CN102206081A - Preparation method of aluminium-nitrogen co-doped silicon carbide absorbing material - Google Patents
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Abstract
The invention provides a preparation method of an aluminium-nitrogen co-doped silicon carbide absorbing material. The method comprises the following steps: selecting initial reaction raw materials of silicon powder with a granularity of 200-400 mesh, carbon black with a granularity of 20-60nm, and ammonium chloride 0.5% -5% of gross weight of the silicon powder and the carbon black; carrying out ball milling on the raw materials for 2-4h; after the ball milling, adding aluminium powder 0.5-10% of gross weight of the silicon powder and the carbon black and tetrafluoroethylene powder 1%-20% of gross weight of the silicon powder and the carbon black into the raw materials for a second ball milling; after the second ball milling, sieving the raw materials with a 60 mesh screen, and disposing the materials in a graphite crucible; disposing the graphite crucible in a high pressure container for vacuum-pumping scrubbing, and filling in nitrogen of 0.5-5Mpa; carrying out self-propagating high temperature synthesis reaction by an electric ignition; carrying out a subsequent processing on reaction synthesis, and removing impurities thereof. The preparation method of the aluminium-nitrogen co-doped silicon carbide absorbing material provided by the present invention has a short production period, and simple equipment and technology; and controllable doping can be realized.
Description
Technical field
The present invention relates to the preparation field of ceramic, particularly relate to the preparation method of a kind of aluminium-nitrogen co-doped silicon carbide absorbing material.
Background technology
Silicon carbide (SiC) is a kind of ideal new type high temperature absorbing material, has that density is little, high temperature resistant, wearability is good, thermostability is high, and the big premium properties that waits of thermal conductivity has widely in fields such as space flight and aviation, national defence, electronics and to use.In recent years, the electromagnetic pollution that electronics and communication system cause not only has a strong impact on human health, and the whole world annual because of its financial loss that causes up to multi-billion dollar.The more important thing is that in military field the research in the electromagnetic shielding material field has important researching value and application prospect about silicon carbide.But the absorbing property of silicon carbide own is very poor, and its dielectric loss is little, and assimilated efficiency is low, and the complex permittivity absorption frequency is narrow, can't satisfy the requirement of electromagnetic shielding material " strong absorption, broadband absorb ".And mix is one of effective way that improves the silicon carbide absorbing property.In at present common adulterating method, mix jointly as simple aluminium (Al), nitrogen (N) or aluminium, nitrogen, the dielectric loss performance of silicon carbide is increased, having proved mixes can strengthen silicon carbide lossy microwave performance.But the simple adulterated silicon carbide powder of aluminium is easy to generate reunion, lack of homogeneity.The oxidation-resistance of simple nitrogen doped silicon carbide powder is poor, does not utilize high temperature to use.
And there are not the problems referred to above in aluminium, nitrogen co-doped silicon carbide powder, the more important thing is to a certain extent and can control the dielectric properties of silicon carbide powder.In the silicon carbide lattice, aluminium mixes can introduce hole carrier, and nitrogen mixes can introduce electronic carrier, by aluminium, nitrogen co-doped in the inner impurity level that forms of silicon carbide.The element that doping is high among both (can produce the many elements of current carrier) plays a leading role aspect dielectric properties.Therefore,,, can change the specific conductivity of silicon carbide,, further control the absorbing property of carbofrax material with the dielectric properties of control silicon carbide by control aluminium, nitrogen doping separately according to the composite principle of hole carrier and electronic carrier.
But people adopt high-temperature heat treatment or laser synthesis method to obtain nitrogen or aluminium doped silicon carbide nano-powder more at present, and the problem of existence is the equipment complexity, the production cycle is long, preparation technology is loaded down with trivial details, cost is high.Therefore, at the silicon carbide absorbing material, how to realize that the high-level efficiency of aluminium, two kinds of elements of nitrogen, mass doping prepare most important.
Summary of the invention
Technical problem to be solved by this invention provides the preparation method of a kind of aluminium-nitrogen co-doped silicon carbide absorbing material, can improve concentration and the electroconductibility and the lossy microwave performance of silicon carbide, with short production cycle, equipment and technology are simple, and can realize controllable doped.
