CN110228995A - A kind of vacuum sintering method of photocuring 3D printing aluminium oxide ceramics biscuit - Google Patents
A kind of vacuum sintering method of photocuring 3D printing aluminium oxide ceramics biscuit Download PDFInfo
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- CN110228995A CN110228995A CN201910551536.5A CN201910551536A CN110228995A CN 110228995 A CN110228995 A CN 110228995A CN 201910551536 A CN201910551536 A CN 201910551536A CN 110228995 A CN110228995 A CN 110228995A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- 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
- C04B35/64—Burning or sintering processes
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
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Abstract
The present invention relates to a kind of vacuum sintering methods of photocuring 3D printing aluminium oxide ceramics biscuit, aluminium oxide ceramics biscuit is placed in Muffle furnace, under the conditions of air atmosphere, it is risen between 300~600 DEG C with 0.1~8 DEG C/min of heating rate, heat preservation 0.5~5 hour, then 800~1050 DEG C are risen to 0.1~8 DEG C/min of heating rate, keeps the temperature 0.5~5 hour；(2) then aluminium oxide ceramics biscuit is transferred in vacuum hotpressing stove, 1 × 10‑3~1 × 10‑ 5It under the high vacuum condition of Pa, is risen between 1100~1300 DEG C with 0.1~8 DEG C/min of heating rate, keeps the temperature 0.5~5 hour to get aluminium oxide ceramics is arrived.The method that the present invention is sintered under degreasing, high vacuum condition at a slow speed by low temperature, reduces the sintering temperature of aluminium oxide ceramics, make sintered alumina ceramic structure uniformly, excellent surface quality, phenomena such as bubble-free, cracking, deformation.Vacuum-sintering temperature provided by the invention reduces 200~400 DEG C than conventional method, is conducive to energy conservation and environmental protection.It can be applied to aluminium oxide ceramics production field.
Description
Technical field
The invention belongs to increases material manufacturing technology field, the vacuum for being related to a kind of photocuring 3D printing aluminium oxide ceramics biscuit is burnt
Knot method.
Background technique
Aluminium oxide ceramics has the excellent performances such as high mechanical strength, high temperature resistance be good, be modern society's purposes most
Extensive ceramics.But since its brittleness is big, the reasons such as difficulty of processing is big limit it in high-precision, complex components field
Application.Michelle L.Griffith realized in nineteen ninety-five using photocuring 3D printing technique printing ceramic material can
It can property (Griffith M L, Halloran J W.Freeform fabrication of ceramics via
stereolithography[J].Journal of the American Ceramic Society,1996,79(10):
2601-2608.).Because photocuring 3D printing technique have the characteristics that efficiently, energy conservation, suitable for the molding of complex components, this
Item technology causes world wide internal medicine scholar's extensive concern.
By containing a large amount of liquid resins in photocuring 3D printing ceramic material slurry therewith, therefore will printing gained ceramic green
Phenomena such as base can deform after being sintered to ceramic material, crack, shrink, these phenomenons limit photocuring 3D printing ceramics skill
The development and application of art.However, not filled for the research in terms of the sintering of photocuring 3D printing alumina ceramic material at present
Point, how to regulate and control sintering procedure, obtain structure uniformly, the ceramic material of excellent surface quality, be to promote photocuring 3D printing skill
The important step of art development and application.
Shanghai Silicate Inst., Chinese Academy of Sciences (Chinese patent, patent No. CN106316369A).Propose using with
Green body embedding and the degumming filled and sintering process are kept ceramic body heated equal by the identical raw material powder of ceramic body ingredient
It is even, it avoids and generates internal stress inside green body, reduce the probability collapsed.Nanjing University of Technology (Chinese patent, the patent No.
CN107129283 a kind of photocuring 3D printing high solid loading ceramic slurry and preparation method thereof) is proposed, can be sintered highly dense
Real, great surface quality ceramic.However not only sintering temperature is higher for the method for these sintered alumina ceramics in air,
Waste of energy, and due under high temperature crystal growth rate it is very fast, be easy to cause material internal cracking, deformation.
The relationship between temperature program, controlled material microstructure and macro property is how controlled, is developed and using light
Solidify the vital step of 3D printing alumina ceramic material.
Summary of the invention
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes a kind of photocuring 3D printing aluminium oxide ceramics biscuit
Vacuum sintering method, by the way that under the conditions of condition of high vacuum degree, the process of slowly heating sintering, the photocuring 3D for preparing good quality is beaten
Print aluminium oxide ceramics.Push the application of photocuring 3D printing technique.The present invention provides a kind of energy conservations, efficient photocuring 3D printing
The sintering method of aluminium oxide ceramics biscuit, suitable for preparing high-precision, complicated ceramic part.
