CN1973983A - Shock wave process and apparatus for synthesizing cubic silicon nitride material - Google Patents
Shock wave process and apparatus for synthesizing cubic silicon nitride material Download PDFInfo
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- CN1973983A CN1973983A CN 200610022182 CN200610022182A CN1973983A CN 1973983 A CN1973983 A CN 1973983A CN 200610022182 CN200610022182 CN 200610022182 CN 200610022182 A CN200610022182 A CN 200610022182A CN 1973983 A CN1973983 A CN 1973983A
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Abstract
The present invention discloses shock wave process and apparatus for synthesizing cubic silicon nitride material. The present invention adopts detonation loading plant to produce shock wave of high pressure and high temperature to synthesize low pressure hexagonal phase silicon nitride material into high pressure cubic silicon nitride material. The present invention makes it possible to obtain great amount of cubic silicon nitride material in low cost, and the preparation process has excellent industrial application foreground.
Description
Technical field
The invention belongs to the synthetic field of superhard material, be specifically related to the synthetic method and the synthesizer of cubic silicon nitride material, especially adopt controlled detonation charger that low pressure six sides (α with β mutually) silicon nitride is pressed into method and the device that changes cubic silicon nitride into through height.
Background technology
Cubic silicon nitride is a kind of new function material of excellent performance, compares with beta silicon nitride with the α that generally uses at present, has more special performance.
At present, the silicon nitride of cube phase structure can be synthetic by high-temperature and high-pressure conditions, as the dynamic high pressure technique that adopts quiet high pressure technique or light-gas gun to make the shock wave load mode is come artificial synthesis of cubic phase silicon nitride material.
In July, 1999 people such as Zerr the Nature magazine on the 400th phase reported first adopt the artificial synthesis of cubic silicon nitride of the quiet high pressure technique of diamond anvil (DAC), but the output that obtains is very limited, 5 * 10-5 milligram of only having an appointment.In July, 2000, the people such as Sekine of Japan's material and Materials Research Institution material research institute delivered the UNDER SHOCK COMPRESSION technology synthesis of cubic silicon nitride that utilizes the gas big gun to load at Appl.Phys.Lett. on the 76th phase, and the output that the single compound experiment obtains also has only about 100 milligrams.The same year, people such as Denmark scholar Jiang and German scholar Schwarz also utilized many tops anvil (MA) high pressure technique synthesis of cubic silicon nitride polycrystalline specimen respectively, but the only about 6-7 milligram of the output (Europhys.Lett. that their single compound experiment obtains, 2000,51:62-67 and Advanced Mater., 2000,12:883-887.).
In sum, utilize the synthetic cubic silicon nitride new material of prior art only can satisfy the needs of laboratory scientific research, can't satisfy commercial Application.Existing technology synthesis of cubic silicon nitride output is low excessively, and the condition harshness, cost costliness, laboratory operation complexity.Be difficult to satisfy the demand of the cheap cubic silicon nitride material of a large amount of preparations.
Summary of the invention
In order to overcome the cubic silicon nitride material preparation condition harshness that prior art exists, the weak point that yields poorly the invention provides a kind of shock wave synthetic method and synthesizer thereof of cubic silicon nitride material.
Shock wave high pressure and hot conditions that the shock wave synthetic method of cubic silicon nitride material of the present invention mainly utilizes synthesizer detonation to produce realize the synthetic of cubic silicon nitride.
The shock wave synthetic method of cubic silicon nitride material of the present invention comprises the following steps: successively
A. be 80%～90% copper powder with the quality percentage composition with content be 10%～20% α mutually (or β phase) beta-silicon nitride powder raw material mix, and put to agate mortar and grind evenly;
B. ground raw mix is joined in the cover of copper raw material chamber, pressurize on hydraulic press with the piston type depression bar, pressure is 2Mpa～10Mpa compacting, and the cover sealing of raw material chamber is formed raw material box;
C. raw material box is placed the retracting device part;
D. again in retracting device part upper end assembling detonation charger part;
E. in the cartridge bottom of detonation charger part the copper film flying is installed;
F. in cartridge, pour the nitromethane liquid explosives into then;
G. at last at powder charge bucket upper end assembling detonator;
H. cap sensitive nitromethane master explosive, the detonation charger is partly worked, the raw material in the compression and back receiving apparatus part in the raw material box, raw material generation phase transition under high pressure is converted into a cube phase silicon nitride.
