CN115714146A - Zinc super-doped silicon, preparation method thereof and application thereof in preparing infrared detector - Google Patents
Zinc super-doped silicon, preparation method thereof and application thereof in preparing infrared detector Download PDFInfo
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- CN115714146A CN115714146A CN202211236162.6A CN202211236162A CN115714146A CN 115714146 A CN115714146 A CN 115714146A CN 202211236162 A CN202211236162 A CN 202211236162A CN 115714146 A CN115714146 A CN 115714146A
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Abstract
The invention discloses a preparation method of zinc super-doped silicon, which comprises the steps of cleaning a silicon substrate, and evaporating or sputtering a zinc film on the surface of the cleaned silicon substrate by adopting a vacuum thermal evaporation or vacuum magnetron sputtering method; and performing scanning radiation on the surface of the zinc film by adopting femtosecond laser to obtain the zinc super-doping. The preparation method is simple and efficient, the invention also provides the zinc super-doped silicon material prepared by the method, the zinc super-doped silicon material has higher zinc doping concentration and better light absorption rate, the invention also provides the application of the zinc super-doped silicon material in preparing the photovoltaic infrared detector, and the prepared infrared detector has better light responsiveness.
Description
Technical Field
The invention belongs to the technical field of silicon-based photoelectron, and particularly relates to zinc super-doped silicon, a preparation method thereof and application thereof in preparing an infrared detector.
Background
The silicon-based photoelectronic technology has the advantages of high speed, low cost, low loss and high integration, faces the historical opportunity of large-scale industrialization and marketization, and is one of the technical fields with development prospects in the modern times. However, for photodetectors integrated in photonic circuits with wavelengths exceeding 1100nm, silicon materials are considered not suitable materials due to their forbidden bandwidth, which greatly restricts the development of silicon-based photonic integration.
Super-doping is considered an effective technique for achieving infrared photoelectric response in silicon. High-concentration doped deep-level impurities are used for introducing high-concentration deep-level centers, and wave functions of the deep-level centers are overlapped with each other to generate delocalization so as to form impurity energy bands. With the help of the impurity band, electrons can realize transition from a valence band to the impurity band and from the impurity band to a conduction band, so that photons with energy lower than the forbidden band width of silicon (1.12 eV) are absorbed. According to the first principle of principle, only when the concentration of deep level impurities is higher than 10 19 cm -3 Then, the formation of the impurity band is possible. Such doping concentrations far exceed the equilibrium solid solubility of typical deep level impurities in silicon. Therefore, a special method is required for doping.
In recent years, due to the extremely short pulse width, the extremely high time resolution and the extremely high peak power of the femtosecond laser, the photoelectric property of the crystalline silicon can be remarkably improved by processing the microstructure on the surface of the crystalline silicon by using the femtosecond laser, and the femtosecond laser receives more and more extensive attention in the field of semiconductor material science. The femtosecond laser is used for irradiating the monocrystalline silicon in the doping environment, and impurities exceeding the equilibrium solid solubility concentration can be doped into the silicon, so that the impurity concentration required by forming an impurity band is achieved, and the silicon responds to infrared light.
At present, the sulfur series elements (sulfur, selenium and tellurium) are successfully super-doped, and corresponding infrared detectors report. The sulfur series element is super-doped by placing silicon in sulfur-containing atmosphere (SF) 6 ) The cavity of (2) is made by scanning with a femtosecond laser. The sulfur super-doped silicon obtained in the way has a surface light trapping structure similar to that of the traditional black silicon, high-concentration sulfur impurities and high infrared light absorption rate. However, the sulfur element has higher electrical activity, so that the super-doped layer has higher free carrier concentration, and the infrared detector based on sulfur super-doped silicon has lower responsivity.
In recent years, the transition metal element is considered to be capable of overcoming the problem of overhigh free carrier concentration of the sulfur series element so as to improve the responsivity of the super-doped silicon-based infrared detector. At present, a super-doped silicon-based infrared detector based on metal elements such as titanium, gold and silver exists, but because the diffusion speed of transition metal in silicon is high, the super-doped silicon of the metal is difficult to prepare and the performance of the super-doped silicon is far from reaching the commercial level. Meanwhile, metals such as gold, silver, titanium and the like also have the defects of high cost, difficult preparation of a doped precursor layer and the like.
Disclosure of Invention
The invention provides a preparation method of zinc super-doped silicon, which is simple and efficient, and also provides a zinc super-doped silicon material prepared by the method, wherein the zinc super-doped silicon material has higher zinc doping concentration and better light absorption rate.
