Reception method of nanostructure silicon base plates

FIELD: physics; semiconductors.

SUBSTANCE: invention concerns processes of chemical machining of slices and can be used for creation of silicon bodies with nanosized structure, applicable as emitters of ions in analytical devices and for creation of light emitting devices. Essence of the invention consists in the reception method of nanostructure silicon base plates by processing of siliceous substances with a gas-vapor mix containing hydrofluoric acid and an oxidising substance, as an oxidising substance halogen or its mix with a oxygen-containing oxidising reagent taken in number of not less than 1.0% is used. Iodine can be used as halogen, and in quality of an oxygen-containing oxidising reagent - a reagent chosen from the group: ozone, peroxide, sulfuric acid, nitric oxide. The invention allows to Iodine can be used as halogen, and in quality of an oxygen-containing oxidising reagent - a reagent chosen from the group: ozone, peroxide, sulfuric acid, nitric oxide.

EFFECT: obtaining of base plates keeping stability of physical and chemical properties of a surface at long storage in natural conditions and providing high uniformity of physical and chemical properties of a surface and, accordingly, higher reproducibility of the analysis at use of such base plates.

8 cl, 6 dwg, 1 tbl

 

The invention relates to processes of chemical processing of semiconductor wafers and can be used to create silicon substrates with nanoscale structure is applicable as emitters ions in analytical instruments, in particular the mass spectrometer. The invention can also be used to create light-emitting devices.

A silicon substrate with a nanocrystalline structure have a number of properties that distinguish them from single-crystal and polycrystalline substrates. In particular, when the laser impact they can become highly effective emitter pre-ions adsorbed on their surface chemical compounds. This property is used in the method of surface-induced laser desorption-ionization (Surface Assisted Laser Desorption-Ionization or " SALDI"), in particular, in one of the most important variants of this method-desorption-ionization on silicon substrates [Alimpiev, S., Nikiforov, S., Karavanskii V., J. Sunner, "On the mechanism of laser induced desorption-ionization of organic compounds from etched silicon and carbon surfaces" J. Chem. Phys., 2001, V.115, P.1891-1901; Zhouxin Shen, John J. Thomas, Claudia Averbuj, Klas M. Broo, Mark Engelhard, John E. Crowell, M.G.Finn and Gary Siuzdak "Porous Silicon as a Versatile Platform for Laser Desorption/Ionization Mass Spectrometry" Anal. Chem, 2001, V.73, P.612-619]. Another property of silicon substrates with a nanocrystalline structure is an intense photoluminescence, which can be and is used to create light-emitting devices.

The formation of the silicon substrates with nanoscale structure is carried out, usually by electrochemical (anodic) etching of monocrystalline silicon in a solution containing hydrofluoric acid. On the back side of the silicon wafer pre-create ohmic contact, for example, by sputtering aluminum. When a positive potential on the silicon electrode (the anode)immersed in a solution containing hydrofluoric acid, flow multistage reactions of dissolution and recovery of silicon. The second electrode (cathode) is usually a platinum plate. The result of this treatment, the formed porous silicon material consisting of nanocrystals and pore size from one to hundreds of nanometers [.Bisi, Stefano Ossicini, L.Pavesi "Porous silicon: a quantum sponge structure for silicon based optoelectronics" Surface Science Reports, 2000, V.38, P.1-126].

A method of processing a silicon substrate for formation of a layer of porous silicon on the surface of the substrate, including anodic etching of n-si in the range of current density from 30 to 150 mA/cm2during the time from 20 to 600 min in concentrated hydrofluoric acid under illumination of the working surface of silicon, for example, an incandescent lamp with a capacity of 200-500 W [RF patent №1459542, CL H01L 21/306, publ. 06.10.2000,].

The known method procedureunrestricted porous silicon substrates by anodic etching in an electrolyte, containing hydrofluoric acid, ethanol and water [J.J.Thomas et al. Desorption-ionization on silicon mass spectrometry: an application in forensics, J. Analytica Chimica acta No. 442, 2001, p.185].

In the known method, the silicon substrate is placed in a Teflon cell with a 25% solution of hydrofluoric acid in ethanol and conduct anodic etching at a current density of 5 mA/cm2within 1 minute. Next, the substrate is treated with ozone followed by etching in a 5% solution of hydrofluoric acid in ethanol for 1 minute. The surface is then washed with ethanol.

