CN106904583B - A kind of silicon nitride magnesium powder and preparation method thereof - Google Patents
A kind of silicon nitride magnesium powder and preparation method thereof Download PDFInfo
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- CN106904583B CN106904583B CN201710184755.5A CN201710184755A CN106904583B CN 106904583 B CN106904583 B CN 106904583B CN 201710184755 A CN201710184755 A CN 201710184755A CN 106904583 B CN106904583 B CN 106904583B
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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
- C01B21/0602—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 two or more other elements chosen from metals, silicon or boron
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Abstract
The present invention relates to a kind of silicon nitride magnesium powders and preparation method thereof.Its technical solution is：Using the inorganic salts of the magnesium powder of 10 ~ 15wt%, the silica of 15 ~ 25wt% and 65 ~ 75wt% as raw material, 0.5 ~ 1h is mixed；Then under the conditions of 0.1 ~ 1MPa and nitrogen atmosphere, medium temperature is warming up to the rate of 5 ~ 10 DEG C/min；Firing temperature is warming up to the rate of 3 ~ 5 DEG C/min again, keeps the temperature 1 ~ 7h, furnace cooling is washed, dry, and silicon nitride magnesium powder is made.Wherein：The firing temperature is 900 ~ 1300 DEG C, and the temperature difference of medium temperature and firing temperature is 100 ~ 200 DEG C.The present invention has the characteristics that simple production process, with short production cycle, raw material resources are enriched and low production cost；Prepared silicon nitride magnesium powder granule is uniform in size and pattern is single.
Description
Technical field
The invention belongs to silicon nitride magnesium technical fields.More particularly to a kind of silicon nitride magnesium powder and preparation method thereof.
Technical background
Silicon nitride magnesium has crystal structure similar with aluminium nitride, i.e., by Mg2+And Si4+Ion substitution Al3+Position.Nitrogen
SiClx magnesium material has higher theoretical thermal conductivity, has in the heat dissipation of high-power electric appliance and high speed circuit and encapsulating material field
Larger potentiality.In ceramic material field, silicon nitride magnesium is mainly as sintering aid, the thermal conductivity for improving silicon nitride ceramics.
In addition to this, silicon nitride magnesium also has higher stress intensity, fracture toughness, hardness and electrical insulating property, attracts more and more grind
The person of studying carefully is researched and developed and is improved to its synthetic method.
Currently, the synthetic method of silicon nitride magnesium is mainly direct nitridation method and carbothermic method.Early in 1969, foreign countries ground
The person of studying carefully is with regard to being prepared for silicon nitride magnesium powder using direct nitridation method and being studied product composition and microstructure.30 years
Afterwards, Japanese Uchida H et al.（Uchida H, Hatani K, Aizawa M, et a1. Preparation of
magnesiam silicon nitride by the carbothermal reduction technique. Advance
Powder Technology. 1999, 10(2): 133-143）With Mg (NO3)2With Si (OC2H5)4Carbon heat is used for raw material also
Former technology successfully prepares silicon nitride magnesium powder.2000, Zelanian Blair R H（R. G. Blmr. The thermal
conductivity of magnesium silicon nitride, MgSiN2, ceramics and related
materials, Eindhoven, The Netherlands, Eindhoven University of Technology,
2000: 177-120）The thermal conductivity of silicon nitride magnesium material is studied in detail in doctoral thesis.The country is to silicon nitride magnesium
Research work start from 2003, Peng Guihua（Peng Guihua, Jiang Guojian, Li Wen orchid self-spread high-temperature synthesizing silicon nitride magnesium powder
Body functional materials, 2004,35：3051-3053）With Mg+Si, Mg2Si and Mg+Si3N4For raw material, using self-propagating synthesis technology
It is prepared for silicon nitride magnesium powder, and the oxygen content and hydration resistance of product are detected.Peng Guihua is in self propagating high temperature
Synthesizing silicon nitride magnesium raw powder's production technology（ZL200410016198.9）In with magnesium powder and α-Si3N4For raw material, ammonium chloride or fluorine
Change ammonium and provides nitrogen source for additive for nitridation reaction.Wang Fei（Wang Fei add the rare gold of burning urea synthesizing silicon nitride magnesium powder body
Belong to material and engineering, 2008,37 (1)：505-508）It is additive in Mg-Si-N systems using urea using combustion synthesis technology
In be prepared for MgSiN2Powder.
