CN104909792B - A kind of continuous lod zirconium carbide based composites and preparation method thereof - Google Patents
A kind of continuous lod zirconium carbide based composites and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of continuous lod zirconium carbide based composites and preparation method thereof, belong to high-temperature hot protective material technical field.Continuous lod zirconium carbide based composites prepared by the present invention has the excellent properties such as lightweight, high temperature resistant and antioxidation, density 1.9～2.2g/cm3, hot strength 96～150MPa, bending/compressive strength 130～180MPa, mass loss only 10 under 2000 DEG C of aerobic environments‑4g/cm2S magnitude, shows preferable combination property advantage, can be applicable to novel hypersonic aircraft, speed reentry aircrafts, the reusable high-temperature hot guard system of maneuvering-vehicle and advanced power systems etc. in-orbit.
Description
Technical field
The present invention relates to a kind of continuous lod zirconium carbide based composites and preparation method thereof, be the company of utilization
Continuous prefabricated carbon fiber body be skeleton, zirconium carbide and carborundum multicomponent mixture be that matrix uses liquid impregnation cracking
Method obtains a kind of continuous lod zirconium carbide based composites, belongs to high-temperature hot protective material technical field.
Background technology
Along with the developing rapidly of competition and space technology of Armada International science and technology, spacecraft to lightweight, efficient,
Quickly, the performance of the aspect such as reliable pursue increasingly stronger, certainly will also Material Field be proposed big challenge.
High-temperature hot protective material refers to keep preferable physics under high temperature, superhigh temperature Service Environment and reaction atmosphere
With a class material of chemical stability, it it is novel hypersonic aircraft, speed reentry aircrafts, repeatable
Use maneuvering-vehicle and advanced power systems in-orbit to succeed in developing and keep excellent war target basis with crucial.
High-temperature hot protective material mainly includes superhigh temperature ceramic material, carbon/carbon, carbon/carborundum etc..Wherein, superhigh temperature
Ceramic material fusing point is high, and antioxygenic property is excellent, but fragility is big, thermal shock resistance is not enough；Carbon/carbon high-temp
Excellent in mechanical performance, but antioxygenic property is not enough；Carbon/carborundum antioxygenic property and mechanical property are all preferable,
But temperature resistant grade is the highest, it is difficult to meet more than 1750 DEG C and use for a long time.Develop 2000 DEG C of high temperature above aerobics
The material used under environment is focus and the difficult point of current thermally protective materials technical field, is also that restriction series is new
One of Pinch technology that type spacecraft is developed.
Summary of the invention
The invention aims to solve existing high-temperature hot protective material difference and meet thermal shock resistance simultaneously
Not enough with antioxygenic property, a kind of continuous lod zirconium carbide based composites and preparation method thereof is proposed,
Having the combination property of excellence under this material at high temperature aerobic environment, the method technical process is simple, is suitable for work
Journeyization is applied.
It is an object of the invention to be achieved through the following technical solutions.
A kind of continuous lod zirconium carbide based composites of the present invention, this material is pre-with continuous carbon fibre
Body processed is that skeleton plays power transmission carrying and keeps the effect of structural reliability effect, and carbon fiber surface has certain thickness
Carbon fiber is played interface protective effect, with the many tuples of zirconium carbide and carborundum by degree (1.5～2.0 μm) matrix carbon
It is divided into matrix that the space between prefabricated carbon fiber body skeleton is filled with, plays high-temperature oxidation resistance effect.
Wherein, carbon fiber is T300 or T700 aerospace level；
Precursor structure is as the criterion three-dimensional or three-dimensional, including acupuncture, carefully compiles puncture；
Zirconium carbide mean diameter 0.5～2 μm；Carborundum mean diameter 0.5～2 μm；Gross mass with composite
Being 100% calculating, carbon fiber mass fraction is 30%～45%, and fiber surface matrix carbon mass fraction is
20%～30%, zirconium carbide mass fraction is 20%～30%, and carborundum mass fraction is 10%～15%.
