CN203529936U - Equipment for producing silicon nitride and nitrogen trifluoride from silicon tetrafluoride and nitrogen - Google Patents
Equipment for producing silicon nitride and nitrogen trifluoride from silicon tetrafluoride and nitrogen Download PDFInfo
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- CN203529936U CN203529936U CN201320626805.8U CN201320626805U CN203529936U CN 203529936 U CN203529936 U CN 203529936U CN 201320626805 U CN201320626805 U CN 201320626805U CN 203529936 U CN203529936 U CN 203529936U
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Abstract
The utility model discloses equipment for producing silicon nitride and nitrogen trifluoride from silicon tetrafluoride and nitrogen. The equipment comprises a plasma generator, a plasma reactor, a cooling chamber, a gas-solid separating chamber and a nitrogen trifluoride refining device, wherein the plasma generator is communicated with the plasma reactor; a discharge port of the plasma reactor is communicated with a feed port of the cooling chamber; the cooling chamber is also provided with a low-temperature nitrogen input; the discharge port of the cooling chamber is communicated with the feed port of the gas-solid separating chamber; a gas-phase discharge port of the gas-solid separating chamber is communicated with the feed port of the nitrogen trifluoride refining device; a solid-phase discharge port of the gas-solid separating chamber is used as a silicon nitride discharge port; the nitrogen trifluoride refining device is provided with a nitrogen trifluoride outlet and a waste gas outlet. The equipment has the advantages that the process line is novel and reasonable, few requirements are proposed for assembly, the reaction is safe, industrial low-energy-consumption production is easily realized, the produced silicon nitride and nitrogen trifluoride are high in purity, high value-added utilization for wastes is realized, the environment is protected, and the economic benefit is brought.
Description
Technical field
The utility model relates to chemical field, particularly with the equipment of silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride.
Background technology
Silicon nitride ceramics has high rigidity, intensity is high, wear-resistant, high temperature resistant, thermal expansivity is little, thermal conductivity is large, good thermal shock, the series of advantages such as density is low, in fields such as ceramic engine, mechanical workout, microtronics, space science and nuclear power engineerings, there is very wide application prospect, thereby also will day by day increase the demand of high-performance silicon nitride powder.In prior art, conventional silicon nitride powder preparation has following several: one, silica flour direct nitridation method, and the method is easy, cost is low, because silicon is thermopositive reaction with reacting of nitrogen, for silica flour can fully be reacted, technology controlling and process more complicated; Simultaneously, due to the doping of the purity of raw material own and the later levigate operation of nitrogenize, cause the purity of powder not high.Two, carbothermic reduction silicon-dioxide method, it is raw material that this method is utilized the very abundant silicon-dioxide of occurring in nature, speed of reaction faster, be particularly suitable for scale operation, but shortcoming is that in product, carbon content is higher in addition.Three, plasma chemistry gas-phase reaction method, the method is utilized the halogenide (SiC1 of silicon
4, SiBr
4deng) or the hydrohalogen (SiHC1 of silicon
3, SiH
2c1
2deng >, add hydrogen generation chemical gas phase reaction with ammonia or nitrogen, or silane (SiH
4) and ammonia or hydrazine (N
2h
4) there is chemical gas phase reaction, generally generate unformed beta-silicon nitride powder; This unformed beta-silicon nitride powder is under nitrogen atmosphere, after Overheating Treatment, can obtain the beta-silicon nitride powder that α phase content is greater than 95%, but this technology is mainly confined to laboratory study at present, because its reaction cost is high, and reaction danger is difficult to control and fails to be produced in batches and practical application always; And the oxygen level that makes powder is greater than 2～3%, and residual chlorine content is higher, reaches 60ppm, finally can affect the performance of silicon nitride ceramics.
Nitrogen trifluoride is the gas of colourless, odorless, stable in properties at normal temperatures, and boiling point is-129 ℃, and fusing point is-208 ℃.In addition, it or a kind of strong oxidizer.Nitrogen trifluoride is as a kind of good plasma etch gases, when ion etching, there is excellent etch-rate and selectivity, and, on etchant surface, do not stay any residue, be very good clean-out system, therefore, at semi-conductor and microelectronic industry, have boundless prospect, in addition, it has also obtained application widely in superlaser field.The preparation method of nitrogen trifluoride has two kinds conventionally: to use NH
3with F
2for raw material is prepared the chemical synthesis that nitrogen trifluoride is representative, due to F
2reactivity is very high, and has stronger toxicity and corrodibility, so this method reactivity hazard is large and many because of the high by product that causes of reaction heat; And with NH
4f-xHF is that raw material is prepared the electrolytic process of nitrogen trifluoride by electrolyzer.The advantage of electrolytic process is that NH is used in production run
3with F
2chemical synthesis comparatively safe purity and the productive rate stable, gas of for raw material, preparing nitrogen trifluoride are all higher, therefore, this method is adopted comparatively widely by a lot of enterprises, but that its maximum shortcoming is production process cost is too high, and the while still exists certain danger.
