CN103508428B - With the instrument and supplies of silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride - Google Patents
With the instrument and supplies of silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride Download PDFInfo
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- CN103508428B CN103508428B CN201310472879.5A CN201310472879A CN103508428B CN 103508428 B CN103508428 B CN 103508428B CN 201310472879 A CN201310472879 A CN 201310472879A CN 103508428 B CN103508428 B CN 103508428B
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Abstract
The invention discloses the equipment and process with silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride, equipment comprises plasma generator, plasma reactor, cooling room, gas solid separation room, nitrogen trifluoride refining plant; Plasma generator is connected with plasma reactor, the discharge port of plasma reactor is connected with the opening for feed of cooling room, cooling room is also provided with low temperature nitrogen input aperture, the discharge port of cooling room is connected with the opening for feed of gas solid separation room, the gas phase discharge port of gas solid separation room is connected with the opening for feed of nitrogen trifluoride refining plant, the solid phase discharge port of gas solid separation room is silicon nitride relief outlet, and nitrogen trifluoride refining plant is provided with nitrogen trifluoride relief outlet and outlet port.Present invention process route is novel, rationally, equipment Requirement is low, and reaction safely, easily realizes industrialized less energy-consumption and produces, and silicon nitride and the nitrogen trifluoride purity of production are high; Realize the high value added utilization of refuse, there is environmental protection and economical effects.
Description
Technical field
The present invention relates to chemical field, particularly with the instrument and supplies 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, thus also will day by day increase the demand of high-performance silicon nitride powder.Silicon nitride powder preparation conventional in prior art has following several: one, silica flour direct nitridation method, and the method is easy, cost is low, because the reaction of silicon and nitrogen is thermopositive reaction, in order to make silica flour fully react, and 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 titanium dioxide silicon process, the silicon-dioxide that this method utilizes occurring in nature very abundant is raw material, in addition speed of reaction faster, be particularly suitable for scale operation, but shortcoming is that in product, carbon content is higher.Three, plasma enhanced chemical vapor reaction method, the method utilizes the halogenide (SiC1 of silicon
4, SiBr
4deng) or the hydrohalogen (SiHC1 of silicon
3, SiH
2c1
2deng > and ammonia or nitrogen hydrogenation generation chemical gas phase reaction, or silane (SiH
4) and ammonia or hydrazine (N
2h
4) there is chemical gas phase reaction, the unformed beta-silicon nitride powder of general generation; This unformed beta-silicon nitride powder in a nitrogen atmosphere, the beta-silicon nitride powder that α phase content is greater than 95% can be obtained after Overheating Treatment, but this technology is mainly limited to laboratory study at present, because its reaction cost is high, and reaction danger is difficult to control and fail to be produced in batches and practical application always; And the oxygen level of obtained powder is greater than 2 ~ 3%, and residual chloride content is higher, reaches 60ppm, finally can affect the performance of silicon nitride ceramics.
Nitrogen trifluoride is colourless, odorless, stable in properties gas at normal temperatures, and boiling point is-129 DEG C, and fusing point is-208 DEG C.In addition, it or a kind of strong oxidizer.Nitrogen trifluoride is as a kind of excellent plasma etch gases, there is when ion etching excellent etch-rate and selectivity, and, any residue is not stayed on etchant surface, be very good clean-out system, therefore, have boundless prospect at semi-conductor and microelectronic industry, in addition, it has also obtained applying widely in superlaser field.The preparation method of nitrogen trifluoride has two kinds usually: namely with NH
3with F
2for raw material prepares the chemical synthesis that nitrogen trifluoride is representative, due to F
2reactivity is very high, and has stronger toxicity and corrodibility, and therefore 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 prepares the electrolytic process of nitrogen trifluoride by electrolyzer.The advantage of electrolytic process is that production run comparatively uses NH
3with F
2for raw material prepare the purity of comparatively safe stable, the gas of the chemical synthesis of nitrogen trifluoride and productive rate all higher, therefore, this method is adopted comparatively widely by a lot of enterprise, but its maximum shortcoming to be production process cost too high, still there is certain danger simultaneously.
Summary of the invention
In order to solve the problem, the invention provides a kind of equipment and process being raw material production silicon nitride and nitrogen trifluoride with silicon tetrafluoride and nitrogen.The technical problem to be solved in the present invention is: provide a kind of operational path novel, reasonable, equipment Requirement is low, and reaction safely, easily realizes the method and apparatus that high purity silicon nitride and nitrogen trifluoride are produced in industrialized less energy-consumption.In order to realize above-mentioned technical purpose, technical scheme of the present invention 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 room, 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 room, the gas phase discharge port of described gas solid separation room is connected with the opening for feed of nitrogen trifluoride refining plant, the solid phase discharge port of described gas solid separation room 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 described discharge port of 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 described opening for feed of sealing gland discharging spiral is connected with the solid phase discharge port of gas solid separation room, 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, described plasma reactor peripheral hardware responds hot water cooler.
