Method for producing gas-penetrable membrane and gas-penetrable membrane

FIELD: technology for producing semi-penetrable membranes for molecular filtration of gas flows and for division of reaction spaces in chemical reactors.

SUBSTANCE: method for producing gas-penetrable membrane includes two-sided electro-chemical etching of monocrystalline plate made of composition AIIIBV of n conductivity type or of semiconductor AIV with width of forbidden zone E≥1,0 electron volts and alloying level 1017-1020 1/cm3. Modes of aforementioned etching are set, providing for generation of simultaneously porous layers, while etching process is performed until moment of spontaneous stopping of electro-chemical process and generation of solid separating layer of stationary thickness on given part of plate area, determined using sharp bend on the curve of temporal dependence of anode current.

EFFECT: gas membrane, produced in accordance to method, has increased penetrability for molecules of light gases and increased selectivity characteristics at room temperature.

2 cl, 3 dwg, 3 ex

 

The invention relates to the manufacture of semi-permeable membranes for molecular filtering gas streams, in particular for the purification of hydrogen and helium, to separate reaction spaces in chemical reactors in the implementation of parallel running of catalytic reactions with the allocation and consumption of hydrogen, and may find application, for example, in a compact fuel cells.

There are two fundamentally different types of gas-permeable membranes, namely: a microporous membrane with dimensions of through pores larger than the diffusing related molecules, and solid, amorphous or polycrystalline membrane, atomic structure characterized by the presence of voids with dimensions sufficient for the introduction of solid phase or only atomic hydrogen (close-Packed crystalline structure of metals), or molecular hydrogen and light monatomic gases such as helium and neon (zeolites, quartz glass). The parameters of the selectivity of the transmission of light gases by membranes of the first type are small in numerical terms range from one to hundreds. In the second case, a partial selective transmittance with respect to the gas molecules, which can dissolve in the solid phase, is determined only by the presence of extended defects in the structure of the filtration layer is the membrane forming the through channels cracks, capillary openings, dislocations, block and intergranular boundaries. Therefore, the best material for the manufacture of filter layers of gas-permeable membranes could be defect-free monocrystalline film that is not used for this purpose up to the present time. An important advantage of single-crystal films must be practical independence selectivity bandwidth gases from their thickness. Thus, when using single-crystal materials, you can increase the absolute permeability of the membranes without loss of quality separation of gas mixtures only by reducing the thickness of the solid filter layer. This, in turn, allows you to extend the range of materials suitable for practical use in the construction of vasoselective membranes.

A known method of obtaining a gas-permeable membrane (see application US No. 20040033180, IPC B 01 J 8/00, publ. 19.02.2004, by forming on the surface of the porous substrate film, the resulting gas-phase reaction in a sealed vessel by heating the silicon source and an aqueous solution of alkali or alkaline solution of a source of aluminum without mixing.

There is a method allows to obtain a gas-permeable membrane with uniform pore size. A disadvantage of the known method of obtaining a gas-permeable membrane is wound is the necessity of using ready-made porous substrate and sophisticated equipment, including temperature-controlled reactor high pressure block evaporation organosilicon compounds and a mechanical input device and rotation of the substrate.

Known gas-permeable membrane obtained as described above is composed of a porous substrate on which is deposited a film based on a zeolite having pores of from 0.02 to 2.00 μm when the porosity of the substrate 10 to 60%.

Known gas-permeable membrane is not continuous and does not provide a high selectivity for the separation of gases.

A method of obtaining a composite gas separation module (see application US No. 20040237779, IPC B 01 D 53/22, publ. 02.12.2004 g)includes applying by chemical vapor deposition on a porous substrate of the intermediate porous layer and the subsequent deposition on it of a continuous layer of palladium, acting vasoselective membrane.

