CN108483447B - A kind of preparation method of micro/nano level spherical carbide silicon materials - Google Patents
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- C01B32/914—Carbides of single elements
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Abstract
The invention belongs to material technology fields, provide a kind of preparation method of micro/nano level spherical carbide silicon materials, spherical carbide silicon materials high-purity, that granularity is controllable are prepared using template, it is characterized in that the carbon ball of size tunable is obtained after hydro-thermal reaction using different organic carbon sources, after gained carbon ball is mixed as template with silicon powder in proportion, reaction product 1 is obtained by high temperature solid state reaction, reaction product 1 obtains the higher spherical carbide silicon materials of pattern uniformity after decarburization, gravity separation method.The present invention can realize the regulation of spherical carbide silicon grain diameter by the selection of organic carbon source and surfactant, the regulation of hydrothermal reaction condition；Then the higher spherical carbide silicon materials of pattern uniformity are obtained by regulation carbon ball with the ratio of silicon powder partial size and using gravity separation method.
Description
Technical field
The invention belongs to material technology fields, and in particular to a kind of preparation method of micro/nano level spherical carbide silicon materials.
Background technique
Silicon carbide have high intensity, high rigidity, high heat conductance, low thermal coefficient of expansion, excellent high-temperature oxidation resistance with
And the performance that stable physicochemical properties etc. are excellent, it is the important advanced structural ceramic of one kind and advanced function ceramics.Therefore
Silicon carbide is widely used in the fields such as abrasive material, metallurgy, refractory material, aerospace, automobile, naval vessel, chemical industry, pipeline manufacture.
Silicon carbide powder is the base stock for preparing silicon carbide ceramics and film, preparation method include: mechanical crushing method,
Sol-gel method, organic matter thermal decomposition method, vapor- phase synthesis reaction method SHS process, carbothermic method etc..Industry at present
Upper prepared silicon carbide powder is mostly particle in irregular shape, has sharp corner angle, poor fluidity.In silicon carbide ceramics system
In product, due to the corner angle that silicon-carbide particle is sharp, causes the loading of silicon carbide powder to be restricted, reduce silicon carbide ceramics
The consistency of product influences its service performance, and as abrasive material in use, sharp corner angle also easily generate scratch.And it is spherical
Particle makes it in each side since its regular shape, good fluidity are easily dispersed, and due to the isotropism of spheric granules
Upward mechanics, electric property etc. are consistent, therefore the preparation of spherical carbide silicon materials industrially has particularly significant answer
With value.
Chinese patent 201310717301.1 uses spray granulation using silicon carbide micro-powder as raw material, is added a certain amount of viscous
Agent is tied, is granulated at high temperature, but gained silicon-carbide particle sphericity is not high.Chinese patent 201510473646.6 uses benzene
Phenol, alkali and formaldehyde prepare performed polymer, obtain thin-film material after performed polymer, high polymer templates, formaldehyde, TEOS are mixed drying,
Thin-film material is heat-treated to obtain spherical carbide silicon, but gained spherical carbide silicon is easy to rupture.Chinese patent
201510487102.5 use carbonaceous mesophase spherules green-ball and silicon powder, obtain after mixing, drying, molding, sintering by spherical shape
The block of silicon-carbide particle composition obtains porous silicon carbide microsphere powder after further decarburization, broken, sieving, but technique is more
It is complicated and need to consume more energy.And in report disclosed above, preparation-obtained spherical carbide Si powder partial size
In the micron-scale.And in actual application, the size of silicon-carbide particle is applied to large effect, therefore is prepared
No matter the controllable spherical carbide silicon particle of granularity is to silicon carbide articles or polishing powder is all necessary.
Summary of the invention
The present invention provides a kind of preparation of micro/nano level spherical carbide silicon materials for deficiency existing for existing technology of preparing
Method.The carbon ball of size tunable is obtained after hydro-thermal reaction using different organic carbon sources, gained carbon ball is as template and silicon
After powder mixes in proportion, reaction product 1 is prepared by high temperature solid state reaction, reaction product 1 obtains after decarburization, gravity separation method
To the higher spherical carbide silicon materials of pattern uniformity.One aspect of the present invention by the selection of organic carbon source and surfactant,
The regulation of the partial size of spherical carbide silicon is realized in the regulation of hydrothermal reaction condition；On the other hand regulate and control the ratio of carbon ball and silicon powder partial size
Value and use gravity separation method obtain the higher spherical carbide silicon materials of pattern uniformity.