Wherein, nitrogen trifluoride refining plant, nitrogen purge retrieving arrangement are the separating-purifying device of mixed gas, and be prior art, therefore not to repeat here for its concrete structure and technological process.
The invention also discloses the technique 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. plasma generator power supply is opened, nitrogen gas plasma is produced in plasma reactor, 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, used up nitrogen in postreaction process;
C. low temperature nitrogen is filled with cooling room, is then together expelled to cooling room and mixes with low temperature nitrogen by reacting the silicon nitride solid of generation, gas of nitrogen trifluoride and unreacted unstripped gas in plasma reactor thus to lower the temperature rapidly;
D. by the silicon nitride solid of lowering the temperature in step C with comprise gas of nitrogen trifluoride, unreacting material gas is expelled to gas solid separation room together with the mixed gas of nitrogen, by silicon nitride solid be separated, discharge from the solid phase discharge port of gas solid separation room; Mixed gas is expelled to nitrogen trifluoride refining plant from the gas phase discharge port of gas solid separation room;
E. the mixed gas of gas of nitrogen trifluoride, unreacting material gas and nitrogen is comprised in nitrogen trifluoride refining plant, through separation and purification, gas of nitrogen trifluoride exports from the nitrogen trifluoride relief outlet of nitrogen trifluoride refining plant, and other mixed gas is discharged from outlet port.
At high temperature react each other to prevent the nitrogen trifluoride that generates in plasma reactor and silicon nitride, regenerate silicon tetrafluoride, thus in step C, low temperature nitrogen is passed in cooling room, to reduce rapidly the temperature of nitrogen trifluoride and silicon nitride extremely lower than 25 DEG C, nitrogen trifluoride and silicon nitride are then more difficult to react.
In such scheme, after described step D, also comprise step D1: the silicon nitride of being discharged by the solid phase discharge port from gas solid separation room is sent in high temperature crystallization furnace through sealing gland discharging spiral and carried out high-temperature fusion crystallization.
In such scheme, after described step e, also comprise step F: export the mixed gas that the outlet port of nitrogen trifluoride refining plant is discharged to nitrogen purge retrieving arrangement, the nitrogen separation in mixed gas is reclaimed, be circulated to plasma reactor and continue to use.
In such scheme, in described step B, the silicon tetrafluoride gas passed into and the mol ratio of nitrogen are 1:4 ~ 1:16.
In such scheme, in described step C, the temperature of low temperature nitrogen is 15 DEG C ~-35 DEG C.
Silicon tetrafluoride and nitrogen react, and generate the reaction formula of silicon nitride and nitrogen trifluoride:
3SiF
4+4N
2→Si
3N
4+4NF
3
Advantage of the present invention and beneficial effect are: the invention provides a kind of equipment and process being raw material production silicon nitride and nitrogen trifluoride with silicon tetrafluoride and nitrogen.Operational path of the present invention is novel, rationally, equipment Requirement is low, and reaction safely, easily realizes industrialized less energy-consumption and produces, and silicon nitride and the nitrogen trifluoride purity of production are high; Silicon tetrafluoride from the byproduct of production of phosphate fertilizer enterprise, also from the converted product silicofluoride (such as Sodium Silicofluoride) of production of phosphate fertilizer enterprise byproduct silicofluoric acid, can realize the high value added utilization of refuse, has environmental protection and economical effects.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is process principle figure of the present invention.
Fig. 2 is the structural representation of the embodiment of the present invention.
