CN105198469A - Forming method of inorganic prefabticated member - Google Patents
Forming method of inorganic prefabticated member Download PDFInfo
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- CN105198469A CN105198469A CN201510568690.5A CN201510568690A CN105198469A CN 105198469 A CN105198469 A CN 105198469A CN 201510568690 A CN201510568690 A CN 201510568690A CN 105198469 A CN105198469 A CN 105198469A
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- Prior art keywords
- inorganic
- prefabricated component
- sponge
- forming method
- slurry
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- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000002002 slurry Substances 0.000 claims abstract description 22
- 230000001590 oxidative effect Effects 0.000 claims abstract description 7
- 239000000835 fiber Substances 0.000 claims description 35
- 239000011230 binding agent Substances 0.000 claims description 21
- 238000002360 preparation method Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 7
- 229910052594 sapphire Inorganic materials 0.000 claims description 7
- 239000010980 sapphire Substances 0.000 claims description 7
- 239000000741 silica gel Substances 0.000 claims description 7
- 229910002027 silica gel Inorganic materials 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 229910052809 inorganic oxide Inorganic materials 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- 238000002525 ultrasonication Methods 0.000 claims description 2
- 238000005245 sintering Methods 0.000 abstract description 6
- 239000000919 ceramic Substances 0.000 abstract description 4
- 229920000642 polymer Polymers 0.000 abstract description 2
- 239000012784 inorganic fiber Substances 0.000 abstract 4
- 239000000571 coke Substances 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 239000007769 metal material Substances 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 238000009210 therapy by ultrasound Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 10
- 238000009826 distribution Methods 0.000 description 5
- 229920000620 organic polymer Polymers 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910001338 liquidmetal Inorganic materials 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000002905 metal composite material Substances 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920001169 thermoplastic Polymers 0.000 description 2
- 239000004416 thermosoftening plastic Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
- Ceramic Products (AREA)
Abstract
The invention provides a forming method of an inorganic prefabticated member. The forming method comprises the steps of (1) adding short inorganic fibers or whiskers to a dispersing agent, and performing ultrasonic treatment for uniformly dispersing and forming slurry; (2) uniformly soaking sponge in the slurry, so as to form the sponge containing the short inorganic fibers or whiskers in a depositional mode; (3) putting the sponge containing the short inorganic fibers or whiskers in a high-temperature furnace in an oxidizing atmosphere, so as to remove polymers from the sponge in a sintering coke exhaust mode and obtain the final ceramic prefabticated member. The obtained ceramic prefabticated member containing the short inorganic fibers or whiskers can be used for multiple purposes of penetrant metal materials and the like.
Description
Technical field
The invention belongs to field of compound material, particularly a kind of forming method of inorganic prefabricated component.
Background technology
The technology of monocrystalline sapphire fiber is prepared in the mass-producing of Niu Ka company of introduction Spain of Dongguan innovation center of Tsing-Hua University; set up monocrystalline sapphire fiber and reinforced composite innovation team thereof, and carry out the applied research of this fiber in ceramic base, metal matrix and polymer-based composite on this basis.During application in fibre-reinforced metal-base composites, except the way of powder metallurgy, usually need to make prefabricated component with fiber, then at high temperature, by under certain pressure or vacuum state, the liquid metal of melting is penetrated into inside prefabricated component, forms the hardware of band fiber reinforcement, thus improve the specific tenacity, wear resistance etc. of hardware.
The application method in metal composite about whisker or inorganic staple fibre, in US Patent No. 5,458,181, US5,335,712, US5,153,057, US5,108,964 and US4,500, what describe in 504 is silicon carbide whisker and paraffin or other thermoplastic organic polymers, forms slurry in the molten state, molded, then utilize high temperature degreasing dewax, then sinter many empty ceramic fiber preform into, more at high temperature infiltrate liquid metal.The prefabricated component preparation of this kind of method, needs the volume range of whisker at 10-50%.And in the paraffin of molten state or the molding process of cooling of other thermoplastic organic polymers and high temperature degreasing dewax process, because the proportion of fiber is comparatively large, easily form layering and Gradient distribution.