In order to address the above problem, the invention discloses the preparation method of a kind of aluminium-nitrogen co-doped silicon carbide absorbing material, may further comprise the steps:
Choose silica flour, carbon black and ammonium chloride and be the reaction starting raw material, the granularity of described silica flour is 200～400 orders, and the sooty granularity is 20～60nm, and the consumption of ammonium chloride is 0.5%～5% of silica flour and a carbon black gross weight;
With above-mentioned reaction starting raw material ball milling 2～4 hours in ball mill;
Raw material behind the ball milling is added the aluminium powder of silica flour and carbon black gross weight 0.5%～10% and the polytetrafluorethylepowder powder of silica flour and carbon black gross weight 1%～20% more respectively, on ball mill, carry out the ball milling second time;
Raw material behind the second time ball milling is crossed 60 mesh sieves, place plumbago crucible;
The plumbago crucible of raw material places high pressure vessel behind the ball milling for the second time with being equipped with, and vacuumizes the gas washing operation, and charges into the nitrogen of 0.5～5MPa, utilizes tungsten filament energising igniting, realizes the self propagating high temperature combustion synthesis reaction;
Carry out subsequent disposal to reacting synthetic material, remove impurity wherein.
Further, described second time ball milling time be 5～15 minutes.
Further, describedly carry out subsequent disposal and comprise removal carbon wherein reacting synthetic material, described removal method is:
The synthetic material of cooled reaction is heated to 600-700 ℃ in air, and is incubated 1～3 hour.
Further, describedly carry out carrying out cleanup acid treatment after subsequent disposal also is included in removal carbon wherein to reacting synthetic material.
Further, described cleanup acid treatment comprises:
Be that 10%～30% hydrochloric acid and concentration are 10%～30% the synthetic material of the described reaction of hydrofluoric acid dips with concentration respectively, the time is 2～5 hours;
The synthetic material of reaction after the described immersion of employing distilled water wash.
Further, the number of times of the synthetic material of the reaction after the described immersion of described distilled water wash is 3 to 5 times.
Further, described ball-milling medium is the silicon carbide ball.
Further, described silica flour and sooty purity are more than or equal to 99%.
Compared with prior art, the present invention has the following advantages:
The preparation method of aluminium of the present invention-nitrogen co-doped silicon carbide absorbing material adopts the self propagating high temperature synthetic technology, utilize reaction self heat release synthetic materials, utilize the outside energy that provides to bring out high heat-producing chemical reaction system generation topochemical reaction (i.e. igniting), form the combustion wave that spreads voluntarily, it is propagated to the unreacted district fast, until spreading whole reaction system, finally obtain synthetic materials.Adopt the high-energy ball milling reaction starting raw material of activation treatment silica flour, carbon black and ammonium chloride in advance, occur between ball-powder-ball by a large amount of collision phenomenons, serious viscous deformation takes place in captive powder under impact effect, high density of defects, distortional strain energy and the nano-interface of powder generation will promote the carrying out of combustion synthesis reaction greatly thus, therefore this kind preparation method's temperature of reaction height, speed of response are fast, temperature rise rate is fast, can save energy and cost.In adulterated process,, can control the dielectric properties of silicon carbide by the aluminium of controlled doping, the proportion of nitrogen, and synthetic aluminium, nitrogen co-doped silicon carbide powder degree of purity of production are higher, therefore production cycle is also shorter, and equipment is simple, can be efficiently and batch preparations.
Description of drawings
Fig. 1 is the schema of the preparation method embodiment of aluminium of the present invention-nitrogen co-doped silicon carbide absorbing material;
Fig. 2 is the XRD figure of the aluminium nitrogen doped silicon carbide of example one of the present invention;
Fig. 3 is the SEM figure of the aluminium nitrogen doped silicon carbide of example one of the present invention;
Fig. 4 is the XRD figure of the aluminium nitrogen doped silicon carbide of example two of the present invention;
Fig. 5 is the SEM figure of the aluminium nitrogen doped silicon carbide of example two of the present invention;
Fig. 6 is the XRD figure of the aluminium nitrogen doped silicon carbide of example three of the present invention;
Fig. 7 is the SEM figure of the aluminium nitrogen doped silicon carbide of example three of the present invention;
Fig. 8 is the XRD figure of the aluminium nitrogen doped silicon carbide of example four of the present invention;
Fig. 9 is the SEM figure of the aluminium nitrogen doped silicon carbide of example four of the present invention;
Figure 10 is the XRD figure of the aluminium nitrogen doped silicon carbide of example five of the present invention;
Figure 11 is the SEM figure of the aluminium nitrogen doped silicon carbide of example five of the present invention.