The technical solution adopted in the present invention is as follows:
Step 1: organic carbon source is soluble in water according to the concentration of 0.1~1mol/L, according to organic carbon source quality
0.1%~5% addition surfactant, obtains uniform mixed solution after stirring；
Step 2: mixed solution is placed in hydrothermal reaction kettle according to certain loading, hydro-thermal reaction is carried out, using second
Alcohol is repeatedly washed and is dried to products therefrom, and carbon ball is obtained；
Step 3: carbon ball is mixed with silicon powder according to certain molar ratio, pressed in high pure nitrogen or ar gas environment
High temperature solid state reaction is carried out according to certain temperature increasing schedule, obtains reaction product 1；
Step 4: reaction product 1 to be aoxidized to 4 hours progress carbonization treatments at 700 DEG C, the powder after carbonization treatment is used
Gravity separation method obtains the relatively narrow spherical carbide silicon materials of particle diameter distribution.
Further, in step 1, the organic carbon source can be glucose, sucrose, maltose, fructose, starch, ring paste
The combination of one or more of essence, resin.
Further, in step 1, the surfactant is oleic acid, calgon, Sodium Polyacrylate, dodecyl
One of benzene sulfonic acid sodium salt, cetyltrimethylammonium bromide.
Further, in step 2, the loading is 10%~60vol%.
Further, in step 2, the heating rate of the hydro-thermal reaction is 1~10 DEG C/min, reaction temperature is 160~
240 DEG C, the reaction time is 2~72 hours.
Further, in step 3, the ratio of the carbon ball and silicon powder partial size is (0.01~1): 1.
Further, in step 3, the molar ratio of the carbon ball and silicon powder is (0.1~2): 1.
Further, in step 3, the temperature increasing schedule is to be warming up to 600~900 DEG C first with 1~20 DEG C/min, is protected
Then temperature 2~6 hours is warming up to 1100~1700 DEG C with 1~10 DEG C/min, keep the temperature 0.5~4 hour, last 1~5 DEG C/min
It is down to room temperature.
Further, in step 4, the technique of gravity separation method is the concentration point by the powder after decarburization according to 20~200g/L
It dissipates and is settled in water, take supernatant liquid after sedimentation, obtain spherical carbide Si powder after dry, needed for the liquid level of every 10cm high
The sedimentation time wanted is 1~30min.
The invention has the benefit that
1, the partial size for regulating and controlling carbon ball by regulation organic carbon source, surfactant, hydrothermal condition, realizes spherical carbide silicon
The regulation of partial size；
2, the higher spherical shape of pattern uniformity is obtained by regulation carbon ball with the ratio of silicon powder partial size and using gravity separation method
Carbofrax material；
3, prepared spherical carbide silicon materials sphericity is higher, and size tunable system, to tens microns, is shown in several hundred nanometers
Write the mobility for improving silicon carbide powder；
4, the preparation process is simple and quick, can be combined in batches.
Detailed description of the invention
Fig. 1 implementation flow chart of the present invention.
Fig. 2 is the XRD object phase result of spherical carbide silicon materials prepared in embodiment 1.
Fig. 3 is the Flied emission scanning mirror photo of spherical carbide silicon materials prepared in embodiment 1.
Fig. 4 is the low magnification Flied emission scanning mirror photo of spherical carbide silicon materials prepared in embodiment 4.
Fig. 5 is the high-amplification-factor Flied emission scanning mirror photo of spherical carbide silicon materials prepared in embodiment 4.
Specific embodiment
Clear and complete description is done to the present invention with reference to the accompanying drawing, so that those skilled in the art is not needing to make
Under conditions of creative work, it can sufficiently implement the present invention.