US4,463,058 method described is that silicon carbide whisker is formed after slurry and adds aluminium powder, molded rear sintering, finally can reach containing whisker 50%(volume percent) matrix material.The preparation method of this kind of powder metallurgy, forms inner bridge formation, by final metal composite densified sintering product, thus cannot have influence on the mechanical property of material when fibre content is higher.
Summary of the invention
The object of this invention is to provide a kind of forming method of inorganic prefabricated component, under the mode of comparatively environmental protection, the uniform prefabricated component of more even, the various distribution of orientations of Fiber Distribution in three dimensions can be prepared.
For realizing above object, technical scheme of the present invention is:
A forming method for inorganic prefabricated component, step comprises: the preparation of a, slurry, is added by inorganic fibre in dispersion agent, and ultrasonication is uniformly dispersed to make it, forms slurry; B, sponge is immersed in slurry prepared by step a; C, the sponge oven dry of will soak fibrous slurry; D, fibrous sponge binder removal, remove the organism of sponge; E, by the prefabricated component sinter molding after binder removal.
Described inorganic fibre be monocrystalline sapphire fiber, polycrystalline alumina fiber, silicon carbide, silicon nitride fiber and his inorganic oxide any one.
Described monocrystalline sapphire fiber diameter range is 0.1-10 micron, and length range is 5-500 micron.
Described dispersion agent is silica gel, and the silica gel concentration range for the preparation of slurry is 5-15%.
In the preparation of step a slurry, the weight percent of inorganic fibre is 10-25%.
The number of times that sponge is soaked in the slurry is 4-8 time, must dry to remove moisture before each immersion.
The environment of steps d fibre-bearing sponge binder removal is that fibrous sponge is placed in 800-1200 DEG C, and binder removal 1-3 hour in the kiln of oxidizing atmosphere is preferably placed in 1000 DEG C of binder removal 1-3 hour.
The temperature of the prefabricated component sinter molding after binder removal is 1200 DEG C to 1800 DEG C; Preferable temperature is 1400 DEG C to 1650 DEG C.
beneficial effect:
1) the present invention is by monocrystalline sapphire fiber dispersion in silica gel, is then inhaled into the space of sponge, and more even, the various distribution of orientations of Fiber Distribution is even in three dimensions for the inorganic prefabricated component of preparation.
2) prefabricated component that the present invention is dried by sponge under certain temperature, sponge binder removal and sintering are made is fine and close, good mechanical property.
Specific embodiment
The present invention is illustrated below by exemplary embodiment.Should be appreciated that scope of the present invention should not be limited to the scope of embodiment.Any do not depart from purport of the present invention change or change and can be understood by those skilled in the art.Protection scope of the present invention is determined by the scope of claims.
Embodiment 1:
It is α-aluminum oxide fiber (the Niu Ka company of 95% by chemical purity, Fibre diameter 0.1-10 micron, length 100-500 micron) add containing silica gel 15% the aqueous solution gradually, add while stirring, continue stirring 4 hours, until thoroughly dispersion forms uniform slurry;
Sponge to be immersed in above-mentioned slurry 5 times, each soak after sponge after draining away the water, be placed in dry 1 hour of the baking oven of 120 DEG C;
The size of 2 green compact obtained is as follows:
(A1) 119.60 × 79.40 × 42.30 millimeters, weight: 89.852 grams
(A2) 116.40 × 83.50 × 42.50 millimeters, weight: 85.464 grams
The organic polymer removing sponge carries out in the kiln of oxidizing atmosphere, and the heating schedule of kiln is:
From room temperature to 600 DEG C, heating rate is 1 DEG C of per minute;
Be 3 DEG C of per minutes from the heating rate of 600 DEG C to 1000 DEG C;
Be 5 DEG C of per minutes from the heating rate of 1000 DEG C to 1400 DEG C;
It is 2 hours the binder removal time of 1400 DEG C.
After binder removal, the size of 2 the ripe bases obtained is as follows:
(A1) 117.06 × 78.35 × 41.60 millimeters, weight: 71.996 grams, volumetric shrinkage 5.01%
(A2) 114.57 × 82.30 × 41.77 millimeters, weight: 72.130 grams, volumetric shrinkage 4.65%
Finally, above-mentioned ripe base is sintered under oxidizing atmosphere, being set as follows of its sintering temperature:
From room temperature to 1425 DEG C, heating rate is 5 DEG C of per minutes;
Binder removal 2 hours at 1425 DEG C;
Hot speed of falling from 1425 DEG C to room temperature is 5 DEG C of per minutes;
The prefabricated component finally obtained does not change dimensionally.