Summary of the invention
In order to address the above problem, the utility model provides a kind of equipment that silicon tetrafluoride and nitrogen is raw material production silicon nitride and nitrogen trifluoride of take.The technical problems to be solved in the utility model is: provide a kind of operational path novel, reasonable, equipment Requirement is low, and reaction safely, easily realizes the equipment that high purity silicon nitride and nitrogen trifluoride are produced in industrialized less energy-consumption.In order to realize above-mentioned technical purpose, the technical solution of the utility model is: with the equipment of silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride, it is characterized in that, comprise plasma generator, plasma reactor, cooling room, gas solid separation chamber, nitrogen trifluoride refining plant; Described plasma generator is connected with plasma reactor, the discharge port of described plasma reactor is connected with the opening for feed of cooling room, described cooling room is also provided with low temperature nitrogen input aperture, the discharge port of described cooling room is connected with the opening for feed of gas solid separation chamber, the gas phase discharge port of described gas solid separation chamber is connected with the opening for feed of nitrogen trifluoride refining plant, the solid phase discharge port of described gas solid separation chamber is silicon nitride relief outlet, and described nitrogen trifluoride refining plant is provided with nitrogen trifluoride relief outlet and outlet port.
In such scheme, also comprise nitrogen purge retrieving arrangement, the opening for feed of described nitrogen purge retrieving arrangement is connected with the outlet port of nitrogen trifluoride refining plant, and the discharge port of described nitrogen purge retrieving arrangement is connected with the opening for feed of plasma reactor.
In such scheme, also comprise sealing gland discharging spiral and high temperature crystallization furnace, the opening for feed of described sealing gland discharging spiral is connected with the solid phase discharge port of gas solid separation chamber, and the discharge port of described sealing gland discharging spiral is connected with the opening for feed of high temperature crystallization furnace.
In such scheme, the described plasma reactor peripheral hardware hot water cooler that responds.
Wherein, the separating-purifying device that nitrogen trifluoride refining plant, nitrogen purge retrieving arrangement are mixed gas, is prior art, and therefore not to repeat here for its concrete structure and technological process.
Use the utility model with silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride, comprise the following steps:
A. whole reactive system is vacuumized, then pass into nitrogen and carry out system airflow cleaning, after cleaning, make whole reactive system be full of nitrogen;
B. open plasma generator power supply, in plasma reactor, produce nitrogen gas plasma, then in plasma reactor, pass into silicon tetrafluoride gas, silicon tetrafluoride gas and nitrogen ion generation chemical reaction, generate silicon nitride solid and gas of nitrogen trifluoride; Meanwhile, also in plasma reactor, pass into nitrogen, the nitrogen that in postreaction process, effect is fallen;
C. low temperature nitrogen is filled with to cooling room, thereby then silicon nitride solid, gas of nitrogen trifluoride, unreacted unstripped gas that in plasma reactor, reaction generates are together expelled to cooling room, mixes cooling rapidly with low temperature nitrogen;
D. the silicon nitride solid of lowering the temperature in step C is expelled to gas solid separation chamber together with the mixed gas that comprises gas of nitrogen trifluoride, unreacting material gas and nitrogen, silicon nitride solid is separated, from the solid phase discharge port of gas solid separation chamber, discharge; Mixed gas is expelled to nitrogen trifluoride refining plant from the gas phase discharge port of gas solid separation chamber;
E. comprise the mixed gas of gas of nitrogen trifluoride, unreacted unstripped gas, nitrogen in nitrogen trifluoride refining plant, through separation and purification, gas of nitrogen trifluoride is from the nitrogen trifluoride relief outlet output of nitrogen trifluoride refining plant, and other mixed gas is discharged from outlet port.
For the nitrogen trifluoride that prevents from generating in plasma reactor at high temperature reacts each other with silicon nitride, regenerate silicon tetrafluoride, thereby in step C, in cooling room, pass into low temperature nitrogen, to reduce rapidly the temperature of nitrogen trifluoride and silicon nitride extremely lower than 25 ℃, nitrogen trifluoride and silicon nitride be more difficult reacting.