Embodiment
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, the present invention is further detailed explanation below in conjunction with the drawings and specific embodiments.
The objective of the invention is to utilize the self propagating high temperature synthetic technology, realize the preparation of aluminium-nitrogen co-doped silicon carbide powder, thereby the dielectric properties of silicon carbide powder are controlled.
With reference to Fig. 1, the preparation method embodiment of aluminium of the present invention-nitrogen co-doped silicon carbide absorbing material is shown, may further comprise the steps:
Step 101 is chosen silica flour, carbon black and ammonium chloride (NH
4Cl) be the reaction starting raw material, the granularity of described silica flour is 200～400 orders, and the sooty granularity is 20～60nm, and the consumption of ammonium chloride is 0.5%～5% of silica flour and a carbon black gross weight.
Wherein, silica flour and sooty purity can be selected according to practical situation, are easier to carry out in order to make reaction, and the impurity of follow-up generation product is less, it is higher relatively that purity needs, among the present invention, choose purity 99.0% more than or equal to silica flour and carbon black as the reaction starting raw material.
Step 102 is with above-mentioned reaction starting raw material ball milling 2～4 hours in ball mill.
Ball mill is a high energy ball mill, and ball-milling medium is the silicon carbide ball.
Step 103 adds the aluminium powder of silica flour and carbon black gross weight 0.5%～10% and the polytetrafluoroethylene (PTFE) powder of silica flour and carbon black gross weight 1%～20% respectively again with the raw material behind the ball milling, carries out the ball milling second time on ball mill.
The time of ball milling can come to determine as the case may be for the second time, various powders can be mixed to get final product, and in the present embodiment, the time of ball milling is generally 5～15 minutes for the second time.
Step 104 is crossed 60 mesh sieves with the raw material behind the second time ball milling, places plumbago crucible.
Wherein, place the quality of the reaction powder of plumbago crucible can determine that the capacity of plumbago crucible is big more, just can place many more reaction powders according to the capacity of plumbago crucible.In the present embodiment, general each 100 grams to 200 grams of getting are put into plumbago crucible.
Step 105, the plumbago crucible of raw material places high pressure vessel behind the ball milling for the second time with being equipped with, and vacuumizes the gas washing operation, and charges into the nitrogen of 0.5～5MPa, utilizes tungsten filament energising igniting, realizes the self propagating high temperature combustion synthesis reaction.
Wherein, nitrogen is high pure nitrogen, and its purity is generally more than or equal to 99.999%.The number of times that vacuumizes gas washing can determine that for example, behind the secondary vacuum pumping gas washing, the gas purity in the high pressure vessel meets the requirements, and then need not to carry out to vacuumize for three times according to the particular case in the high pressure vessel.Generally speaking, in order to guarantee the gas purity in the high pressure vessel, the number of times that vacuumizes mostly is three times.In addition, the gas that charges into adopts nitrogen, and nitrogen-atoms wherein can participate in reaction, enters in the middle of the lattice of silicon carbide, thereby obtains the required adulterated nitrogen of silicon carbide.Synthetic product furnace cooling under nitrogen after reaction finishes.
Step 106 is carried out subsequent disposal to reacting synthetic material, removes impurity wherein.
Generally speaking, can comprise impurity such as carbon, silicon and silicon-dioxide in the synthetic material of reaction.When subsequent disposal, can at first in air, be heated to 600-700 ℃ to the synthetic material of cooled reaction, and be incubated 1～3 hour, thereby remove carbon wherein, carry out cleanup acid treatment with certain density hydrochloric acid and hydrofluoric acid respectively then, remove impurity such as silicon and silicon-dioxide, thereby obtain highly purified aluminium-nitrogen co-doped silicon carbide powder product.Wherein, the treating processes of pickling is, is that 10%～30% hydrochloric acid and concentration are 10%～30% the synthetic material of the described reaction of hydrofluoric acid dips with concentration respectively, and the time is 2～5 hours; Adopt the synthetic material of reaction after the described immersion of distilled water wash then.The number of times of the synthetic material of reaction after distilled water wash soaks is generally 3 to 5 times.
