CN104316372A - Preparation method of breaking tenacity sample made of ceramic material - Google Patents
Preparation method of breaking tenacity sample made of ceramic material Download PDFInfo
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- CN104316372A CN104316372A CN201410565994.1A CN201410565994A CN104316372A CN 104316372 A CN104316372 A CN 104316372A CN 201410565994 A CN201410565994 A CN 201410565994A CN 104316372 A CN104316372 A CN 104316372A
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Abstract
The invention discloses a preparation method of a breaking tenacity sample made of a ceramic material, which adopts a specially-made mould and a tenacity sheet. The preparation method comprises the following steps: firstly fixing the tenacity sheet with certain size on a certain position in the cavity of the mould, so that the tenacity sheet after slip casting is just embedded the gap position where the sample appears; preparing a sizing agent with good mobility according to a set formula, pouring the sizing agent into the specially-made mould, supplementing materials continuously till the sizing agent does not sink; opening the mould after 1h, taking out the ceramic biscuit after pouring, and placing the ceramic biscuit in a dry and shady place; sintering the ceramic biscuit according to set sintering schedule after 2-3 days. With the method for preparing the breaking tenacity sample made of fine ceramic, the ceramic sample having the gap with width being smaller than or equal to 0.15mm can be obtained, the root of the gap has an original crack, so as to meet the requirements of most ceramic breaking tenacity detection methods requiring precracks for samples.
Description
Technical field
The present invention relates to a kind of detection method of material mechanical performance, particularly relate to a kind of detection method of hard brittle material fracture mechanical property, be applied to hard brittle material forming technique and Quality Control Technology field.
Background technology
Fine ceramics material has high rigidity, high-melting-point, the excellent performance such as wear-resistant, corrosion-resistant, therefore has important application in fields such as metallurgy, aerospace, the energy, machinery, optics.But the same with most stupalith, most of fine ceramics is also a kind of hard brittle material, the mode of its fracture is brittle fracture, so fine ceramics material is very responsive to crackle.Based on this characteristic of fine ceramics, fracture mechanical property is the important indicator evaluating its mechanical property, wherein uses the most general breaking mechanics parameter to be fracture toughness K
iC.
At present, the method of testing of ceramic materials fracture toughness mainly contains SENB (SENB, Single Edge Nothed Beam) method, micro indentation (MI, Microfracture Indentation) method, crease strength (ISB, Indentation Strength in Beam) method, double cantilever beam (DCB, Double Cantilever beam) method, twoly turn round (DT, Double Torsion) method etc.Wherein Single edge notch beam and hardness method use comparatively general.
Micro indentation (MI) method is a kind of method that the crack length that produced by impression and corner thereof Vickers hardness measures while and Vickers hardness number are tried to achieve, advantage is easily operation and less demanding to sample, shortcoming refer to more approximate condition in the derivation of computing formula, the fracture toughness obtained can produce the deviation being approximately 20% ~ 30%, and this just makes the measuring accuracy of MI method and reliability all receive impact to a certain degree.
SENB (SENB) method uses the most general method, is also universally recognized standard method of test, because SENB law theory is perfect, method of testing simple, records K
iCthe result that value obtains than additive method is accurate, and is applicable to test in high temperature or atmosphere.When adopting SENB method test ceramic materials fracture toughness, the method of usual employing machining cuts out in test specimen stress surface side the breach that width is 0.25 ~ 0.30 mm, replacing crackle with this breach, then using the method for three-point bending to be broken, by calculating the fracture toughness of material.But for a lot of brittle ceramic materials, conventional machining is difficult to the breach obtaining 0.25 ~ 0.30 mm width, and breach is wider, and the stress concentration degree produced is less, and the Fracture Toughness recorded is then higher.Strictly speaking, obtain Fracture Toughness accurately, test should adopt the sample with Original Cracks to test.Therefore, it is a committed step that the notch base gone out in machining carries out presplitting process.The method producing crackle at present mainly contains: press-pressure cyclic fatigue method, bridge indentation method, polishing, carve people's method, the front system of sintering splits method and stress corrosion method etc.Pressure-pressure cyclic fatigue method is often used in the presplitting of metal material sample, and for fine ceramics material, because having firmly crisp characteristic, using and pressing cyclic fatigue method more much more difficult than metal to cause Original Cracks.Bridge platen press is the method for a kind of precrack for hard brittle material proposition, GB/T 23806-2009, namely fine ceramics fracture toughness test method monolateral pre-CRACKED BEAM (SEPB) method has made detailed description to bridge platen press crackle fabricated device and using method, the method does not need the experimental facilities of complex and expensive, simple to operate, national standard is chosen to be, i.e. JIS R1617-2002: one of fine ceramic fracture toughness test method under high temperature in Japan.But the problems such as bridge platen press exists that the degree of depth of crackle is wayward, the xsect of the direction of crack initiation and test specimen is not parallel, easily produce the drift angle being greater than 10 °, and the impact being subject to impression quality are very large.