Technical solution
A kind of vacuum sintering method of photocuring 3D printing aluminium oxide ceramics biscuit, it is characterised in that steps are as follows:
Step 1: aluminium oxide ceramics biscuit being placed in Muffle furnace, under the conditions of air atmosphere, with 0.1~8 DEG C/min
Heating rate rises between 300~600 DEG C, keeps the temperature 0.5~5 hour, is then risen to 0.1~8 DEG C/min of heating rate
800~1050 DEG C, keep the temperature 0.5~5 hour；
Step 2: aluminium oxide ceramics biscuit being transferred in vacuum hotpressing stove, 1 × 10-3~1 × 10-5The high vacuum of Pa
Under the conditions of, it is risen between 1100~1300 DEG C with 0.1~8 DEG C/min of heating rate, keeps the temperature 0.5~5 hour to get oxygen is arrived
Change aluminium ceramics.
The aluminium oxide ceramics biscuit is printed by aluminium oxide ceramics slurry.
The alumina slurry is made of photosensitive resin and alumina powder.
Powder quality percentage composition is not less than 35% in the aluminium oxide ceramics slurry of the printing aluminium oxide ceramics biscuit, no
Higher than 85%.
The alumina slurry is made of photosensitive resin and alumina powder.
The photosensitive resin is acrylic resin, can be trimethylolpropane trimethacrylate, 1,6- hexylene glycol dipropyl
One of olefin(e) acid ester, hydroxyethyl methacrylate are a variety of.
Beneficial effect
A kind of vacuum sintering method of photocuring 3D printing aluminium oxide ceramics biscuit proposed by the present invention, aluminium oxide ceramics element
Base is obtained by photocuring 3D printing aluminium oxide ceramics slurry.Specific sintering method is as follows: (1) aluminium oxide ceramics biscuit being placed in horse
Not in furnace, under the conditions of air atmosphere, risen between 300~600 DEG C with 0.1~8 DEG C/min of heating rate, heat preservation 0.5~
5 hours, 800~1050 DEG C then are risen to 0.1~8 DEG C/min of heating rate, keeps the temperature 0.5~5 hour；(2) then by oxygen
Change aluminium biscuit of ceramics to be transferred in vacuum hotpressing stove, 1 × 10-3~1 × 10-5Under the high vacuum condition of Pa, with 0.1~8 DEG C/
The heating rate of minute rises between 1100~1300 DEG C, keeps the temperature 0.5~5 hour to get aluminium oxide ceramics is arrived.The present invention passes through
The method that low temperature is sintered under degreasing, high vacuum condition at a slow speed, reduces the sintering temperature of aluminium oxide ceramics, makes sintered oxidation
Aluminium ceramic structure uniformly, excellent surface quality, bubble-free, cracking, deformation phenomena such as.Vacuum-sintering temperature ratio provided by the invention
Conventional method reduces 200~400 DEG C, is conducive to energy conservation and environmental protection.It can be applied to aluminium oxide ceramics production field.
Beneficial effects of the present invention have the following:
1, method of the present invention by being sintered under low temperature at a slow speed degreasing, high vacuum condition, reduces the burning of aluminium oxide ceramics
Junction temperature, make sintered alumina ceramic structure uniformly, excellent surface quality, bubble-free, cracking, deformation phenomena such as.
2, vacuum-sintering temperature provided by the invention reduces 200~400 DEG C than conventional method, is conducive to energy conservation and environmental protection.It can
Applied to aluminium oxide ceramics production field.Photocuring 3D printing aluminum oxide technology is conducive to high precision, complicated part
Molding has a good application prospect in terms of ceramic core, biomedical aluminium oxide.Light through the invention
Solidify the sintering method of 3D printing biscuit of ceramics, it is photocuring that available structure is uniform, excellent surface quality ceramic product
The application of 3D printing aluminium oxide ceramics technology provides the foundation.
Detailed description of the invention
Fig. 1 is the vacuum sintering method flow chart of photocuring 3D printing aluminium oxide ceramics biscuit.
Fig. 2 is vacuum-sintering posterior photocuring 3D printing aluminium oxide ceramics pictorial diagram.
Specific embodiment
Now in conjunction with embodiment, attached drawing, the invention will be further described:
Based on the present Research of photocuring 3D printing aluminium oxide ceramics technology, it is sintered out the pottery that structure is uniform, has excellent performance
Porcelain slurry is the critical issue of this technical application.
By deploying photosensitive resin, dispersing agent, alumina powder, defoaming agent and UV absorbers carry out photocuring 3D and beat
Print the preparation of aluminium oxide ceramics slurry.Wherein dispersing agent mass percentage is 2%~25%, and quality of alumina percentage composition is
40%~85%, surplus is photosensitive resin.
Dispersing agent is added dropwise in photosensitive resin and is stirred evenly, alumina powder is then gradually added into photosensitive resin
In.
Obtained mixture is stirred evenly, defoaming agent is added in ball milling after 2~6 hours, add after ball milling 2~6 hours again
Enter UV absorbers, after mixing evenly, ultrasonic vibration 0.5~6 hour, then proceedes to ball milling 2~6 hours.
By the mixture vacuumize process 0.5~6 hour after ball milling to get arriving aluminium oxide ceramics slurry.