Copper screw rod is adopted in raw material chamber cover sealing among the step b.
Copper film flying among the step e is diameter 60mm, the copper coin sheet of thick 1mm.
Nitromethane liquid explosives explosive payload among the step f is 1.5kg～2.0kg.
The synthesizer that is used for the shock wave synthetic method of cubic silicon nitride material comprises retracting device part, detonation charger part.
The outermost end parts of retracting device part are a momentum ring, and the momentum ring is become by the cylindrical iron system of hollow; Be provided with an iron lining topmost in the ring of momentum ring, lay raw material box in the iron lining, raw material box is made up of raw material chamber cover and screw rod, and the material of raw material box is a copper; The lower end is provided with cylindrical iron body momentum piece in the ring of momentum ring.
The detonation charger partly contains detonator, main explosive and film flying, and film flying is arranged on the bottom of cartridge; The main explosive of adorning is the nitromethane liquid explosives in the cartridge; Detonator is equipped with in powder charge bucket upper end.Detonation charger part places retracting device part upper end by pole.
Low pressure six side's beta-silicon nitride powders refer to α phase or beta phase silicon nitride powder, and the granularity of powder material is about 1 μ m～10 μ m, and the quality percentage composition is 10%～20%.
The quality percentage composition of the copper powder that adds is 80%～90%, and granularity is 200 orders～300 orders, and copper powder here as being cooling agent, mainly plays a part to cool.
The compacting of copper powder and low pressure phase silicon nitride powder mixture is to utilize the piston type depression bar to pressurize on hydraulic press, and pressure is 2Mpa～10Mpa.
What the explosive in the plane film flying charger that explosive detonation drives adopted is the nitromethane liquid explosives, and the film flying material is an oxygen-free copper, involves the higher target speed of hitting to obtain planar impact.
Raw material chamber cover and copper screw rod in the retracting device part all adopt oxygenless copper material, with effective protection raw material box body not by impact wreckage and realize the complete recovery of raw material.
For protect the raw material box body not by impact wreckage realizing the complete recovery of raw material, and not with low pressure six side's silicon nitride powder precursor reactants, adopted oxygen-free copper to make the raw material box material.For avoiding raw material box fried chamber under the high-temperature and high-pressure conditions effect, to occur, in the retracting device partial design momentum piece so that the effective pressure in the unloading raw material box fast.As detonation charger part, adopt the nitromethane liquid explosives, to obtain the good planar impact ripple of flatness, the collision film flying adopts oxygenless copper material, can improve impact velocity, drive during the work of detonation charger and hit target film flying high-speed motion, the raw material box in the retracting device part is subjected to the high-speed impact of film flying, and the raw material that loads will experience UNDER SHOCK COMPRESSION in the box.After the pulse compression of the shock wave pressure of the coupling that is subjected to shock wave pressure 50Gpa～60Gpa, impact temperature 3600K～5000K and temperature, α mutually or beta phase silicon nitride raw material generation phase transition under high pressure be converted into cubic silicon nitride.
Adopt preparation method of the present invention, can obtain in a large number, more cheap cubic silicon nitride material.The product volume of single compound experiment reaches the gram magnitude.Method of the present invention has better industrial application prospects, helps people more fully to understand and be familiar with the characteristic of cubic silicon nitride, expands its range of application in industrial technology.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples.
Fig. 1 is the structural representation of synthesizer of the present invention.
Fig. 2 is the X-ray diffractogram that adopts the powder body of cubic silicon nitride of the present invention's preparation.
1. detonators, 2. upper cover plates, 3. cartridges, 4. main explosive 5. film flyings 6. lower covers 7. poles 8. iron linings 9. raw material box 10. filling raw materials 11. momentum rings 12. momentum pieces among the figure
The specific embodiment
In the shock wave synthetic method of cubic silicon nitride material of the present invention, it is synthetic with the phase transformation that realizes material to have adopted special-purpose synthesizer to produce HTHP, promptly utilize the blast of explosive can drive film flying high velocity impact raw material box, in raw material box, produce instantaneous HTHP, make that being filled in α in the target box or beta phase silicon nitride raw material undergone phase transition by the pulse shock compression to change into cubic silicon nitride.