The preparation method of a kind of continuous lod zirconium carbide based composites of the present invention, the method is with carbon
Fiber preform is reinforcement, introduces certain content matrix carbon by gas-phase permeation technique and fiber is played interface
Protection, with liquid impregnation, solidification, the cracking technology certain content zirconium carbide of introducing and carborundum as matrix,
During introducing, in order to improve the introducing efficiency of different times, design has selected early stage to adulterate with ceramic powders
Resin is physics introducing method and the later stage chemical introducing method with ceramic forerunner as carrier of carrier, effectively
Solve and introduce content and introduce the contradictory problems of uniformity, it is achieved that ceramic matrix component efficient, uniform
Introduce, on the premise of keeping mechanical property, structural reliability and the antioxygenic property of material is greatly improved.
Concretely comprising the following steps of the method:
1) continuous carbon fibre precast body is carried out interface sink carbon process, treatment temperature is 950～1050 DEG C, insulation
1～2h, totally 2～3 times, obtain low-density fibre skeleton blank；
2) by zirconium carbide powder and silicon carbide powder with dehydrated alcohol as dispersant, carry out point initially with ultrasonic
Dissipating, then carry out high speed ball milling, finally carry out rotary evaporator evaporation and dry, the ultrasonic disperse time is 1～2h,
Ball-milling Time is 8～10h, obtains hybrid ceramic powder body；
3) by step 2) ceramic powder that obtains mixes with phenolic resin, dehydrated alcohol, obtains mixture,
Ceramic powder and phenolic resin mass ratio are 1:1～3, and ceramic powder is 1:0.5～2 with the mass ratio of dehydrated alcohol.
Mixture sequentially passes through high speed machine stirring, ultrasonic disperse, high speed sand milling, and high speed machine mixing time is
0.5-1h, the ultrasonic disperse time 0.5～1h, the high speed sand milling time 1～2h, the resin obtaining doped ceramics powder body is molten
Liquid；
4) step 3 is utilized) resin solution that obtains is to step 1) the low-density fibre skeleton blank that obtains depends on
Secondary carry out impregnating, solidify, carbonization and Pintsch process.Dipping point vacuum impregnation and pressure impregnation, first carried out
Vacuum impregnation, then carries out pressure impregnation, and vacuum impregnation pressure is gauge pressure-0.1MPa, the dwell time 2～4h,
Pressure impregnation pressure is 1～5MPa, pressurize 2～4h；Solidification temperature is 180～220 DEG C, insulation 2～4h；Carbon
Changing temperature is 750～900 DEG C, insulation 2～5h, and Pintsch process temperature is 1800～2200 DEG C, insulation 1～3h.
Repeat 3～4 times, obtain half densified fiber and strengthen zirconium carbide based composites；
5) Polymer ceramic precursor is utilized to step 4) to strengthen carbonization zirconio multiple for half densified fiber that obtains
Condensation material impregnates further, solidifies, carbonization and cracking.Dipping, solidification, the same step 4) of carbonization technique,
Pintsch process temperature is 1300～1600 DEG C, is incubated 2～4h.Repeat 6～8 times, obtain the continuous fiber of densification
Strengthen zirconium carbide based composites.
The continuous lod zirconium carbide based composites prepared by said method carries out mechanical property and antioxidation
Performance test, and microstructure after its bearer properties and oxidation is observed and analyzed.
Beneficial effect
Continuous lod zirconium carbide based composites prepared by the present invention has lightweight, high temperature resistant and antioxidation
Deng excellent properties, density 1.9～2.2g/cm3, hot strength 96～150MPa, bending/compressive strength
130～180MPa, mass loss only 10 under 2000 DEG C of aerobic environments-4g/cm2S magnitude, shows preferably
Combination property advantage, can be applicable to novel hypersonic aircraft, speed reentry aircrafts, reusable
The high-temperature hot such as maneuvering-vehicle and advanced power systems guard system in-orbit.
