CN115490234A - Self-propagating synthesis method and application of iron carbide material - Google Patents
Self-propagating synthesis method and application of iron carbide material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 28
- 229910001567 cementite Inorganic materials 0.000 title claims abstract description 24
- 238000001308 synthesis method Methods 0.000 title claims abstract description 6
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 239000012621 metal-organic framework Substances 0.000 claims abstract description 10
- 238000002485 combustion reaction Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 8
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000007036 catalytic synthesis reaction Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000013206 MIL-53 Substances 0.000 claims description 7
- 238000005554 pickling Methods 0.000 claims description 7
- 238000003786 synthesis reaction Methods 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 230000002194 synthesizing effect Effects 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 49
- 229910052742 iron Inorganic materials 0.000 abstract description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 10
- 239000001301 oxygen Substances 0.000 abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 3
- 238000004134 energy conservation Methods 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 21
- 229910052759 nickel Inorganic materials 0.000 description 10
- 239000003054 catalyst Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 230000003197 catalytic effect Effects 0.000 description 6
- 239000007787 solid Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000004502 linear sweep voltammetry Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000005049 combustion synthesis Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- PSVSZBOMJGAVRS-UHFFFAOYSA-N 2,3-diaminoterephthalic acid Chemical compound NC1=C(N)C(C(O)=O)=CC=C1C(O)=O PSVSZBOMJGAVRS-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000004832 voltammetry Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention relates to a self-propagating synthesis method and application of an iron carbide material, wherein a metal-organic framework precursor and a combustion improver are ground and uniformly mixed, ignited by a tungsten wire, acid-washed and dried to obtain the iron carbide material Fe 3 C or nitrogen doped iron carbide material Fe 3 C (N) has the characteristics of short reaction time, energy conservation and the like. Synthetic iron carbide material Fe 3 C and Fe 3 The C (N) has good oxygen evolution performance, effectively reduces the overpotential of electrolysis, and can be applied to the field of water electrolysis or electrolytic catalytic synthesis.
Description
Technical Field
The invention relates to the field of materials, in particular to a method for quickly synthesizing an iron carbide material by using a metal-organic framework as a precursor and adopting a self-propagating method and application thereof.
Background
The self-spreading high-temp. synthesis method is also called self-spreading combustion synthesis method or combustion synthesis method, and the main principle of said process is that all the reaction substances are mixed together, and ignited to produce chemical reaction to produce strong heat energy, i.e. self-spreading high-temp. synthesis reaction, i.e. self-spreading reaction, is a new material synthesis technology, and has high practical application value in the field of synthesis of new material.
In the field of energy, water is electrolyzed into high-energy environment-friendly energy hydrogen and environment-friendly oxygen by means of electrolysis, and the method has important research significance. In the process of water electrolysis, the kinetics process of the oxygen evolution reaction of the anode is relatively slow and is a main factor of the energy consumption of water electrolysis.
Disclosure of Invention
The invention aims to provide a method for self-propagating synthesis of iron carbide materials, which adopts a metal-organic framework Fe-MIL-53 or Fe-MIL-53-NH 2 Adding a certain amount of combustion improver into a precursor, and quickly synthesizing the iron carbide material Fe by adopting a self-propagating method 3 C or Fe 3 And the C (N) has the advantages of short reaction time, energy conservation and the like, and electrochemical research shows that the synthesized iron carbide material has good performance in the oxygen evolution reaction and has a certain application prospect in the field of new energy.
In order to achieve the aim, the invention provides a method for self-propagating synthesis of an iron carbide material, which comprises the following steps:
(1) Mixing: uniformly mixing the metal-organic framework precursor and the combustion improver in proportion by grinding to obtain a mixture;
(2) And (3) combustion: igniting the mixture by a tungsten wire;
(3) Acid washing: after the combustion is finished, pickling the combusted substances by using a pickling agent;
(4) And (3) drying: drying the product after acid washing in vacuum or in the air to obtain an iron carbide material;
the metal-organic framework precursor is Fe-MIL-53 or Fe-MIL-53-NH 2 ；
The combustion improver is aluminum powder, magnesium powder or a mixture thereof;
the acid pickling agent is sulfuric acid, hydrochloric acid, hydrofluoric acid or a mixture of any two or three of the sulfuric acid, the hydrochloric acid and the hydrofluoric acid.
The iron carbide material Fe synthesized by the invention 3 C and Fe 3 The C (N) has good oxygen evolution performance, can be applied to the field of electrolytic water or electrolytic catalytic synthesis, and can effectively reduce the overpotential of electrolysis.
Drawings
FIG. 1 is Fe 3 C and Fe 3 XRD pattern of C (N).
FIG. 2 is Fe 3 C and Fe 3 Linear Sweep Voltammetry (LSV) profile of C (N).
FIG. 3 is Fe 3 C and Fe 3 Tafel slope curve for C (N).
FIG. 4 is Fe 3 C and Fe 3 Nyquist plot for C (N).
FIG. 5 is Fe 3 C and Fe 3 And C (N) cyclic voltammogram of the non-Faraday region.
