CN104891455A - Preparation method for silicon nitride nano-material - Google Patents
Preparation method for silicon nitride nano-material Download PDFInfo
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- CN104891455A CN104891455A CN201510248180.XA CN201510248180A CN104891455A CN 104891455 A CN104891455 A CN 104891455A CN 201510248180 A CN201510248180 A CN 201510248180A CN 104891455 A CN104891455 A CN 104891455A
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- silicon nitride
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- nitride nano
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 35
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 12
- 239000010935 stainless steel Substances 0.000 claims abstract description 12
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims abstract description 9
- IDBFBDSKYCUNPW-UHFFFAOYSA-N lithium nitride Chemical compound [Li]N([Li])[Li] IDBFBDSKYCUNPW-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000005049 silicon tetrachloride Substances 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 11
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 3
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 238000007789 sealing Methods 0.000 abstract description 2
- 239000012300 argon atmosphere Substances 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 230000000877 morphologic effect Effects 0.000 abstract 1
- 230000007935 neutral effect Effects 0.000 abstract 1
- 238000005554 pickling Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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Abstract
Belonging to preparation methods of ceramic materials, the invention relates to a preparation method for a silicon nitride nano-material. The method includes: in argon atmosphere, placing the mixture of silicon tetrachloride and lithium nitride in a special stainless steel reaction kettle and performing sealing, putting the special stainless steel reaction kettle into a resistance crucible furnace and conducting heating, subjecting the product to alcohol washing, acid pickling and water washing to neutral, and carrying out separation and drying so as to obtain the silicon nitride nano-material. The preparation method for the silicon nitride nano-material has the characteristics of simple equipment, low reaction temperature, short reaction time, environment-friendliness, simple and easily controllable operation, good shape morphological product, cheap raw materials, mild reaction conditions, simple operation, and easy realization of industrial production, provides further convenience for application in relevant fields, and has significant practical value.
Description
Technical field
The invention belongs to stupalith field, relate to a kind of preparation method of silicon nitride nano-material.
Background technology
Silicon nitride nano-material is because having stable insulativity, and high heat and chemical stability, special mechanics and electric property and receive much concern, have a good application prospect in nano electron device and nanostructured ceramic material etc.
The preparation method of current silicon nitride nano-material has: metal catalysed processes, pyrolysis method, ball milling-annealing method, copyrolysis method and ammonia direct nitridation method, arc discharge, Electron-beam irradiation, laser evaporization method, chemical Vapor deposition process (CVD) and laser ablation method etc., aforesaid method or needs in relatively high temperature of reaction, or rely on large-scale instrument and equipment.
Therefore, at lower temperatures, preparing silicon nitride nano-material under milder condition, having the meaning of particularly important for promoting silicon nitride and related compound material and broadened application thereof.
Summary of the invention
The object of this invention is to provide a kind of preparation method of silicon nitride nano-material, realize the low-temperature growth of silicon nitride nano-material.
The present invention is achieved in that with silicon tetrachloride and lithium nitride for raw material, and through sealing solid state reaction, prepare silicon nitride nano-material, concrete technical scheme is as follows:
0.030 mol silicon tetrachloride, 0.040 mol lithium nitride are joined 50 milliliters of special stainless steel cauldrons, and seal by step 1. in argon atmospher;
Special stainless steel cauldron is put into resistance crucible furnace by step 2., by temperature controller with the temperature rise rate of 10 DEG C/min constant temperature 12-24 hour under 400-600 oC;
The special stainless steel cauldron of step 3 takes out by step 3., naturally cools to room temperature, opens reactor, takes out product in reactor;
The product ethanol of step 3 is embathed 30 minutes by step 4., through centrifugation, washes 30 minutes with acidleach, with distillation washing 3-5 time, then washes 2-3 time with ethanol;
Step 5. by the product centrifugation of step 4 and in vacuum drier under 60 C dry 6 hours, obtains dark gray powder product, i.e. silicon nitride nano-material.