Summary of the invention
In order to solve prior art problem, the object of the invention is to the deficiency overcoming prior art existence, a kind of fracture toughness specimen preparation method of stupalith is provided, the sample of preparation is with Original Cracks, and one-step shaping, does not need expensive device, simple to operate, and customization is strong, can meet the geomery requirement of most of fracture toughness specimen, especially be applicable to being applied to the preparation for fine ceramics fracture toughness specimen.
Create object for reaching foregoing invention, the present invention adopts following technical proposals:
A fracture toughness specimen preparation method for stupalith, comprises the steps:
A. the preparation of sectional die: adopt sectional die shape system, mould is made to have two parts matched moulds module, according to outer contoured shape and the dimensional requirement of the fracture toughness specimen of stupalith, the mold cavity of processing customization hollow, when two parts matched moulds block merging is assembled into full die, one end open along mold cavity depth direction forms sprue gate, mould adopts gypsum or lime to make, need the dimensional requirement of prefabricated breach according to the fracture toughness specimen of test experiments to stupalith simultaneously, make the toughness flake of a slice Hou Du≤0.15mm, and according to the position of breach at the fracture toughness specimen of stupalith, toughness flake is mounted on the corresponding position in the groove of a module of mould, thus toughness flake is assembled in mold cavity, make the plane orthogonal of toughness flake in die cavity depth direction, when mould sprue gate upwards time, mold cavity depth direction is parallel with vertical direction, and toughness flake's level is horizontally disposed with, it is the die tip shell of one of them module of mould directly over toughness flake, cast slurry injects from the sprue gate of mould and freely falls into the not direct impact flexibility thin slice of process bottom mold cavity, the material that described toughness flake adopts incendivity to decompose is made,
B. the fracture toughness specimen raw material of stupalith prepares: take ceramic sample feed composition material respectively according to the fracture toughness specimen constituent mass ratio of stupalith, wherein ceramic powders takes 100 parts, deionized water takes 0 ~ 14 part, gum arabic takes 0 ~ 14 part, spreading agent takes 0 ~ 0.16 part, Li Du≤the 1.8um of ceramic powders, is evenly fully mixed and made into ceramic sample slurry for subsequent use by each feed composition;
C. ceramic sample slurry cast: the ceramic sample slurry prepared in described step b is slowly poured in the mould prepared in described step a, along with the slurry in mold cavity constantly sinks to carrying out to continue to supplement the feeding of ceramic sample slurry, until the slurry in mold cavity no longer sinks, at least after cast starts 1h, carry out die sinking, obtain ceramic sample biscuit, ceramic sample biscuit is taken out, be placed in dry sunshade place for subsequent use, the toughness flake prepared in described step a is embedded on ceramic sample biscuit;
D. ceramic sample sintering: after the ceramic sample biscuit being embedded with toughness flake prepared in described step c is placed 2-3 days, experimentally test the sintering schedule of the pottery used, ceramic sample element is sintered, after toughness flake's combustion decomposition, make ceramic sample predetermined position to leave width and be not more than 0.15mm breach, after sintering process completes, obtain the fracture toughness specimen being with stupalith that is jagged and that crack at root of notch.
The length of the notch depth on the fracture toughness specimen of above-mentioned stupalith and root of notch crackle is preferentially adjusted by the shape and size of toughness flake.
Lime mould is made in preferred employing water and unslaked lime reaction solidification.
Above-mentioned toughness flake is preferably polyvinyl chloride film.