Detailed description of the invention
A kind of continuous lod zirconium carbide based composites, skeleton is continuous carbon fibre precast body, its surface
For deposition carbon protective layer, matrix is the refractory ceramics component such as zirconium carbide, carborundum.With gross mass for 100%
Calculating, carbon fiber mass fraction is 30%～45%, and fiber surface matrix carbon mass fraction is 20%～30%, carbon
Changing zirconium mass fraction is 25%～30%, and carborundum mass fraction is 5%～10%；
Fiber is T300 or T700 aerospace grade carbon fiber, and precursor structure is as the criterion three-dimensional or three-dimensional, including pin
Thorn, the puncture of thin volume etc.；Zirconium carbide, carborundum, mean diameter is 0.5～2 μm, and purity is more than 99.5%；
The preparation method of a kind of continuous lod zirconium carbide based composites, concretely comprises the following steps:
1) continuous fiber precast body is carried out interface sink carbon process, treatment temperature is 950～1050 DEG C, insulation
1～2h, totally 2～3 times, obtain low-density fibre skeleton blank；
2) zirconium carbide powder, silicon carbide powder 4:1～3:2 in mass ratio is mixed, with dehydrated alcohol for dispersion
Agent, uses ultrasonic disperse, high speed ball milling and rotary evaporator evaporation to dry, and the ultrasonic disperse time is 1～2h,
Ball-milling Time is 8～10h, obtains hybrid ceramic powder body；
3) by step 2) ceramic powder that obtains mixes with phenolic resin, dehydrated alcohol, ceramic powder and phenol
Urea formaldehyde mass ratio is 1:1～3, and ceramic powder is 1:0.5～2 with the mass ratio of dehydrated alcohol.Stir through high speed machine
Mix, ultrasonic disperse, high speed sand milling, high speed machine stirring and the ultrasonic disperse time 0.5～1h, during high speed sand milling
Between 1～2h, obtain the resin solution of doped ceramics powder body；
4) step 3 is utilized) resin solution that obtains is to step 1) the low-density fibre skeleton blank that obtains enters
Row dipping, solidification, carbonization and Pintsch process.Dipping point vacuum impregnation and pressure impregnation, vacuum impregnation pressure
For gauge pressure-0.1MPa, dwell time 2～4h, pressure impregnation pressure is 1～5MPa, pressurize 2～4h；Solidification temperature
Degree is 180～220 DEG C, insulation 2～4h；Carburizing temperature is 750～900 DEG C, insulation 2～5h, Pintsch process temperature
Degree is 1800～2200 DEG C, insulation 1～3h.Repeat 3～4 times, obtain half densified fiber and strengthen carbonization zirconio
Composite；
5) Polymer ceramic precursor is utilized to step 4) to strengthen carbonization zirconio multiple for half densified fiber that obtains
Condensation material impregnates further, solidifies, carbonization and cracking.Dipping, solidification, the same step 4) of carbonization technique,
Pintsch process temperature is 1300～1600 DEG C, is incubated 2～4h.Repeat 6～8 times, obtain the continuous fiber of densification
Strengthen zirconium carbide based composites.
Below in conjunction with embodiment, the invention will be further described.But present disclosure is not only confined to
The following examples.
Embodiment 1
A kind of continuous lod zirconium carbide based composites, this material is with T700 carbon fiber needling preform
For skeleton, carbon fiber mass fraction 30%, carbon fiber surface interface matrix carbon-coating mass fraction 30%, carbonization
Zirconium, carborundum mean diameter are 0.5～2 μm, and zirconium carbide mass fraction is 30%, carborundum mass fraction
It is 10%.
The preparation method of a kind of continuous lod zirconium carbide based composites, concretely comprises the following steps:
1) choose a size of 150mm × 150mm × 100mm needling structure precast body and carry out interface deposited carbon layer
Processing, treatment temperature is 1050 DEG C, is incubated 2h, and totally 3 times, the thickness of the carbon-coating of deposition is 5-10 μm,
To low-density fibre skeleton blank,；
2) by zirconium carbide powder more than 99.5% of mean diameter 0.5～2 μm, purity and silicon carbide powder by matter
Measure and mix than 3:1, put in excess dehydrated alcohol and disperse, use ultrasonic disperse, high speed ball milling and rotary evaporation
Device evaporation is dried, and the ultrasonic disperse time is 1h, and Ball-milling Time is 10h, obtains hybrid ceramic powder body；
3) by step 2) ceramic powder that obtains mixes with phenolic resin, dehydrated alcohol, ceramic powder and phenol
Urea formaldehyde mass ratio is 1:1, and ceramic powder is 1:2 with the mass ratio of dehydrated alcohol.Stir through high speed machine,
Ultrasonic disperse, high speed sand milling, high speed machine stirring and ultrasonic disperse time 1h, high speed sand milling time 2h,
Resin solution to doped ceramics powder body；
4) step 3 is utilized) resin solution that obtains is to step 1) the low-density fibre skeleton blank that obtains enters
Row dipping, solidification, carbonization and Pintsch process.Dipping point vacuum impregnation and pressure impregnation, vacuum impregnation pressure
For gauge pressure-0.1MPa, dwell time 2h, pressure impregnation pressure is 3MPa, pressurize 2h；Solidification temperature is 190 DEG C,
Insulation 2h；Carburizing temperature is 850 DEG C, insulation 2h, and Pintsch process temperature is 2000 DEG C, insulation 2h.Repeat
3 times, obtain half densified fiber and strengthen zirconium carbide based composites；
5) Polymer ceramic precursor is utilized to step 4) to strengthen carbonization zirconio multiple for half densified fiber that obtains
Condensation material impregnates further, solidifies, carbonization and cracking.Dipping, solidification, the same step 4) of carbonization technique,
Pintsch process temperature is 1500 DEG C, is incubated 2h.It is repeated 8 times, obtains the continuous lod zirconium carbide of densification
Based composites.