Embodiment 2:
It is α-aluminum oxide fiber (the Dongguan Niu Ka novel material company of 99.7% by chemical purity, Fibre diameter 0.1-10 micron, length 100-500 micron) add containing silica gel 15% the aqueous solution gradually, add while stirring, continue stirring 4 hours, until thoroughly dispersion forms uniform slurry;
Sponge to be immersed in above-mentioned slurry 5 times, each soak after sponge after draining away the water, be placed in dry 1 hour of the baking oven of 120 DEG C;
The size of 2 green compact obtained is as follows:
(B1) 120.80 × 83.50 × 42.50 millimeters, weight: 101.530 grams
(B2) 122.70 × 83.80 × 42.50 millimeters, weight: 117.175 grams
The organic polymer removing sponge carries out in the kiln of oxidizing atmosphere, and the heating schedule of kiln is:
From room temperature to 600 DEG C, heating rate is 1 DEG C of per minute;
Be 3 DEG C of per minutes from the heating rate of 600 DEG C to 1000 DEG C;
Be 5 DEG C of per minutes from the heating rate of 1000 DEG C to 1400 DEG C;
It is 2 hours the binder removal time of 1400 DEG C.
After binder removal, the size of 2 the ripe bases obtained is as follows:
(B1) 119.15 × 82.70 × 42.09 millimeters, weight: 85.517 grams, volumetric shrinkage 3.25%
(B2) 121.60 × 82.90 × 42.00 millimeters, weight: 100.786 grams, volumetric shrinkage 3.11%
Finally, above-mentioned ripe base is sintered under oxidizing atmosphere, being set as follows of its sintering temperature:
From room temperature to 1600 DEG C, heating rate is 5 DEG C of per minutes;
Binder removal 2 hours at 1600 DEG C;
Hot speed of falling from 1600 DEG C to room temperature is 5 DEG C of per minutes;
The prefabricated component finally obtained does not shrink dimensionally.
Above-described embodiment is only and technological thought of the present invention and feature is described, it describes comparatively concrete and detailed, its object is to enable those of ordinary skill in the art understand content of the present invention and implement according to this, and be not limited in signle crystal alumina fiber, other inorganic staple fibre or whisker all can make prefabricated component by this kind of method.Therefore only the scope of the claims of the present invention can not be limited with this, it should be noted that, for the person of ordinary skill of the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made, namely all do according to the embodiment of the present invention any amendment, equivalent variations and modification, all still belong in the scope of technical scheme of the present invention.
Claims (10)
1. a forming method for inorganic prefabricated component, step comprises: the preparation of a, slurry, is added by inorganic fibre in dispersion agent, and ultrasonication is uniformly dispersed to make it, forms slurry; B, sponge is immersed in slurry prepared by step a; C, the sponge oven dry of will soak fibrous slurry; D, fibrous sponge binder removal, remove the organism of sponge; E, by the prefabricated component sinter molding after binder removal.
2. the forming method of inorganic prefabricated component according to claim 1, described inorganic fibre be monocrystalline sapphire fiber, polycrystalline alumina fiber, silicon carbide, silicon nitride fiber and his inorganic oxide any one.
3. the forming method of inorganic prefabricated component according to claim 2, described monocrystalline sapphire fiber diameter range is 0.1-10 micron, and length range is 5-500 micron.
4. the forming method of inorganic prefabricated component according to claim 1, described dispersion agent is silica gel, and the silica gel concentration range for the preparation of slurry is 5-15%.
5. the forming method of inorganic prefabricated component according to claim 1, in the preparation of step a slurry, the weight percent of inorganic fibre is 10-25%.
6. the forming method of inorganic prefabricated component according to claim 1, the number of times that sponge is soaked in the slurry is 4-8 time, must dry to remove moisture before each immersion.
7. the forming method of inorganic prefabricated component according to claim 1, the environment of steps d fibre-bearing sponge binder removal is that fibrous sponge is placed in 800-1200 DEG C, binder removal 1-3 hour in the kiln of oxidizing atmosphere.