The preparation method of aluminium of the present invention-nitrogen co-doped silicon carbide absorbing material adopts the self propagating high temperature synthetic technology, utilize reaction self heat release synthetic materials, utilize the outside energy that provides to bring out high heat-producing chemical reaction system generation topochemical reaction (i.e. igniting), form the combustion wave that spreads voluntarily, it is propagated to the unreacted district fast, until spreading whole reaction system, finally obtain synthetic materials.Adopt the high-energy ball milling reaction starting raw material of activation treatment silica flour, carbon black and ammonium chloride in advance, occur between ball-powder-ball by a large amount of collision phenomenons, serious viscous deformation takes place in captive powder under impact effect, high density of defects, distortional strain energy and the nano-interface of powder generation will promote the carrying out of combustion synthesis reaction greatly thus, therefore this kind preparation method's temperature of reaction height, speed of response are fast, temperature rise rate is fast, can save energy and cost.In adulterated process, by the aluminium of controlled doping, the proportion of nitrogen, can control the dielectric properties of silicon carbide, and synthetic aluminium, nitrogen co-doped silicon carbide powder degree of purity of production are higher, the production cycle is also shorter, therefore can be efficiently and batch preparations.
Preparation method embodiment to aluminium of the present invention-nitrogen co-doped silicon carbide absorbing material is elaborated below in conjunction with concrete example.
Example one
Carbon black and the 2 gram ammonium chlorides of 140 grams, 250 purpose silica flours, 60 gram 50nm are placed high energy ball mill, and ball milling 3 hours, ball-milling medium are the silicon carbide ball.Add 1 gram aluminium (Al) powder, 12 gram polytetrafluoroethylene (PTFE) powder then, uniform mixing is 10 minutes again.To cross 60 mesh sieves through mixed uniformly powder, and get 100 grams and place plumbago crucible.Place high pressure vessel with the crucible of handling the back powder is housed, carry out vacuumizing again for 3 times the gas washing operation after, charge into the high pure nitrogen of 3MPa, utilize tungsten filament energising igniting, the pilot combustion building-up reactions, after reaction was finished, products of combustion is furnace cooling under nitrogen atmosphere.Combustion synthesized product is heated to 600 ℃ in air, and is incubated 2 hours.Be that 15% hydrochloric acid and concentration are 10% hydrofluoric acid acid-leached product respectively with concentration again, soaking the product time respectively is 3 hours, behind 5 distilled water washs, obtains final synthetic product.
With reference to Fig. 2, to analyze as can be known by the XRD (X-ray diffraction, X-ray diffraction) of final synthetic product, synthetic product mainly is the SiC of cubic structure, its lattice parameter is compared with doped SIC sample not, has reduced
Show that Al, N have entered in the lattice of SiC, prepared product is Al, N codoped SiC powder.
With reference to Fig. 3, SEM (the scanning electron microscope of final synthetic product, scanning electronic microscope) analysis revealed, prepared Al, N doped SIC powder mainly are made up of the equi-axed crystal of the about 200nm of mean diameter, and tactical rule, crystal boundary are clearly demarcated.In 8.0GHz～12.4GHz range of frequency, the dielectric loss value of prepared SiC powder never doped SIC 0.07 bring up to 0.22.
Example two
With 136.5 grams, 300 order silica flours, 60 gram 50nm carbon blacks and 1.965 gram ammonium chlorides place high energy ball mill, and ball milling 3 hours, ball-milling medium are the silicon carbide ball.Add 3.93 gram aluminium (Al) powder and 11.79 gram polytetrafluoroethylene (PTFE) powder then, uniform mixing is 10 minutes again.To cross 60 mesh sieves through mixed uniformly powder, and get 100 grams and place plumbago crucible.Place high pressure vessel with the crucible of handling the back powder is housed, carry out vacuumizing again for 3 times the gas washing operation after, charge into the high pure nitrogen of 3MPa, utilize tungsten filament energising igniting, the pilot combustion building-up reactions, after reaction was finished, products of combustion is furnace cooling under nitrogen atmosphere.Combustion synthesized product is heated to 600 ℃ in air, and is incubated 2 hours.Be that 15% hydrochloric acid and concentration are 10% hydrofluoric acid acid-leached product respectively with concentration again, soaking the product time respectively is 3 hours, behind 5 distilled water washs, obtains final synthetic product.