Preferential employing wet ball grinding method prepares above-mentioned ceramic sample slurry.
Preferably take ceramic sample feed composition material respectively according to the fracture toughness specimen constituent mass ratio of stupalith, pour in the ball grinder of 500ml after each for the ceramic sample taken feed composition material is mixed, add the zirconia ceramics ball of at least 4 9g and the zirconia ceramics ball of at least 18 4g again, then ball grinder is placed in tumbling ball mill ball milling at least 9h, rotating speed is adjusted at least 10r/min, prepares ceramic sample slurry.
The present invention compared with prior art, has following apparent outstanding substantive distinguishing features and remarkable advantage:
The present invention prepares the method for fine ceramics fracture toughness specimen, essence belongs to ceramic grout moulding process, in order to obtain being with ceramic sample jaggy, first water before sintering and outpour one is inlayed PVC thin slice biscuit at gap position, concrete implementation method is in advance at the PVC thin slice being fixed certain size by the position of the corresponding breach in the cavity poured into a mould, and after the cast demoulding, PVC thin slice will be embedded in biscuit; Then during sintering, PVC thin slice can the too high and combustion decomposition of Yin Wendu, and then leave breach, the simultaneously burn expansion that causes of PVC thin slice is understood and be cracked at root of notch, the degree of depth of breach and the length of crackle can be adjusted by the length of PVC thin slice, the inventive method is simple, there is obvious economy and practicality, the ceramic fracture toughness detection method of major part needs precrack can be met to the requirement of sample.
Accompanying drawing explanation
Fig. 1 is the sectional die matched moulds using state schematic diagram of the preferred embodiment of the present invention.
Fig. 2 is a module and toughness flake's installment state schematic diagram of the sectional die of the preferred embodiment of the present invention.
Fig. 3 is the ceramic sample biscuit figure of the cast gained of the preferred embodiment of the present invention.
Fig. 4 is the enlarged drawing of empty wire frame positions in Fig. 3.
Fig. 5 is the fracture toughness specimen figure of the stupalith after the preferred embodiment of the present invention has sintered.
Fig. 6 is the enlarged drawing of empty wire frame positions in Fig. 5.
Fig. 7 is the three-point bending resistance test sketch of the fracture toughness specimen of the stupalith using the preferred embodiment of the present invention to prepare.
Fig. 8 is the post-rift assay maps of fracture toughness specimen of stupalith prepared by the preferred embodiment of the present invention.
Embodiment
Details are as follows for the preferred embodiments of the present invention:
In the present embodiment, see Fig. 1 ~ Fig. 8, a kind of fracture toughness specimen preparation method of stupalith, comprises the steps:
A. the preparation of sectional die: adopt sectional die shape system, mould is made to have two parts matched moulds module (1, 2), matched moulds module (1, 2) in-profile is all step shape, according to outer contoured shape and the dimensional requirement of the fracture toughness specimen 5 of stupalith, the mold cavity of processing customization hollow, when two parts matched moulds block merging is assembled into full die, one end open along mold cavity depth direction forms sprue gate 3, mould adopts water and unslaked lime reaction solidification to make lime mould, need the dimensional requirement of prefabricated breach according to the fracture toughness specimen 5 of test experiments to stupalith simultaneously, make the toughness flake 4 that a slice thickness is 0.15mm, and according to the position of breach at the fracture toughness specimen 5 of stupalith, toughness flake 4 is mounted on the middle position of the inner rectangular groove of a module of mould, thus toughness flake 4 is assembled in mold cavity, make the plane orthogonal of toughness flake 4 in die cavity depth direction, when mould sprue gate 3 upwards time, mold cavity depth direction is parallel with vertical direction, and toughness flake 4 level is horizontally disposed with, it is the die tip shell of one of them module of mould directly over toughness flake 4, cast slurry injects from the sprue gate 3 of mould and freely falls into the not direct impact flexibility thin slice 4 of process bottom mold cavity, the vinyl chloride PVC film that described toughness flake 4 adopts the incendivity of cutting to decompose is made, see Fig. 1 and Fig. 2,