The continuous carbon fibre preparing said method strengthens zirconium carbide based composites and is sampled analyzing, permissible
Find out white phase be zirconium carbide, ash form and aspect be carborundum, zirconium carbide, carborundum are dispersed in fiber interfascicular
Inside cellulose, one layer of deposited carbon layer, average thickness 1.7～2.0 μm are uniformly wrapped up in fibre bundle surface.
The continuous carbon fibre preparing said method strengthens zirconium carbide based composites and carries out performance test and evaluation
Characterize.Test result is: it is 2.1g/cm that (1) drainage records density of material3；(2) universal testing machine is surveyed
Obtain tensile strength of material 96.1MPa, bending strength 130MPa, compressive strength 134MPa；(3) at 2100 DEG C
Under aerobic environment, mass loss rate is 2.0 × 10-4g/cm2s。
Embodiment 2
A kind of continuous lod zirconium carbide based composites, this material is with T700 carbon fiber needling preform
For skeleton, carbon fiber mass fraction 30%, carbon fiber surface boundary layer mass fraction 30%, zirconium carbide, carbon
SiClx mean diameter 0.5～2 μm, zirconium carbide mass fraction is 25%, and carborundum mass fraction is 15%.
The preparation method of a kind of continuous lod zirconium carbide based composites, concretely comprises the following steps:
1) choose a size of 150mm × 150mm × 100mm needling structure precast body and carry out interface deposited carbon layer
Processing, treatment temperature is 1050 DEG C, is incubated 2h, and totally 3 times, the thickness of the carbon-coating of deposition is 5-10 μm,
To low-density fibre skeleton blank；
2) by zirconium carbide powder more than 99.5% of mean diameter 0.5～2 μm, purity and silicon carbide powder by matter
Measure and mix than 5:3, put in excess dehydrated alcohol and disperse, use ultrasonic disperse, high speed ball milling and rotary evaporation
Device evaporation is dried, and the ultrasonic disperse time is 2h, and Ball-milling Time is 8h, obtains hybrid ceramic powder body；
3) by step 2) ceramic powder that obtains mixes with phenolic resin, dehydrated alcohol, ceramic powder and phenol
Urea formaldehyde mass ratio is 1:2, and ceramic powder is 1:1 with the mass ratio of dehydrated alcohol.Stir through high speed machine,
Ultrasonic disperse, high speed sand milling, high speed machine stirring and ultrasonic disperse time 0.5h, high speed sand milling time 1h,
Obtain the resin solution of doped ceramics powder body；
4) step 3 is utilized) resin solution that obtains is to step 1) the low-density fibre skeleton blank that obtains enters
Row dipping, solidification, carbonization and Pintsch process.Dipping point vacuum impregnation and pressure impregnation, vacuum impregnation pressure
For gauge pressure-0.1MPa, dwell time 3h, pressure impregnation pressure is 3MPa, pressurize 3h；Solidification temperature is 190 DEG C,
Insulation 2h；Carburizing temperature is 850 DEG C, insulation 2h, and Pintsch process temperature is 2000 DEG C, insulation 2h.Repeat
2 times, obtain half densified fiber and strengthen zirconium carbide based composites；
5) Polymer ceramic precursor is utilized to step 4) to strengthen carbonization zirconio multiple for half densified fiber that obtains
Condensation material impregnates further, solidifies, carbonization and cracking.Dipping, solidification, the same step 4) of carbonization technique,
Pintsch process temperature is 1500 DEG C, is incubated 2h.It is repeated 10 times, obtains the continuous lod carbonization of densification
Zirconium based composite material.