Either direct nitridation method, carbothermic method or self-propagating synthesis technology all have the shortcomings that common, such as preparation
Period is long, energy consumption mostly and complex technical process.
Invention content
The present invention is directed to overcome prior art defect, and it is an object of the present invention to provide a kind of simple production process, with short production cycle, former
Expect resourceful and low production cost silicon nitride magnesium raw powder's production technology, prepared silicon nitride magnesium powder granule size
Uniformly, pattern is single.
To achieve the above object, the technical solution adopted in the present invention is：With the magnesium powder of 10 ~ 15wt%, 15 ~ 25wt% two
The inorganic salts of silica and 65 ~ 75wt% are raw material, mix 0.5 ~ 1h；Then under the conditions of 0.1 ~ 1MPa and nitrogen atmosphere, with 5 ~
The rate of 10 DEG C/min is warming up to medium temperature；Firing temperature is warming up to the rate of 3 ~ 5 DEG C/min again, 1 ~ 7h is kept the temperature, with stove
It is cooling, it washs, it is dry, silicon nitride magnesium powder is made.
The firing temperature is 900 ~ 1300 DEG C, and the temperature difference of medium temperature and firing temperature is 100 ~ 200 DEG C.
The Mg contents of the magnesium powder are 90 ~ 99wt%, and the granularity of the magnesium powder is one in 0.02 ~ 44 μm and 44 ~ 88 μm
Kind.
The SiO of the silicon dioxide powder2Content is 85 ~ 99wt%, and the granularity of the silicon dioxide powder is 44 ~ 74 μm, 0.02
One kind in ~ 44 μm and≤0. 02 μm.
The inorganic salts be sodium chloride, potassium chloride, lithium chloride, magnesium chloride, sodium fluoride and potassium fluoride in one kind, two kinds or
Three kinds.
Solution used in the washing is one kind in hydrochloric acid, sulfuric acid and nitric acid, a concentration of 1mol/ of the cleaning fluids
L。
Due to the adoption of the above technical scheme, the present invention has following good effect compared with prior art：
The present invention prepares nitridation using abundant silica and magnesium powder as raw material, using fused salt auxiliary magnesiothermic reduction nitriding
Silicon magnesium powder body, makes the cost of raw material substantially reduce.Fused salt auxiliary magnesiothermic reduction nitriding prepares silicon nitride magnesium powder can be relatively low
Temperature and short period complete, also with the short advantage of simple production process and period.
The magnesium that the present invention uses i.e. fusible formation liquid magnesium, magnesium during entire reduction nitridation under the conditions of 650 DEG C
Reaction is participated in the form of liquid and gaseous, the enthalpy of system significantly increases, and significantly reduces the initial temperature of reaction.Due to magnesium
The a large amount of heat of thermal reduction reaction process releasing, reaction are not necessarily to the spontaneous progress of extraneous offer energy response energy after starting, and
Higher system reaction temperature can be reached at a lower temperature.The present invention is assisted using fused salt, and preparation process is not required to
Want special equipment, inorganic salts melt to form ion melt at lower temperature, significantly improve reactant mass transfer velocity and
Particle agglomeration is effectively prevented, obtained powder granule is uniform in size, and pattern is single.
Therefore, the present invention has simple production process, with short production cycle, raw material resources abundant and the spy of low production cost
Point；Prepared silicon nitride magnesium powder granule is uniform in size and pattern is single.
Description of the drawings
Fig. 1 is a kind of SEM figures of silicon nitride magnesium powder prepared by the present invention.
Specific implementation mode
The invention will be further described with reference to the accompanying drawings and detailed description, not to the limit of its protection domain
System.
In present embodiment：The Mg contents of the magnesium powder are 90 ~ 99wt%；The SiO of the silicon dioxide powder2Content
For 85 ~ 99wt%；A concentration of 1mol/L of the cleaning fluids.It is repeated no more in embodiment.
