CN108059133A - Nano-silicon nitride and preparation method thereof - Google Patents
Nano-silicon nitride and preparation method thereof Download PDFInfo
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- CN108059133A CN108059133A CN201711311855.6A CN201711311855A CN108059133A CN 108059133 A CN108059133 A CN 108059133A CN 201711311855 A CN201711311855 A CN 201711311855A CN 108059133 A CN108059133 A CN 108059133A
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/068—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with silicon
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Abstract
The invention belongs to inorganic compound field of nanometer material technology, and in particular to a kind of nano-silicon nitride and preparation method thereof, the nano-silicon nitride and preparation method thereof are that silicate is carried out ball-milling treatment, obtain powdered silicate；According to mass ratio it is 1 by obtained powdered silicate and magnesium powder, magnesium chloride, ammonium chloride：(0.6‑1)：(3‑5)：(0.6 1.8) it is uniformly mixed and obtains mixture, then obtained mixture is heated to 800 1000 DEG C of 6 18h of heat preservation with the heating rate of 8 20 DEG C/min again, mixture after being reacted after cooling, the mixture after obtained reaction carry out pickling, nano-silicon nitride are obtained after pickling.
Description
Technical field
The invention belongs to inorganic compound field of nanometer material technology, more particularly to a kind of nano-silicon nitride and its preparation side
Method.
Technical background
Silicon nitride is a kind of advanced engineering ceramics and semi-conducting material, the material have high room temperature and elevated temperature strength,
High rigidity, resistance to abrasion, inoxidizability and good heat shock resistance and mechanical shock performance, by material supply section, educational circles is considered structure
High comprehensive performance in ceramic field, be most hopeful to substitute nickel-base alloy obtained in high-tech, high-temperature field it is widely applied
A kind of new material.For example, Si3N4Whisker is due to its excellent high temperature resistant, high-modulus, high intensity, low-expansion coefficient and good
Thermal stability and chemical stability can be used as constituent element to add in plastic substrate, metallic matrix and ceramic matrix, play enhancing, increase
Tough effect, it is considered to be the preferable constituent element of enhancing light metal and ceramic material receives increasing attention；Si3N4Nano wire is excellent
Semi-conducting material is the ideal material for preparing high-temperature nano device, has extraordinary application prospect.
It is well known that Si3N4There are two types of crystal forms, i.e. α-Si3N4With β-Si3N4.The preparation side of silicon nitride nano structural material
Method has very much, common are sol-gel method, silica flour direct nitridation method, carbon thermal reduction titanium dioxide silicon process, organo-silicon compound ammonia
Solution, combustion synthesis method, chemical vapour deposition technique etc..Such as Chinese patent (notification number：1134404) disclose it is a kind of prepare α-
Si3N4The method of whisker.This method uses the SiO 2 powder of appropriate granularity as raw material, in the nitrogen atmosphere of certain pressure
Under, through directly reaction generation crystal structure is complete between 1200 DEG C -1600 DEG C, list of excellent surface quality in crystal vessel
Brilliant α-Si3N4Whisker；Chinese patent (notification number：CN1092825A) also disclose and a kind of prepare zero defect Si3N4The side of whisker
Method.It with silicon tetrachloride is silicon source that this method, which is, and ammonia makees nitrogen source, and the two at room temperature, is reacted in alumina reaction tube.
Then reactant in high temperature furnace is heated, and is gradually heating to 1100 DEG C or more, nitridation is generated after product amides deamination
Silicon superfine powder is finally warming up to 1400 DEG C -1480 DEG C, when constant temperature 1-3 is small, obtains Si3N4Whisker.Due to the nitridation of special appearance
Silicon nanostructure material has great scientific value and potential application prospect, therefore for special appearance silicon nitride nano knot
It synthesizes structure material, has caused the great interest of people.Due to preparing the method for silicon nitride nano-material above-mentioned, have
Used raw material is toxic, the price that has costly, the harsher and made Si of the reaction condition that has3N4It is pure
Degree is not high, affects its performance, has certain limitation.
