CN104072147B - A kind of preparation method of silicon nitride honeycomb pottery - Google Patents
A kind of preparation method of silicon nitride honeycomb pottery Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of silicon nitride honeycomb pottery, comprising: step 1) preparation has the silicon nitride honeycomb base substrate of parallel channels; 2) binder removal of silicon nitride honeycomb base substrate or degreasing; 3) calcine silicon nitride honeycomb base substrate, obtain the silicon nitride honeycomb pottery with duct inner wall extend whisker structure.The obtained ceramic matrix partial particulate of the inventive method combines closely, and honeycomb hole inwall grows into whisker, and this ceramic honey comb has the premium propertiess such as high strength, low density, high temperature resistant, resistance to chemical attack, is applicable to filtration and the purification of multiple fluid.Ceramic honey comb after using is easy to adopt multiple method to remove filtrate, reusable.Preparation method's technique of the present invention is simple, low for equipment requirements, convenient operation and control, and production efficiency is high, is applicable to large-scale industrial and produces.
Description
Technical field
The present invention relates to field of material technology, particularly, relate to one and have the preparation method of the silicon nitride honeycomb pottery of " whisker intert parallel channels " structure.
Background technology
Ceramic honey comb has parallel through pore texture, have that osmotic pressure is high, geometric jacquard patterning unit surface is large, diffusion length is short, be conducive to counting of particle and discharge with gas and to reduce advantages such as filtering volume, have a wide range of applications in the purifying treatment etc. of the filtration, purification of industrial gaseous waste, motor-vehicle tail-gas and other life waste gas, the heat exchange of metallurgical industry and the filtration of molten metal, the toxic gas of mining industry and liquid.
Ceramic honey comb has the special channel architecture that is parallel to each other.Based on different pore-forming principles, the preparation of ceramic honey comb mainly contains the several methods such as mould extrusion moulding, impregnation sintering and lyophilize.
The first size according to required honeycomb hole of extrusion moulding and shape (trilateral, rhombus, rectangle, hexagon etc.) prepare mould, then prepare the ceramic honey comb of duct arrangement high-sequential by the extrusion of ceramic size.Corning company of the U.S. and Japanese NGK company comparatively ripe in this technical grasp, realized industrialization produce.The ceramic honey comb of preparation is mainly used in vehicle exhaust and heat accumulation block materials.To be material aperture limit by the preparation of mould for the greatest problem of the method, is difficult to prepare the cellular material of aperture in tens micron dimensions.The up-to-date ceramic honey comb product of Corning company can prepare 1200 through holes at most on the cross section of 1 square inch, and be the limit that current known the method can prepare ceramic honey comb aperture, further reduced bore is very difficult.
Impregnation sintering method is that the tinsel first thickness being about 0.1mm is rolled into spination paillon foil, after being sticked into through-hole structure, then enters in ceramic size by this through-hole structure matrix with binding agent, and final drying, sintering are prepared into ceramic honey comb.Problem and the mould extrusion moulding of the method are similar, are all mechanical hole fabrication technique, and aperture is by the restriction of spination paillon foil rolling process, and further reduced bore is very difficult.
Freeze drying process is relatively new ceramic honey comb moulding process, not yet realizes large-scale commercial production at present.First this technique add the volatile materials of low temperature easy crystallization high temperature such as water, amphene, camphor in ceramic size, then ceramic size is injected the container of the surrounding heat insulation bottom heat conduction be placed on refrigerant, realized the solvent continuously-directional crystallization in slurry by control temperature gradient, be separated with powder granule simultaneously.After lyophilize, ice crystal distils under vacuo, and the microtexture that ice crystal is formed is retained, thus obtains the base substrate with directed through-hole structure, then through sintering obtained porous ceramics.The method is by chemicrystallization, distillation and phase disengagement method pore-forming, has broken away from mechanical processing technique restriction, and 80 microns can be down in the ceramic honey comb aperture of preparation.But, in the freezing casting process of this technique, be difficult to the synchronous change of the thermograde controlling same level, cause the straight parallel general character in the duct of prepared ceramic honey comb poor, this is the subject matter of the method, and in addition, this technique exists a series of technology barrier in large-scale application fashion, processing condition and process are difficult to accurate control, constrain it and apply on a large scale.