Detailed Description
The invention is further described with reference to specific examples.
Metal-organic framework precursors Fe-MIL-53 and Fe-MIL-53-NH 2 According to the method of the literature (Horcajada P et al, JACS,2008,130 (21): 6774-6780), the specific synthesis method is as follows: carrying out hydrothermal reaction for 15h at 150 ℃ according to the molar ratio of ferric chloride hexahydrate, terephthalic acid or diaminoterephthalic acid and N, N-dimethylformamide being 1.
Example 1
Self-propagating synthesis of iron carbide material Fe 3 C：
(1) Weighing a metal-organic framework precursor Fe-MIL-53, aluminum powder and magnesium powder according to a mass ratio of 4;
(2) Placing the mixture on qualitative filter paper, and igniting the mixture through a tungsten filament to enable the mixture to fully react to obtain a black solid substance;
(3) Grinding the black solid into black powder, and mixing the black powder at 0.5mol/LH 2 SO 4 Soaking and acid washing for 12h, washing for 2-3 times by using pure water and absolute ethyl alcohol respectively, and performing centrifugal separation;
(4) Putting the centrifugally separated solid in a vacuum drying oven, drying at the constant temperature of 70 ℃ for 4h, cooling to room temperature, and taking out to obtain a black crude product;
(5) Placing the crude product in a volume ratio of 2:1, soaking and pickling in a mixed solution of HF and HCl for 12 hours; washing with pure water and absolute ethyl alcohol for 2-3 times, drying in vacuum drying oven at 70 deg.C for 4 hr, and cooling to room temperature to obtain black solid iron carbide material Fe 3 C。
According to the same method, with a metal-organic framework Fe-MIL-53-NH 2 Obtaining nitrogen-doped iron carbide material Fe as a precursor 3 C(N)。
Example 2
Iron carbide material Fe 3 C and Fe 3 Electrocatalytic performance study of C (N):
preparation of a working electrode: 20mg of catalyst (Fe) was added to the prepared beaker 3 C or Fe 3 C (N)) was added a certain amount of PTFE emulsion (10% by weight) and absolute ethanol (1 2 And drying the substrate in a vacuum furnace at 60 ℃ for 12 hours to obtain the working electrode with the electrochemical oxygen evolution characteristic.
The Chenhua CHI660D is used as a testing device, and a conventional three-electrode system is adopted: the method comprises the steps of taking an HgO/Hg electrode as a reference electrode, taking foamed nickel filled with a catalyst as a working electrode, testing the electrochemical performance of the electrode in a 1.0mol/LKOH solution, starting the test after 30min of nitrogen is introduced, and continuously introducing nitrogen in the test process, so as to remove oxygen in the solution and remove errors caused by resistance generated by bubbles.
Linear Sweep Voltammetry (LSV) is currently the most common method for determining the electrochemical performance of a catalyst, and is to apply a linear voltage to an electrode to make the voltage and the applied voltage have a linear relationship, and use an LSV curve to obtain an overpotential and a current density at a specific potential, so as to determine the electrochemical performance of the catalyst.
The Tafel curve (Tafel) conforms to the Tafel equation, and the catalytic performance of the catalyst can be shown, and the Tafel formula is as follows: q = blogj + a, where q is the overpotential, b is the Tafel slope, j is the current density, and in the electrolytic method, the overpotential is proportional to the logarithm of the current density, and the lower the Tafel slope, the better the catalytic characteristics of the catalyst.
Electrochemical impedance testing (EIS) involves the application of a relatively low frequency alternating current potential wave to the electrochemical system under test, and the frequency of the sine wave is used to determine the ratio of alternating current potential to current. Its working frequency is 0.1-100000 Hz, and its amplitude is 5.0mA.
(4) Electrochemical active area (ECSA)
To evaluate the catalytic activity of a catalyst, it is necessary to analyze its surface, i.e. the electrochemically active area. The double layer capacitance (Cd) was used in the experiment, and two methods were used to obtain electrochemical double layer capacitors: (1) linear fitting was performed with non-faraday spaced electric double layer capacitance currents at different scan speeds. (2) Corresponding impedance under different frequencies is obtained through electrochemical impedance spectroscopy; the electrochemically active area is typically associated with the electrochemical double layer capacitance (Cdl). Cdl estimates that: ECSA = Cdl/Cs, cs being ideal unit capacitance under the same electrolyte condition, generally 20-60 μ F/cm 2 In this test, 40. Mu.F/cm 2 。
And (4) analyzing results:
scanning the sample by X-ray, wherein the scanning angle is 2 theta = 5-80 degrees, and the precursors (b) and (c) in figure 1 are Fe-MIL-53 and Fe-MIL-53-NH 2 The XRD patterns of the target precursors Fe-MIL-53 and Fe-MIL-53-NH are successfully synthesized 2 . In the figure, (d) and (e) are Fe synthesized by self-propagating 3 C and Fe 3 An XRD pattern of C (N) shows that 2 theta =38.4, 44.7, 65.2 and 78.2 are diffraction peaks of the aluminum simple substance. 2 θ =35.5, 42.8, 62.4 respectively ascribed to Fe 3 The 020, 200 and 114 crystal planes of C have strong diffraction peaks of aluminum, so that other diffraction peaks are not obvious enough.