The content of the invention
For the disadvantages described above or Improvement requirement of the prior art, received the present invention provides one kind by raw material preparation of silicate
The method of rice silicon nitride and the nano-silicon nitride that is obtained by this method, its object is to by with silicate powder powder stock,
Using ammonium chloride as nitrogen source, using magnesium chloride as fused salt, reacted under glass melting state, nanometer most is prepared through pickling afterwards
Thus silicon nitride solves prior art nanometer, nitridation silicon preparation method severe reaction conditions, of high cost, porous structure and is not easy to obtain
Or the technical problems such as structural instability.
To achieve the above object, one side according to the invention provides a kind of preparation method of nano-silicon nitride, should
Method includes the following steps：
(1) silicate is subjected to ball-milling treatment, obtains powdered silicate；
(2) the powdered silicate for obtaining step (1) is 1 according to mass ratio with magnesium powder, magnesium chloride, ammonium chloride：
(0.6-1)：(3-5)：(0.6-1.8) is uniformly mixed and obtains mixture；
(3) mixture for obtaining step (2) is heated to 800-1000 DEG C of heat preservation 6- with the heating rate of 8-20 DEG C/min
18h, the mixture after being reacted after cooling；
(4) mixture after the reaction for obtaining step (3) carries out pickling, and nano-silicon nitride is obtained after pickling.
In a preferred embodiment, the silicate is sodium metasilicate or calcium silicates, it is further preferred that the silicate is
Sodium metasilicate.
In a preferred embodiment, powdered silicate granularity described in step (1) is ＜ 0.74mm, further preferably
Ground, the powdered silicate granularity are ＜ 0.55mm.
In a preferred embodiment, which is characterized in that the granularity of the magnesium powder is 0.035-0.05mm, specific described
The granularity of magnesium powder can be 0.035mm, 0.037mm, 0.039mm, 0.041mm, 0.043mm, 0.045mm, 0.047mm, 0.05mm
And any number in the scope that is formed of any two in these numerical value.
In a preferred embodiment, the purity of the ammonium chloride is ＞ 99.5%.
In a preferred embodiment, the acid pickling step is specially：First cleaned in hydrochloric acid, it is then clear in hydrofluoric acid
It washes.It is further preferred that the pH value of the hydrochloric acid is 3-5, the pH value of the hydrofluoric acid is 4-6.
On the other hand the present invention also provides a kind of nano-silicon nitride, the nano-silicon nitride is based on above-mentioned nano-silicon nitride
Preparation method is made.
In a preferred embodiment, the aperture of the nano-silicon nitride is 16-80nm, the specific nano-silicon nitride
Aperture for 16nm, 20nm, 24nm, 28nm, 32nm, 36nm, 40nm, 44nm, 48nm, 52nm, 56nm, 60nm, 64nm, 68nm,
Any number in the scope that any two in 72nm, 76nm, 80nm and these numerical value is formed.
In a preferred embodiment, the granularity of the nano-silicon nitride is 6-18nm, it is further preferred that the nanometer nitrogen
The granularity of SiClx is 8-12nm.
In a preferred embodiment, the specific surface area of the nano-silicon nitride is 160-240m2/ g, it is further preferred that
The specific surface area of the nano-silicon nitride is 200-220m2/g。
In general, by the above technical scheme conceived by the present invention compared with prior art, it can obtain down and show
Beneficial effect：
(1) present invention prepares nano-silicon nitride by raw material of silicate, and silicate is of low cost, is a kind of of high quality and at a reasonable price
Nano-silicon nitride raw materials for production；
(2) present invention prepares the nano-si 3 n 4 ceramics of high added value using silicate and ammonium chloride as starting material, both
Can considerable economic benefits can be brought with environmental protection again, the potentiality with sustainable development, product high-purity nm silicon nitride
With being widely applied very much；
(3) each step cooperative cooperating of the preparation method of nano-silicon nitride of the present invention constitutes a set of independent technical solution,
Excellent nano-silicon nitride has been prepared.The present invention selects silicate as raw material, using magnesium chloride as fused salt, since the two exists
It is molten state between 800-1000 DEG C, can so realizes that molten state is reacted, while is realized using ammonium chloride as nitrogen source
Good mass transfer, and silicate utilizes reactive liquid solution mass-and heat-transfer, ingredient point in itself due to containing the symbiosis such as sodium, calcium wherein
The uniform advantage of cloth so that sodium, the oxide of calcium and fused salt are uniformly distributed in reaction product, with the formal distribution of three-dimensional perforation
In the product, finally by pickling reaction product, nano-silicon nitride has been obtained.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph for the silicon nitride nano particles that the embodiment of the present invention 1 is prepared；
Fig. 2 is the transmission electron microscope picture for the silicon nitride nano particles that the embodiment of the present invention 1 is prepared；
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, it is right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Conflict is not formed each other to can be combined with each other.