Can say, the preparation difficult point of ceramic honey comb and focus concentrate on the hole count increasing further unit surface always, i.e. in the research of reduced bore.But, it is pointed out that the aperture of i.e. enable further reduction ceramic honey comb is reduced to micron dimension, its aperture reduce the increase suddenly that gas will be caused by resistance, thus reduce filtration efficiency.That is, single honeycomb structure is relied on to be difficult to the small-bore required by the filtration of solution subparticle and to keep air-flow this contradiction unimpeded simultaneously.
Whisker is the single crystal of a kind of high strength beard shape synthesized under manual control condition, and its crystalline structure is more complete, and subsurface defect is few, and its strength and modulus is all close to ideal crystal.Therefore, whisker Chang Zuowei reinforcing component join metal matrix, ceramic base and polymer-based in the effect of its activeness and quietness.Modal whisker has Si
3n
4, SiC, Al
2o
3deng.But at present about the research of whisker mainly concentrate on whisker preparation and in matrix activeness and quietness effect, rarely have report about the research of whisker in other purposes.In the preparation research of whisker, report is had to point out to utilize hole can growth in situ whisker, as patent CN102251284A (a kind of method preparing beta-silicon nitride whisker), and document (Ji Xiaoli, Xu Fei, power is national, Wan Weiwei, On In-situ Synthesis of Mullite Whisker strengthens foam silicon carbide ceramics, Chinese powder technology, 2011,17 (3): 33-36) and document (Lv Chenjing, Tian Xiushu, Han Yufang, fabricated in situ contains Al
2o
3whisker Al
2o
3the research of/Ti-Al matrix material mechanism), but former concerns is in the preparation of whisker, and rear both pay close attention to the reinforced effects of whisker to matrix or foam base plate.Meanwhile, the porous body prepared by above document and the hole in parts are closed pore, are difficult to use in filtration.
The present invention is based on hole provides space can the principle of growth in situ whisker, selects Si
3n
4for raw material, by controlling sintering condition, prepare the New Si of " duct inner wall extend whisker "
3n
4ceramic honey comb.The present invention is intended to utilize parallel channels to ensure the unimpeded of fluid, utilizes the filtration of whisker increase to fine particle of duct inner wall extend.The present invention first at honeycomb structure situ synthesizing whisker, and develops whisker and is filtering and the new opplication of field of purification in conjunction with honeycomb structure.
Summary of the invention
The invention provides a kind of preparation method of silicon nitride honeycomb pottery, comprise the following steps:
1) preparation has the silicon nitride honeycomb base substrate also drying of parallel channels;
2) organic eliminating is carried out to dried base substrate;
3) calcine silicon nitride honeycomb base substrate, obtain body portion particle and combine closely, hole inner wall extend has the silicon nitride honeycomb pottery of whisker.
Wherein, the silicon nitride honeycomb base substrate in step 1) with parallel channels adopts extrusion moulding preparation.In the art, extruding forming method prepares the conventional method of ceramic honey comb, can directly prepare silicon nitride honeycomb base substrate.
In the inventive method, in step 1), silicon nitride honeycomb base substrate also can adopt dry pressing, gel casting forming method or direct coagulation casting method first to prepare biscuit, then adopts mechanical hole building method to obtain the silicon nitride honeycomb base substrate with parallel channels.
In embodiments of the invention, be adopt self-control Multi needle to become punch die, the obtained silicon nitride honeycomb base substrate with parallel channels.
In the inventive method, be raw material with beta-silicon nitride powder in step 1), and add sintering agent, shaping medium, dispersion agent mix, and prepares silicon nitride base substrate.
Described beta-silicon nitride powder particle diameter 0.5 μm ~ 2.5 μm, untreated or through oxide treatment.In step 1), beta-silicon nitride powder addition is 65 ~ 90wt% of the powder gross weight comprising silicon nitride powder, sintering agent and dispersion agent.
Described sintering agent is aluminum oxide powder and yttrium oxide powder, aluminum oxide powder particle diameter 0.3 μm ~ 5.0 μm, and addition is the 2-4wt% of beta-silicon nitride powder; Yttrium oxide particle diameter is 0.1 μm ~ 5.0 μm, and addition is the 6-8wt% of beta-silicon nitride powder.