With reference to Fig. 4, by the XRD analysis of final synthetic product as can be known, synthetic product mainly is the SiC of cubic structure, and its lattice parameter is compared with doped SIC sample not, has reduced
Show that Al, N have entered in the lattice of SiC, prepared product is Al, N codoped SiC powder.
With reference to Fig. 5, the typical sem analysis result of final synthetic product shows that prepared Al, N doped SIC powder mainly are made up of the equi-axed crystal of the about 100nm of mean diameter, and tactical rule, crystal boundary are clearly demarcated.In 8.0GHz～12.4GHz range of frequency, the dielectric loss value of prepared SiC powder never doped SIC 0.07 bring up to 0.10.
Example three
133 grams, 250 order silica flours, 60 gram 50nm carbon blacks and 1.93 gram ammonium chlorides are placed high energy ball mill, and ball milling 3 hours, ball-milling medium are the silicon carbide ball.Add 5.79 gram aluminium (Al) powder, 11.58 gram polytetrafluoroethylene (PTFE) powder then, uniform mixing is 10 minutes again.To cross 60 mesh sieves through mixed uniformly powder, and get 100 grams and place plumbago crucible.Place high pressure vessel with the crucible of handling the back powder is housed, carry out vacuumizing again for 3 times the gas washing operation after, charge into the high pure nitrogen of 1MPa, utilize tungsten filament energising igniting, the pilot combustion building-up reactions, after reaction was finished, products of combustion is furnace cooling under nitrogen atmosphere.Combustion synthesized product is heated to 600 ℃ in air, and is incubated 2 hours.Be that 15% hydrochloric acid and concentration are 10% hydrofluoric acid acid-leached product respectively with concentration again, soaking the product time respectively is 3 hours, behind 5 distilled water washs, obtains final synthetic product.
With reference to Fig. 6, by the XRD analysis of final synthetic product as can be known, synthetic product mainly is the SiC of cubic structure, and its lattice parameter is compared with doped SIC sample not, has increased
Show that Al, N have entered in the lattice of SiC, prepared product is Al, N codoped SiC powder.
With reference to Fig. 7, the sem analysis of final synthetic product shows that prepared Al, N doped SIC powder mainly are made up of the equi-axed crystal of the about 70nm of mean diameter, and tactical rule, crystal boundary are clearly demarcated.In 8.0GHz～12.4GHz range of frequency, the dielectric loss value of prepared SiC powder never doped SIC 0.07 bring up to 0.18.
Example four
129.5 grams, 300 order silica flours, 60 gram 50nm carbon blacks and 1.895 gram ammonium chlorides are placed high energy ball mill, and ball milling 3 hours, ball-milling medium are the silicon carbide ball.Add 7.58 gram aluminium (Al) powder, 11.37 gram polytetrafluoroethylene (PTFE) powder then, uniform mixing is 10 minutes again.To cross 60 mesh sieves through mixed uniformly powder, and get 100 grams and place plumbago crucible.Place high pressure vessel with the crucible of handling the back powder is housed, carry out vacuumizing again for 3 times the gas washing operation after, charge into the high pure nitrogen of 1MPa, utilize tungsten filament energising igniting, the pilot combustion building-up reactions, after reaction was finished, products of combustion is furnace cooling under nitrogen atmosphere.Combustion synthesized product is heated to 600 ℃ in air, and is incubated 2 hours.Be that 15% hydrochloric acid and concentration are 10% hydrofluoric acid acid-leached product respectively with concentration again, soaking the product time respectively is 3 hours, behind 5 distilled water washs, obtains final synthetic product.
With reference to Fig. 8, the XRD analysis of final synthetic product as can be known, product mainly is made up of the SiC of cubic structure, its lattice parameter is compared with doped SIC sample not, has increased
Show that Al, N have entered in the lattice of SiC, prepared product is Al, N codoped SiC powder.