For making unformed beta-silicon nitride powder be converted into alpha-phase silicon nitride powder, after step D, can also comprise step D1: the silicon nitride that the solid phase discharge port from gas solid separation chamber is discharged carries out high-temperature fusion crystallization through sealing gland discharging spiral is sent into high temperature crystallization furnace.
For reducing costs, cut the waste and pollute, after described step e, can also comprise step F: the mixed gas that the outlet port of nitrogen trifluoride refining plant is discharged exports nitrogen purge retrieving arrangement to, the nitrogen separation in mixed gas is reclaimed, be circulated to plasma reactor and continue to use.
In step B, the silicon tetrafluoride gas passing into and the mol ratio of nitrogen are 1:4～1:16.
In step C, the temperature of low temperature nitrogen is 15 ℃～-35 ℃.
Silicon tetrafluoride reacts with nitrogen, generates the reaction formula of silicon nitride and nitrogen trifluoride:
3SiF
4+4N
2→Si
3N
4+4NF
3
Advantage of the present utility model and beneficial effect are: the utility model provides a kind of equipment that silicon tetrafluoride and nitrogen is raw material production silicon nitride and nitrogen trifluoride of take.Operational path of the present utility model is novel, reasonable, and equipment Requirement is low, and reaction safely, easily realizes industrialized less energy-consumption and produces, and the silicon nitride of production and nitrogen trifluoride purity are high; Silicon tetrafluoride can also can for example, be realized the high value added utilization of refuse from the converted product silicofluoride (Sodium Silicofluoride) of production of phosphate fertilizer enterprise byproduct silicofluoric acid from the byproduct of production of phosphate fertilizer enterprise, has environmental protection and economical effects.
Accompanying drawing explanation
In order to be illustrated more clearly in the utility model embodiment or technical scheme of the prior art, to the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described below, apparently, accompanying drawing in the following describes is only embodiment more of the present utility model, for those of ordinary skills, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is the structural representation of the utility model embodiment.
In figure: 1, plasma generator 2, plasma reactor 3, cooling room
4, gas solid separation chamber 5, nitrogen trifluoride refining plant 6, nitrogen purge tripping device
7, the low temperature nitrogen input aperture 9 of reaction heat water cooler 8, cooling room, sealing gland discharging spiral
10, high temperature crystallization furnace
Embodiment
Below in conjunction with drawings and Examples, embodiment of the present utility model is further described.Following examples are only for the technical solution of the utility model is more clearly described, and can not limit protection domain of the present utility model with this.
As shown in Figure 1, the utility model is a kind of equipment with silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride.Comprise plasma generator 1, plasma reactor 2, cooling room 3, gas solid separation chamber 4, nitrogen trifluoride refining plant 5, nitrogen purge tripping device 6, plasma generator 1 is connected with plasma reactor 2, the plasma reactor 2 peripheral hardwares hot water cooler 7 that responds, the discharge port of plasma reactor 2 is connected with the opening for feed of cooling room 3, cooling room 3 is also provided with low temperature nitrogen input aperture 8, the discharge port of cooling room 3 is connected with the opening for feed of gas solid separation chamber 4, the gas phase discharge port of gas solid separation chamber 4 is connected with the opening for feed of nitrogen trifluoride refining plant 5, the solid phase discharge port of gas solid separation chamber 4 is silicon nitride relief outlet, silicon nitride relief outlet is connected with the opening for feed of sealing gland discharging spiral 9, the discharge port of sealing gland discharging spiral 9 is connected with the opening for feed of high temperature crystallization furnace 10, nitrogen trifluoride refining plant 5 is provided with nitrogen trifluoride relief outlet and outlet port.The opening for feed of nitrogen purge retrieving arrangement 6 is connected with the outlet port of nitrogen trifluoride refining plant 5, and the discharge port of nitrogen purge retrieving arrangement 6 is connected with the opening for feed of plasma reactor 2.