A preparation method of zinc super-doped silicon comprises the following steps:
(1) Cleaning a silicon substrate, and evaporating or sputtering a zinc film on the surface of the cleaned silicon substrate;
(2) Performing scanning radiation on the surface of the zinc film obtained in the step (1) by adopting femtosecond laser to obtain the zinc super-doped silicon, wherein the pulse width of the femtosecond laser is 100-200fs, and the energy flux density is 0.5-1.5J/cm -2 。
This application makes zinc can dissolve in silicon fast through carrying out femto second laser scanning on the zinc film, has avoided leading to the phenomenon of appearing in the follow silicon because the quick diffusion of zinc to obtain the silicon of even super doping zinc, and then have higher zinc doping concentration, exceed the threshold value concentration that forms the impurity area, the energy band structure that forms can assist and absorb near infrared light. The prepared zinc super-doped silicon surface has a continuous periodic pointed cone-shaped structure through reasonable femtosecond laser parameters, incident light is reflected for multiple times in the structure, and a light trapping structure is formed to increase the light absorption rate.
The femtosecond laser scanning can melt the silicon chip and the surface zinc metal film and solidify the silicon chip and the surface zinc metal film at a very high speed, the process is an unbalanced process, and impurities far exceeding the equilibrium solid solubility can be doped into silicon, so that the aim of super doping is fulfilled.
And cleaning the silicon substrate by adopting an RCA cleaning program to remove impurities and an oxide layer on the surface of the silicon.
And sequentially carrying out ultrasonic cleaning, hydrofluoric acid soaking, deionized water cleaning and nitrogen blow-drying on the cleaned silicon substrate. For removing the naturally formed oxide layer.
The vacuum degree of the vacuum thermal evaporation or vacuum magnetron sputtering is 1 multiplied by 10 -4 Pa or less.
The thickness of the zinc film obtained in the step (1) is 20-40nm. The zinc film is too thin, which causes the film thickness to be uneven, and further can cause the doping to be uneven; too thick a zinc film can result in blocking of the laser and result in insufficient doping depth.
The number of single-point pulses is higher than 20.
The surface appearance of the silicon wafer is determined by the single-point pulse frequency and the laser energy flux density, and when the energy flux density is high, a pointed cone-shaped surface light trapping structure can be formed by the lower single-point pulse frequency; when the energy flux density is low, a higher number of single-point pulses is needed to form the surface light trapping structure.
The invention also provides zinc super-doped silicon prepared by the preparation method of the zinc super-doped silicon, wherein the surface of the zinc super-doped silicon has a continuous periodic taper-shaped structure, and the effective doping concentration of zinc is higher than 10 19 cm -3 。
The invention also provides a preparation method of the photovoltaic zinc super-doped silicon-based infrared detector, which comprises the following steps:
(1) Carrying out ultrasonic cleaning and annealing treatment on the zinc super-doped silicon;
(2) Putting the zinc super-doped silicon obtained in the step (1) into a hydrofluoric acid solution for cleaning to remove a surface oxide layer;
(3) Placing a mask on the upper surface of the zinc super-doped silicon obtained in the step (2), and then carrying out thermal evaporation on the upper surface of the zinc super-doped silicon to obtain a top electrode;
(4) And (4) blade-coating an indium-gallium alloy on the lower surface of the zinc super-doped silicon obtained in the step (3) to obtain the photovoltaic zinc super-doped silicon-based infrared detector.
In the step (3), the top electrode is a hollow square gold electrode.
The invention also provides a preparation method of the photoconductive zinc super-doped silicon-based infrared detector, which comprises the following steps:
(1) Carrying out ultrasonic cleaning and annealing treatment on the zinc super-doped silicon;
(2) Putting the zinc super-doped silicon obtained in the step (1) into a hydrofluoric acid solution for cleaning to remove a surface oxide layer;
(3) Placing a mask on the upper surface of the zinc super-doped silicon obtained in the step (2), and then carrying out thermal evaporation and evaporation on the upper surface of the zinc super-doped silicon to obtain inserted finger-shaped gold electrodes which are used as two electrodes of the light guide type detector, so as to obtain the light guide type zinc super-doped silicon-based infrared detector;
the channel width of the two electrodes of the interdigitated gold electrode is 50-100 μm.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the method, the femtosecond laser method is utilized to enable the zinc film to be rapidly dissolved in the silicon, the problem that the effective doping concentration of zinc in the silicon is low due to the fact that zinc is separated out from the silicon due to rapid diffusion of the zinc is solved, and the effective doping concentration of the zinc in the silicon exceeds 10 by utilizing the method 19 cm -3 Over a threshold concentration for forming an impurity band, soThe formed energy band structure can assist in absorbing near infrared light. Meanwhile, by setting reasonable femtosecond laser parameters, the microstructure of the silicon surface can enable incident light to be reflected for multiple times, the optical path length of the incident light on the super-doped layer is increased, and the light absorption rate of the incident light serving as a light trapping structure is increased.