The disadvantages of this method are its multi-stage, complexity and long duration of operations in time

Known composite gas separation module, obtained as described above, includes a porous substrate made of stainless steel or alloys containing chromium and Nickel, the intermediate porous metal layer of palladium or palladium and metal 1B group and a continuous layer of palladium (˜20 μm), perform the function of gazosa the unbiased membrane.

A disadvantage of the known composite gas separation module is its rapid degradation when used in conditions of significant temperature fluctuations. Moreover, the discontinuity of the filtering layer of palladium comes from even a single cooling in a hydrogen-containing atmosphere to a temperature T<150-180°C.

A method of obtaining a composite gas separation module (see application US No. 20040237780, IPC B 01 D 53/22, publ. 2.12.2004,), including the application by sequential chemical vapor deposition on a porous substrate intermediate porous combined metal layer in the form of three layers of palladium, separated by two layers of metal element 1B group (copper or silver), application in several stages in the intermediate layer is thicker (˜10 μm) layer of palladium, mechanical grinding formed surface and the subsequent application of a continuous layer of palladium.

The disadvantages of this method are its multi-stage, complexity and long duration of operations in time.

A known design of a composite gas separation module, obtained as described above. The module consists of a porous metal substrate, covering the intermediate porous metal layer and a solid metal membrane, sat the active permeable to hydrogen, lying on the intermediate porous layer. The intermediate porous layer is made up of three layers of palladium, separated by two layers of metal element 1B group (copper or silver), on top of which bears more than a thick (˜10 μm) layer of palladium on the polished surface of which is coated with a continuous layer of palladium or its alloy (˜20 μm), perform the function vasoselective membrane. The obtained composite module are operated at temperatures of 350-500°and has a high selectivity bandwidth of hydrogen.

A disadvantage of the known composite gas separation module is its rapid degradation when used in conditions of significant temperature fluctuations. Moreover, the discontinuity of the filtering layers of palladium and its alloys come from even a single cooling in a hydrogen-containing atmosphere to a temperature T<150-180°C. it is Known that the dissolution of hydrogen in metals is accompanied by the dissociation of molecules and the formation of solid solutions, in which atomic hydrogen is chemically associated with the atoms of the crystal lattice of the metal. With a sharp decrease in temperature from the saturated solid solution of hydrogen in palladium begins the evolution of precipitates hydride phase, which causes internal stresses, leading to the formation of cracks in the filter layer, m is mpany. In addition, to the destruction of the palladium layer of the composite membrane can lead to deformation caused by differences in coefficients of thermal expansion of the layer and the material of the porous substrate.

A method of obtaining vodorodopronitsaemosti oxide membranes (see US patent No. 5453298, IPC 01 D 71/02, publ. 26.09.1995,), including the formation within the porous glass or ceramic substrate, a continuous layer of oxide formed by filing reagents from opposite sides of the substrate. As reagents can be halides of silicon, boron, aluminum and titanium; CHLOROSILANES or chloralosane. The precipitation product is in the process of hydrolysis reagent water vapor at temperatures of from 100 to 800°depending on the composition of the resulting oxide. The resulting structures are subjected to long-term (from 5 to 15 days) high-temperature annealing in an atmosphere of wet nitrogen, providing a sintering the deposited oxide material of the porous substrate and the formation of a continuous filter layer.

The disadvantages of this method include the complexity of hardware design and duration of operations required to achieve the desired result. In addition, the possibility of obtaining a solid films inside the microporous substrate is limited to the original pore sizes.

Water is vodopronitsaema oxide membrane, obtained as described above, consists of microporous (pore size from 2.5 to 12 nm) glass or ceramic (aluminum oxide) substrate, made in the form of a tube. Inside the porous substrate is formed by a continuous layer of oxide in the form of a continuous filter layer. Selectivity bandwidth hydrogen such membrane in relation to nitrogen varies from hundred to several thousand at operating temperatures from 800 to 450°C.