8. the forming method of inorganic prefabricated component according to claim 1, the environment of steps d fibre-bearing sponge binder removal is that fibrous sponge is placed in 1000 DEG C of binder removal 1-3 hour.
9. the forming method of inorganic prefabricated component according to claim 1, the temperature of the prefabricated component sinter molding after binder removal is 1200 DEG C to 1800 DEG C.
10. the forming method of inorganic prefabricated component according to claim 9, the temperature of the prefabricated component sinter molding after binder removal is 1400 DEG C to 1650 DEG C.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510568690.5A CN105198469B (en) | 2015-09-09 | 2015-09-09 | A kind of forming method of inorganic prefabricated component |
| PCT/CN2015/093602 WO2017041356A1 (en) | 2015-09-09 | 2015-11-02 | Forming method of inorganic prefabricated member |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510568690.5A CN105198469B (en) | 2015-09-09 | 2015-09-09 | A kind of forming method of inorganic prefabricated component |
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| Publication Number | Publication Date |
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| CN105198469A true CN105198469A (en) | 2015-12-30 |
| CN105198469B CN105198469B (en) | 2017-12-08 |
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| WO (1) | WO2017041356A1 (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011817A (en) * | 2012-12-24 | 2013-04-03 | 中国科学院金属研究所 | Preparation method of yttrium-silicon-oxygen porous high-temperature ceramic material |
| CN103803934A (en) * | 2013-12-23 | 2014-05-21 | 中国建筑材料科学研究总院 | Nanosized silica thermal insulation material and preparation method based on normal-temperature drying wet process thereof |
| CN104726734A (en) * | 2013-12-20 | 2015-06-24 | 中国科学院上海硅酸盐研究所 | Preparation method of silicon carbide reinforced aluminum base composite material |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4866011A (en) * | 1988-05-02 | 1989-09-12 | Swiss Aluminium, Ltd. | Process for forming a ceramic foam |
| US5382396A (en) * | 1992-06-15 | 1995-01-17 | Industrial Technology Research Institute | Method of making a porous ceramic filter |
| JP4213612B2 (en) * | 2004-03-24 | 2009-01-21 | 独立行政法人産業技術総合研究所 | Method for producing porous structure |
| EP2123618A1 (en) * | 2008-05-13 | 2009-11-25 | L'AIR LIQUIDE, Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude | Ceramic foam with gradient of porosity in heterogeneous catalysis |
| CN102372499A (en) * | 2010-08-20 | 2012-03-14 | 湖北工业大学 | Method for preparing porous Ti2AlN ceramic by organic foam impregnation process |
| CN104073669B (en) * | 2014-07-01 | 2016-08-31 | 南京工程学院 | A kind of method prepared containing graded metal three-dimensional network pottery |
-
2015
- 2015-09-09 CN CN201510568690.5A patent/CN105198469B/en active Active
- 2015-11-02 WO PCT/CN2015/093602 patent/WO2017041356A1/en active Application Filing
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011817A (en) * | 2012-12-24 | 2013-04-03 | 中国科学院金属研究所 | Preparation method of yttrium-silicon-oxygen porous high-temperature ceramic material |
| CN104726734A (en) * | 2013-12-20 | 2015-06-24 | 中国科学院上海硅酸盐研究所 | Preparation method of silicon carbide reinforced aluminum base composite material |
| CN103803934A (en) * | 2013-12-23 | 2014-05-21 | 中国建筑材料科学研究总院 | Nanosized silica thermal insulation material and preparation method based on normal-temperature drying wet process thereof |
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| Publication number | Publication date |
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| CN105198469B (en) | 2017-12-08 |
| WO2017041356A1 (en) | 2017-03-16 |
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Effective date of registration: 20231115 Address after: 523000 Building 1, No.1 Xuefu Road, Songshanhu Park, Dongguan City, Guangdong Province Patentee after: Guangdong Qingda Innovation Research Institute Co.,Ltd. Address before: 523000 Innovation Science Park, Songshan Lake High-tech Industrial Development Zone, Dongguan City, Guangdong Province, 8 Tsinghua Dongguan Innovation Center Patentee before: TSINGHUA INNOVATION CENTER IN DONGGUAN |
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