Embodiment 1
A kind of silicon nitride magnesium powder and preparation method thereof.With the magnesium powder of 8 ~ 13wt%, the silica of 15 ~ 18wt% and 71 ~
The inorganic salts of 75wt% are raw material, mix 0.5 ~ 1h；Then under the conditions of 0.1 ~ 1MPa and nitrogen atmosphere, with 5 ~ 10 DEG C/min's
Rate is warming up to medium temperature；Firing temperature is warming up to the rate of 3 ~ 5 DEG C/min again, keeps the temperature 1 ~ 7h, furnace cooling is washed,
It is dry, silicon nitride magnesium powder is made.
The firing temperature is 900 ~ 1100 DEG C, and the temperature difference of medium temperature and firing temperature is 100 ~ 160 DEG C.
The granularity of the magnesium powder is 0.02 ~ 44 μm.
The granularity of the silicon dioxide powder is 44 ~ 74 μm.
The inorganic salts are sodium chloride.
Solution used in the washing is hydrochloric acid.
Embodiment 2
A kind of silicon nitride magnesium powder and preparation method thereof.Remaining is the same as embodiment 1 in addition to following：
The granularity of the silicon dioxide powder is 0.02 ~ 44 μm.
The inorganic salts are potassium chloride.
Solution used in the washing is sulfuric acid.
Embodiment 3
A kind of silicon nitride magnesium powder and preparation method thereof.Remaining is the same as embodiment 1 in addition to following：
The granularity of the silicon dioxide powder≤0. 02 μm.
The inorganic salts are the mixture of sodium fluoride and potassium fluoride.
Solution used in the washing is nitric acid.
Embodiment 4
A kind of silicon nitride magnesium powder and preparation method thereof.Remaining is the same as embodiment 1 in addition to following：
The granularity of the magnesium powder is 44 ~ 88 μm.
The inorganic salts are the mixture of lithium chloride and magnesium chloride.
Embodiment 5
A kind of silicon nitride magnesium powder and preparation method thereof.Remaining is the same as embodiment 1 in addition to following：
The granularity of the magnesium powder is 44 ~ 88 μm.
The granularity of the silicon dioxide powder is 0.02 ~ 44 μm.
The inorganic salts are the mixture of lithium chloride, magnesium chloride and sodium fluoride.
Solution used in the washing is sulfuric acid.
Embodiment 6
A kind of silicon nitride magnesium powder and preparation method thereof.Remaining is the same as embodiment 1 in addition to following：
The granularity of the magnesium powder is 44 ~ 88 μm.
The granularity of the silicon dioxide powder≤0. 02 μm.
The inorganic salts are the mixture of potassium chloride, lithium chloride and magnesium chloride.
Solution used in the washing is nitric acid.
Embodiment 7
A kind of silicon nitride magnesium powder and preparation method thereof.With the magnesium powder of 9 ~ 14wt%, the silica of 18 ~ 22wt% and 68 ~
The inorganic salts of 71wt% are raw material, mix 0.5 ~ 1h；Then under the conditions of 0.1 ~ 1MPa and nitrogen atmosphere, with 5 ~ 10 DEG C/min's
Rate is warming up to medium temperature；Firing temperature is warming up to the rate of 3 ~ 5 DEG C/min again, keeps the temperature 1 ~ 7h, furnace cooling is washed,
It is dry, silicon nitride magnesium powder is made.
The firing temperature is 1000 ~ 1200 DEG C, and the temperature difference of medium temperature and firing temperature is 120 ~ 180 DEG C.
The granularity of the magnesium powder is 0.02 ~ 44 μm.
The granularity of the silicon dioxide powder is 44 ~ 74 μm.
The inorganic salts are lithium chloride.
Solution used in the washing is hydrochloric acid.
Embodiment 8
A kind of silicon nitride magnesium powder and preparation method thereof.Remaining is the same as embodiment 7 in addition to following：
The granularity of the silicon dioxide powder is 0.02 ~ 44 μm.
The inorganic salts are magnesium chloride.
Solution used in the washing is sulfuric acid.
Embodiment 9
A kind of silicon nitride magnesium powder and preparation method thereof.Remaining is the same as embodiment 7 in addition to following：
The granularity of the silicon dioxide powder≤0. 02 μm.
The inorganic salts are the mixture of sodium chloride and potassium chloride.
Solution used in the washing is nitric acid.