Aluminium oxide ceramics biscuit is placed in Muffle furnace, under the conditions of air atmosphere, with 0.1~8 DEG C/min of heating speed
Rate rises between 300~600 DEG C, keeps the temperature 0.5~5 hour, then 800 are risen to 0.1~8 DEG C/min of heating rate~
1050 DEG C, keep the temperature 0.5~5 hour.
Aluminium oxide ceramics biscuit is transferred in vacuum hotpressing stove, 1 × 10-3~1 × 10-5Under the high vacuum condition of Pa,
It is risen between 1100~1300 DEG C with 0.1~8 DEG C/min of heating rate, keeps the temperature 0.5~5 hour and make pottery to get to aluminium oxide
Porcelain.
Embodiment 1.
Step 1: photocuring 3D printing aluminium oxide ceramics biscuit being placed in Muffle furnace, under the conditions of air atmosphere, with 2
DEG C/min heating rate rise to 500 DEG C, keep the temperature 2 hours, then rise to 1000 DEG C with 5 DEG C/min of heating rate, heat preservation 2
Hour.
Step 2: and then aluminium oxide ceramics biscuit is transferred in vacuum hotpressing stove, 1 × 10-4The high vacuum condition of Pa
Under, 1200 DEG C are risen to 5 DEG C/min of heating rate, keeps the temperature 2 hours to get uniform, excellent surface quality, no gas to structure
Bubble, cracking, the aluminium oxide ceramics deformed.As shown in Figure 2.
Embodiment 2.
Step 1: photocuring 3D printing aluminium oxide ceramics biscuit being placed in Muffle furnace, under the conditions of air atmosphere, with 7
DEG C/min heating rate rise to 600 DEG C, keep the temperature 5 hours, then rise to 1000 DEG C with 5 DEG C/min of heating rate, heat preservation 5
Hour.
Step 2: and then aluminium oxide ceramics biscuit is transferred in vacuum hotpressing stove, 1 × 10-4The high vacuum condition of Pa
Under, 1100 DEG C are risen to 2 DEG C/min of heating rate, keeps the temperature 3 hours to get uniform, excellent surface quality, no gas to structure
Bubble, cracking, the aluminium oxide ceramics deformed.As shown in Figure 2.
Embodiment 1.
Step 1: photocuring 3D printing aluminium oxide ceramics biscuit being placed in Muffle furnace, under the conditions of air atmosphere, with 3
DEG C/min heating rate rise to 400 DEG C, keep the temperature 3 hours, then rise to 900 DEG C with 3 DEG C/min of heating rate, heat preservation 4
Hour.
Step 2: and then aluminium oxide ceramics biscuit is transferred in vacuum hotpressing stove, 1 × 10--3The high vacuum condition of Pa
Under, 1200 DEG C are risen to 4 DEG C/min of heating rate, keeps the temperature 4 hours to get uniform, excellent surface quality, no gas to structure
Bubble, cracking, the aluminium oxide ceramics deformed.As shown in Figure 2.
Vacuum-sintering temperature provided by the invention reduces 200~400 DEG C than conventional method, is conducive to energy conservation and environmental protection.It can answer
For aluminium oxide ceramics production field.
Claims (3)
1. a kind of vacuum sintering method of photocuring 3D printing aluminium oxide ceramics biscuit, it is characterised in that steps are as follows:
Step 1: aluminium oxide ceramics biscuit being placed in Muffle furnace, under the conditions of air atmosphere, with 0.1~8 DEG C/min of heating
Rate rises between 300~600 DEG C, keeps the temperature 0.5~5 hour, then 800 are risen to 0.1~8 DEG C/min of heating rate~
1050 DEG C, keep the temperature 0.5~5 hour；
Step 2: aluminium oxide ceramics biscuit being transferred in vacuum hotpressing stove, 1 × 10-3~1 × 10-5The high vacuum condition of Pa
Under, it is risen between 1100~1300 DEG C with 0.1~8 DEG C/min of heating rate, keeps the temperature 0.5~5 hour to get aluminium oxide is arrived
Ceramics.
2. the vacuum sintering method of photocuring 3D printing aluminium oxide ceramics biscuit according to claim 1, it is characterised in that: institute
Aluminium oxide ceramics biscuit is stated to be printed by aluminium oxide ceramics slurry.
3. the vacuum sintering method of photocuring 3D printing aluminium oxide ceramics biscuit according to claim 1, it is characterised in that: institute
It states powder quality percentage composition in the aluminium oxide ceramics slurry of printing aluminium oxide ceramics biscuit and is not higher than 85% not less than 35%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111302772A (en) * | 2020-02-23 | 2020-06-19 | 西北工业大学 | Argon atmosphere sintering method for 3D printing ceramic core |
| CN112110725A (en) * | 2020-09-01 | 2020-12-22 | 有研资源环境技术研究院(北京)有限公司 | High-density annular oxide coating material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111302772A (en) * | 2020-02-23 | 2020-06-19 | 西北工业大学 | Argon atmosphere sintering method for 3D printing ceramic core |
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Application publication date: 20190913 |