Embodiment 1
Whole reactive system is vacuumized, then pass into nitrogen and carry out system airflow cleaning, after cleaning, make whole reactive system be full of nitrogen; Open plasma generator power supply, nitrogen plasma is entered and be full of plasma reactor, the power of the present embodiment applying plasma reactor is 10 kilowatts, then in plasma reactor, pass into silicon tetrafluoride gas and nitrogen, the mol ratio of controlling silicon tetrafluoride and nitrogen by under meter is 1:4; Nitrogen ion generation chemical reaction in silicon tetrafluoride gas and nitrogen plasma, generates silicon nitride solid and gas of nitrogen trifluoride; The low temperature nitrogen of-35 ℃ is filled with to cooling room, thereby then silicon nitride solid, gas of nitrogen trifluoride, unreacted unstripped gas that in plasma reactor, reaction generates are together expelled to cooling room, mixes cooling rapidly with low temperature nitrogen; Silicon nitride solid after cooling is expelled to gas solid separation chamber together with mixed gas, indoor in gas solid separation, silicon nitride solid is separated, from the solid phase discharge port of gas solid separation chamber, discharge; The mixed gas that comprises gas of nitrogen trifluoride, unreacted unstripped gas, nitrogen is expelled to nitrogen trifluoride refining plant from the gas phase discharge port of gas solid separation chamber; The mixed gas that comprises gas of nitrogen trifluoride, unreacted unstripped gas, nitrogen is in nitrogen trifluoride refining plant, through separation and purification, nitrogen trifluoride relief outlet output by gas of nitrogen trifluoride from nitrogen trifluoride refining plant, other mixed gas is expelled to nitrogen purge retrieving arrangement from outlet port, nitrogen separation in mixed gas is reclaimed, be circulated to plasma reactor and continue to use.
After 180 minutes reaction times, collect silicon nitride solid 57kg, gas of nitrogen trifluoride 112.6kg.Wherein silicon nitride solid is amorphous silicon nitride powder, in order to make product possess better industrial applicability, this amorphous silicon nitride is sent into and in high temperature crystallization furnace 10, carried out high-temperature fusion phase inversion and crystallization is processed by sealing gland discharging spiral 9 transhipment, obtain alpha-phase silicon nitride powder.
Whole reactive system is vacuumized, then pass into nitrogen and carry out system airflow cleaning, after cleaning, make whole reactive system be full of nitrogen; Open plasma generator power supply, nitrogen plasma is entered and be full of plasma reactor, the power of the present embodiment applying plasma reactor is 10 kilowatts, then in plasma reactor, pass into silicon tetrafluoride gas and nitrogen, the mol ratio of controlling silicon tetrafluoride and nitrogen by under meter is 1:8; Nitrogen ion generation chemical reaction in silicon tetrafluoride gas and nitrogen plasma, generates silicon nitride solid and gas of nitrogen trifluoride; The low temperature nitrogen of 0 ℃ is filled with to cooling room, thereby then silicon nitride solid, gas of nitrogen trifluoride, unreacted unstripped gas that in plasma reactor, reaction generates are together expelled to cooling room, mixes cooling rapidly with low temperature nitrogen; Silicon nitride solid after cooling is expelled to gas solid separation chamber together with mixed gas, indoor in gas solid separation, silicon nitride solid is separated, from the solid phase discharge port of gas solid separation chamber, discharge; The mixed gas that comprises gas of nitrogen trifluoride, unreacted unstripped gas, nitrogen is expelled to nitrogen trifluoride refining plant from the gas phase discharge port of gas solid separation chamber; The mixed gas that comprises gas of nitrogen trifluoride, unreacted unstripped gas, nitrogen is in nitrogen trifluoride refining plant, through separation and purification, nitrogen trifluoride relief outlet output by gas of nitrogen trifluoride from nitrogen trifluoride refining plant, other mixed gas is expelled to nitrogen purge retrieving arrangement from outlet port, nitrogen separation in mixed gas is reclaimed, be circulated to plasma reactor and continue to use.
After 200 minutes reaction times, collect silicon nitride solid 60kg, gas of nitrogen trifluoride 119.3kg.Wherein silicon nitride solid is amorphous silicon nitride powder, in order to make product possess better industrial applicability, this amorphous silicon nitride is sent into and in high temperature crystallization furnace 10, carried out high-temperature fusion phase inversion and crystallization is processed by sealing gland discharging spiral 9 transhipment, obtain alpha-phase silicon nitride powder.