A specific embodiment of the invention is as follows:
Embodiment 1
A kind of preparation method of micro/nano level spherical carbide silicon materials, comprising the following steps: (1) by glucose according to
The concentration of 0.4mol/L is soluble in water, adds oleic acid according to the 1% of organic carbon source quality, is uniformly mixed after stirring molten
Liquid；(2) mixed solution is placed in hydrothermal reaction kettle according to loading 60%, carry out hydro-thermal reaction, heating rate be 10 DEG C/
Min, reaction temperature are 220 DEG C, and the reaction time is 4 hours, and products therefrom is repeatedly washed and dried using ethyl alcohol；(3)
Carbon ball is mixed with silicon powder according to molar ratio 2:1, wherein the ratio of carbon ball and silicon powder partial size is 0.01:1, in high-purity argon gas
In environment, 900 DEG C are warming up to using 10 DEG C/min first, keeps the temperature 2 hours, is then warming up to 1500 DEG C with 3 DEG C/min, heat preservation 2
Hour, last 4 DEG C/min is down to room temperature, obtains reaction product 1；(4) reaction product 1 is aoxidized 4 hours at 700 DEG C and is taken off
Carbon processing, the powder after decarburization are dispersed in water according to the concentration of 20g/L, are taken supernatant liquid after settling 5min, are obtained after dry
The relatively narrow spherical carbide silicon materials of particle diameter distribution.The main component of prepared sample is as shown in Fig. 2, be the silicon carbide of beta crystal, field
Emit electromicroscopic photograph as shown in figure 3, the partial size of spherical carbide silicon is about 300nm.
Embodiment 2
A kind of preparation method of micro/nano level spherical carbide silicon materials, comprising the following steps: (1) by maltose according to
The concentration of 1mol/L is soluble in water, adds Sodium Polyacrylate according to the 5% of maltose quality, is uniformly mixed after stirring molten
Liquid；(2) mixed solution being placed in hydrothermal reaction kettle according to loading 0.1, carries out hydro-thermal reaction, heating rate is 5 DEG C/min,
Reaction temperature is 100 DEG C, and the reaction time is 72 hours, and products therefrom is repeatedly washed and dried using ethyl alcohol；(3) by carbon
Ball is mixed with silicon powder according to molar ratio 1:1, and wherein the ratio of carbon ball and silicon powder partial size is 1:1, in high-purity argon gas environment,
600 DEG C are warming up to using 20 DEG C/min first, keeps the temperature 6 hours, is then warming up to 1700 DEG C with 2 DEG C/min, keeps the temperature 0.5 hour,
Last 2 DEG C/min is down to room temperature, obtains reaction product 1；(4) reaction product 1 is aoxidized at 700 DEG C at progress decarburization in 4 hours
Reason, the powder after decarburization are dispersed in water according to the concentration of 100g/L, are taken supernatant liquid after settling 15min, are obtained grain after dry
The spherical carbide silicon materials of diameter narrow distribution.
Embodiment 3
A kind of preparation method of micro/nano level spherical carbide silicon materials, comprising the following steps: (1) by fructose according to
The concentration of 0.1mol/L is soluble in water, adds neopelex according to the 3% of fructose quality, obtains after stirring uniform
Mixed solution；(2) mixed solution is placed in hydrothermal reaction kettle according to loading 0.4, carries out hydro-thermal reaction, heating rate 2
DEG C/min, reaction temperature is 240 DEG C, and the reaction time is 2 hours, and products therefrom is repeatedly washed and dried using ethyl alcohol；
(3) carbon ball is mixed with silicon powder according to molar ratio 0.1:1, wherein the ratio of carbon ball and silicon powder partial size is 0.5:1, high-purity
In nitrogen environment, 700 DEG C are warming up to using 15 DEG C/min first, 4 hours is kept the temperature, is then warming up to 1300 DEG C with 10 DEG C/min,
Heat preservation 3 hours, last 5 DEG C/min is down to room temperature, obtains reaction product 1；(4) it is small that above-mentioned reaction product is aoxidized to 4 at 700 DEG C
Shi Jinhang carbonization treatment, the powder after decarburization are dispersed in water according to the concentration of 50g/L, take supernatant liquid after settling 10min, are done
The relatively narrow spherical carbide silicon materials of particle diameter distribution are obtained after dry.