B. the fracture toughness specimen raw material of stupalith prepares: take ceramic sample feed composition material respectively according to the fracture toughness specimen 5 constituent mass ratio of stupalith, ginseng is shown in Table 1:
Pour into after mixing in the ball grinder of 500ml, add the zirconia ceramics ball of 4 9g and the zirconia ceramics ball of 18 4g again, then ball grinder is placed in tumbling ball mill ball milling 9h, rotating speed is adjusted to 10r/min, each feed composition is evenly fully mixed and made into ceramic sample slurry for subsequent use;
C. ceramic sample slurry cast: the ceramic sample slurry prepared in described step b is slowly poured in the mould prepared in described step a, due to the water sorption of mould, slurry in chamber can constantly sink, along with the slurry in mold cavity constantly sinks to carrying out to continue to supplement the feeding of ceramic sample slurry, until the slurry in mold cavity no longer sinks, die sinking is carried out after cast starts 1h, obtain ceramic sample biscuit, ceramic sample biscuit is taken out, be placed in dry sunshade place for subsequent use, the toughness flake 4 prepared in described step a is embedded on ceramic sample biscuit, see Fig. 3 and Fig. 4,
D. ceramic sample sintering: after the ceramic sample biscuit being embedded with toughness flake 4 prepared in described step c is placed 3 days, experimentally test the sintering schedule of the pottery used, ceramic sample element is sintered, after toughness flake 4 combustion decomposition, make ceramic sample predetermined position to leave width and be not more than 0.15mm breach, after sintering process completes, obtain the fracture toughness specimen 5 being with stupalith that is jagged and that crack at root of notch, see Fig. 5 and Fig. 6.
This example is according to ASTM E399-09(Standard Test Method for Linear-Elastic Plane-Strain Fracture Toughness K
iCof Metallic Materials) require to prepare composite conductor oxygen-permeating film ceramic materials fracture toughness sample to the sample of SENB method.The mould used as depicted in figs. 1 and 2.Should notice during making that sprue gate 3 can not be positioned at directly over PVC thin slice, in case grouting material directly drops on PVC thin slice and hit curved or shoot down, see Fig. 2.
A certain amount of BaCo is taken respectively according to the formula in table 1
0.7fe
0.2nb
0.1o
3-δceramic powder, water, Arabic tree
Glue, spreading agent, pour into after mixing in the ball grinder of 500ml, add the zirconia ceramics ball of 4 9g and the zirconia ceramics ball of 18 4g again, then ball grinder is placed in tumbling ball mill ball milling under the rotating speed of 10r/min, taking out slurry after 9h uses ready gypsum mold to pour into a mould, period repeatedly feed supplement till slurry does not sink.Die sinking after 1h.As shown in Figure 3 and Figure 4, cast obtains rectangular specimen, as Fig. 3 to the biscuit sample obtained; Dotted box portion in 3 is amplified, can see that PVC thin slice is embedded in sample well and needs to occur on the position of breach, as Fig. 4.Finally according to the sintering schedule sintering biscuit of regulation.As shown in Figure 5, the requirement of the rectangular specimen size conforms ASTM E399-09 obtained, as Fig. 5 for the sample finally obtained; Dotted box portion in Fig. 5 is amplified, find that the PVC thin slice be originally embedded on biscuit sample disappears, the substitute is the breach that the degree of depth is specimen height half, width is less than or equal to 0.15mm, and root of notch creates the Original Cracks consistent with notch depth direction, its degree of depth is about 1mm, as shown in Figure 6.Fine ceramics fracture toughness specimen prepared by the present embodiment contains the ceramic sample of the breach of Kuan Du≤0.15mm, and root of notch has Original Cracks, can meet the ceramic fracture toughness detection method of major part needs precrack to the requirement of sample.
the fracture experiment of the fracture toughness specimen of the stupalith using the present invention to prepare:
The using method of the composite conductor oxygen-permeating film ceramic materials fracture toughness sample obtained by the preferred embodiment of the present invention, see the Fig. 7 in figure; Existing composition graphs 7 is described below:
Use three-point bending resistance measurement device sample fracture toughness, the sample prepared is placed by shown in Fig. 7, the two ends of the fracture toughness specimen 5 of stupalith are point using fulcrum 6 as pressure support, should be noted that and make containing side jaggy down, and breach to be positioned at the position, middle of two fixed support axles.
