CN108017396A - The drying means of water base pulp gel injection moulding base substrate - Google Patents
The drying means of water base pulp gel injection moulding base substrate Download PDFInfo
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- CN108017396A CN108017396A CN201711123960.7A CN201711123960A CN108017396A CN 108017396 A CN108017396 A CN 108017396A CN 201711123960 A CN201711123960 A CN 201711123960A CN 108017396 A CN108017396 A CN 108017396A
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- base substrate
- injection moulding
- base
- gel injection
- drying
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- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6269—Curing of mixtures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
- B28B11/243—Setting, e.g. drying, dehydrating or firing ceramic articles
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- 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
- C04B35/01—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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- 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
- C04B35/01—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
- C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
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- 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
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/0605—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances by sublimating
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- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6023—Gel casting
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Structural Engineering (AREA)
- Manufacturing & Machinery (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
The invention belongs to ceramic manufacturing field, and in particular to a kind of drying means of water base pulp gel injection moulding base substrate.Comprise the following steps：The wet base that water base pulp gel injection moulding obtains is immersed in tertiary butanol aqueous solution and is dried；Then by after its pre-freeze, then vacuum freeze drying is carried out, obtains dried base substrate.The volume fraction of the tert-butyl alcohol is 10~70% in tertiary butanol aqueous solution.Liquid phase is dried and is combined with vacuum freeze drying by the present invention, using the characteristics of tert-butyl alcohol saturated vapour pressure is high, fusing point is low, surface tension is low, moisture is replaced to exclusion from wet base, the concentration gradient of moisture is formed, promotes hydrone displacement；It can complete to be freeze-dried at relatively high temperatures, freeze efficient, good energy saving property；The internal stress of moisture evaporation generation is reduced, the shrinking percentage of base substrate is reduced, improves dimensional accuracy, it is high using the dry billet surface quality of the present invention, the defects of cracking will not be produced, deformed.
Description
Technical field
The invention belongs to ceramic manufacturing field, and in particular to a kind of drying side of water base pulp gel injection moulding base substrate
Method.
Background technology
Ceramic material has been widely used in the industrial circles such as electronics, machinery, national defence because of its unique performance.But due to it
Itself brittleness is larger, is difficult to be machined out after sintering, so how to obtain complex-shaped ceramic component and ensure that it has
Accurate size becomes the key issue in practical application.High polymer monomer polymerization is incorporated into ceramic shaping by gel casting forming
In technique, the method can prepare complex-shaped ceramic component, and gained blank structure is uniform, intensity is high, can carry out certain
Machining, be a kind of ceramic near-net-shape technique, thus be subject to the extensive concern of academia and industrial quarters.Gel injection-moulding
It is most widely used due to economic, environmental protection usually using two class solvent of water and alcohol, wherein water in shaping.
The usual water content of base substrate obtained by gel casting forming is larger (volume ratio commonly reaches 30~50%).Moisture is with liquid
Form is present in base substrate, and in drying process, moisture is constantly migrated from inside to surface, in surface evaporation or diffusion, causes interior
Outer water content is different；At the same time under the effect of gravity, vapor rises, and moisture declines, and causing base substrate, moisture is different up and down.On
Stating the gradation of moisture causes the contraction of base substrate each several part inconsistent, while the surface tension of water is larger, is produced in moisture exclusion process
The defects of larger capillary force, causes inside there are stress, cracking, deformation.Therefore, drying is in gel casting forming
One of the key link.It is that gel casting forming is wet to make water translocation by way of heating so as to be dried in drying oven
The most common drying mode of base, for avoid because caused by rate of drying is too fast billet surface crack the defects of, researcher passes through
Control temperature lifts speed, humidity decrease speed and drying time or controlled by way of pulse air-supply to be contained inside and outside base substrate
Water rate is poor, reduces shrinking percentage difference inside and outside base substrate, but this mode is less efficient.Liquid displacement drying is to insert base substrate to water
Point have in the solvent of strong affinity, be more than osmotic pressure in hydrous objects by water using osmotic pressure of the water in liquid drier
Split and change in solution, achieve the purpose that dry.In the method, dried medium surface tension used is smaller, is contacted more with base substrate
Fully so that base substrate each several part rate of drying approaches, while can effectively reduce capillary force, reduce stress generation and by
The defects of this caused warpage, cracking.Patent (CN101486579A, CN102887711B) uses alcohols, the ketone of low molecular weight
Class, aldehydes and ethers organic matter solution carry out liquid phase drying to the wet base of gel injection-moulding.But small molecule chain is in liquid phase drying process
In it is readily permeable enter wet base, cause drying effect low, drying be not thorough.Patent (CN106892662A) is with polyethylene glycol
Dry liquid improves degree of drying.Above-mentioned patent is both placed in drying oven after liquid phase drying to be completed to obtain by heated-air drying
Final dry base substrate, essence be by reduce solvent surface tension improve product quality, but heated-air drying in itself lack
Falling into can not still overcome.