Dispersion agent is mainly used in the colloidal formation such as gel injection molding and forming technology, direct coagulation casting technique, and the present invention does not also rely on specific dispersion agent, as long as dispersion agent can make ceramic powder suitably disperse in sauce.Operable dispersion agent is ammonium polyacrylate, Tetramethylammonium hydroxide, ammonium citrate, ammonium polymethacrylate, Tetramethyl Ethylene Diamine, Sodium hexametaphosphate 99 etc.
According to different forming methods, select corresponding shaping medium.Extrusion moulding generally selects water, polyvinyl alcohol, poly-hydroxyl ethanol acid etc. as shaping medium.Gel casting forming selects water base acrylamide polymers to be shaping medium, and wherein monomer is acrylamide, and linking agent is N, N '-methylene-bisacrylamide, and initiator is 8% ammonium persulfate solution, and catalyzer is N,N,N′,N′ tetramethylethylene diamine.Direct coagulation casting selects urea and urease to be shaping medium.
Raw material beta-silicon nitride powder involved in the present invention, sintering agent powder and the additive such as dispersion agent, shaping medium are common commercial powder, its purity is commercial level, but further according to adjusting the requirement of product purity, also can adopt the grade reagents such as analytical pure.
The powder granularity of raw material beta-silicon nitride powder involved in the present invention, sintering agent powder and dispersion agent, shaping medium etc. is more little is more conducive to sintering, preferably less than 2.0 μm powders, but is not limited thereto scope.
According to different forming methods, additive such as dispersion agent, shaping medium etc. can be different, and the solid load of base substrate also can be different.
In the inventive method, step 2) in the drying of silicon nitride honeycomb base substrate be that room temperature is dried in the shade or 40 DEG C ~ 60 DEG C oven dry, the parallel construction in maintenance honeycomb duct.
Step 2) in organism eliminating is carried out to dried base substrate, temperature is at 500 DEG C ~ 800 DEG C, and the time is 0.5 ~ 3 hour.
According to different forming methods, its time of drying/temperature/humidity is different, to keep base substrate indeformable for standard.Because organic content in different forming method base substrate is different, so it is different to get rid of organic program.In extrusion moulding, dry-pressing formed prepared base substrate, organic content is higher, depending on base substrate size, need the 1 little independent degreasing process up to 1 day, and in gel casting forming and the base substrate prepared by direct coagulation casting, organic content is lower, is easy to binder removal in rapid heating condition before sintering.This process is familiar with by those skilled in the art.
In the inventive method, calcined by silicon nitride honeycomb base substrate in step 3), calcining temperature is 1650 DEG C ~ 1750 DEG C, insulation 0.5h ~ 3h.
Preferably, calcined by silicon nitride honeycomb base substrate in step 3), calcining temperature is 1700 DEG C, and soaking time is 3h.
Present invention also offers the preparation-obtained silicon nitride honeycomb pottery of above-mentioned preparation method.
The present invention proposes on the framework of ceramic honey comb base substrate, hole is utilized to grow the principle of whisker, prepare the silicon nitride honeycomb pottery that hole wall is " whisker intert parallel channels " novel texture of whisker, the whisker stretched in this novel texture silicon nitride honeycomb ceramic channel walls effectively can carry out the filtration of fine particle, and its original basic honeycomb parallel via holes structure in turn ensure that the smoothness of fluid.
The ceramic honey comb of " duct inner wall extend whisker " novel texture proposed by the invention, is not only applicable to silicon nitride, is also applicable to the material such as silicon carbide, aluminum oxide simultaneously generating whisker under similar or catalytic condition.The ceramic honey comb of " duct inner wall extend whisker " novel texture of preparation, is not limited to pore size, increases the efficiency such as filtration, separation, enrichment by hole by aperture inner wall extend whisker.Ceramic honey comb after using is easy to adopt multiple method to remove filtrate, reusable.