Embodiment 4
A kind of preparation method of micro/nano level spherical carbide silicon materials, comprising the following steps: (1) by starch according to
The concentration of 0.3mol/L is soluble in water, adds calgon according to the 1% of starch quality, is uniformly mixed after stirring molten
Liquid；(2) mixed solution being placed in hydrothermal reaction kettle according to loading 0.2, carries out hydro-thermal reaction, heating rate is 1 DEG C/min,
Reaction temperature is 200 DEG C, and the reaction time is 10 hours, and products therefrom is repeatedly washed and dried using ethyl alcohol；(3) by carbon
Ball is mixed with silicon powder according to molar ratio 0.5:1, and wherein the ratio of carbon ball and silicon powder partial size is 0.3:1, in High Purity Nitrogen compression ring
In border, 800 DEG C are warming up to using 10 DEG C/min first, keeps the temperature 3 hours, is then warming up to 1600 DEG C with 3 DEG C/min, heat preservation 1 is small
When, last 1 DEG C/min is down to room temperature, obtains reaction product 1；(4) above-mentioned reaction product is aoxidized 4 hours at 700 DEG C and is carried out
Carbonization treatment, the powder after decarburization are dispersed in water according to the concentration of 200g/L, supernatant liquid are taken after settling 30min, after dry
Obtain the relatively narrow spherical carbide silicon materials of particle diameter distribution.The Flied emission electromicroscopic photograph of prepared sample is as shown in Figure 4 and Figure 5, institute
The obtained spherical carbide silicon materials overwhelming majority is spherical carbide silicon particle, and the uniformity of pattern is higher, spherical carbide silicon grain diameter
About 7 μm.
Embodiment 5
A kind of preparation method of micro/nano level spherical carbide silicon materials, comprising the following steps: (1) by grape sugar and starch
(molar ratio 2:1) is soluble in water according to the concentration of 0.3mol/L, according to 3% addition hexa metaphosphoric acid of glucose and starch quality
Sodium obtains uniform mixed solution after stirring；(2) mixed solution is placed in hydrothermal reaction kettle according to loading 0.5, carries out water
Thermal response, heating rate are 6 DEG C/min, and reaction temperature is 180 DEG C, and the reaction time is 24 hours, using ethyl alcohol to products therefrom
It is repeatedly washed and is dried；(3) carbon ball is mixed with silicon powder according to molar ratio 0.4:1, wherein carbon ball and silicon powder partial size
Ratio be 0.7:1, in high pure nitrogen environment, be warming up to 800 DEG C using 10 DEG C/min first, keep the temperature 2.5 hours, then with
7 DEG C/min is warming up to 1400 DEG C, keeps the temperature 2.5 hours, last 3 DEG C/min is down to room temperature, obtains reaction product 1；It (4) will be above-mentioned anti-
Product is answered to aoxidize 4 hours progress carbonization treatments at 700 DEG C, the powder after decarburization is dispersed in water according to the concentration of 80g/L, is sunk
Supernatant liquid is taken after drop 5min, obtains the relatively narrow spherical carbide silicon materials of particle diameter distribution after dry.
Presently preferred embodiments of the present invention is described above, it should be pointed out that the invention is not limited to above-mentioned
Particular implementation, devices and structures not described in detail herein should be understood as gives reality with the common mode in this field
It applies；Anyone skilled in the art, without departing from the scope of the technical proposal of the invention, technology according to the present invention
Essence any simple modifications, equivalents, and modifications made to the above embodiment still fall within technical solution of the present invention protection
In the range of.
Claims (3)
1. a kind of preparation method of micro/nano level spherical carbide silicon materials, which comprises the following steps:
Step 1: organic carbon source is soluble in water according to the concentration of 0.1~1mol/L, according to the 0.1~5% of organic carbon source quality
Surfactant is added, uniform mixed solution is obtained after stirring；
Step 2: mixed solution is placed in hydrothermal reaction kettle according to certain loading, hydro-thermal reaction is carried out, using ethyl alcohol pair
Products therefrom is repeatedly washed and is dried, and carbon ball is obtained；
Step 3: carbon ball is mixed with silicon powder according to certain molar ratio, pressed in high pure nitrogen, argon gas or vacuum environment
High temperature solid state reaction is carried out according to certain temperature increasing schedule, obtains reaction product 1；
Step 4: reaction product 1 to be aoxidized to 4 hours progress carbonization treatments at 700 DEG C, the powder after carbonization treatment uses gravity treatment
Method obtains the relatively narrow spherical carbide silicon materials of particle diameter distribution；
In step 1, the organic carbon source is one of glucose, sucrose, maltose, fructose, starch, cyclodextrin, resin
Or several combinations；
In step 1, the surfactant is oleic acid, in calgon, Sodium Polyacrylate, neopelex
One kind；
In step 2, the loading is 10%~60vol%；
In step 2, the heating rate of the hydro-thermal reaction is 1~10 DEG C/min, and reaction temperature is 100~240 DEG C, reaction
Time is 2~72 hours；
In step 3, the ratio of the carbon ball and silicon powder partial size is (0.01~1): 1；
In step 3, the molar ratio of the carbon ball and silicon powder is (0.1~2): 1.
