing machine 18 respectively with light spectral instrument 2, quartz crystal film thickness monitor 3, pulsed laser 4 connection; For the sequential of regulating impulse laser instrument 4 and fiber spectrometer 2, store and analyze the LIBS signal that fiber spectrometer spreads out of, obtaining each composition that laser ablation target 7 produces, i.e. film forming component, percentage information; Also for obtain that quartz crystal film thickness monitor 3 spreads out of become film thickness information; The measurement result of the two combines the most at last, draws pulsed laser deposition plated film film stoichiometry when each composition quality.Pulsed laser 4 and fiber spectrometer 2 time ordered pair LIBS signal intensity have a great impact, be obtain optimum signal-noise ratio, need repeatedly debug this value.
Wherein, described first quartz window 12, second quartz window 20, vacuum gauge 14, vacuum pump group 11, air intake opening 16 are arranged on the flange of vacuum chamber 1.
The invention has the beneficial effects as follows: the present invention is based on pulsed laser deposition coating technique, LIBS, QCM (Quartz Crystal Microbalance) survey thickness technology, energy real-time in-situ on-line measurement pulsed laser deposition plated film film stoichiometry when each composition quality, and interference can not be had to coating process, and build simple, be easy to operation; Be applicable to pulsed laser deposition plated film field.
Accompanying drawing explanation
Fig. 1 is the structural representation of a kind of on-line measurement of the present invention PLD film stoichiometry when device of each composition quality.
Accompanying drawing identifies: 1-vacuum chamber, 2-fiber spectrometer, 3-quartz crystal film thickness monitor, 4-pulsed laser, 5-oscillator, 6-rotatable target platform, 7-target, the rotatable base station of 8-, 9-substrate, 10-first condenser lens, 11-vacuum pump group, 12-first quartz window, 13-plasma plume, 14-vacuum gauge, 15-optical fiber, 16-air intake opening, 17-quartz crystal sensor, 18-computing machine, 19-second condenser lens, 20-second quartz window, 21-quartz crystal.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in detail.
With reference to Fig. 1, the device of a kind of on-line measurement of the present invention PLD film stoichiometry when each composition quality, comprising: pulsed deposition coating system (PLD), Laser-induced Breakdown Spectroscopy (LIBS) measuring system, QCM (Quartz Crystal Microbalance) (QCM) measuring system, data analysis system.
Described pulsed laser deposition plated film (PLD) system is used for the film in substrate deposition specific function, comprising: vacuum chamber 1, pulsed laser 4, rotatable target platform 6, target 7, rotatable base station 8, substrate 9, first condenser lens 10; Described vacuum chamber 1 outer wall is provided with vacuum pump group 11, vacuum gauge 14, air intake opening 16, first quartz window 12, for the formation of the environmental gas condition needed for plated film, vacuum chamber 1 is evacuated to vacuum state by vacuum pump group 11, and in experimentation, maintain the stability of its vacuum state; Described target 7, substrate 9 are placed in rotatable target platform 6 in vacuum chamber 1, rotatable base station 8 respectively; It is interior and corresponding with the first quartz window 12 of vacuum chamber 1 that described first condenser lens 10 is placed on vacuum chamber 1; It is outside that described pulsed laser 4 is positioned at vacuum chamber 1.
Pulsed laser 4 sends pulse laser, enters vacuum chamber 1 through the first quartz window 12, focuses on target 7 surface, as the energy source of ablation sputtering target material through the first condenser lens 10; The substrate 9 that rotatable base station 8 is placed, as the substrate of growing film; The target 9 that rotatable target platform 8 is placed, as the source of film substrate.
Described Laser-induced Breakdown Spectroscopy (LIBS) measuring system for the formation of and store the LIBS spectrum of laser splash target plasma plume, comprising: fiber spectrometer 2, second condenser lens 19, optical fiber 15; It is interior and corresponding with the second quartz window 20 of vacuum chamber 1 that described second condenser lens 19 is placed on vacuum chamber 1; Described fiber spectrometer 2 gathers LIBS spectrum by optical fiber 13.