With reference to Fig. 9, the sem analysis result of final synthetic product shows that prepared Al, N doped SIC powder mainly are made up of the equi-axed crystal of the about 40nm of mean diameter, and tactical rule, crystal boundary are clearly demarcated.In 8.0GHz～12.4GHz range of frequency, the dielectric loss value of prepared SiC powder never doped SIC 0.07 bring up to 0.21.
Example five
127 grams, 250 order silica flours, 60 gram 50nm carbon blacks and 1.87 gram ammonium chlorides are placed high energy ball mill, and ball milling 3 hours, ball-milling medium are the silicon carbide ball.Add 9.35 gram aluminium (Al) powder, 11.22 gram polytetrafluoroethylene (PTFE) powder then, uniform mixing is 10 minutes again.To cross 60 mesh sieves through mixed uniformly powder, and get 100 grams and place plumbago crucible.Place high pressure vessel with the crucible of handling the back powder is housed, carry out vacuumizing again for 3 times the gas washing operation after, charge into the high pure nitrogen of 1MPa, utilize tungsten filament energising igniting, the pilot combustion building-up reactions, after reaction was finished, products of combustion is furnace cooling under nitrogen atmosphere.Combustion synthesized product is heated to 600 ℃ in air, and is incubated 2 hours.Be that 15% hydrochloric acid and concentration are 10% hydrofluoric acid acid-leached product respectively with concentration again, soaking the product time respectively is 3 hours, behind 5 distilled water washs, obtains final synthetic product.
With reference to Figure 10, by the XRD analysis of final synthetic product as can be known, synthetic product mainly is the SiC of cubic structure, and its lattice parameter is compared with doped SIC sample not, has increased
Show that Al, N have entered in the lattice of SiC, prepared product is Al, N codoped SiC powder.
With reference to Figure 11, the sem analysis result of final synthetic product shows that prepared Al, N doped SIC powder mainly are made up of the equi-axed crystal of the about 20nm of mean diameter, and tactical rule, crystal boundary are clearly demarcated.In 8.0GHz～12.4GHz range of frequency, the dielectric loss value of prepared SiC powder never doped SIC 0.07 bring up to 0.27.
Each embodiment in this specification sheets all adopts the mode of going forward one by one to describe, and what each embodiment stressed all is and the difference of other embodiment that identical similar part is mutually referring to getting final product between each embodiment.
More than the preparation method of aluminium provided by the present invention-nitrogen co-doped silicon carbide absorbing material is described in detail, used specific case herein principle of the present invention and embodiment are set forth, the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof; Simultaneously, for one of ordinary skill in the art, according to thought of the present invention, the part that all can change in specific embodiments and applications, in sum, this description should not be construed as limitation of the present invention.
Claims (8)
1. the preparation method of aluminium-nitrogen co-doped silicon carbide absorbing material is characterized in that, may further comprise the steps:
Choose silica flour, carbon black and ammonium chloride and be the reaction starting raw material, the granularity of described silica flour is 200～400 orders, and the sooty granularity is 20～60nm, and the consumption of ammonium chloride is 0.5%～5% of silica flour and a carbon black gross weight;
With above-mentioned reaction starting raw material ball milling 2～4 hours in ball mill;
Raw material behind the ball milling is added 1%～20% polytetrafluorethylepowder powder of 0.5%～10% aluminium powder of silica flour and carbon black gross weight and silica flour and carbon black gross weight more respectively, on ball mill, carry out the ball milling second time;
Raw material behind the second time ball milling is crossed 60 mesh sieves, place plumbago crucible;
The plumbago crucible of raw material places high pressure vessel behind the ball milling for the second time with being equipped with, and vacuumizes the gas washing operation, and charges into the nitrogen of 0.5～5MPa, utilizes tungsten filament energising igniting, realizes the self propagating high temperature combustion synthesis reaction;
Carry out subsequent disposal to reacting synthetic material, remove impurity wherein.
2. the method for claim 1 is characterized in that, the time of ball milling described second time is 5～15 minutes.
3. the method for claim 1 is characterized in that, describedly carries out subsequent disposal and comprises removal carbon wherein reacting synthetic material, and described removal method is:
The synthetic material of cooled reaction is heated to 600-700 ℃ in air, and is incubated 1～3 hour.