The content of the invention
For prior art blank cracking, problem on deformation, the object of the present invention is to provide a kind of water base pulp gel injection
The drying means of molding blank, reduces the internal stress that moisture evaporation produces, and reduces the shrinking percentage of base substrate, improves dimensional accuracy, adopt
Dry billet surface quality is high, and dry contraction is small, the defects of will not producing cracking, deform.
The drying means of water base pulp gel injection moulding base substrate of the present invention, comprises the following steps：
The wet base that water base pulp gel injection moulding obtains is immersed in tertiary butanol aqueous solution and is dried；Then it is its is pre-
After jelly, then vacuum freeze drying is carried out, obtain dried base substrate.
Wherein：
Water base pulp gel injection moulding is common process well known in the art, first will be needed during gel casting forming
Ceramic powder is added to the suspension that high solid loading is configured in solution, and the solution used in the process is most commonly used that
Water.
The volume fraction of the tert-butyl alcohol is 10~70% in tertiary butanol aqueous solution, and the present invention utilizes tert-butyl alcohol saturated vapor pressure
Low, the characteristics of surface tension is low, first displaces the water in wet base, so as to improve green body quality.The tert-butyl alcohol in tertiary butanol aqueous solution
Volume fraction is 10~70%, and replacement result is optimal.
Pre-freezing temperature is -40~-60 DEG C, and the time is 2~4h.
The drying condition of vacuum freeze drying is：Vacuum is less than 15Pa, and temperature is -5~-20 DEG C.The present invention is using cold
Freeze, then vacuum freeze drying, directly from solid state sublimation be gaseous state by water, so as to fulfill dry purpose.Moisture one in wet base
As exist with liquid, therefore need first by its pre-freeze once, be changed into solid-state.
As a kind of perferred technical scheme, the drying side of water base pulp gel injection moulding base substrate of the present invention
Method, step are as follows：
(1) the wet base for obtaining water base pulp gel injection moulding is put on grid beam, then soaks wet base and grid beam
Steep in tertiary butanol aqueous solution, interruption weighs base substrate weight, until its constant weight, obtains the ceramic body of liquid phase drying；
(2) it is fully crystallized it in -40~-60 DEG C of 2~4h of pre-freeze the ceramic body that step (1) obtains；
(3) base substrate that step (2) obtains is carried out vacuum refrigeration under the conditions of vacuum is less than 15Pa, -5~-20 DEG C to do
Dry, interruption is weighed, and is no longer changed to weight, you can obtain dried base substrate.
Soaking time in step (1) is 2~6h.
Grid beam in step (1) is aluminum porous web screen work, the purpose wet base being placed on grid beam be in order to
Base substrate is played a supporting role, while is allowd and be carried out at the same time during liquid displacement from multiple directions, avoids deforming.
Vacuum freeze drying carries out in vacuum freeze drier.
Compared with prior art, the present invention has the following advantages：
(1) tert-butyl alcohol surface tension is smaller, can be reduced in drying process as caused by internal stress as liquid drier
Cracking, deformation.
(2) tert-butyl alcohol solidification point is high, saturated vapor pressure is high, volatile, can greatly improve freeze-drying temperature, improves dry
Dry efficiency, achievees the purpose that energy saving.
(3) the billet surface quality that this method obtains is high, dry contraction is small, has higher dimensional accuracy.
(4) liquid phase is dried and is combined with vacuum freeze drying by the present invention, utilizes tert-butyl alcohol saturated vapour pressure height, fusing point
Low, the characteristics of surface tension is low, moisture is replaced to exclusion from wet base, the concentration gradient of moisture is formed, promotes hydrone to orient
It is mobile；It can complete to be freeze-dried at relatively high temperatures, freeze efficient, good energy saving property.
(5) inventive method reduces the internal stress that moisture evaporation produces, the shrinking percentage of base substrate is reduced, passes through this method
Dry base substrate shrinking percentage is less than 5%, and shrinking percentage, which reduces, causes base substrate and design size goodness of fit higher, therefore dimensional accuracy carries
Height, the billet surface quality using this method drying is high, it is dry shrink it is small, obtained dried base substrate will not produce cracking,
The defects of deformation.
Embodiment
With reference to embodiment, the present invention will be further described.
Embodiment 1
The aluminum oxide porous block base substrate that water base pulp gel injection moulding is obtained is put into pre-configured drying liquid
Immersion 2h in (tertiary butanol aqueous solution, tert-butyl alcohol volume fraction 70%), then putting it into -40 DEG C of pre-freeze 2h in refrigerator makes it
It is fully crystallized, finally in vacuum 10Pa, -5 DEG C of freeze-dryings are until parch, you can it is 3.5%, without cracking to obtain shrinking percentage
Alumina porous ceramic base substrate.