(2) The method for preparing the zinc super-doped silicon uses a zinc material with reasonable cost, and adopts a simple thermal evaporation or sputtering method, so that the preparation method is simple and has reasonable cost.
(3) The photovoltaic silicon-based infrared detector made of zinc super-doped silicon forms an effective photodiode through a pn junction formed by a p-type super-doped layer and a substrate, can generate light response from visible light to near infrared bands, and generates considerable light response to 1310nm and 1550nm of key communication wavelengths which cannot generate response of a common silicon-based photoelectric detector. The photoconductive infrared detector made of zinc super-doped silicon also generates photoelectric response to infrared light energy.
Drawings
Fig. 1 is a schematic view of femtosecond laser processing provided in embodiment 1, in which fig. 1a is a schematic view of processing, and fig. 1b is a diagram of a scanning path of the femtosecond laser;
fig. 2 is scanning electron micrographs of the surface topography of the zinc super-doped silicon provided in examples 1 and 2 and comparative examples 1 and 2, wherein fig. 2a is the scanning electron micrograph of the surface topography of the zinc super-doped silicon provided in comparative example 1, fig. 2b is the scanning electron micrograph of the surface topography of the zinc super-doped silicon provided in comparative example 2, fig. 2c is the scanning electron micrograph of the surface topography of the zinc super-doped silicon provided in example 2, and fig. 2d is the scanning electron micrograph of the surface topography of the zinc super-doped silicon provided in example 1;
FIG. 3 is a spectrum of visible-infrared absorption spectrum of zinc super-doped silicon prepared in example 1;
FIG. 4 is a schematic structural view of a photovoltaic super-doped silicon-based infrared detector prepared in application example 1;
FIG. 5 is a response curve diagram of a photovoltaic super-doped silicon-based infrared detector prepared in application example 1;
fig. 6 is a schematic structural view of the photoconductive super-doped silicon-based infrared detector prepared in application example 2.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention.
Example 1
The specific manufacturing method of the zinc super-doped silicon comprises the following steps: cleaning, coating and femtosecond laser scanning, and the specific description is as follows:
the specific steps of cleaning comprise: adopting a standard RCA cleaning program, carrying out alcohol ultrasonic treatment on the cut silicon wafer, and sequentially carrying out ultrasonic treatment on the silicon wafer in an RCAI number solution (volume ratio NH) under the condition of 80 ℃ water bath 3 ·H 2 O:H 2 O 2 :H 2 O =1 2 O 2 :H 2 O = 1). NH 3 ·H 2 O, HCl and H 2 O 2 The concentrations of the solutions were 28%,37% and 30%, respectively. And placing the cleaned silicon wafer in deionized water for ultrasonic cleaning for 3 minutes. The sonicated sample was soaked with a dilute hydrofluoric acid solution (about 2%) for 2 minutes to remove the naturally formed oxide layer on the surface. And thoroughly washing the silicon wafer with deionized water, blow-drying with a nitrogen gun, placing in a culture dish, and storing in a vacuum environment for later use.
The specific steps of coating comprise: fixing the clean silicon wafer on a vacuum thermal evaporation sample stage, sealing the sample chamber, and vacuumizing to 1 × 10 by a mechanical pump and a molecular pump -4 Pa or less. The evaporation boat adopts a tungsten boat, and the evaporation source adopts zinc particles with the purity of more than 99.99 percent. The evaporation rate and time were controlled so that the thickness of the evaporated Zn metal film was 30nm. The samples after completion of the thermal evaporation were stored in a nitrogen glove box to avoid surface oxidation.