4. method as claimed in claim 3 is characterized in that, describedly carries out carrying out cleanup acid treatment after subsequent disposal also is included in removal carbon wherein to reacting synthetic material.
5. method as claimed in claim 4 is characterized in that, described cleanup acid treatment comprises:
Be that 10%～30% hydrochloric acid and concentration are 10%～30% the synthetic material of the described reaction of hydrofluoric acid dips with concentration respectively, the time is 2～5 hours;
The synthetic material of reaction after the described immersion of employing distilled water wash.
6. method as claimed in claim 5 is characterized in that, the number of times of the synthetic material of the reaction after the described immersion of described distilled water wash is 3 to 5 times.
7. the method for claim 1 is characterized in that, described ball-milling medium is the silicon carbide ball.
8. the method for claim 1 is characterized in that, described silica flour and sooty purity are more than or equal to 99%.
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| CN103253678A (en) * | 2013-05-06 | 2013-08-21 | 南京航空航天大学 | Titanium diboride ceramic powder low-temperature solid-phase synthesizing method |
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| CN109181637A (en) * | 2018-08-24 | 2019-01-11 | 东南大学 | A kind of lamination shape Mo2CTx/ nitrogen-doped carbon micro-nano hybridization compounding absorbing material and preparation method thereof |
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| CN111960452A (en) * | 2020-08-27 | 2020-11-20 | 北京理工大学 | Preparation method of aluminum fluoride powder |
| CN114038934A (en) * | 2021-09-24 | 2022-02-11 | 北京科技大学 | Preparation method of high-temperature ultraviolet photoelectric detector based on co-doped one-dimensional SiC nanostructure |
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| CN103253678A (en) * | 2013-05-06 | 2013-08-21 | 南京航空航天大学 | Titanium diboride ceramic powder low-temperature solid-phase synthesizing method |
| CN103253678B (en) * | 2013-05-06 | 2016-01-27 | 南京航空航天大学 | A kind of low-temperature solid-phase synthesis method of diboride ceramic powder |
| WO2016177935A1 (en) | 2015-05-07 | 2016-11-10 | Teknologian Tutkimuskeskus Vtt Oy | A method for forming powder particles and a product |
| US11247269B2 (en) | 2015-05-07 | 2022-02-15 | Teknologian Tutkimuskeskus Vtt Oy | Method for forming powder particles and a product |
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| CN105293499B (en) * | 2015-11-30 | 2017-10-24 | 西安电子科技大学 | A kind of preparation method of B, N codope nanometer silicon carbide absorbing material |
| JP2020029390A (en) * | 2018-08-24 | 2020-02-27 | 国立研究開発法人産業技術総合研究所 | Method for producing aluminum silicon carbide |
| CN109181637B (en) * | 2018-08-24 | 2021-02-09 | 东南大学 | Laminated Mo2CTxNitrogen-doped carbon micro-nano hybrid composite wave-absorbing material and preparation method thereof |
| CN109181637A (en) * | 2018-08-24 | 2019-01-11 | 东南大学 | A kind of lamination shape Mo2CTx/ nitrogen-doped carbon micro-nano hybridization compounding absorbing material and preparation method thereof |
| JP7145488B2 (en) | 2018-08-24 | 2022-10-03 | 国立研究開発法人産業技術総合研究所 | Method for producing aluminum silicon carbide |
| CN111960452A (en) * | 2020-08-27 | 2020-11-20 | 北京理工大学 | Preparation method of aluminum fluoride powder |
| CN114038934A (en) * | 2021-09-24 | 2022-02-11 | 北京科技大学 | Preparation method of high-temperature ultraviolet photoelectric detector based on co-doped one-dimensional SiC nanostructure |
| CN114038934B (en) * | 2021-09-24 | 2024-02-09 | 北京科技大学 | Preparation method of high-temperature ultraviolet photoelectric detector based on co-doped one-dimensional SiC nano structure |
| CN117464203A (en) * | 2023-12-28 | 2024-01-30 | 南京曼杰科电子工程有限公司 | Wave-absorbing material apparatus for producing |
| CN117464203B (en) * | 2023-12-28 | 2024-03-19 | 南京曼杰科电子工程有限公司 | Wave-absorbing material apparatus for producing |
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