Embodiment 10
A kind of silicon nitride magnesium powder and preparation method thereof.Remaining is the same as embodiment 7 in addition to following：
The granularity of the magnesium powder is 44 ~ 88 μm.
The inorganic salts are the mixture of sodium chloride and potassium fluoride.
Embodiment 11
A kind of silicon nitride magnesium powder and preparation method thereof.Remaining is the same as embodiment 7 in addition to following：
The granularity of the magnesium powder is 44 ~ 88 μm.
The granularity of the silicon dioxide powder is 0.02 ~ 44 μm.
The inorganic salts are the mixture of magnesium chloride, sodium fluoride and potassium fluoride.
Solution used in the washing is sulfuric acid.
Embodiment 12
A kind of silicon nitride magnesium powder and preparation method thereof.Remaining is the same as embodiment 7 in addition to following：
The granularity of the magnesium powder is 44 ~ 88 μm.
The granularity of the silicon dioxide powder≤0. 02 μm.
The inorganic salts are the mixture of lithium chloride, magnesium chloride and sodium fluoride.
Solution used in the washing is nitric acid.
Embodiment 13
A kind of silicon nitride magnesium powder and preparation method thereof.With the magnesium powder of 10 ~ 15wt%, the silica of 22 ~ 25wt% and 65 ~
The inorganic salts of 68wt% are raw material, mix 0.5 ~ 1h；Then under the conditions of 0.1 ~ 1MPa and nitrogen atmosphere, with 5 ~ 10 DEG C/min's
Rate is warming up to medium temperature；Firing temperature is warming up to the rate of 3 ~ 5 DEG C/min again, keeps the temperature 1 ~ 7h, furnace cooling is washed,
It is dry, silicon nitride magnesium powder is made.
The firing temperature is 1100 ~ 1300 DEG C, and the temperature difference of medium temperature and firing temperature is 140 ~ 200 DEG C.
The granularity of the magnesium powder is 0.02 ~ 44 μm.
The granularity of the silicon dioxide powder is 44 ~ 74 μm.
The inorganic salts are sodium fluoride.
Solution used in the washing is hydrochloric acid.
Embodiment 14
A kind of silicon nitride magnesium powder and preparation method thereof.Remaining is the same as embodiment 13 in addition to following：
The granularity of the silicon dioxide powder is 0.02 ~ 44 μm.
The inorganic salts are potassium fluoride.
Solution used in the washing is sulfuric acid.
Embodiment 15
A kind of silicon nitride magnesium powder and preparation method thereof.Remaining is the same as embodiment 13 in addition to following：
The granularity of the silicon dioxide powder≤0. 02 μm.
The inorganic salts are the mixture of potassium chloride and lithium chloride.
Solution used in the washing is nitric acid.
Embodiment 16
A kind of silicon nitride magnesium powder and preparation method thereof.Remaining is the same as embodiment 13 in addition to following：
The granularity of the magnesium powder is 44 ~ 88 μm.
The inorganic salts are the mixture of magnesium chloride and sodium fluoride.
Embodiment 17
A kind of silicon nitride magnesium powder and preparation method thereof.Remaining is the same as embodiment 13 in addition to following：
The granularity of the magnesium powder is 44 ~ 88 μm.
The granularity of the silicon dioxide powder is 0.02 ~ 44 μm.
The inorganic salts are the mixture of potassium chloride, lithium chloride and magnesium chloride.
Solution used in the washing is sulfuric acid.
Embodiment 18
A kind of silicon nitride magnesium powder and preparation method thereof.Remaining is the same as embodiment 13 in addition to following：
The granularity of the magnesium powder is 44 ~ 88 μm.
The granularity of the silicon dioxide powder≤0. 02 μm.
The inorganic salts are the mixture of sodium chloride, potassium chloride and lithium chloride.
Solution used in the washing is nitric acid.
Present embodiment has following good effect compared with prior art：
Present embodiment assists magnesiothermic reduction nitriding using abundant silica and magnesium powder as raw material, using fused salt
Silicon nitride magnesium powder is prepared, the cost of raw material is made to substantially reduce.Fused salt auxiliary magnesiothermic reduction nitriding prepares silicon nitride magnesium powder
It can be completed in lower temperature and short period, also with the short advantage of simple production process and period.