In known vodorodopronitsaemosti oxide membrane, the possibility of obtaining a solid films inside the microporous substrate is limited to the original pore sizes. Therefore, high selectivity bandwidth hydrogen such membranes can only be achieved if the small size of pores in the substrate and, accordingly, with its high initial resistance to the gas stream, which may exceed the resistance of the solid filter layer.

A known method of obtaining a gas-permeable membrane (see PCT application no WO 9905344, IPC B 01 J 8/00, publ. 04.02.1999 g), which coincides with the inventive method by the greatest number of significant features and adopted for the prototype. Prototype method includes unilateral electrochemical etching one side is fixed in the holder monocrystalline wafer of semiconductor AndIVwith the doping level of 1017-10191/cm3when although nom the light exposure of the other side plate for forming a layer of porous material.

Known gas-permeable porous membrane prototype has dimensions of through pores, greatly exceeding the size of the diffusing related molecules, resulting in the selective transmission of light gases such membrane is extremely low, including at room temperature.

Known gas-permeable membrane obtained as described above (see US patent No. 6328876, IPC C 25 F 3.12, published 11.12.2001,), comprising a layer of porous monocrystalline silicon formed from the original monocrystalline wafer of semiconductor AndIVwith the doping level of 1017-10191/cm3by one-sided electrochemical etching, while the porous layer is enclosed in a frame of the above-mentioned monolithic single-crystal semiconductor AndIVmade in the form of a closed loop.

Known gas-permeable membrane has a very low selectivity transmittance of light gases, including at room temperature.

The task of the invention is to develop a method for creating gas-permeable membrane having high permeability to molecules of light gases (hydrogen and helium) and a high prevalence of selectivity at room temperature.

The problem is solved by a group of inventions, a single component is first inventive concept.

In terms of how the task is solved in that a method of obtaining a gas-permeable membrane includes bilateral electrochemical etching of single-crystal plate of the connection AndIIIBVn-type conductivity or of semiconductor AndIVwith bandgap E≥1,0 eV and the doping level of 1017-10201/cm3while installing the modes mentioned etching for the formation of homogeneous porous layers, and the etching process leading up to the moment of its spontaneous termination and formation of a solid separation layer fixed thickness on a given part of the square plate, which is determined by the kink in the curve of the time dependence of the anode current.

As monocrystalline plates can be availed plate, for example, from silicon, indium phosphide or gallium arsenide.

The method provides for obtaining a gas-permeable membrane of the nanoscale thickness of monocrystalline layers of semiconductor of group IV elements or compounds AndIIIBVembedded in the porous volume of the crystal of the same composition. The method is based on the effect of spontaneous termination of the electrochemical process on a collision fronts of steam formation in semiconductor crystals when reaching a thickness separating these fronts undisturbed layer, corresponding in the military the layer thickness of the space charge in the semiconductor.

The formation of porous layers occurs in materials AndIIIBVonly n-type conductivity when the width of the forbidden zone E>1 eV. This: InP; GaAs; GaP; AlAs, and their solid solutions, as well as all of nitrides of group III elements. Regardless of the composition of the electrolyte used for the anodic etching, the degree of homogeneity of porous layers in single crystals AndIIIBVincreases, and the dispersion of the pore size decreases with increasing doping level of the semiconductor. Therefore, for the fabrication of membranes comfortable enough highly doped (1018cm-3) inserts AIIIBV.

In the part of the device, the task is solved in that the gas-permeable membrane includes nanoscale semiconductor layer located between the layers of porous material, which are formed from the original single-crystal plate of the connection AndIIIBVn-type conductivity or of semiconductor AndIVwith bandgap E≥1,0 eV and the doping level of 1017-10201/cm3through bilateral electrochemical etching with modes, providing the formation of a homogeneous porous layers, until his spontaneous termination and formation of a solid separation layer of fixed thickness, which is determined by the kink in the curve of the time dependence of the anode current.

Nano is asmany layer mainly has a thickness of δ equal to 10-20 nm.

The original single-crystal plate can be made of silicon or gallium arsenide.