Present embodiment discloses a kind of preparation methods of nano-silicon nitride, and this method comprises the following steps：
(1) silicate is subjected to ball-milling treatment, obtains powdered silicate；
(2) the powdered silicate for obtaining step (1) is 1 according to mass ratio with magnesium powder, magnesium chloride, ammonium chloride：
(0.6-1)：(3-5)：(0.6-1.8) is uniformly mixed and obtains mixture；
(3) mixture for obtaining step (2) is heated to 800-1000 DEG C of heat preservation 6- with the heating rate of 8-20 DEG C/min
18h, the mixture after being reacted after cooling；
(4) mixture after the reaction for obtaining step (3) carries out pickling, and nano-silicon nitride is obtained after pickling.
The present embodiment also discloses a kind of nano-silicon nitride, and method of the nano-silicon nitride based on the present embodiment is made.
It is embodiment below：
Embodiment 1
A kind of preparation method of nano-silicon nitride, carries out in accordance with the following steps：
(1) 5g sodium metasilicate is subjected to ball-milling treatment, obtains powdered silicate；
(2) the powdered sodium metasilicate for obtaining step (1) is 1 according to mass ratio with magnesium powder, magnesium chloride, ammonium chloride：
0.6：3：0.6 be uniformly mixed obtain mixture；
(3) mixture for obtaining step (2) is heated to 800 DEG C of heat preservation 6h with the heating rate of 8 DEG C/min, after cooling
Mixture after to reaction；
(4) for the mixture after the reaction for obtaining step (3) successively in the hydrochloric acid that pH value is 3, pH value is in 4 hydrofluoric acid
Carry out pickling.
It is embodiment 1 based on nano-silicon nitride made from the present embodiment method
Phenetic analysis is carried out to the nano silicon nitride silicon particle being prepared：
From the scanning electron microscope (SEM) photograph of Fig. 1, the silicon nitride that embodiment 1 is prepared belongs to the silicon nitride of Nano grade.
From the transmission electron microscope picture of Fig. 2, silicon nitride product that embodiment 1 is prepared has excellent pore passage structure and whole
Body structure is not destroyed, and is connected with each other between nano silicon nitride silicon particle, has hole, porous silicon nitride between nano silicon nitride silicon particle
Specific surface area be 220m2/ g, for pore-size distribution between 16-80nm, the silicon nitride of the method synthesis has the specific surface of superelevation
Product and excellent pore structure, therefore the nano-silicon nitride of the present invention industrially can be mass produced and applied.
Embodiment 2
A kind of preparation method of nano-silicon nitride, carries out in accordance with the following steps：
(1) 5g sodium metasilicate is subjected to ball-milling treatment, obtains powdered silicate；
(2) the powdered sodium metasilicate for obtaining step (1) is 1 according to mass ratio with magnesium powder, magnesium chloride, ammonium chloride：
0.7：3.6：0.8 be uniformly mixed obtain mixture；
(3) mixture for obtaining step (2) is heated to 850 DEG C of heat preservation 8h with the heating rate of 10 DEG C/min, after cooling
Mixture after being reacted；
(4) for the mixture after the reaction for obtaining step (3) successively in the hydrochloric acid that pH value is 3, pH value is in 5 hydrofluoric acid
Carry out pickling.
It is embodiment 2 based on nano-silicon nitride made from the present embodiment method.
Phenetic analysis is carried out to the nano silicon nitride silicon particle being prepared：
The silicon nitride product that embodiment 2 is prepared has excellent pore passage structure and overall structure is not destroyed, nanometer nitrogen
It is connected with each other between silicon carbide particle, there is hole, the specific surface area of silicon nitride is 200m between nano silicon nitride silicon particle2/ g, aperture
It is distributed between 16-80nm, the silicon nitride of the method synthesis has the specific surface area of superelevation and excellent pore structure, therefore this hair
Bright nano-silicon nitride industrially can be mass produced and applied.