The magnesium that present embodiment uses under the conditions of 650 DEG C, that is, fusible formation liquid magnesium, in entire reduction nitridation
Magnesium participates in reaction in the form of liquid and gaseous in the process, and the enthalpy of system significantly increases, and significantly reduces the starting temperature of reaction
Degree.Since magnesiothermic reduction reaction process releases a large amount of heat, reaction can be spontaneous without the extraneous energy response that provides after starting
It carries out, and higher system reaction temperature can be reached at a lower temperature.Present embodiment is made using fused salt
Auxiliary, preparation process do not need special equipment, and inorganic salts melt to form ion melt at lower temperature, significantly improve anti-
It answers the mass transfer velocity of object and effectively prevents particle agglomeration, obtained silicon nitride magnesium is as described in Figure 1, and Fig. 1 makes for embodiment 10
A kind of SEM of standby silicon nitride magnesium powder schemes.As can be seen from Figure 1：Powder granule is uniform in size, and pattern is single.
Therefore, present embodiment has simple production process, with short production cycle, raw material resources abundant and production cost
Cheap feature；Prepared silicon nitride magnesium powder granule is uniform in size and pattern is single.
Claims (5)
1. a kind of silicon nitride magnesium raw powder's production technology, it is characterised in that：With the magnesium powder of 10~15wt%, 15~25wt% two
The inorganic salts of silica and 65~75wt% are raw material, mix 0.5~1h；Then under the conditions of 0.1~1MPa and nitrogen atmosphere,
It is warming up to medium temperature with the rate of 5~10 DEG C/min, then firing temperature is warming up to the rate of 3~5 DEG C/min, heat preservation 1~
7h, furnace cooling are washed, dry, and silicon nitride magnesium powder is made；
The firing temperature is 900~1300 DEG C, and the temperature difference of medium temperature and firing temperature is 100~200 DEG C.
2. silicon nitride magnesium raw powder's production technology according to claim 1, it is characterised in that the Mg contents of the magnesium powder are
90~99wt%, the granularity of the magnesium powder are one kind in 0.02~44 μm and 44~88 μm.
3. silicon nitride magnesium raw powder's production technology according to claim 1, it is characterised in that the SiO of the silicon dioxide powder2
Content is 85~99wt%, and the granularity of the silicon dioxide powder is one kind in 44~74 μm, 0.02~44 μm and≤0.02 μm.
4. silicon nitride magnesium raw powder's production technology according to claim 1, it is characterised in that the inorganic salts be sodium chloride,
One kind in potassium chloride, lithium chloride, magnesium chloride, sodium fluoride and potassium fluoride, two kinds or three kinds.
5. silicon nitride magnesium raw powder's production technology according to claim 1, it is characterised in that solution is used in the washing
One kind in hydrochloric acid, sulfuric acid and nitric acid, a concentration of 1mol/L of the cleaning fluids.
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| CN109775674A (en) * | 2019-04-02 | 2019-05-21 | 青岛瓷兴新材料有限公司 | A kind of silicon nitride magnesium raw powder's production technology |
| CN110218080A (en) * | 2019-05-31 | 2019-09-10 | 武汉科技大学 | Nitridation in situ generates silicon nitride magnesium combination magnesia-carbon refractory material and preparation method thereof |
| CN110240132B (en) * | 2019-05-31 | 2022-12-02 | 武汉科技大学 | Silicon-magnesium nitride powder based on molten salt method and preparation method thereof |
| CN110143808B (en) * | 2019-05-31 | 2021-07-06 | 武汉科技大学 | Low-carbon magnesia-carbon refractory material added with silicon-magnesium nitride powder and preparation method thereof |
| CN113666752A (en) * | 2021-08-05 | 2021-11-19 | 陕西中钒昌盛新材料科技有限公司 | Novel technology for producing silicon nitride magnesium by using waste magnesium refractory material |
| CN117550900A (en) * | 2023-11-13 | 2024-02-13 | 中国人民解放军国防科技大学 | Si prepared by adopting molten salt method 3 N 4 /MgSiN 2 Method for preparing high-heat-conductivity silicon nitride ceramic from composite powder |
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