The invention is illustrated by drawings, where:

Figure 1 shows a schematic diagram of an installation for implementing the inventive method;

figure 2 schematically shows a perspective view of the gas-permeable membrane;

figure 3 shows a transverse image of the structure of gas-permeable silicon membrane obtained by electron microscope.

Installation for the implementation of the proposed method consists of a PTFE vessel 1 with the electrolyte solution 2, which contains the original single-crystal plate 3, with two opposite sides which has a platinum cathodes 4. Plate 3 is connected with the positive pole of the power source (not shown). As the material of the original single-crystal plates can be availed connection AndIIIBVn-type conductivity and the semiconductor AndIVwith bandgap E≥1,0 eV and the doping level of 1017-10201/cm3such as gallium arsenide or silicon.

Obtained by the claimed method gas-permeable membrane consists of two porous layers 5, between which is enclosed nanoscale semiconductor layer 6.

The inventive method of obtaining the gas-permeable MEM the Ana is as follows.

The original single-crystal plate 3 from the connection AndIIIBVn-type conductivity or semiconductor AndIVwith bandgap E≥1,0 eV cover acid resist, in which the open window, symmetrically located on opposite sides of the plate, and is placed, for example, in the installation shown in figure 1. Carry out the known process of bilateral electrochemical etching plate 3 until spontaneous termination of the electrochemical process. The onset of spontaneous termination of the electrochemical process and the formation of a solid separation layer 6 fixed thickness is determined by the kink in the curve of the time dependence of the anode current. The fraction of the area of the layer 6 with respect to the area of Windows opened on the original surface of the plate 3, is estimated as the ratio of the magnitude of the current downturn to its value at the break point of the current curve.

Example 1. Manufacturer of gas-permeable membranes made of silicon, consisting of two porous layers separated solid monocrystalline layer thickness of 10÷15 nm.

The source material was a silicon single crystal plate of p-type conductivity with a carrier concentration of 2·1019cm-3(the width of the bandgap of silicon Eg=1,18 eV), oriented in the plane (100). The cover plate is Ali acid resist, which was opened window, symmetrically located on opposite sides of the plate. Anodic treatment, the plates were held at room temperature in a mixture of ethanol with hydrofluoric acid[HF]=40%) in a volume ratio of 1:1. The process of steam formation is conducted in potentiostatic mode with an initial value of the current density of 70 mA/cm2. The onset of spontaneous termination of the electrochemical process and the formation of a solid separation stationary layer thickness was determined by the kink in the curve of the time dependence of the anode current. The fraction of the area of this layer with respect to the area of Windows opened on the original surface of the plate was estimated as the ratio of the magnitude of the current downturn to its value at the break point of the current curve.

The resulting membrane is characterized by the following parameters: permeability to hydrogen at 20° - 3,1·10-7·mol m-2with-1PA-1and at 100° - 1,4·10-6·mol m-2with-1PA-1; permeability for helium at 20° - 1,1·10-7·mol m-2with-1PA-1and at 100°With a 1.5·10-6·mol m-2with-1PA-1. Indicators selectivity bandwidth of hydrogen relative to the argon and oxygen in the temperature range from 20°to 150°respectively (9÷7)·103 and (4÷3)·104.

Example 2. Manufacturer of gas-permeable membranes made of indium phosphide, consisting of two porous layers separated by a continuous single-crystal layer thickness of 40÷50 nm.

The source material was a single crystal wafer of indium phosphide n-type conductivity with a carrier concentration of 5×1018cm-3oriented in the plane (100). The plate was covered with an acid resist, which was opened window, symmetrically located on opposite sides of the plate. Anodic treatment of the plates was carried out in an aqueous solution of hydrazinehydrate (N2H4·2HCl) with a concentration of 1 M. the Process of steam formation is conducted in potentiostatic mode with an initial value of the current density of 300 mA/cm2. The onset of spontaneous termination of the electrochemical process and the formation of a continuous separating layer of finite thickness is determined by the kink in the curve of the time dependence of the anode current. The fraction of the area of this layer with respect to the area of Windows opened on the original surface of the plate, is estimated as the ratio of the magnitude of the current downturn to its value at the break point of the current curve. After anodic treatment was carried out by annealing the wafer in an atmosphere of inert gas at a temperature of 350°C.