Pulsed laser is sent out 4 and is gone out pulse laser, enters vacuum chamber 1 through the first quartz window 12, focuses on target material surface through the first condenser lens 10, forms plasma plume; Second condenser lens 19 focuses on optical fiber 15 receiving surface for the light sent by plasma plume 13; Optical fiber 15 is for transmitting LIBS spectrum; Fiber spectrometer 2 is for gathering LIBS spectrum.
Described QCM (Quartz Crystal Microbalance) (QCM) measuring system, for measuring film thickness information, comprising: quartz crystal film thickness monitor 3, oscillator 5, quartz crystal sensor 17, quartz crystal 21; Described quartz crystal 21 to be fixed on quartz crystal sensor 17 and to be placed in vacuum chamber 1; Described quartz crystal sensor 17, oscillator 5, quartz crystal film thickness monitor 3 are connected by BNC cable successively.
Quartz crystal 21 is for deposit film, and quartz crystal sensor 17 gives the electric current of quartz crystal 21 for transmission oscillator 5, make quartz crystal 21 vibration at high speed, and the electric signal transmission produced by quartz crystal 21 is to oscillator 5; Electronic signal is delivered to quartz crystal film thickness monitor 3 by oscillator 5; Quartz crystal film thickness monitor 3 is for controlling quartz crystal sensor 17 and recording the change of thickness; High temperature, high heat load all can reduce the performance of quartz crystal 21, in order to keep the life-span of quartz crystal 21, when not needing to measure, the baffle plate of quartz crystal sensor 9 should be closed, and quartz crystal 21 is become certain distance with detected materials.
Described data analysis system and computing machine 18; Described computing machine respectively with light spectral instrument, quartz crystal film thickness monitor 3, pulsed laser 4 connection; For the sequential of regulating impulse laser instrument 4 and fiber spectrometer 2, store and analyze the LIBS signal that fiber spectrometer spreads out of, obtaining each composition that laser ablation target 7 produces, i.e. film forming component, percentage information; Also for obtain that quartz crystal film thickness monitor 3 spreads out of become film thickness information; The measurement result of the two combines the most at last, draws pulsed laser deposition plated film film stoichiometry when each composition quality.Pulsed laser 4 and fiber spectrometer 2 time ordered pair LIBS signal intensity have a great impact, be obtain optimum signal-noise ratio, need repeatedly debug this value.
Wherein, described first quartz window 12, second quartz window 20, vacuum gauge 14, vacuum pump group 11, air intake opening 16 are arranged on the flange of vacuum chamber 1.
Described fiber spectrometer 2(is for Ocean Optics of U.S. LIBS2500+), can gather spectral range 200-980 nm, resolution 0.1 nm (FWHM), detection 14,336 pixel CCD, frame speed is by conputer controlled 10 Hz; Trigger delay is-121us to+135us in 500ns, by OOILIBS software control, is used for gathering LIBS spectrum, can carries out real-time qualitative measurement, have ppb and pieck stage sensitivity.Optical fiber 15 is by collected optical transport to fiber spectrometer, and computing machine 18 controls the duty of fiber spectrometer 2, stores and analyzes obtained spectral information.
Described quartz crystal film thickness monitor 3(is for INFICON company SQM 160), use the speed in quartz crystal sensor commercial measurement film deposition process and thickness, be 0.03Hz in 10 frequency resolutions read under value/second, within the scope of whole service, temperature stability is 2 ppm.Quartz crystal 21 is positioned on baffled quartz crystal sensor 9, for collecting the material that laser splash goes out.
Described pulsed laser 4(is for French Quantel company Brilliant EaZy model Nd:YAG nanosecoud pulse laser) the high-energy ps pulsed laser and ns pulsed laser of 1064nm, 532nm, 355nm tri-kinds of wavelength can be provided, as the lasing light emitter of sharp pld (pulsed laser deposition) and LIBS.
Measuring process of the present invention comprises the following steps:
Step 1: need according to plated film, select suitable target 7, substrate 9 and environmental gas.