However, known methods for producing silicon substrates with nanoscale structure by anodic etching in an electrolyte containing hydrofluoric acid, have the following drawbacks:

in the process of electrochemical etching is contamination of the silicon substrate by chemical substances, in particular alkali and alkaline earth metals. Mass spectra obtained by the use of such substrates as emitters ions, characterized by chemical noise that makes it difficult, and in some cases makes it impossible for detection of defined compounds;

- heterogeneity of the obtained silicon substrates with nanoscale structure. In particular, the local sensitivity (ionization efficiency) nonuniformly distributed over the surface that bring the low reproducibility of the analysis when using these substrates as the emitter ions. The heterogeneity of the substrate also leads to uncontrolled changes in the photoluminescence spectra obtained with different surface areas;

- the inability to store the substrate in aerobic conditions. Upon contact with the air is sufficiently rapid oxidation of the surface silicon atoms. Formed as a result of oxidation of the oxide layer is an insulator, which excludes the possibility of applying such a surface as the emitter of ions in analytical devices. When storing the substrate in aerobic conditions also rapid degradation photoluminescent properties. Therefore, when using silicon substrates prepared by a known method, an ion emitter or light emitting structures you can either use only freshly prepared samples, or during storage to take special measures to prevent contact of the substrate with air.

An additional disadvantage of known methods is the necessity of establishing electrical contact with the silicon substrate and electrochemical equipment, which complicates the process of obtaining nanostructured silicon substrates and increases their value.

The closest technical solution is the way to obtain nanostructured silicon substrates by arr the processing silicon-containing materials by gas-vapour mixture, containing vapors of nitric NGO3and HF hydrofluoric acid [M.Saadoun, N.Mliki, H.Kaabi, K.Daoudi, B.Bessais, H.Ezzaouia, R.Bennaceur "Vapour-etching-based porous silicon: a new approach" Thin Solid Films, 2002, V.405, P.29-34]. In the known method the silicon substrate is placed in a polypropylene cell partially filled with a mixture of NGO3(65%) and HF (40%), at a distance of 2.5 cm above the surface of the above-mentioned mixture. The cuvette is placed in a thermostat and maintain at a constant temperature. Gas-vapor mixture formed by the evaporation placed in the cuvette of nitric and hydrofluoric acids, reacts with the silicon substrate, resulting in the surface of the substrate layer is formed mesoporous silicon nanocrystalline structure. In the temperature range from 20°C to 30°C processing time of the substrate does not exceed 30 minutes, because when increasing the exposure time to completely violated the homogeneity of the porous layer. At a temperature of 40°With the processing of the substrate is 2 to 20 minutes At a temperature of 60°With the duration of treatment is limited to 2 minutes

In a known method of obtaining nanostructured silicon substrates latter is not in contact with solutions of acids, resulting in forming nanocrystalline porous layer is characterized by a high degree of purity. When using such substrates as emitters ion intensity hee the systematic noise is small and does not interfere with the detection of the analyzed compounds.

In addition, the known method does not involve the creation of electrical contact with the silicon substrate and electrochemical equipment that simplifies the method of obtaining nanostructured silicon substrates and reduces their cost.

However, the known method of obtaining silicon substrates with nanoscale structure has drawbacks:

- when processing a silicon substrate by a known method get though to a lesser extent than in counterparts, but still fairly large heterogeneity of the obtained silicon substrates with nanoscale structure. Different parts of the surface have substantially different physical and chemical properties. In particular, the local sensitivity (ionization efficiency) nonuniformly distributed over the surface, resulting in low reproducibility of the analysis when using these substrates as the emitter ions. In addition, they differ in the photoluminescence spectra obtained with different surface areas, which significantly complicates the use of such substrates in light-emitting devices.

- the inability to store the substrate in aerobic conditions. Like its competitors, when in contact with air is sufficiently rapid oxidation of the surface silicon atoms. Formed as a result of oxidation of the oxide is Loy is dielectric, that excludes the possibility of applying such a surface as the emitter of ions in analytical devices. When storing the substrate in aerobic conditions also rapid degradation photoluminescent properties. Therefore, when using silicon substrates prepared by a known method, an ion emitter or light emitting structures, you can either use only freshly prepared samples, or during storage to take special measures to prevent contact of the substrate with air.