After sample places, directly over breach, position applies pressure at right angle, and as shown in Figure 7, note using suitable loading velocity depending on material fragility, this test loading velocity is 0.5 mm/min.Under the effect of load up, sample, is expanded for source vertically downward with the pre-crackle of root of notch, and post-rift sample as shown in Figure 8.Fracture Toughness is calculated according to ASTM E399-09 standard meter after fracture.
By reference to the accompanying drawings the embodiment of the present invention is illustrated above; but the invention is not restricted to above-described embodiment; multiple change can also be made according to the object of innovation and creation of the present invention; change, the modification made under all Spirit Essences according to technical solution of the present invention and principle, substitute, combination, to simplify; all should be the substitute mode of equivalence; as long as goal of the invention according to the invention; only otherwise deviate from know-why and the inventive concept of the fracture toughness specimen preparation method of stupalith of the present invention, all protection scope of the present invention is belonged to.
Claims (6)
1. a fracture toughness specimen preparation method for stupalith, is characterized in that, comprise the steps:
A. the preparation of sectional die: adopt sectional die shape system, mould is made to have two parts matched moulds module, according to outer contoured shape and the dimensional requirement of the fracture toughness specimen of stupalith, the mold cavity of processing customization hollow, when two parts matched moulds block merging is assembled into full die, one end open along mold cavity depth direction forms sprue gate, mould adopts gypsum or lime to make, need the dimensional requirement of prefabricated breach according to the fracture toughness specimen of test experiments to stupalith simultaneously, make the toughness flake of a slice Hou Du≤0.15mm, and according to the position of breach at the fracture toughness specimen of stupalith, toughness flake is mounted on the corresponding position in the groove of a module of mould, thus toughness flake is assembled in mold cavity, make the plane orthogonal of toughness flake in die cavity depth direction, when mould sprue gate upwards time, mold cavity depth direction is parallel with vertical direction, and toughness flake's level is horizontally disposed with, it is the die tip shell of one of them module of mould directly over toughness flake, cast slurry injects from the sprue gate of mould and freely falls into the not direct impact flexibility thin slice of process bottom mold cavity, the material that described toughness flake adopts incendivity to decompose is made,
B. the fracture toughness specimen raw material of stupalith prepares: take ceramic sample feed composition material respectively according to the fracture toughness specimen constituent mass ratio of stupalith, wherein ceramic powders takes 100 parts, deionized water takes 0 ~ 14 part, gum arabic takes 0 ~ 14 part, spreading agent takes 0 ~ 0.16 part, Li Du≤the 1.8um of ceramic powders, is evenly fully mixed and made into ceramic sample slurry for subsequent use by each feed composition;
C. ceramic sample slurry cast: the ceramic sample slurry prepared in described step b is slowly poured in the mould prepared in described step a, along with the slurry in mold cavity constantly sinks to carrying out to continue to supplement the feeding of ceramic sample slurry, until the slurry in mold cavity no longer sinks, at least after cast starts 1h, carry out die sinking, obtain ceramic sample biscuit, ceramic sample biscuit is taken out, be placed in dry sunshade place for subsequent use, the toughness flake prepared in described step a is embedded on ceramic sample biscuit;
D. ceramic sample sintering: after the ceramic sample biscuit being embedded with toughness flake prepared in described step c is placed 2-3 days, experimentally test the sintering schedule of the pottery used, ceramic sample element is sintered, after toughness flake's combustion decomposition, make ceramic sample predetermined position to leave width and be not more than 0.15mm breach, after sintering process completes, obtain the fracture toughness specimen being with stupalith that is jagged and that crack at root of notch.
2. the fracture toughness specimen preparation method of stupalith according to claim 1, is characterized in that: the length of the notch depth on the fracture toughness specimen of stupalith and root of notch crackle is adjusted by the shape and size of toughness flake.
3. the fracture toughness specimen preparation method of stupalith according to claim 1 or 2, is characterized in that: in described step a, adopts water and unslaked lime reaction solidification to make lime mould.
4. the fracture toughness specimen preparation method of stupalith according to claim 1 or 2, it is characterized in that: in described step a, described toughness flake is polyvinyl chloride film.