The specific steps of the femtosecond laser scanning, as shown in fig. 1a and 1b, include: and performing femtosecond laser scanning on the coated silicon wafer by adopting a pulse laser galvanometer system with the central wavelength of 380nm and the pulse width of 200 fs. The scanning mode is progressive scanning. Setting proper scanning speed and line spacing to adjust the average pulse number per point on the silicon chip to 50 times,the different pulse times can make the surface topography of the silicon wafer generate larger difference, as shown in fig. 2d, the surface of the silicon wafer is in a continuous periodic pointed cone-shaped structure, and the structure can make the incident light reflected therein for multiple times to form a light trapping structure to increase the light absorption rate. The energy flux density of the adopted laser is 0.5-1.5J cm -2 Meanwhile, the zinc super-doped silicon is obtained, as shown in fig. 3, the absorption rate of the common silicon wafer to infrared light with the wavelength of more than 1100nm is close to 0%, and the absorption rate of the zinc super-doped silicon wafer to the infrared light with the wavelength of 1100-2000nm is generally more than 50%, which proves that the zinc super-doped silicon has a very significant effect on expanding the infrared absorption of silicon.
Example 2
Unlike the embodiment 1, the plating step includes: by vacuum magnetron sputtering. The clean silicon chip is fixed on a vacuum magnetron sputtering sample table, a sample cavity is sealed, and the vacuum degree is pumped to below 1 multiplied by 10 < -4 > Pa by a mechanical pump and a molecular pump. The sputtering source uses a zinc target with the purity of more than 99.99 percent, and the sputtering rate and the sputtering time are controlled by adjusting proper voltage and power under the protection of argon gas, so that the thickness of the sputtered metal film is 30nm. The sputtered samples were stored in a glove box under nitrogen to avoid surface oxidation. The pulse width is 100fs, the average number of pulses received per dot is 20, and as shown in fig. 2c, the surface forms a pointed cone-shaped surface light trapping structure.
Comparative example 1
Unlike example 1, when the number of single-point pulses is less than 5, as shown in fig. 2a, the surface of the silicon wafer is dotted and the light absorption is low.
Comparative example 2
Unlike example 1, when the number of single-point pulses is less than 10, the surface of the silicon wafer shows a striped undulation as shown in fig. 2b, and the light absorption rate is low.
Application example 1
The manufacturing method of the photovoltaic super-doped silicon-based infrared detector comprises the following steps: cleaning, heat treatment, top electrode growth and back electrode scrape coating, and the specific description is as follows:
the zinc super-doped silicon is ultrasonically cleaned in acetone to remove nano-particle silicon, impurities and dirt which are possibly generated in the processing process. And annealing the zinc super-doped silicon subjected to ultrasonic cleaning at the temperature of 600-800 ℃ for 30 minutes, and performing heat treatment in a quartz tube furnace under the protection of argon. After raising the temperature of the tube furnace to a predetermined temperature, the sample was put in after introducing a protective gas (argon gas) for about 5 minutes, and was kept at a constant temperature for 30 minutes, followed by furnace cooling. The annealing process can repair the lattice defects caused by the femtosecond laser super doping process and activate the doped impurities. After the annealing process is completed, the super-doped silicon wafer is soaked in a diluted hydrofluoric acid solution (about 2%) for 2 minutes to remove the oxide layer on the surface.
The top electrode is obtained by thermal evaporation under the cover of a mask. Fixing the thermally treated super-doped silicon wafer on a vacuum thermal evaporation sample stage, covering with an electrode mask (rectangular frame mask for photovoltaic detector and finger-inserted mask for photoconductive detector) having a shape corresponding to the required shape, sealing the sample chamber, and vacuumizing to 1 × 10 by mechanical pump and molecular pump -4 Pa or less. The evaporation boat adopts a tungsten boat, and the evaporation source adopts gold particles with the purity of more than 99.99 percent. The gold electrode can form good ohmic contact with the p-type super-doped layer, has extremely high conductivity, and can improve carrier collection efficiency, thereby improving the responsivity of the detector. The evaporation rate and evaporation time were controlled so that the electrode thickness was 150nm, and too thin an electrode resulted in uneven electrode thickness affecting the contact, and too thick an electrode wasted material.
And after the top electrode is grown, the back surface of the top electrode is required to be coated with indium-gallium alloy in a scraping mode to serve as a back electrode. A pn junction is formed between the super-doped layer and the bottom silicon substrate due to the difference of carrier concentration, reverse bias is applied through the upper electrode and the lower electrode, photo-generated carriers can be generated when light irradiates a top surface photosensitive area, and the photo-generated carriers are separated under the action of the external bias and collected by the upper electrode and the lower electrode to generate photocurrent, so that the purpose of light detection is achieved.
As shown in fig. 4, the photovoltaic super-doped silicon-based infrared detector has a structure that the lower surface of n-type silicon is coated with indium-gallium alloy as a back electrode, the upper surface of the n-type silicon is formed with zinc super-doped silicon, and a gold top electrode is plated on the surface of the zinc super-doped silicon.