The technical objective of the proposed solutions is to obtain nanostructured silicon substrates that remain stable physico-chemical properties of the surface during prolonged storage under natural conditions and providing higher compared to the prototype of the homogeneity of the physico-chemical properties of the surface and a higher reproducibility of the analysis when using such substrates as the emitter of ions in the methods of mass spectrometry and ion mobility spectrometry.

The technical problem is solved in that in a method of producing nanostructured silicon substrates by processing the silicon-containing material gas mixture containing hydrofluoric acid and an oxidizing agent, an oxidizing agent is used, the halogen is whether its mixture with oxygen-containing oxidizing reagent, taken in an amount not less than 1.0%.

Preferable as the halogen to use iodine, and as the oxygen-containing oxidizing reagent to use a reagent selected from the group of: ozone, hydrogen peroxide, sulfuric acid, oxides of nitrogen.

It is advisable to use a gas-vapor mixture obtained by mixing at a given temperature saturated vapor of iodine and equilibrium vapor of hydrofluoric acid and oxygen-containing oxidizing reagent.

It is advisable to use 5-50% aqueous solution of hydrofluoric acid, and the processing carried out when the temperature of the silicon-containing material 15-90°C.

Preferably the processing of silicon-containing materials to conduct the flow of gas mixture with temperaturas last 15-90°C.

Figure 1 presents a photograph in fluorescent microscope sample of nanostructured silicon, prepared by the method of the prototype.

Figure 2 - photograph of a fluorescent microscope sample of nanostructured silicon, prepared by the proposed method.

Figure 3 - the photoluminescence spectra of nanostructured silicon obtained by the method prototype. Spectra are taken under identical conditions with different surface areas.

Figure 4 - the photoluminescence spectra of nanostructured silicon obtained by the proposed the method. Spectra are taken under identical conditions with different surface areas.

Figure 5 is the Raman spectrum obtained on one of the sections of nanostructured silicon, prepared by the method of the prototype, and Raman spectra obtained at several sites nanostructured silicon, prepared by the proposed method.

Figure 6 - the Raman spectrum obtained on the second site of nanostructured silicon, prepared by the method of the prototype.

The use of halogen as an oxidant in the composition of the gas mixture (ASG) to obtain nanostructured silicon substrates allows retaining the benefits of steam etching, to improve the key parameters - uniformity and stability.

This is due to the significant difference in the mechanisms of oxidation of the silicon substrate pairs nitric acid (by way of a prototype) and halogen free (by the present method).

When exposed to nitric acid vapor, the formation of the oxide phase silicon SiO2, which then reacts with the hydrofluoric acid with the formation of volatile silicon tetrafluoride SiF4. When a certain ratio of the concentration of vapors of nitric and hydrofluoric acids formed nanostructured porous leucemia. However, different parts of such a layer can have a different structure and chemical composition. In particular, some areas may form ammonium nitrate as the product of the interaction of silicon with nitric acid (see figures 1, 5 and 6).

In addition, the surface of the formed layer is saturated with hydrogen, resulting in a main surface chemical groups of freshly prepared nanostructured silicon substrates are group Si-Hn(where n=1, 2, 3). These groups are in contact with air is quickly replaced with oxygen-containing groups, resulting on the surface of the silicon oxide layer is formed.

When used as an oxidizer vapor of the halogen oxidation mechanism is different, in particular, in the oxidation process does not result in formation of an oxide phase silicon SiO2. The halogen molecules adsorbed on the surface of a silicon substrate are efficient electron acceptors. Therefore, the adsorption of vapors halides leads to the formation of positively charged holes on the surface of a silicon substrate, and to provide reactivity of the silicon atoms in the interaction with pairs of hydrofluoric acid. The result is a nanostructured silicon layer with a high degree of uniformity and consistency of khimicheskogo the composition (see 2 and 5).

The surface of the formed layer is passivated by halogen and is chemically inert. Unlike the prototype of nanostructured silicon substrate obtained by the present method may be stored in contact with air without changing their chemical composition.