In the preparation method of above-mentioned silicon nitride nano-material, described rare gas element is preferably argon gas.
In the preparation method of above-mentioned silicon nitride nano-material, described ethanol is preferably 95%-100% ethanol.
In the preparation method of above-mentioned silicon nitride nano-material, described acid is preferably the mixed solution of hydrochloric acid, sulfuric acid, nitric acid and/or its arbitrary volume ratio.Wherein, described acid optimum is 1mol/L hydrochloric acid.
In the preparation method of above-mentioned silicon nitride nano-material, described vacuum-drying temperature is 60 ± 1 C, and time of drying is 6 ± 0.5 hours.
Beneficial effect, owing to have employed such scheme,
(1) the present invention is with silicon tetrachloride and lithium nitride for raw material, adopts solid-phase synthesis to prepare silicon nitride nano-material, solve pollution problem in silicon nitride nano-material preparation process in argon atmospher;
(2) instant invention overcomes silicon nitride nano-material preparation process in literature method and rely on the defect of main equipment;
Reach object of the present invention.
advantage:this prepares the method for silicon nitride nano-material, required equipment is simple, temperature of reaction is lower, the reaction times shortens, environmental friendliness, easy control simple to operate, products therefrom pattern is better, cheaper starting materials, reaction conditions is gentle, easy and simple to handle, is easy to realize suitability for industrialized production, provide further convenience in the application of association area, there is great practical value.
Embodiment
Further describe the present invention by following examples, but scope of the present invention should be noted not by the restriction of these embodiments.
embodiment 1:a kind of preparation method of silicon nitride nano-material
Take 0.030 mol silicon tetrachloride and 0.040 mol lithium nitride, above-mentioned substance is joined 50 milliliters of special stainless steel cauldrons in argon gas environment and fully mixing, then be placed in electric furnace after autoclave being sealed, by temperature controller with the temperature rise rate of 10 DEG C/min constant temperature 24 hours under 400 oC, it is then allowed to naturally cool to room temperature.Drive still, products therefrom embathes through 95% ethanol, and 1mol/L hydrochloric acid embathes, and is washed to pH neutrality, and centrifugation is also placed in vacuum drying oven under 60 C dry 6 hours, finally obtains dark gray powder product, i.e. silicon nitride nano-material.
embodiment 2:a kind of preparation method of silicon nitride nano-material
Take 0.015 mol silicon tetrachloride and 0.020 mol lithium nitride, above-mentioned substance is joined 50 milliliters of special stainless steel cauldrons in argon gas environment and fully mixing, then be placed in electric furnace after autoclave being sealed, by temperature controller with the temperature rise rate of 8 DEG C/min constant temperature 16 hours under 500 oC, it is then allowed to naturally cool to room temperature.Drive still, products therefrom embathes through 95% ethanol, and 1mol/L hydrochloric acid embathes, and is washed to pH neutrality, and centrifugation is also placed in vacuum drying oven under 60 C dry 6 hours, finally obtains dark gray powder product, i.e. silicon nitride nano-material.
embodiment 3:a kind of preparation method of silicon nitride nano-material
Take 0.045 mol silicon tetrachloride and 0.060 mol lithium nitride, above-mentioned substance is joined 80 milliliters of special stainless steel cauldrons in argon gas environment and fully mixing, then be placed in electric furnace after autoclave being sealed, by temperature controller with the temperature rise rate of 5 DEG C/min constant temperature 12 hours under 600 oC, it is then allowed to naturally cool to room temperature.Drive still, products therefrom embathes through 95% ethanol, and 1mol/L hydrochloric acid embathes, and is washed to pH neutrality, and centrifugation is also placed in vacuum drying oven under 60 C dry 6 hours, finally obtains dark gray powder product, i.e. silicon nitride nano-material.