Fig. 1 is the structural representation of synthesizer of the present invention, and synthesizer comprises detonation charger part and retracting device part, and whole device profile is cylindric.
Among the figure, the detonation charger partly contains detonator 1, main explosive 4, film flying 5, upper cover plate 2 and lower cover 6, and the top of cartridge 3 and bottom are respectively arranged with upper cover plate 2 and lower cover 6, and film flying 5 is arranged on the bottom of cartridge 3; Adorn main explosive 4 in the cartridge 3 and be the nitromethane liquid explosives; Detonator 1 is equipped with in powder charge bucket 3 upper ends, and detonation charger part places retracting device part upper end by pole 7.
The outermost end parts of retracting device part are a momentum ring 11, and momentum ring 11 is become by the cylindrical iron system of hollow; Be provided with an iron lining 8 topmost in the ring of momentum ring 11, lay raw material box 9 in the iron lining 8, raw material box 9 is made up of raw material chamber cover and screw rod, and the material of raw material box 9 is a copper; The lower end is provided with cylindrical iron body momentum piece 12 in the ring of momentum ring 11.
The course of work of the present invention is: by detonator 1 main explosive 4 is ignited, main then explosive 4 detonation driven film flyings 5 high-speed motions, film flying 5 high-speed impacts produce the filling raw material 10 in the instantaneous compression and back receiving apparatus part of shock wave; Retracting device partly is provided with and absorbs residue shock wave energy, the momentum ring 11 that is used to realize the complete recovery of raw material, momentum piece 12.
In synthesizer of the present invention, nitromethane master explosive 4 doses of being adorned in the cartridge 3 are 1.5kg～2.0kg, and copper film flying 5 is the disk of diameter 60mm.Determined main explosive 4 doses and film flying 5 parameters, just can guarantee detonation charger part can export synthesize required coupling shock wave pressure and temperature, i.e. shock wave pressure 50Gpa～60Gpa, impact temperature 3600K～5000K.Adopt the good copper product of ductility to make film flying 5, enough impact strengths are arranged, guarantee that raw material box 9 does not break, raw material can intactly be reclaimed to guarantee retracting device.
Embodiment 1
The α phase silicon nitride powder that takes by weighing 2.3 gram particle degree and be 1 μ m～10 μ m is made initial feed, taking by weighing 9.2 gram particle degree again is that 200 orders～300 purpose copper powders and α phase silicon nitride raw material mix, wherein copper powder is an additive, mainly play a part to cool, its quality percentage composition is 90%, the α phase silicon nitride powder is a raw material, and its quality percentage composition is 10%.Mixed raw material put to agate mortar grinds half an hour, subsequently ground compound is poured in the cover of copper raw material chamber, again with press with mixed material compacting in the cover of raw material chamber, pressure is 5Mpa.Raw material box 9 is placed the retracting device part, again in retracting device part upper end assembling detonation charger part, the diameter of packing in cartridge 3 bottoms is 60mm, thick is the copper film flying 5 of 1mm, in cartridge 3, pour nitromethane liquid master explosive 4 into then, institute's explosive payload is about 1.6kg, at last at powder charge bucket 3 upper ends assembling detonator 1.
Detonator 1 is ignited nitromethane master explosive 4, and the detonation charger is partly worked, and drives copper film flying 5 high-speed motions, and the raw material box 9 in the retracting device part is subjected to the high-speed impact of copper film flying 5, and the filling raw material 10 in the raw material box 9 will experience UNDER SHOCK COMPRESSION.After the pulse compression of the shock wave pressure of the coupling that is subjected to shock wave pressure 50Gpa～60Gpa, impact temperature 3600K～5000K and temperature, α mutually or beta phase silicon nitride raw material generation phase transition under high pressure be converted into cubic silicon nitride.