Step 2: be placed on by target 7 on rotatable target platform 6, is placed on substrate 9 in rotatable base station 8.
Step 3: the position regulating rotatable target platform 6, rotatable base station 8, first condenser lens 10, second condenser lens 19, make target 7 be parallel to target 7 with target 7 one-tenth miter angle, optical fiber 15 in the face of substrate 9, quartz crystal 21, and gather spectral position at the focus place being positioned at the focus place of condenser lens apart from target 71 ~ 2mm place, target 7, optical fiber 15 is positioned at the second condenser lens 19.
Step 4: by vacuum pump group 11 by vacuum chamber 1 vacuum state, then use vacuum gauge 14 measurement of vacuum, until air pressure is less than 10
-3mbar:; Need to be filled with corresponding gas from air intake opening 16 according to plated film.
Step 5: according to the needs of coating film thickness, computing machine 18 carries control software design by fiber spectrometer 2 and arranges laser pulse number, regulates laser instrument Q time delay, arranges the sequential of pulsed laser 4 and fiber spectrometer 2, start plated film and gather LIBS spectrum.
Step 6: while pulsed laser 4 is started working, computing machine 18 shows and records the change of quartz crystal 21 resonant frequency with the pulsed laser deposition plated film time in real time.
Step 7: analyze LIBS signal with free scaling method, calculate each compositional stoichiometry ratio in film;
The characteristic spectral line intensity of the particle recorded can be expressed as:
Wherein,
for the line strength measured, k, i are respectively the high and low energy level of electronic transition corresponding to characteristic wavelength, and λ is the wavelength of the characteristic spectral line of selection analysis; F is test parameters, C
sfor the atom content corresponding to selected emission line; g
kfor high level degeneracy, A
kifor k energy level is to the transition probability of i energy level, E
kfor high level energy, k
bfor Boltzmann constant, T is plasma temperature, U
s(T) be partition function.E
k, g
kand A
kican check in from atomic spectrum standard and technical data library NIST; F, T and
result is determined by experiment;
Definition x=E
k,
,
,
, then y=mx+q
s.Draw the relation curve of (x, y), with least square fitting, the slope reaction and plasma temperature obtained, the concentration of the intercept obtained reaction institute amalyzing substances.
Constant F is determined by normalization:
;
Describedly freely determine calibration method, based on following hypothesis:
L () thinks the material composition of the composition energy actual response analytic target of atom in laser plasma;
(2) think that laser plasma is in local thermal equilibrium;
(3) do not consider the self absorption effect of plasma, think that this laser plasma is an optically thin plasma.
Step 8: the change analyzing quartz crystal 21 resonant frequency, calculates total deposition;
The natural resonance frequency f of the quartz chip piezoelectric effect of AT cutting is:
(1)
Wherein, n is harmonic number, n=1,3,5, d
qfor the thickness of quartz crystal, c is shear elasticity coefficient; ρ is the density (2.65 × 10 of quartz crystal
3kg/m
3);
Can Hua Wei ﹕ for conventional first-harmonic (n=1) (1) formula
?(2)
Wherein,
(AT cutting), is called the frequency constant of crystal; d
qfor the thickness of crystal.
(2) are declined and get:
the physical significance of above formula is, if thickness is d
qquartz crystal increase thickness deltat d
q, then the vibration frequency of crystal has changed Δ f, and the negative sign in formula represents that the frequency of crystal reduces along with the increase of thickness.Assuming that the rete of deposit does not change quartz crystal mode of oscillation, by quartz crystal thickness increment Δ d
qrepresented by mass transfer and become thicknesses of layers increment Delta d
m.Then:
(3)
And the rete of in fact deposit has changed the vibration mode of quartz itself, by the vibration mode of homogenous material, become the mixing vibration pattern of bi-material; Consider that quartz crystal is become mixing vibration pattern by after rete deposit, the formula of following calculating thickness of having derived:
(4)
Wherein, A
ffor film thickness, unit dust (); N
q-AT-cut crystal frequency constant, 1.668 × 10
13hertz. dust (Hz); D
qfor quartzy density, 2.648g/cm
3; π is constant, 3.1415926; D
ffor film material density, unit g/cm
3; Z is material Z coefficient,
, Z
macoustic impedance (the unit gcm of deposition membrane
2s), Z
qacoustic impedance (the unit gcm of quartz crystal
2s); F
qfor the resonant frequency of quartz crystal; F
ccrystal frequency after deposition materials.