Embodiment 3
A kind of preparation method of nano-silicon nitride, carries out in accordance with the following steps：
(1) 5g sodium metasilicate is subjected to ball-milling treatment, obtains powdered silicate；
(2) the powdered sodium metasilicate for obtaining step (1) is 1 according to mass ratio with magnesium powder, magnesium chloride, ammonium chloride：
0.8：4：1 be uniformly mixed obtain mixture；
(3) mixture for obtaining step (2) is heated to 880 DEG C of heat preservation 10h, cooling with the heating rate of 12 DEG C/min
Mixture after being reacted afterwards；
(4) for the mixture after the reaction for obtaining step (3) successively in the hydrochloric acid that pH value is 4, pH value is in 5 hydrofluoric acid
Carry out pickling.
It is embodiment 3 based on nano-silicon nitride made from the present embodiment method.
Phenetic analysis is carried out to the nano silicon nitride silicon particle being prepared：
The silicon nitride product that embodiment 3 is prepared has excellent pore passage structure and overall structure is not destroyed, nanometer nitrogen
It is connected with each other between silicon carbide particle, there is hole, the specific surface area of silicon nitride SiClx is 200m between nano silicon nitride silicon particle2/ g,
Pore-size distribution is between 16-80nm, and the silicon nitride of the method synthesis has the specific surface area of superelevation and excellent pore structure, therefore
The nano-silicon nitride of the present invention industrially can be mass produced and applied.
Embodiment 4
A kind of preparation method of nano-silicon nitride, carries out in accordance with the following steps：
(1) 5g sodium metasilicate is subjected to ball-milling treatment, obtains powdered silicate；
(2) the powdered sodium metasilicate for obtaining step (1) is 1 according to mass ratio with magnesium powder, magnesium chloride, ammonium chloride：
0.9：4：1.2 be uniformly mixed obtain mixture；
(3) mixture for obtaining step (2) is heated to 900 DEG C of heat preservation 12h, cooling with the heating rate of 14 DEG C/min
Mixture after being reacted afterwards；
(4) for the mixture after the reaction for obtaining step (3) successively in the hydrochloric acid that pH value is 3, pH value is in 5 hydrofluoric acid
Carry out pickling.
It is embodiment 4 based on nano-silicon nitride made from the present embodiment method.
Phenetic analysis is carried out to the nano silicon nitride silicon particle being prepared：
The silicon nitride product that embodiment 4 is prepared has excellent pore passage structure and overall structure is not destroyed, nanometer nitrogen
It is connected with each other between silicon carbide particle, there is hole, the specific surface area of silicon nitride is 210m between nano silicon nitride silicon particle2/ g, aperture
It is distributed between 16-80nm, the silicon nitride of the method synthesis has the specific surface area of superelevation and excellent pore structure, therefore this hair
Bright nano-silicon nitride industrially can be mass produced and applied.
Embodiment 5
A kind of preparation method of nano-silicon nitride, carries out in accordance with the following steps：
(1) 5g sodium metasilicate is subjected to ball-milling treatment, obtains powdered silicate；
(2) the powdered sodium metasilicate for obtaining step (1) is 1 according to mass ratio with magnesium powder, magnesium chloride, ammonium chloride：1：
4.8：1.6 be uniformly mixed obtain mixture；
(3) mixture for obtaining step (2) is heated to 950 DEG C of heat preservation 14h, cooling with the heating rate of 16 DEG C/min
Mixture after being reacted afterwards；
(4) for the mixture after the reaction for obtaining step (3) successively in the hydrochloric acid that pH value is 4, pH value is in 6 hydrofluoric acid
Carry out pickling.
It is embodiment 5 based on nano-silicon nitride made from the present embodiment method.
Phenetic analysis is carried out to the nano silicon nitride silicon particle being prepared：
The silicon nitride product that embodiment 5 is prepared has excellent pore passage structure and overall structure is not destroyed, nanometer nitrogen
It is connected with each other between silicon carbide particle, there is hole, the specific surface area of silicon nitride is 210m between nano silicon nitride silicon particle2/ g, aperture
It is distributed between 16-80nm, the silicon nitride of the method synthesis has the specific surface area of superelevation and excellent pore structure, therefore this hair
Bright nano-silicon nitride industrially can be mass produced and applied.