2. a kind of preparation method of micro/nano level spherical carbide silicon materials according to claim 1, which is characterized in that step
In three, the temperature increasing schedule is to be warming up to 600~900 DEG C first with 1~20 DEG C/min, keeps the temperature 2~6 hours, then with 1~
10 DEG C/min is warming up to 1100~1700 DEG C, keeps the temperature 0.5~4 hour, last 1~5 DEG C/min is down to room temperature.
3. a kind of preparation method of micro/nano level spherical carbide silicon materials according to claim 1, which is characterized in that step
In four, the technique of the gravity separation method is to be dispersed in water the powder after decarburization according to the concentration of 20~200g/L to sink
Drop, takes supernatant liquid after sedimentation, obtain spherical carbide Si powder after dry, and the sedimentation time required for the liquid level of every 10cm high is
1~30min.
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| CN109502590B (en) * | 2018-11-23 | 2020-07-03 | 山东天岳先进材料科技有限公司 | Method for improving yield of silicon carbide powder |
| CN110003536A (en) * | 2019-02-20 | 2019-07-12 | 谭美英 | A kind of preparation method of heat-dissipation type wear-resistant rubber material |
| CN112794302A (en) * | 2019-11-14 | 2021-05-14 | 中国科学院大连化学物理研究所 | Spherical carbon material and preparation method thereof |
| CN111392728B (en) * | 2020-02-28 | 2022-04-08 | 山东天岳先进科技股份有限公司 | Raw material for producing silicon carbide crystal and preparation method and application thereof |
| CN111704139A (en) * | 2020-06-29 | 2020-09-25 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Preparation method of high-purity silicon carbide powder |
| CN111995406A (en) * | 2020-08-10 | 2020-11-27 | 裴小罗 | SiC wear-resistant refractory material based on nano carbon material modification |
| CN114105120A (en) * | 2020-08-28 | 2022-03-01 | 中国科学院大连化学物理研究所 | Preparation method and application of small-size carbon sphere material |
| CN112876281B (en) * | 2021-01-28 | 2022-06-03 | 哈尔滨工业大学（威海） | Preparation method and application of biological ceramic support with hollow microsphere surface micro-nano structure |
| CN113415798B (en) * | 2021-05-12 | 2023-02-24 | 江西农业大学 | Preparation method of phosphorus-doped microporous, mesoporous and macroporous coexisting grade pore structure carbon nanospheres |
| RU2767270C1 (en) * | 2021-08-25 | 2022-03-17 | Кирилл Борисович ИГНАТЬЕВ | Method for obtaining silicon carbide |
| CN114368970B (en) * | 2022-01-12 | 2022-12-06 | 西北工业大学 | Submicron ZrC-SiC composite ceramic microsphere and preparation method thereof |
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| CN102897763B (en) * | 2012-10-08 | 2014-08-13 | 北京科技大学 | Low-temperature rapid synthesis method of alpha-SiC micropowder |
| CN105347328A (en) * | 2015-12-06 | 2016-02-24 | 杭州飞山浩科技有限公司 | Method for preparing monodisperse carbon microspheres by using cane sugar as carbon source |
| CN105417541A (en) * | 2015-12-22 | 2016-03-23 | 中国电子科技集团公司第二研究所 | Method for preparing high-purity silicon carbide powder |
| CN107721429B (en) * | 2017-11-15 | 2020-02-21 | 中国科学院福建物质结构研究所 | Zirconium carbide-silicon carbide composite powder material and preparation method thereof |
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