Fe 3 C and Fe 3 And C (N) is subjected to a polarization curve obtained by a linear volt-ampere scanning test in a 1.0mol/L KOH solution within a potential range of 1.2-2.0V, as shown in figure 2, and the polarization curve of the electrocatalytic oxygen evolution reaction of blank foamed nickel under the same condition is also tested, blank comparison is carried out, and the influence of the factors of the foamed nickel on the experiment is eliminated. As can be seen from FIG. 2, fe 3 C (N) has an oxidation peak at a scanning potential of 1.36V. When the current density reaches 100mA cm -2 Of (i) Fe 3 C (N) minimum overpotential required, comparable Fe 3 C requires a slightly higher catalytic reaction potential, which is the worst of the blank nickel foam. Thus, fe 3 C (N) has better catalytic activity, while blank foam nickel is the least, in comparison with Fe 3 C and Fe 3 C (N), using the same solvent, at the same current density, fe 3 C (N) has better catalytic activity, and Fe can be seen from linear voltammetry 3 C (N) has better oxygen evolution reaction characteristics.
The smaller the slope of the Tafel curve is, the smaller the overpotential of the electrocatalytic reaction is, and the better the catalytic performance of the catalyst is. From FIG. 3, fe can be seen 3 C(72.2mV·dec -1 ) And Fe 3 C(N)(61.4mV·dec -1 ) The Tafel slope of the polymer is less than NF (186.8 mV dec) -1 ) Tafel slope of (1). Fe 3 The Tafel gradient of C is 72.2mV dec -1 The electrochemical process of the material is better, and Fe 3 The Tafel slope of C (N) was 61.4mV dec -1 Thus, the catalyst shows excellent electrocatalytic performance.
The self-supporting electrode made of the foamed nickel substrate can improve the stability of the electrode, and can also improve the interface resistance and the conduction of electric charges, thereby improving the electrocatalysis performance of the electrode. FIG. 4 is Fe 3 C/Ni，Fe 3 Nyquist plots (Nyquist plots) for C (N)/Ni and Ni, fe in FIG. 4 3 C (N)/Ni and Fe 3 The Nyquist plot for C/Ni has an arc radius significantly less than that of Ni, indicating Fe 3 C (N)/Ni and Fe 3 C/Ni is more conductive than Ni and has less charge transfer resistance.
The double layer capacitance (Cdl) can be obtained from CV curves of the non-faraday region in experiments at different scan speeds. A certain proportional relation exists between ECSA and Cdl, and the Cdl value can directly reflect the electrochemical activity area of the electrocatalyst. Thus, for Fe 3 C and Fe 3 The electric double layer capacitance of C (N) was measured: (1) Cyclic voltammetry scanning with different frequencies is carried out in the non-Faraday region, and scanning is carried out at least twice when the scanning speed is set every time so as to ensure the reliability and the accuracy of data; (2) Calculating the difference between the anode current density and the cathode current density under the selected overpotential according to each scanning datum, and drawing by taking the current density difference (j) as an ordinate and the scanning speed as an abscissa; (3) The linear trend of the curve was observed and a slope twice the capacitance of the double layer at the solid-solution interface was obtained by linear fitting. The results show that Fe 3 C、Fe 3 The capacitor capacity of C (N) is 1.91mF cm -2 、1.51mF cm -2 。
The above results all show that (Fe) 3 C) And Fe 3 The C (N) has good oxygen evolution performance, excellent electrocatalysis performance and better conductivity, can be applied to the fields of electrolytic water and electrolytic catalysis, and can effectively reduce the overpotential of electrolysis.
Claims (6)
1. A self-propagating synthesis method of an iron carbide material is characterized by comprising the following steps:
(1) Uniformly mixing the metal-organic framework precursor and the combustion improver in proportion by grinding;
(2) Igniting the mixed substances by a tungsten wire;
(3) After the combustion is finished, pickling the product by using a pickling agent;
(4) Drying the product after acid washing in vacuum or in air to obtain an iron carbide material; the metal-organic framework precursor is Fe-MIL-53 or Fe-MIL-53-NH 2 。
2. The self-propagating process for synthesizing iron carbide material of claim 1, wherein: the combustion improver is aluminum powder, magnesium powder or a mixture of the aluminum powder and the magnesium powder.
3. A method of self-propagating synthesis of iron carbide material as claimed in claim 2, characterized in that: the acid pickling agent is sulfuric acid, hydrochloric acid, hydrofluoric acid or a mixture of any two or three of the sulfuric acid, the hydrochloric acid and the hydrofluoric acid.
4. The self-propagating method for synthesizing iron carbide material according to claim 1, wherein: and (4) vacuum drying is adopted.
5. Use of the iron carbide material of claim 1 for electrolysis of water.
6. Use of the iron carbide material of claim 1 in electrolytic catalytic synthesis.
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