Finally it should be noted that the above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof, to the greatest extent
Pipe is described in detail the present invention with reference to above-described embodiment, and those of ordinary skill in the art still can be to this hair
Bright specific embodiment is modified or replaced equivalently, these without departing from the spirit and scope of the present invention any modification or
Person's equivalent substitution is being applied within pending claims.
Claims (10)
1. a kind of preparation method of nano-silicon nitride, which is characterized in that this method comprises the following steps：
(1) silicate is subjected to ball-milling treatment, obtains powdered silicate；
(2) the powdered silicate for obtaining step (1) is 1 according to mass ratio with magnesium powder, magnesium chloride, ammonium chloride：(0.6-
1)：(3-5)：(0.6-1.8) is uniformly mixed and obtains mixture；
(3) mixture for obtaining step (2) is heated to 800-1000 DEG C of heat preservation 6-18h with the heating rate of 8-20 DEG C/min,
Mixture after being reacted after cooling；
(4) mixture after the reaction for obtaining step (3) carries out pickling, and nano-silicon nitride is obtained after pickling.
2. the preparation method of nano-silicon nitride according to claim 1, which is characterized in that the silicate is sodium metasilicate or silicon
Sour calcium.
3. the preparation method of nano-silicon nitride according to claim 1, which is characterized in that powder described in the step (1)
The silicate granularity of shape is ＜ 0.74mm.
4. the preparation method of nano-silicon nitride according to claim 1, which is characterized in that the granularity of the magnesium powder is 0.035-
0.05mm。
5. the preparation method of nano-silicon nitride according to claim 1, which is characterized in that the purity of the ammonium chloride is ＞
99.5%.
6. the preparation method of nano-silicon nitride according to claim 1, which is characterized in that the acid pickling step is specially：First
It cleans in hydrochloric acid, is then cleaned in hydrofluoric acid.
7. a kind of nano-silicon nitride, which is characterized in that the nano-silicon nitride is based on any one institute in the claims 1-6
The preparation method for stating nano-silicon nitride is made.
8. nano-silicon nitride according to claim 7, which is characterized in that the aperture of the nano-silicon nitride is 16-80nm.
9. nano-silicon nitride according to claim 7, which is characterized in that the granularity of the nano-silicon nitride is 6-18nm.
10. nano-silicon nitride according to claim 7, which is characterized in that the specific surface area of the nano-silicon nitride is
160-240m2/g。
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| US20050080285A1 (en) * | 2003-10-10 | 2005-04-14 | Ziyun Wang | Monosilane or disilane derivatives and method for low temperature deposition of silicon-containing films using the same |
| CN104671795A (en) * | 2015-02-05 | 2015-06-03 | 武汉科技大学 | Single-phase alpha-Si3N4 micropowder and preparation method thereof |
| CN107140641A (en) * | 2017-05-09 | 2017-09-08 | 武汉科技大学 | A kind of method that three-dimensional porous silicon is prepared by raw material of silicate glass |
| CN107416837A (en) * | 2017-05-09 | 2017-12-01 | 武汉科技大学 | A kind of method that porous nano carborundum is prepared using silicate glass as raw material |
-
2017
- 2017-12-11 CN CN201711311855.6A patent/CN108059133A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050080285A1 (en) * | 2003-10-10 | 2005-04-14 | Ziyun Wang | Monosilane or disilane derivatives and method for low temperature deposition of silicon-containing films using the same |
| CN104671795A (en) * | 2015-02-05 | 2015-06-03 | 武汉科技大学 | Single-phase alpha-Si3N4 micropowder and preparation method thereof |
| CN107140641A (en) * | 2017-05-09 | 2017-09-08 | 武汉科技大学 | A kind of method that three-dimensional porous silicon is prepared by raw material of silicate glass |
| CN107416837A (en) * | 2017-05-09 | 2017-12-01 | 武汉科技大学 | A kind of method that porous nano carborundum is prepared using silicate glass as raw material |
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