The obtained membrane characterized the following parameters: permeability to hydrogen at 20° With - 1,6·10-7·mol m-2with-1PA-1and at 100° - 5,0·10-7·mol m-2with-1PA-1. Indicators selectivity bandwidth of hydrogen relative to the argon and oxygen in the temperature range from 20°to 150°respectively (6÷4)·103and (2÷1)·104.

Example 3. Manufacturer of gas-permeable membranes made of gallium arsenide, consisting of two porous layers separated solid monocrystalline layer thickness of 60÷70 nm.

The source material was a single crystal wafer of gallium arsenide of n-type conductivity with a carrier concentration of 2·1018cm-3oriented in the plane (100). The plate was covered with an acid resist, which was opened window, symmetrically located on opposite sides of the plate. Anodic treatment of the plates was carried out in aqueous solution H2SO4(2.0 M). The process of steam formation is conducted in potentiostatic mode with an initial value of current density of 50 mA/cm2. The onset of spontaneous termination of the electrochemical process and the formation of a continuous separating layer of finite thickness is determined by the kink in the curve of the time dependence of the anode current. The fraction of the area of this layer with respect to the area of Windows opened on the outcome of the second surface of the plate, is estimated as the ratio of the magnitude of the current downturn to its value at the break point of the current curve. After anodic treatment was carried out by annealing the wafer in an atmosphere of inert gas at a temperature of 350°C.

The resulting membrane is characterized by the following parameters: permeability to hydrogen at 20° - 9·10-8·mol m-2with-1PA-1and at 100°C - 2.0-110-7·mol m-2with-1PA-1. Indicators selectivity bandwidth of hydrogen relative to the argon and oxygen in the temperature range from 20°to 150°respectively (8÷7)·103and (3÷2)·104.

1. A method of obtaining a gas-permeable membranes, including bilateral electrochemical etching of single-crystal plate of the connection AndIIIBVn-type conductivity or of semiconductor AndIVwith bandgap E≥1,0 eV and the doping level of 1017-10201/cm3while installing the modes mentioned etching for the formation of homogeneous porous layers, and the etching process are until spontaneous termination of the electrochemical process and the formation of a solid separation layer fixed thickness on a given part of the square plate, which is determined by the kink in the curve of the time dependence of the Academy of Sciences of the underwater current.

2. The method according to claim 1, characterized in that the conduct referred to bilateral electrochemical etching of single-crystal silicon wafers.

3. The method according to claim 1, characterized in that the conduct referred to bilateral electrochemical etching of single-crystal wafer of gallium arsenide.

4. The method according to claim 1, characterized in that the conduct referred to bilateral electrochemical etching of single-crystal wafer of indium phosphide.

5. Gas-permeable membrane comprising nanosized semiconductor layer located between the layers of porous material, which are formed from the original single-crystal plate of the connection AndIIIBVn-type conductivity or of semiconductor AndIVwith bandgap E≥1,0 eV and the doping level of 1017-10201/cm3by bilateral electrochemical etching with modes, providing the formation of a homogeneous porous layers, until his spontaneous termination and formation of a solid separation layer of fixed thickness, which is determined by the kink in the curve of the time dependence of the anode current.

6. The membrane according to claim 5, characterized in that the said original plate is made of silicon.

7. The membrane according to claim 6, characterized in that the nanoscale layer has a thickness of the at δ equal to 10-20 nm.

8. The membrane according to claim 5, characterized in that the said original plate is made of gallium arsenide.

9. The membrane according to claim 5, characterized in that the said original plate is made of indium phosphide.



 

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