In figure: 1, the low temperature nitrogen input aperture 9 of plasma generator 2, plasma reactor 3, cooling room 4, gas solid separation room 5, nitrogen trifluoride refining plant 6, nitrogen purge tripping device 7, reaction heat water cooler 8, cooling room, sealing gland discharging spiral 10, high temperature crystallization furnace
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is further described.Following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
As shown in Figure 2, the present invention is a kind of with the equipment of silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride.Comprise plasma generator 1, plasma reactor 2, cooling room 3, gas solid separation room 4, nitrogen trifluoride refining plant 5, nitrogen purge tripping device 6, plasma generator 1 is connected with plasma reactor 2, plasma reactor 2 peripheral hardware responds hot water cooler 7, 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 room 4, the gas phase discharge port of gas solid separation room 4 is connected with the opening for feed of nitrogen trifluoride refining plant 5, the solid phase discharge port of gas solid separation room 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 passes 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 is full of plasma reactor, in the present embodiment, the power of plasma reactor is 10 kilowatts, then in plasma reactor, pass into silicon tetrafluoride gas and nitrogen, the mol ratio being controlled 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 DEG C is filled with cooling room, then by reacting the silicon nitride solid of generation in plasma reactor, gas of nitrogen trifluoride, unreacted unstripped gas is together expelled to cooling room and mixes with low temperature nitrogen thus lower the temperature rapidly; Silicon nitride solid after cooling is expelled to gas solid separation room together with mixed gas, indoor in gas solid separation, silicon nitride solid is separated, discharges from the solid phase discharge port of gas solid separation room; By comprise gas of nitrogen trifluoride, unreacted unstripped gas, nitrogen mixed gas be expelled to nitrogen trifluoride refining plant from the gas phase discharge port of gas solid separation room; Comprise gas of nitrogen trifluoride, unreacted unstripped gas, nitrogen mixed gas in nitrogen trifluoride refining plant, through separation and purification, the nitrogen trifluoride relief outlet of gas of nitrogen trifluoride from nitrogen trifluoride refining plant is exported, other mixed gas is expelled to nitrogen purge retrieving arrangement from outlet port, nitrogen separation in mixed gas is reclaimed, is circulated to plasma reactor and continues 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, better industrial applicability is possessed in order to make product, this amorphous silicon nitride is transported to send in high temperature crystallization furnace 10 by sealing gland discharging spiral 9 and carries out high-temperature fusion phase inversion and crystallization process, obtain alpha-phase silicon nitride powder.
Embodiment 2
Whole reactive system is vacuumized, then passes 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 is full of plasma reactor, in the present embodiment, the power of plasma reactor is 10 kilowatts, then in plasma reactor, pass into silicon tetrafluoride gas and nitrogen, the mol ratio being controlled 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 DEG C is filled with cooling room, then by reacting the silicon nitride solid of generation in plasma reactor, gas of nitrogen trifluoride, unreacted unstripped gas is together expelled to cooling room and mixes with low temperature nitrogen thus lower the temperature rapidly; Silicon nitride solid after cooling is expelled to gas solid separation room together with mixed gas, indoor in gas solid separation, silicon nitride solid is separated, discharges from the solid phase discharge port of gas solid separation room; By comprise gas of nitrogen trifluoride, unreacted unstripped gas, nitrogen mixed gas be expelled to nitrogen trifluoride refining plant from the gas phase discharge port of gas solid separation room; Comprise gas of nitrogen trifluoride, unreacted unstripped gas, nitrogen mixed gas in nitrogen trifluoride refining plant, through separation and purification, the nitrogen trifluoride relief outlet of gas of nitrogen trifluoride from nitrogen trifluoride refining plant is exported, other mixed gas is expelled to nitrogen purge retrieving arrangement from outlet port, nitrogen separation in mixed gas is reclaimed, is circulated to plasma reactor and continues 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, better industrial applicability is possessed in order to make product, this amorphous silicon nitride is transported to send in high temperature crystallization furnace 10 by sealing gland discharging spiral 9 and carries out high-temperature fusion phase inversion and crystallization process, obtain alpha-phase silicon nitride powder.
Embodiment 3
Whole reactive system is vacuumized, then passes 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 is full of plasma reactor, in the present embodiment, the power of plasma reactor is 10 kilowatts, then in plasma reactor, pass into silicon tetrafluoride gas and nitrogen, the mol ratio being controlled 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 DEG C is filled with cooling room, then by reacting the silicon nitride solid of generation in plasma reactor, gas of nitrogen trifluoride, unreacted unstripped gas is together expelled to cooling room and mixes with low temperature nitrogen thus lower the temperature rapidly; Silicon nitride solid after cooling is expelled to gas solid separation room together with mixed gas, indoor in gas solid separation, silicon nitride solid is separated, discharges from the solid phase discharge port of gas solid separation room; By comprise gas of nitrogen trifluoride, unreacted unstripped gas, nitrogen mixed gas be expelled to nitrogen trifluoride refining plant from the gas phase discharge port of gas solid separation room; Comprise gas of nitrogen trifluoride, unreacted unstripped gas, nitrogen mixed gas in nitrogen trifluoride refining plant, through separation and purification, the nitrogen trifluoride relief outlet of gas of nitrogen trifluoride from nitrogen trifluoride refining plant is exported, other mixed gas is expelled to nitrogen purge retrieving arrangement from outlet port, nitrogen separation in mixed gas is reclaimed, is circulated to plasma reactor and continues 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, better industrial applicability is possessed in order to make product, this amorphous silicon nitride is transported to send in high temperature crystallization furnace 10 by sealing gland discharging spiral 9 and carries out high-temperature fusion phase inversion and crystallization process, obtain alpha-phase silicon nitride powder.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
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 room, 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 room, the gas phase discharge port of described gas solid separation room is connected with the opening for feed of nitrogen trifluoride refining plant, the solid phase discharge port of described gas solid separation room is silicon nitride relief outlet, and described nitrogen trifluoride refining plant is provided with nitrogen trifluoride relief outlet and outlet port.