Production technique of the present invention is simple, low for equipment requirements, convenient operation and control, and production efficiency is high, is applicable to large-scale industrial and produces.The ceramic honey comb prepared by method of the present invention is silicon nitride material, there is the premium propertiess such as high strength, low density, high temperature resistant, resistance to chemical attack, be applicable to filtration and the purification of multiple fluid, as the filtration, purification of fine particle in air, waste gas that various commercial run produces, its other life waste gas of motor-vehicle tail-gas, also can be used for the tabular adsorbent of analysis chromatographic column, to the filtration of the heat exchange of metallurgical industry and molten metal, to the toxic gas of mining industry and the purifying treatment etc. of liquid.Scanning electron microscope (SEM) shows ceramic honey comb body portion particle of the present invention and combines closely, and honeycomb hole inwall grows into whisker, forms parallel channels.This structure makes ceramic honey comb of the present invention can be kept the smoothness of fluid in use by straight channels, and the whisker of passing hole channel inner wall extend filters further, cleansing fluid.
Accompanying drawing explanation
Fig. 1 is silicon nitride ceramics " duct inner wall extend whisker " the SEM photo that embodiment 1 obtains.
Fig. 2 is silicon nitride ceramics " the duct inner wall extend whisker " XRD figure that embodiment 1 obtains.
Embodiment
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.Without departing from the spirit and substance of the case in the present invention, the amendment do the inventive method, step or condition or replacement, all belong to scope of the present invention.
If do not specialize, chemical feedstocks used in embodiment is conventional commercial raw material, the conventional means that technique means used in embodiment is well known to those skilled in the art.
Silicon nitride honeycomb pottery and performance thereof are prepared in embodiment 1 extrusion moulding
Getting 200g particle diameter is 2 μm of silicon nitride powders, and 5g particle diameter is 3 μm of aluminum oxide and 15g particle diameter is 2 μm of yttrium oxide, mixes, obtains powdered mixture.The acid of water, polyvinyl alcohol and poly-hydroxyl ethanol is pressed the weight ratio mixing of 70:10:20, stir obtained homogeneous solution, solution is mixed with the weight ratio of above-mentioned powder mixture according to 100:70, fully mixing 0.75 hour of normal temperature in the mixing roll (BL-6175-B) at normal temperatures and pressures, under normal temperature and pressure old 3 hours, obtain pug.Pug is crossed 60 mesh sieves and carry out filtration, purification, the honeycomb biscuit with parallel channels is extruded by honeycomb ceramic extruding machine (BL-6177), 40 DEG C of dryings 6 hours, after dry, sample is at 600 DEG C of binder removal organics removal 2h, then the honeycomb biscuit after binder removal is put into sintering oven, be warming up to 1700 DEG C with 10 DEG C/min, under the nitrogen pressure of 0.5MPa, sinter 2.5 hours, be there is " duct inner wall extend whisker " structure silicon nitride honeycomb pottery.Fig. 1 is shown in by its SEM photo, and XRD figure is shown in Fig. 2.Scanning electron microscope (SEM) shows the obtained silicon nitride honeycomb ceramic matrix partial particulate of the present embodiment and combines closely, and honeycomb hole inwall grows into whisker, forms parallel channels.
This ceramic honey comb aperture is 0.5mm, and void content is 68%.The method specified according to GB/T1964 detects, and obtaining horizontal ultimate compression strength is 9MPa, axial compression strength 21MPa.After placing 24 hours again after ceramic honey comb is boiled 0.5 hour with 10% salpeter solution, solution is water white transparency, and resist chemical performance is good.After testing, the silicon nitride honeycomb pottery of preparation has that osmotic pressure is high, geometric jacquard patterning unit surface is large, diffusion length is short, is conducive to counting of particle and discharges with gas and to reduce filtration volume, the excellent specific properties such as the smoothness of fluid.