5. the fracture toughness specimen preparation method of stupalith according to claim 1 or 2, is characterized in that: in described step b, adopts wet ball grinding method to prepare ceramic sample slurry.
6. the fracture toughness specimen preparation method of stupalith according to claim 5, it is characterized in that: in described step b, ceramic sample feed composition material is taken respectively according to the fracture toughness specimen constituent mass ratio of stupalith, pour in the ball grinder of 500ml after each for the ceramic sample taken feed composition material is mixed, add the zirconia ceramics ball of at least 4 9g and the zirconia ceramics ball of at least 18 4g again, then ball grinder is placed in tumbling ball mill ball milling at least 9h, rotating speed is adjusted at least 10r/min, prepares ceramic sample slurry.
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Cited By (10)
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| CN106769284A (en) * | 2016-11-29 | 2017-05-31 | 南华大学 | It is a kind of that the method containing closure crack cube model is prepared based on cement mortar material |
| CN106904983A (en) * | 2017-03-27 | 2017-06-30 | 湘潭大学 | A kind of preparation method containing Embedded defect ceramic sample |
| CN107382266A (en) * | 2017-07-26 | 2017-11-24 | 长沙楚风陶社陶艺有限公司 | A kind of processing technology of crack ceramic utensil |
| CN108896379A (en) * | 2018-03-26 | 2018-11-27 | 扬州大学 | A kind of device making concrete coped beam test specimen notch |
| CN109849152A (en) * | 2018-04-25 | 2019-06-07 | 水利部交通运输部国家能源局南京水利科学研究院 | The high-precision method for prefabricating and device of concrete component micro-crack |
| CN110146360A (en) * | 2019-06-14 | 2019-08-20 | 中国建筑材料科学研究总院有限公司 | The method of brittle ceramic precrack, the bracket of precrack and its application |
| CN112146960A (en) * | 2020-10-14 | 2020-12-29 | 中国矿业大学(北京) | Method for manufacturing cement mortar test piece with built-in open crack |
| CN113466038A (en) * | 2021-06-21 | 2021-10-01 | 长江存储科技有限责任公司 | Detection sample for fracture toughness and detection method thereof |
| CN117949277A (en) * | 2024-03-25 | 2024-04-30 | 中国航发四川燃气涡轮研究院 | Defect prefabrication structure and method for circumferential high-stress part of wheel disc |
| CN117949277B (en) * | 2024-03-25 | 2024-06-04 | 中国航发四川燃气涡轮研究院 | Defect prefabrication structure and method for circumferential high-stress part of wheel disc |
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| CN106769284B (en) * | 2016-11-29 | 2019-05-31 | 南华大学 | A method of based on cement mortar material preparation crack cube model containing closure |
| CN106769284A (en) * | 2016-11-29 | 2017-05-31 | 南华大学 | It is a kind of that the method containing closure crack cube model is prepared based on cement mortar material |
| CN106904983A (en) * | 2017-03-27 | 2017-06-30 | 湘潭大学 | A kind of preparation method containing Embedded defect ceramic sample |
| CN107382266A (en) * | 2017-07-26 | 2017-11-24 | 长沙楚风陶社陶艺有限公司 | A kind of processing technology of crack ceramic utensil |
| CN108896379A (en) * | 2018-03-26 | 2018-11-27 | 扬州大学 | A kind of device making concrete coped beam test specimen notch |
| CN109849152B (en) * | 2018-04-25 | 2019-12-17 | 水利部交通运输部国家能源局南京水利科学研究院 | method and device for prefabricating microcracks of concrete member |
| CN109849152A (en) * | 2018-04-25 | 2019-06-07 | 水利部交通运输部国家能源局南京水利科学研究院 | The high-precision method for prefabricating and device of concrete component micro-crack |
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| CN113466038A (en) * | 2021-06-21 | 2021-10-01 | 长江存储科技有限责任公司 | Detection sample for fracture toughness and detection method thereof |
| CN113466038B (en) * | 2021-06-21 | 2022-05-20 | 长江存储科技有限责任公司 | Detection sample for fracture toughness and detection method thereof |
| CN117949277A (en) * | 2024-03-25 | 2024-04-30 | 中国航发四川燃气涡轮研究院 | Defect prefabrication structure and method for circumferential high-stress part of wheel disc |
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