2. according to claim 1 with the equipment of silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride, 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 described discharge port of nitrogen purge retrieving arrangement is connected with the opening for feed of plasma reactor.
3. according to claim 1 with the equipment of silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride, it is characterized in that, also comprise sealing gland discharging spiral and high temperature crystallization furnace, the described opening for feed of sealing gland discharging spiral is connected with the solid phase discharge port of gas solid separation room, and the discharge port of described sealing gland discharging spiral is connected with the opening for feed of high temperature crystallization furnace.
4. described to it is characterized in that with the equipment of silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride according to claims 1 to 3 is arbitrary, described plasma reactor peripheral hardware responds hot water cooler.
5., with the technique of silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride, it is characterized in that, 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. plasma generator power supply is opened, nitrogen gas plasma is produced in plasma reactor, 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, used up nitrogen in postreaction process;
C. low temperature nitrogen is filled with cooling room, is then together expelled to cooling room and mixes with low temperature nitrogen by reacting the silicon nitride solid of generation, gas of nitrogen trifluoride and unreacted unstripped gas in plasma reactor thus to lower the temperature rapidly;
D. by the silicon nitride solid of lowering the temperature in step C with comprise gas of nitrogen trifluoride, unreacting material gas is expelled to gas solid separation room together with the mixed gas of nitrogen, by silicon nitride solid be separated, discharge from the solid phase discharge port of gas solid separation room; Mixed gas is expelled to nitrogen trifluoride refining plant from the gas phase discharge port of gas solid separation room;
E. the mixed gas of gas of nitrogen trifluoride, unreacting material gas and nitrogen is comprised in nitrogen trifluoride refining plant, through separation and purification, gas of nitrogen trifluoride exports from the nitrogen trifluoride relief outlet of nitrogen trifluoride refining plant, and other mixed gas is discharged from outlet port.
6. according to claim 5 with the technique of silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride, it is characterized in that, after described step D, also comprise step D1: the silicon nitride of being discharged by the solid phase discharge port from gas solid separation room is sent in high temperature crystallization furnace through sealing gland discharging spiral and carried out high-temperature fusion crystallization.
7. arbitrary described with the technique of silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride according to claim 5 or 6, it is characterized in that, also step F is comprised: export the mixed gas that the outlet port of nitrogen trifluoride refining plant is discharged to nitrogen purge retrieving arrangement after described step e, nitrogen separation in mixed gas is reclaimed, is circulated to plasma reactor and continues to use.
8. arbitrary described with the technique of silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride according to claim 5 or 6, it is characterized in that, in described step B, the silicon tetrafluoride gas passed into and the mol ratio of nitrogen are 1:4 ~ 1:16.
9. arbitrary described with the technique of silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride according to claim 5 or 6, it is characterized in that, in described step C, the temperature of low temperature nitrogen is 15 DEG C ~-35 DEG C.
10. according to claim 7 with the technique of silicon tetrafluoride and nitrogen production silicon nitride and nitrogen trifluoride, it is characterized in that, in described step B, the silicon tetrafluoride gas passed into and the mol ratio of nitrogen are 1:4 ~ 1:16; In described step C, the temperature of low temperature nitrogen is 15 DEG C ~-35 DEG C.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4227907A (en) * | 1979-10-22 | 1980-10-14 | The United States Of America As Represented By The Secretary Of The Army | Laser photochemical synthesis coating of optical fiber |
| CN1445161A (en) * | 2002-11-29 | 2003-10-01 | 白万杰 | Technique for preparing silicon nitride powders with high alpha phase by using plasma chemical vapor phase process |
| CN203529936U (en) * | 2013-10-11 | 2014-04-09 | 应悦 | Equipment for producing silicon nitride and nitrogen trifluoride from silicon tetrafluoride and nitrogen |
-
2013
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4227907A (en) * | 1979-10-22 | 1980-10-14 | The United States Of America As Represented By The Secretary Of The Army | Laser photochemical synthesis coating of optical fiber |
| CN1445161A (en) * | 2002-11-29 | 2003-10-01 | 白万杰 | Technique for preparing silicon nitride powders with high alpha phase by using plasma chemical vapor phase process |
| CN203529936U (en) * | 2013-10-11 | 2014-04-09 | 应悦 | Equipment for producing silicon nitride and nitrogen trifluoride from silicon tetrafluoride and nitrogen |
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