Thus, the halogen performs not only the function of the oxidizing agent, but also the function of the protective layer.

Below are examples of implementation of the proposed method.

Example 1.

At the bottom of the Teflon beaker with a volume of 100 ml was placed two containers with a volume of 15 ml each. The first tank is filled with an aqueous solution of hydrofluoric acid (25%), second - iodine. Teflon beaker is covered with a plate of monocrystalline silicon brand KES-0.01 at a distance of 2.5 cm above the surface of hydrofluoric acid and iodine are placed in a thermostat and incubated for 2.5 h at 40°C. in the volume of the Teflon Cup, free from placed two containers are formed saturated vapors of iodine and equilibrium pairs of hydrofluoric acid, which interact with the silicon substrate. As a result of such interaction on the surface of the silicon substrate layer is formed of nanocrystalline silicon with a thickness of about 1 μm.

Example 2.

At the bottom of the Teflon beaker with a volume of 150 ml was placed three volumes of 10 ml each. The first tank is filled with an aqueous solution of hydrofluoric acid (49%), second - iodine, and the third aqueous solution of hydrogen peroxide (10%). Teflon beaker is covered with a plate of monocrystalline silicon brand KES-0.005 at a distance of 3.5 cm from the top edge of the containers, placed in a thermostat and incubated for 2.5 h at 30°C. in the volume of the Teflon Cup, free from the three placed containers are formed saturated vapors of iodine and equilibrium pairs of hydrofluoric acid and hydrogen peroxide, which interact with the silicon substrate. As a result of such interaction on the surface of the silicon substrate layer is formed of nanocrystalline silicon with a thickness of about 1 μm.

Example 3.

In flow Teflon chamber is placed a monocrystalline silicon wafer mark KDB-0.01. The camera is at room temperature. Through the chamber pumped gas-vapor mixture obtained by mixing saturated at 40°C of iodine vapor and equilibrium at 20°C vapour 49% hydrofluoric acid and 5% sulfuric acid. The carrier gas is air, gas tract thermostatic at 40°C. for 30 minutes this treatment on the surface of the silicon substrate layer is formed of nanocrystalline silicon with a thickness of about 1 μm.

For detailed mapping of the main physico-chemical parameters characterizing the state of the surface, kremna the substrate s, obtained by the method of the prototype and the claimed method were analyzed by the methods of fluorescent spectroscopy, Raman spectroscopy and " SALDI " -mass spectrometry. The results obtained indicate that the substrate obtained by the claimed method differs from substrates prototype both in physical structure and chemical composition. Thus, large-scale heterogeneity patterns can be clearly seen on the photo luminescence samples of nanostructured silicon obtained by the method of the prototype (Figure 1), and absent in the samples prepared according to the claimed method (Figure 2). Additional information gives a comparison of the photoluminescence spectra taken from different places of the surface of nanostructured silicon, which was obtained by the method of the prototype (Figure 3, curves 1, 2 and 3). It is known that the intensity of photoluminescence and its range depends on the size of the silicon nanocrystallites and the chemical composition of the surface. The observed figure 3 differences in the intensity of photoluminescence, as well as the shift of the maximum of the spectrum shows significant small-scale heterogeneity patterns. At the same time nanostructured silicon layer obtained by the proposed method is characterized by a high degree of homogeneity and consistency of Henichesk the first composition. This, in particular, shows that the photoluminescence spectra taken from different places of the surface, is almost identical (Figure 4, curves 1, 2 and 3).

The difference in the chemical composition nanostrukturirovannogo silicon, prepared by the method of the prototype illustrates the Raman spectra taken from two different sites (Figure 5-6).

On the first plot (Figure 5) in the spectrum is observed only unbalanced line crystalline silicon 521 cm-1(a small broadening of the line in the region of smaller values of the shift indicates the formation of nanocrystallites). The second part of (6) in the spectrum there are a number of new lines that are apparently associated with the formation of the oxidized phase of silicon and ammonium nitrate (product of the interaction of nitric acid with silicon).

At the same time, all Raman spectra taken from different areas of nanostructured silicon obtained by the present method, had the form shown in Figure 5.