Embodiment 2 gel casting forming prepares silicon nitride honeycomb pottery and performance thereof
By monomeric acrylamide and linking agent N, N '-methylene-bisacrylamide is water-soluble, monomeric acrylamide concentration is 15wt%, crosslinker concentration is 0.5wt%, form monomer premixed liquid, in 100ml monomer premixed liquid, add particle diameter is 0.5 μm of beta-silicon nitride powder 230g, the particle diameter adding silicon nitride powder body burden 2.5% is the particle diameter of 0.3 μm of sintering agent aluminum oxide powder 5.75g and silicon nitride powder body burden 7.5% is 0.1 μm of yttrium oxide powder 17.25g, dispersion agent is ammonium citrate 2g, stir and obtain the ceramic size that solid load is about 40%, catalyst n is added in above-mentioned slurry, N, N ', N '-Tetramethyl Ethylene Diamine 25 μ l, then stir, add initiator 8% ammonium persulfate solution 50 μ l again, mould is injected at once after stirring, and self-control Multi needle is become punch die (syringe needle φ=2mm, 4 hole/square centimeters) insert in slurry, be the demoulding after gel until slurry, obtain honeycomb to wet base.Wet base is put into baking oven 50 DEG C of dryings 24 hours, dry base substrate is put into multifunctional sintering furnace (HIGH-MUTLI5000), be warming up to 1650 DEG C with speed 10 DEG C/min, in temperature-rise period, organism completes eliminating, and under the nitrogen pressure of 0.5MPa, 1650 DEG C sinter 2 hours.Be there is " duct inner wall extend whisker " structure silicon nitride honeycomb pottery.The SEM photo of the silicon nitride honeycomb pottery that the present embodiment prepares and XRD figure and the obtained silicon nitride honeycomb ceramic-like of embodiment 1 are seemingly.
This ceramic honey comb aperture is 0.1mm, and void content is 65%.The method specified according to GB/T1964 detects, and obtaining horizontal ultimate compression strength is 13MPa, axial compression strength 28MPa.After placing 24 hours again after ceramic honey comb is boiled 0.5 hour with 10% salpeter solution, solution is water white transparency, and resist chemical performance is good.After testing, the silicon nitride honeycomb pottery of preparation has that osmotic pressure is high, geometric jacquard patterning unit surface is large, diffusion length is short, is conducive to counting of particle and discharges with gas and to reduce filtration volume, the excellent specific properties such as the smoothness of fluid.
Embodiment 3 is dry-pressing formed prepares silicon nitride honeycomb pottery and performance thereof
Be 2.5 μm of beta-silicon nitride powders and 5g particle diameter by 200g particle diameter be 5 μm of sintering agent aluminum oxide powders and 15g particle diameter be that 2 μm of yttrium oxide powders mix, add alcohol and abrading-ball wet-milling 24 hours, after drying and screening, add using material 5wt% paraffin after sieving as forming agent, rectangular sample (long 10cm is pressed in punching block, wide 5cm, high 5cm), pressure is 120MPa, the Multi needle of press-in self-control subsequently becomes punch die (syringe needle φ=2mm, 4 hole/square centimeters) and extract, obtained honeycomb body, this honeycomb body is put into draft glue discharging furnace be warming up to 800 DEG C and be incubated dewaxing in 3 hours, dry base substrate is put into multifunctional sintering furnace (HIGH-MUTLI5000), 1700 DEG C are warming up to speed 10 DEG C/min, 1.5 hours are sintered under the nitrogen pressure of 0.5MPa.Be there is " duct inner wall extend whisker " structure silicon nitride honeycomb pottery.The SEM photo of the silicon nitride honeycomb pottery that the present embodiment prepares and XRD figure and the obtained silicon nitride honeycomb ceramic-like of embodiment 1 are seemingly.
This ceramic honey comb aperture is 0.1mm, and void content is 62%.The method specified according to GB/T1964 detects, and obtaining horizontal ultimate compression strength is 10MPa, axial compression strength 21MPa.After placing 24 hours again after ceramic honey comb is boiled 0.5 hour with 10% salpeter solution, solution is water white transparency, and resist chemical performance is good.After testing, the silicon nitride honeycomb pottery of preparation has that osmotic pressure is high, geometric jacquard patterning unit surface is large, diffusion length is short, is conducive to counting of particle and discharges with gas and to reduce filtration volume, the excellent specific properties such as the smoothness of fluid.