Whole reactive system is vacuumized, then pass into nitrogen and carry out system airflow cleaning, after cleaning, make whole reactive system be full of nitrogen; Open plasma generator power supply, nitrogen plasma is entered and be full of plasma reactor, the power of the present embodiment applying plasma reactor is 10 kilowatts, then in plasma reactor, pass into silicon tetrafluoride gas and nitrogen, the mol ratio of controlling silicon tetrafluoride and nitrogen by under meter is 1:16; Nitrogen ion generation chemical reaction in silicon tetrafluoride gas and nitrogen plasma, generates silicon nitride solid and gas of nitrogen trifluoride; The low temperature nitrogen of 15 ℃ is filled with to cooling room, thereby then silicon nitride solid, gas of nitrogen trifluoride, unreacted unstripped gas that in plasma reactor, reaction generates are together expelled to cooling room, mixes cooling rapidly with low temperature nitrogen; Silicon nitride solid after cooling is expelled to gas solid separation chamber together with mixed gas, indoor in gas solid separation, silicon nitride solid is separated, from the solid phase discharge port of gas solid separation chamber, discharge; The mixed gas that comprises gas of nitrogen trifluoride, unreacted unstripped gas, nitrogen is expelled to nitrogen trifluoride refining plant from the gas phase discharge port of gas solid separation chamber; The mixed gas that comprises gas of nitrogen trifluoride, unreacted unstripped gas, nitrogen is in nitrogen trifluoride refining plant, through separation and purification, nitrogen trifluoride relief outlet output by gas of nitrogen trifluoride from nitrogen trifluoride refining plant, other mixed gas is expelled to nitrogen purge retrieving arrangement from outlet port, nitrogen separation in mixed gas is reclaimed, be circulated to plasma reactor and continue to use.
After 185 minutes reaction times, collect silicon nitride solid 56.5kg, gas of nitrogen trifluoride 107.1kg.Wherein silicon nitride solid is amorphous silicon nitride powder, in order to make product possess better industrial applicability, this amorphous silicon nitride is sent into and in high temperature crystallization furnace 10, carried out high-temperature fusion phase inversion and crystallization is processed by sealing gland discharging spiral 9 transhipment, obtain alpha-phase silicon nitride powder.
The foregoing is only preferred embodiment of the present utility model; not in order to limit the utility model; all within spirit of the present utility model and principle, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection domain of the present utility model.
Claims (4)
1. with the equipment of silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride, it is characterized in that, comprise plasma generator, plasma reactor, cooling room, gas solid separation chamber, nitrogen trifluoride refining plant; Described plasma generator is connected with plasma reactor, the discharge port of described plasma reactor is connected with the opening for feed of cooling room, described cooling room is also provided with low temperature nitrogen input aperture, the discharge port of described cooling room is connected with the opening for feed of gas solid separation chamber, the gas phase discharge port of described gas solid separation chamber is connected with the opening for feed of nitrogen trifluoride refining plant, the solid phase discharge port of described gas solid separation chamber is silicon nitride relief outlet, and described nitrogen trifluoride refining plant is provided with nitrogen trifluoride relief outlet and outlet port.
2. the equipment with silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride according to claim 1, it is characterized in that, also comprise nitrogen purge retrieving arrangement, the opening for feed of described nitrogen purge retrieving arrangement is connected with the outlet port of nitrogen trifluoride refining plant, and the discharge port of described nitrogen purge retrieving arrangement is connected with the opening for feed of plasma reactor.
3. the equipment with silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride according to claim 1, it is characterized in that, also comprise sealing gland discharging spiral and high temperature crystallization furnace, the opening for feed of described sealing gland discharging spiral is connected with the solid phase discharge port of gas solid separation chamber, and the discharge port of described sealing gland discharging spiral is connected with the opening for feed of high temperature crystallization furnace.
4. according to the arbitrary described equipment with silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride of claim 1～3, it is characterized in that the described plasma reactor peripheral hardware hot water cooler that responds.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320626805.8U CN203529936U (en) | 2013-10-11 | 2013-10-11 | Equipment for producing silicon nitride and nitrogen trifluoride from silicon tetrafluoride and nitrogen |
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|---|---|---|---|
| CN201320626805.8U CN203529936U (en) | 2013-10-11 | 2013-10-11 | Equipment for producing silicon nitride and nitrogen trifluoride from silicon tetrafluoride and nitrogen |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103508428A (en) * | 2013-10-11 | 2014-01-15 | 应悦 | Equipment and process for producing silicon nitride and nitrogen trifluoride by using silicon tetrafluoride and nitrogen gas |
-
2013
- 2013-10-11 CN CN201320626805.8U patent/CN203529936U/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103508428A (en) * | 2013-10-11 | 2014-01-15 | 应悦 | Equipment and process for producing silicon nitride and nitrogen trifluoride by using silicon tetrafluoride and nitrogen gas |
| CN103508428B (en) * | 2013-10-11 | 2015-09-23 | 应悦 | With the instrument and supplies of silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride |
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| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20140409 Effective date of abandoning: 20150923 |
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| RGAV | Abandon patent right to avoid regrant |