Claims (7)
1. a preparation method for silicon nitride nano-material, is characterized in that being made up of the following step:
0.03 mol silicon tetrachloride and 0.04 mol lithium nitride are joined 50 milliliters of special stainless steel cauldrons by step 1. in argon atmospher, and seal;
Special stainless steel cauldron is put into resistance crucible furnace by step 2., by temperature controller with the temperature rise rate of 5-10 DEG C/min constant temperature 12-24 hour under 400-600 oC;
The special stainless steel cauldron of step 3 takes out by step 3., naturally cools to room temperature, opens reactor, takes out product in reactor;
The product ethanol of step 3 is embathed 30 minutes by step 4., through centrifugation, washes 30 minutes with acidleach, with distillation washing 3-5 time, then washes 2-3 time with ethanol;
Step 5. by the product centrifugation of step 4 and in vacuum drier under 60 C dry 6 hours, obtains dark gray powder product, i.e. silicon nitride nano-material.
2. the preparation method of silicon nitride nano-material according to claim 1, is characterized in that: the silicon tetrachloride consumption described in step 1 is 0.030mol, and lithium nitride consumption is 0.040 mol, and special stainless steel cauldron volume is 50 ± 1 milliliters.
3. the preparation method of silicon nitride nano-material according to claim 1, is characterized in that: the temperature rise rate described in step 2 is 5-10 DEG C/min, Heating temperature 400-600 C in resistance crucible furnace, and the time is 12-24 hour.
4. the preparation method of silicon nitride nano-material according to claim 1, is characterized in that: the product ethanol of step 4 embathes 30 ± 1 minutes, washes 30 ± 1 minutes with acidleach, with distillation washing 3-5 time, washes 2-3 time with ethanol.
5. the preparation method of silicon nitride nano-material according to claim 1, is characterized in that: the acid described in step 4 is preferably the mixed solution of hydrochloric acid, sulfuric acid, nitric acid and/or its arbitrary volume ratio.
6. wherein, described acid optimum is 1mol/L hydrochloric acid.
7. the preparation method of silicon nitride nano-material according to claim 1, is characterized in that: the vacuum-drying temperature described in step 5 is 60 ± 1 C, and time of drying is 6 ± 0.5 hours.
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| CN201510248180.XA CN104891455A (en) | 2015-05-15 | 2015-05-15 | Preparation method for silicon nitride nano-material |
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| CN201510248180.XA CN104891455A (en) | 2015-05-15 | 2015-05-15 | Preparation method for silicon nitride nano-material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109095443A (en) * | 2018-10-22 | 2018-12-28 | 青岛瓷兴新材料有限公司 | A kind of method that liquid phase auxiliary combustion is synthetically prepared high purity silicon nitride silicon powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1955110A (en) * | 2006-09-07 | 2007-05-02 | 暨南大学 | Preparation method of silicon nitride nanowire and nanoribbon powder material |
| CN102674271A (en) * | 2012-06-04 | 2012-09-19 | 蔡佩君 | Method for preparing boron nitride nanotube |
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- 2015-05-15 CN CN201510248180.XA patent/CN104891455A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1955110A (en) * | 2006-09-07 | 2007-05-02 | 暨南大学 | Preparation method of silicon nitride nanowire and nanoribbon powder material |
| CN102674271A (en) * | 2012-06-04 | 2012-09-19 | 蔡佩君 | Method for preparing boron nitride nanotube |
Non-Patent Citations (1)
| Title |
|---|
| ARTHUR J. ANDERSON ET AL.: "Microwave initiated solid-state metathesis routes to Li2SiN2", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109095443A (en) * | 2018-10-22 | 2018-12-28 | 青岛瓷兴新材料有限公司 | A kind of method that liquid phase auxiliary combustion is synthetically prepared high purity silicon nitride silicon powder |
| CN109095443B (en) * | 2018-10-22 | 2021-05-28 | 青岛瓷兴新材料有限公司 | Method for preparing high-purity silicon nitride powder by liquid-phase auxiliary combustion synthesis |
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Application publication date: 20150909 |