Claims (7)
1. the shock wave synthetic method of a cubic silicon nitride material is characterized in that: comprise the following steps successively
A. copper powder and the content that with the quality percentage composition is 80%-90% be 10%-20% α mutually (or β phase) beta-silicon nitride powder raw material mix, and put to agate mortar and grind evenly;
B. ground raw mix is joined in the cover of copper raw material chamber, pressurize on hydraulic press with the piston type depression bar, pressure is 2Mpa～10Mpa compacting, and sealing raw material chamber cover forms raw material box;
C. raw material box is placed the retracting device part;
D. again in retracting device part upper end assembling detonation charger part;
E. in the cartridge bottom of detonation charger part the copper film flying is installed;
F. in cartridge, pour the nitromethane liquid explosives into then;
G. at last at powder charge bucket upper end assembling detonator;
H. cap sensitive nitromethane master explosive, the detonation charger is partly worked, the raw material in the compression and back receiving apparatus in the raw material box, raw material generation phase transition under high pressure is converted into a cube phase silicon nitride.
2. according to the shock wave synthetic method of the cubic silicon nitride material of claim 1, it is characterized in that: copper screw rod is adopted in the raw material chamber cover sealing among the step b.
3. according to the shock wave synthetic method of the cubic silicon nitride material of claim 1, it is characterized in that: the copper film flying among the step e is diameter 60mm, the copper coin sheet of thick 1mm.
4. according to the shock wave synthetic method of the cubic silicon nitride material of claim 1, it is characterized in that: the nitromethane liquid explosives explosive payload among the step f is 1.5kg～2.0kg.
5. be used for the synthesizer of shock wave synthetic method of the cubic silicon nitride material of claim 1, it is characterized in that: described synthesizer comprises retracting device part, detonation charger part.
6. the synthesizer that is used for the shock wave synthetic method of cubic silicon nitride material according to claim 5 is characterized in that: the outermost end parts of described retracting device part are a momentum ring (11), and momentum ring (11) is become by the cylindrical iron system of hollow; Be provided with an iron lining (8) topmost in the ring of momentum ring (11), lay raw material box (9) in the iron lining (8), raw material box (9) is made up of raw material chamber cover and screw rod, and the material of raw material box (9) is a copper; The lower end is provided with cylindrical iron body momentum piece (12) in the ring of momentum ring (11).
7. the synthesizer that is used for the shock wave synthetic method of cubic silicon nitride material according to claim 5, it is characterized in that: described detonation charger partly contains detonator (1), main explosive (4), film flying (5), upper cover plate (2) and lower cover (6), the top of cartridge (3) and bottom are respectively arranged with upper cover plate (2) and lower cover (6), and film flying (5) is arranged on the bottom of cartridge (3); Institute's main explosive of adorning (4) is the nitromethane liquid explosives in the cartridge (3); Detonator (1) is equipped with in powder charge bucket (3) upper end, and the detonation charger partly places the upper end of retracting device part by pole (7).
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530956A (en) * | 2011-12-07 | 2012-07-04 | 中国工程物理研究院流体物理研究所 | Explosive impact synthesis method for RuSi |
| CN103245574A (en) * | 2013-05-04 | 2013-08-14 | 太原科技大学 | Method and device for driving loading of metal flying piece by multistage detonation of explosive |
| CN103386279A (en) * | 2012-05-10 | 2013-11-13 | 丰映科技股份有限公司 | Continuous chemical reaction method and detonation reactor using continuous chemical reaction method |
| CN114777585A (en) * | 2022-03-22 | 2022-07-22 | 中国工程物理研究院流体物理研究所 | Fixing device and method for measuring action time of detonator |
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2006
- 2006-11-02 CN CN 200610022182 patent/CN1973983A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530956A (en) * | 2011-12-07 | 2012-07-04 | 中国工程物理研究院流体物理研究所 | Explosive impact synthesis method for RuSi |
| CN103386279A (en) * | 2012-05-10 | 2013-11-13 | 丰映科技股份有限公司 | Continuous chemical reaction method and detonation reactor using continuous chemical reaction method |
| CN103386279B (en) * | 2012-05-10 | 2015-06-24 | 丰映科技股份有限公司 | Continuous chemical reaction method and detonation reactor using continuous chemical reaction method |
| CN103245574A (en) * | 2013-05-04 | 2013-08-14 | 太原科技大学 | Method and device for driving loading of metal flying piece by multistage detonation of explosive |
| CN114777585A (en) * | 2022-03-22 | 2022-07-22 | 中国工程物理研究院流体物理研究所 | Fixing device and method for measuring action time of detonator |
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