To compare the stability of nanostructured silicon substrates obtained by the method of the prototype and the proposed method, during prolonged storage under natural conditions, were also determined relative changes in the analytical signal. The results of one analysis are given in the table.

Table
The shelf life of the substrate, weeksThe relative change of the analytical signal from the substrate prepared by the method of the prototype, %The relative change of the analytical signal from the substrate prepared by the present method, %
1223
2561
3675
4852
5965

From the data obtained it follows that the substrate obtained by the method of the prototype, quickly degrade, and after 5 weeks of the analytical signal is reduced more than 20 times. At the same time nanostructured silicon obtained by the present method, stable, and analytical signal accurate to measurement error does not change.

1. The method of obtaining nanostructured silicon substrates by processing the silicon-containing materials combined cycle is MESU, containing hydrofluoric acid and an oxidizer, wherein the oxidizer agents use halogen or a mixture of oxygen-containing oxidizing reagent, taken in an amount not less than 1.0%.

2. The method according to claim 1, characterized in that as the use of halogen iodine.

3. The method according to claim 1, characterized in that the use of oxygen-containing oxidizing reagent selected from the group of: ozone, hydrogen peroxide, sulfuric acid, oxides of nitrogen.

4. The method according to claim 1, characterized in that use gas-vapor mixture obtained by mixing at a given temperature saturated vapor of iodine and equilibrium vapor of hydrofluoric acid and oxygen-containing oxidizing reagent.

5. The method according to claim 1 or 4, characterized in that use 5-50%aqueous solution of hydrofluoric acid.

6. The method according to claim 1, characterized in that the treatment is carried out at a temperature of silicon-containing material 15-90°C.

7. The method according to claim 1, characterized in that the processing of silicon-containing materials lead the flow of gas mixture.

8. The method according to claim 1 or 7, characterized in that the processing of silicon-containing materials lead the flow of gas mixture with temperaturas last 15-90°C.



 

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8 cl, 6 dwg, 3 tbl

FIELD: nanotechnology.

SUBSTANCE: invention relates to method of receiving of powder of nano-crystalline calcium hydroxyapatite. Nano-crystalline calcium hydroxyapatite is received by interaction of calcium hydroxide and solution, containing phosphate-ions, herewith suspension of calcium hydroxide is prepared directly before interaction with solution, containing phosphate-ions from solutions of calcium acetate and potassium hydroxide, herewith amount of calcium hydroxide is from 50 up to 100% in mixture of calcium-bearing components.

EFFECT: receiving of hydroxyapatite powder with particles size 30 - 50 nm.

3 dwg, 1 tbl, 1 ex

FIELD: nanotechnology.

SUBSTANCE: invention relates to method of receiving of nano-crystalline hydroxyapatite. According to the invention calcium nano-crystalline hydroxyapatite is received by interaction of compound of calcium and ammonium hydro-phosphate. In the capacity of calcium compound it is used sugar lime C12H22-2nO11Can, at n, which is situated in the range from 0.5 up to 2. Particles size of the received hydroxyapatite is 30-50 nm.

EFFECT: receiving of nano-crystalline powder of calcium hydroxyapatite, which contains unaggressive biocompatible accompaniment of the reaction and that provides its usage in medicine.

3 dwg, 1 tbl, 1 ex

FIELD: carbon materials.

SUBSTANCE: weighed quantity of diamonds with average particle size 4 nm are placed into press mold and compacted into tablet. Tablet is then placed into vacuum chamber as target. The latter is evacuated and after introduction of cushion gas, target is cooled to -100оС and kept until its mass increases by a factor of 2-4. Direct voltage is then applied to electrodes of vacuum chamber and target is exposed to pulse laser emission with power providing heating of particles not higher than 900оС. Atomized target material form microfibers between electrodes. In order to reduce fragility of microfibers, vapors of nonionic-type polymer, e.g. polyvinyl alcohol, polyvinylbutyral or polyacrylamide, are added into chamber to pressure 10-2 to 10-4 gauge atm immediately after laser irradiation. Resulting microfibers have diamond structure and content of non-diamond phase therein does not exceed 6.22%.

EFFECT: increased proportion of diamond structure in product and increased its storage stability.

2 cl

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