The continuous carbon fibre preparing said method strengthens zirconium carbide based composites and is sampled analyzing, permissible
Find out white phase be zirconium carbide, ash form and aspect be carborundum, zirconium carbide, carborundum are dispersed in fiber interfascicular
Inside cellulose, one layer of deposited carbon layer, average thickness 1.5～1.9 μm are uniformly wrapped up in fibre bundle surface.
The continuous carbon fibre preparing said method strengthens zirconium carbide based composites and carries out performance test and evaluation
Characterize.Test result is: it is 1.95g/cm that (1) drainage records density of material3；(2) universal testing machine
Record tensile strength of material 98MPa, bending strength 135MPa, compressive strength 140MPa；(3) at 2000 DEG C
Under aerobic environment, mass loss rate is 3.6 × 10-4g/cm2s。
Embodiment 3
A kind of continuous lod zirconium carbide based composites, this material is carefully to compile puncture knot with T300 carbon fiber
Structure precast body is skeleton, carbon fiber mass fraction 45%, carbon fiber surface boundary layer mass fraction 20%, carbon
Changing zirconium, carborundum mean diameter 0.5～2 μm, zirconium carbide mass fraction is 25%, and carborundum mass fraction is
10%.
The preparation method of a kind of continuous lod zirconium carbide based composites, concretely comprises the following steps:
1) choose a size of 120mm × 120mm × 100mm needling structure precast body and carry out interface deposition processes,
Treatment temperature is 1050 DEG C, is incubated 2h, and totally 3 times, the thickness of the carbon-coating of deposition is 5-10 μm, obtains low close
Degree fiber reinforcement blank；
2) by zirconium carbide powder more than 99.5% of mean diameter 0.5～2 μm, purity and silicon carbide powder by matter
Measure ratio 2.5:1 mixing, put in excess dehydrated alcohol and disperse, use ultrasonic disperse, high speed ball milling and rotate steaming
Sending out device evaporation to dry, the ultrasonic disperse time is 2h, and Ball-milling Time is 8h, obtains hybrid ceramic powder body；
3) by step 2) ceramic powder that obtains mixes with phenolic resin, dehydrated alcohol, ceramic powder and phenol
Urea formaldehyde mass ratio is 1:3, and ceramic powder is 1:1 with the mass ratio of dehydrated alcohol.Stir through high speed machine,
Ultrasonic disperse, high speed sand milling, high speed machine stirring and ultrasonic disperse time 1h, high speed sand milling time 2h,
Resin solution to doped ceramics powder body；
4) step 3 is utilized) resin solution that obtains is to step 1) the low-density fibre skeleton blank that obtains enters
Row dipping, solidification, carbonization and Pintsch process.Dipping point vacuum impregnation and pressure impregnation, vacuum impregnation pressure
For gauge pressure-0.1MPa, dwell time 2h, pressure impregnation pressure is 3MPa, pressurize 2h；Solidification temperature is 190 DEG C,
Insulation 2h；Carburizing temperature is 850 DEG C, insulation 2h, and Pintsch process temperature is 2000 DEG C, insulation 2h.Repeat
3 times, obtain half densified fiber and strengthen zirconium carbide based composites；
5) Polymer ceramic precursor is utilized to step 4) to strengthen carbonization zirconio multiple for half densified fiber that obtains
Condensation material impregnates further, solidifies, carbonization and cracking.Dipping, solidification, the same step 4) of carbonization technique,
Pintsch process temperature is 1500 DEG C, is incubated 2h.It is repeated 8 times, obtains the continuous lod zirconium carbide of densification
Based composites.
The continuous carbon fibre preparing said method strengthens zirconium carbide based composites and is sampled analyzing, permissible
Find out white phase be zirconium carbide, ash form and aspect be carborundum, zirconium carbide, carborundum are dispersed in fiber interfascicular
Inside cellulose, one layer of deposited carbon layer, average thickness 1.8～2.0 μm are uniformly wrapped up in fibre bundle surface.