Embodiment 4 direct coagulation casting prepares silicon nitride honeycomb pottery and performance thereof
Be 2 μm of beta-silicon nitride powders and 8.5g particle diameter by 340g particle diameter be 3 μm of sintering agent aluminum oxide powders and 255g particle diameter be that 3 μm of yttrium oxide powders mix, add 100ml deionized water fully to stir, slurry is cooled to about 5 DEG C, adds analytically pure urea 1g and urease 20unit/mg, be stirred well to evenly, slurry is warming up to 25 DEG C, punch die is become to put into slurry Multi needle, static 1 hour, slurry curing, take out Multi needle and become punch die, obtained silicon nitride honeycomb base substrate.Base substrate is put into baking oven 40 DEG C of dryings 12 hours, dry base substrate is put into dry base substrate is put into multifunctional sintering furnace (HIGH-MUTLI5000), be warming up to 1700 DEG C with speed 10 DEG C/min, in temperature-rise period, organism completes eliminating, and under the nitrogen pressure of 0.5MPa, 1700 DEG C sinter 3 hours.Be there is " duct inner wall extend whisker " structure silicon nitride honeycomb pottery.The SEM photo of the silicon nitride honeycomb pottery that the present embodiment prepares and XRD figure and the obtained silicon nitride honeycomb ceramic-like of embodiment 1 are seemingly.
This ceramic honey comb aperture is 0.1mm, and void content is 72%.The method specified according to GB/T1964 detects, and obtaining horizontal ultimate compression strength is 12MPa, axial compression strength 28MPa.After placing 24 hours again after ceramic honey comb is boiled 0.5 hour with 10% salpeter solution, solution is water white transparency, and resist chemical performance is good.After testing, the silicon nitride honeycomb pottery of preparation has that osmotic pressure is high, geometric jacquard patterning unit surface is large, diffusion length is short, is conducive to counting of particle and discharges with gas and to reduce filtration volume, the excellent specific properties such as the smoothness of fluid.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (7)
1. a preparation method for silicon nitride honeycomb pottery, is characterized in that, described method comprises the following steps:
1) preparation has the silicon nitride honeycomb base substrate also drying of parallel channels;
2) organic eliminating is carried out to dried base substrate;
3) calcine silicon nitride honeycomb base substrate, obtain body portion particle and combine closely, hole inner wall extend has the silicon nitride honeycomb pottery of whisker;
Wherein, step 1) in be raw material with beta-silicon nitride powder, and add sintering agent, dispersion agent, shaping medium, deionized water mix, and prepares silicon nitride base substrate;
Step 1) described beta-silicon nitride powder particle diameter 0.5 μm ~ 2.5 μm, beta-silicon nitride powder addition is 65 ~ 90wt% of the powder gross weight comprising silicon nitride powder, sintering agent and dispersion agent;
Described sintering agent is aluminum oxide powder and yttrium oxide powder, aluminum oxide powder particle diameter 0.3 μm ~ 5.0 μm, and addition is the 2-4wt% of beta-silicon nitride powder; Yttrium oxide particle diameter is 0.1 μm ~ 5.0 μm, and addition is the 6-8wt% of beta-silicon nitride powder;
Step 3) in calcining temperature be less than 1700 DEG C for being greater than 1650 DEG C, insulation 0.5h ~ 3h, pressure 0.5MPa.
2. preparation method as claimed in claim 1, is characterized in that, step 1) in there is parallel channels silicon nitride honeycomb base substrate adopt extrusion moulding preparation.
3. preparation method as claimed in claim 1, it is characterized in that, step 1) in silicon nitride honeycomb base substrate adopt dry pressing, gel casting forming method or direct coagulation casting method first to prepare biscuit, then adopt mechanical hole building method to obtain the silicon nitride honeycomb base substrate with parallel channels.
4. method as claimed in claim 3, it is characterized in that, the particle diameter of silicon nitride powder is 2 μm; Described sintering agent is aluminum oxide powder and yttrium oxide powder, aluminum oxide powder particle diameter 3.0 μm, and addition is the 2.5wt% of beta-silicon nitride powder; Yttrium oxide particle diameter is 2.0 μm, and addition is the 7.5wt% of beta-silicon nitride powder.
5. the method as described in as arbitrary in claims 1 to 3, is characterized in that, step 1) in the drying means of silicon nitride honeycomb base substrate be that room temperature is dried in the shade or 40 DEG C ~ 60 DEG C oven dry, the parallel construction in maintenance honeycomb duct.
6. the method for claim 1, is characterized in that, step 2) in organism eliminating is carried out to dried base substrate, temperature is at 500 DEG C ~ 800 DEG C, and the time is 0.5 ~ 3 hour.
7. the preparation-obtained silicon nitride honeycomb pottery of preparation method according to claim 1.
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