As shown in fig. 5, the zinc-super-doped silicon-based photovoltaic detector exhibits the rectifying characteristic of a pn junction when not illuminated (corresponding to the black dark current curve in the figure). When reverse voltage is applied, no matter white light or infrared light is adopted to irradiate the detector, obvious photocurrent can be generated, which shows that the zinc super-doped silicon-based photovoltaic detector has good photoresponse to visible light and infrared light.
Application example 2
Different from the application example 1, the photoconductive detector is manufactured after the top electrode is grown, and the insertion finger-shaped electrodes at two sides are respectively used as a positive electrode and a negative electrode to be connected into a circuit. When the electrodes at two ends are loaded with bias voltage, if the channel region between the insertion fingers at two sides is irradiated by light, the generated photon-generated carriers are separated under the applied voltage to generate photocurrent, thereby achieving the purpose of optical detection. The structure of the photoconductive detector is shown in fig. 6, zinc super-doped silicon is formed on the surface of a silicon wafer, and finger-inserted Au electrodes are plated on the surface of the zinc super-doped silicon.
Claims (10)
1. A preparation method of zinc super-doped silicon is characterized by comprising the following steps:
(1) Cleaning a silicon substrate, and evaporating or sputtering a zinc film on the surface of the cleaned silicon substrate;
(2) Performing scanning radiation on the surface of the zinc film obtained in the step (1) by adopting femtosecond laser to obtain the zinc super-doped silicon, wherein the pulse width of the femtosecond laser is 100-200fs, and the energy flux density is 0.5-1.5J/cm -2 。
2. The method for preparing zinc-super-doped silicon according to claim 1, wherein the silicon substrate is cleaned by an RCA cleaning procedure to remove impurities and an oxide layer on the surface of the silicon.
3. The method according to claim 1, wherein the cleaned silicon substrate is sequentially subjected to ultrasonic cleaning, hydrofluoric acid soaking, deionized water cleaning and nitrogen blow-drying.
4. The method for preparing zinc-super doped silicon according to claim 1,it is characterized in that the vacuum degree of the vacuum thermal evaporation or vacuum magnetron sputtering is 1 multiplied by 10 -4 Pa or less.
5. The method for preparing zinc super-doped silicon according to claim 1, wherein the thickness of the zinc thin film obtained in the step (1) is 20-40nm.
6. The method according to claim 1, wherein the number of single-point pulses is greater than 20.
7. The zinc-doped silicon prepared by the preparation method of zinc-doped silicon according to any one of claims 1 to 6, wherein the surface of the zinc-doped silicon has a continuous periodic pointed cone-shaped structure, and the effective doping concentration of zinc is higher than 10 19 cm -3 。
8. A preparation method of a photovoltaic zinc super-doped silicon-based infrared detector is characterized by comprising the following steps:
(1) Carrying out ultrasonic cleaning and annealing treatment on the zinc super-doped silicon according to claim 7;
(2) Putting the zinc super-doped silicon obtained in the step (1) into a hydrofluoric acid solution for cleaning to remove a surface oxide layer;
(3) Placing a mask on the upper surface of the zinc super-doped silicon obtained in the step (2), and then carrying out thermal evaporation and evaporation on the upper surface of the zinc super-doped silicon to obtain a top electrode, wherein the top electrode is a hollow square gold electrode;
(4) And (4) blade-coating an indium-gallium alloy on the lower surface of the zinc super-doped silicon obtained in the step (3) to obtain the photovoltaic zinc super-doped silicon-based infrared detector.
9. A method for preparing a photoconductive zinc super-doped silicon-based infrared detector is characterized by comprising the following steps:
(1) Subjecting the zinc-super-doped silicon of claim 7 to ultrasonic cleaning and annealing treatment;
(2) Putting the zinc super-doped silicon obtained in the step (1) into a hydrofluoric acid solution for cleaning to remove a surface oxide layer;
(3) And (3) placing a mask on the upper surface of the zinc super-doped silicon obtained in the step (2), and then carrying out thermal evaporation and evaporation on the upper surface of the zinc super-doped silicon to obtain two finger-inserted gold electrodes, thereby obtaining the photoconductive zinc super-doped silicon-based infrared detector.
10. The method for preparing the photoconductive zinc-heavily-doped silicon-based infrared detector as claimed in claim 9, wherein the channel widths of the two electrodes of the finger-inserted gold electrode are 50-100 μm.
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