The continuous carbon fibre preparing said method strengthens zirconium carbide based composites and carries out performance test and evaluation table
Levy.Test result is: it is 2.0g/cm that (1) drainage records density of material3；(2) universal testing machine records
Tensile strength of material 150MPa, bending strength 180MPa, compressive strength 175MPa；(3) at 2000 DEG C
Under aerobic environment, mass loss rate is 5.6 × 10-4g/cm2s。
Claims (1)
1. a preparation method for continuous lod zirconium carbide based composites, this composite is with carbon fiber
Precast body is skeleton, and carbon fiber surface has matrix carbon, fills zirconium carbide and carborundum between the space of skeleton；
Zirconium carbide mean diameter 0.5～2 μm；Carborundum mean diameter 0.5～2 μm；Gross mass with composite
Being 100% calculating, carbon fiber mass fraction is 30%～45%, and matrix carbon mass fraction is 20%～30%, carbon
Changing zirconium mass fraction is 20%～30%, and carborundum mass fraction is 10%～15%；
It is characterized in that steps of the method are:
1) prefabricated carbon fiber body is carried out interface sink carbon process, treatment temperature is 950～1050 DEG C, be incubated 1～2h,
Obtain low-density fibre skeleton blank；
2) by zirconium carbide powder and silicon carbide powder with dehydrated alcohol as dispersant, carry out point initially with ultrasonic
Dissipating, then carry out high speed ball milling, finally carry out rotary evaporator evaporation and dry, the ultrasonic disperse time is 1～2h,
Ball-milling Time is 8～10h, obtains hybrid ceramic powder body；
3) by step 2) ceramic powder that obtains mixes with phenolic resin, dehydrated alcohol, obtains mixture,
Ceramic powder and phenolic resin mass ratio are 1:1～3, and ceramic powder is 1:0.5～2 with the mass ratio of dehydrated alcohol；
Mixture sequentially passes through high speed machine stirring, ultrasonic disperse, high speed sand milling, and high speed machine mixing time is
0.5-1h, the ultrasonic disperse time 0.5～1h, the high speed sand milling time 1～2h, the resin obtaining doped ceramics powder body is molten
Liquid；
4) step 3 is utilized) resin solution that obtains is to step 1) the low-density fibre skeleton blank that obtains depends on
Secondary carry out impregnating, solidify, carbonization and Pintsch process；Dipping point vacuum impregnation and pressure impregnation, first carried out
Vacuum impregnation, then carries out pressure impregnation, and vacuum impregnation pressure is gauge pressure-0.1MPa, the dwell time 2～4h,
Pressure impregnation pressure is 1～5MPa, pressurize 2～4h；Solidification temperature is 180～220 DEG C, insulation 2～4h；Carbon
Changing temperature is 750～900 DEG C, insulation 2～5h, and Pintsch process temperature is 1800～2200 DEG C, insulation 1～3h；
Obtain half densified fiber and strengthen zirconium carbide based composites；
5) utilize zirconium carbide, carborundum Polymer ceramic precursor to step 4) the half fine and close chemical fibre that obtains
Dimension strengthen zirconium carbide based composites impregnate further, solidify, carbonization and cracking；Dipping point Vaccum Permeating
Stain and pressure impregnation, first carry out vacuum impregnation, then carry out pressure impregnation, and vacuum impregnation pressure is gauge pressure
-0.1MPa, dwell time 2～4h, pressure impregnation pressure is 1～5MPa, pressurize 2～4h；Solidification temperature is
180～220 DEG C, insulation 2～4h；Carburizing temperature is 750～900 DEG C, insulation 2～5h, and cracking temperature is
1300～1600 DEG C, it is incubated 2～4h, obtains the continuous lod zirconium carbide based composites of densification.
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| CN111875400B (en) * | 2020-08-13 | 2022-12-23 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of high-temperature heat-insulating material containing zirconium carbide |
| CN112409003B (en) * | 2020-11-09 | 2022-09-27 | 航天材料及工艺研究所 | Hybrid matrix silicon carbide-based composite material and preparation method thereof |
| CN117945775A (en) * | 2024-03-21 | 2024-04-30 | 西安源创航空科技有限公司 | C (C)fPreparation method of ZrC ceramic composite material |
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2015
- 2015-05-27 CN CN201510280643.0A patent/CN104909792B/en active Active
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| CN107746278A (en) * | 2017-10-30 | 2018-03-02 | 湖北三江航天江北机械工程有限公司 | The manufacture method of solid propellant rocket gas regulator butterfly valve |
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