Step 9: the result of LIBS and the result of QCM are combined, obtains the quality of each composition in film;
Produce n kind material after assumes samples laser ablation, i-th kind of material concentration (relative concentration) that LIBS measurement obtains is C
si; QCM records crystal frequency after deposition materials
, then total ablation amount M is:
, wherein S is quartz crystal receiving area.
By Σ
iΜ
i=Μ and Σ
sc
s=1, the ablation amount of various ablation resultant can be obtained
.
Above content is the further description done the present invention in conjunction with optimal technical scheme, can not assert that the concrete enforcement of invention is only limitted to these explanations.Concerning general technical staff of the technical field of the invention, under the prerequisite not departing from design of the present invention, simple deduction and replacement can also be made, all should be considered as protection scope of the present invention.
Claims (2)
1. the device of an on-line measurement PLD film stoichiometry when each composition quality, it is characterized in that, the device of described a kind of on-line measurement pld (pulsed laser deposition) stoichiometry when each composition quality comprises: pulsed laser deposition coating system, Laser-induced Breakdown Spectroscopy measuring system, QCM (Quartz Crystal Microbalance) measuring system, data analysis system;
Described pulsed laser deposition coating system comprises: vacuum chamber (1), pulsed laser (4), rotatable target platform (6), target (7), rotatable base station (8), substrate (9), the first condenser lens (10); Described vacuum chamber (1) outer wall is provided with vacuum pump group (11), vacuum gauge (14), air intake opening (16), the first quartz window (12); Described target (7), substrate (9) are placed in vacuum chamber (1) interior rotatable target platform (6), rotatable base station (8) respectively; It is interior and corresponding with first quartz window (12) of vacuum chamber (1) that described first condenser lens (10) is placed on vacuum chamber (1); It is outside that described pulsed laser (4) is positioned at vacuum chamber (1), corresponding to the first quartz window and the first condenser lens;
Described Laser-induced Breakdown Spectroscopy measuring system comprises: fiber spectrometer (2), the second condenser lens (19), optical fiber (15); It is interior and corresponding with second quartz window (20) of vacuum chamber (1) that described second condenser lens (19) is placed on vacuum chamber (1); Described fiber spectrometer (2) gathers LIBS spectrum by optical fiber (15);
Described QCM (Quartz Crystal Microbalance) (QCM) measuring system comprises: quartz crystal film thickness monitor (3), oscillator (5), quartz crystal sensor (17), quartz crystal (21); Described quartz crystal (21) is fixed on quartz crystal sensor (17) and goes up and be placed in vacuum chamber (1); Described quartz crystal sensor (17), oscillator (5), quartz crystal film thickness monitor (3) are connected by BNC cable successively;
Described data analysis system and computing machine (18); Described computing machine (18) respectively with fiber spectrometer (2), quartz crystal film thickness monitor (3), pulsed laser (4) connection.
2. the device of a kind of on-line measurement PLD film stoichiometry according to claim 1 when each composition quality, it is characterized in that, described first quartz window (12), the second quartz window (20), vacuum gauge (14), vacuum pump group (11), air intake opening (16) are arranged on the flange of vacuum chamber (1).
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| CN107478175A (en) * | 2017-08-18 | 2017-12-15 | 东南大学 | A kind of atomic layer deposition thin film in-situ monitoring control system |
| CN112924437B (en) * | 2019-12-06 | 2023-02-21 | 核工业西南物理研究院 | Laser-induced breakdown spectroscopy absolute quantitative analysis method |
| CN115181942B (en) * | 2022-07-19 | 2024-04-02 | 重庆华谱科学仪器有限公司 | Plasma grating pulse laser deposition coating method |
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