Embodiment 2
Water base pulp gel injection moulding is obtained into aluminum oxide porous block base substrate and is put into pre-configured drying liquid (uncle
Butanol aqueous solution, tert-butyl alcohol volume fraction 10%) in immersion 6h, then putting it into -60 DEG C of pre-freeze 2h in refrigerator makes its complete
Holocrystalline, finally in vacuum 10Pa, -20 DEG C of freeze-dryings are until parch, you can it is 4.7%, without cracking to obtain shrinking percentage
Alumina porous ceramic base substrate.
Embodiment 3
The water base pulp gel injection moulding acquisition bar-shaped base substrate of aluminium oxide is put into the pre-configured drying liquid (tert-butyl alcohol
Aqueous solution, tert-butyl alcohol volume fraction 50%) in immersion 4h, then putting it into -40 DEG C of pre-freeze 2h in refrigerator makes it tie completely
Crystalline substance, finally in vacuum 10Pa, -5 DEG C of freeze-dryings are until parch, you can obtain shrinking percentage as the 4.3%, aluminium oxide without cracking
Bar shaped ceramic base substrate.
Embodiment 4
Water base pulp gel injection moulding acquisition zirconium oxide ring-type base substrate is put into the pre-configured drying liquid (tert-butyl alcohol
Aqueous solution, tert-butyl alcohol volume fraction 70%) in immersion 2h, then putting it into -40 DEG C of pre-freeze 2h in refrigerator makes it tie completely
Crystalline substance, finally in vacuum 10Pa, -5 DEG C of freeze-dryings are until parch, you can obtain shrinking percentage as the 3.9%, zirconium oxide without cracking
Ring-shaped pottery base substrate.
Claims (8)
- A kind of 1. drying means of water base pulp gel injection moulding base substrate, it is characterised in that：Comprise the following steps：The wet base that water base pulp gel injection moulding obtains is immersed in tertiary butanol aqueous solution and is dried；Then by its pre-freeze Afterwards, then vacuum freeze drying is carried out, obtains dried base substrate.
- 2. the drying means of water base pulp gel injection moulding base substrate according to claim 1, it is characterised in that：The tert-butyl alcohol The volume fraction of the tert-butyl alcohol is 10~70% in aqueous solution.
- 3. the drying means of water base pulp gel injection moulding base substrate according to claim 1, it is characterised in that：Pre-freeze temperature Spend for -40~-60 DEG C, the time is 2~4h.
- 4. the drying means of water base pulp gel injection moulding base substrate according to claim 1, it is characterised in that：Vacuum is cold Freezing dry drying condition is：Vacuum is less than 15Pa, and temperature is -5~-20 DEG C.
- 5. according to the drying means of any water base pulp gel injection moulding base substrates of claim 1-4, it is characterised in that： Step is as follows：(1) the wet base for obtaining water base pulp gel injection moulding is put on grid beam, is then dipped into wet base and grid beam In tertiary butanol aqueous solution, interruption weighs base substrate weight, until its constant weight, obtains the ceramic body of liquid phase drying；(2) it is fully crystallized it in -40~-60 DEG C of 2~4h of pre-freeze the ceramic body that step (1) obtains；(3) base substrate that step (2) obtains is subjected to vacuum freeze drying under the conditions of vacuum is less than 15Pa, -5~-20 DEG C, It is disconnected to weigh, no longer change to weight, you can obtain dried base substrate.
- 6. the drying means of water base pulp gel injection moulding base substrate according to claim 5, it is characterised in that：Step (1) soaking time in is 2~6h.
- 7. the drying means of water base pulp gel injection moulding base substrate according to claim 5, it is characterised in that：Step (1) grid beam in is aluminum porous web screen work.
- 8. the drying means of water base pulp gel injection moulding base substrate according to claim 5, it is characterised in that：Vacuum is cold It is lyophilized dry to be carried out in vacuum freeze drier.
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| CN201711123960.7A CN108017396A (en) | 2017-11-14 | 2017-11-14 | The drying means of water base pulp gel injection moulding base substrate |
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| CN201711123960.7A CN108017396A (en) | 2017-11-14 | 2017-11-14 | The drying means of water base pulp gel injection moulding base substrate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111925217A (en) * | 2020-07-17 | 2020-11-13 | 长沙理工大学 | Method for drying wet gel blank of ceramic precursor and method for preparing ceramic body |
| CN113664970A (en) * | 2021-08-26 | 2021-11-19 | 苏州炻原新材料科技有限公司 | Device for liquid phase drying of gel injection molding blank and using method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111925217A (en) * | 2020-07-17 | 2020-11-13 | 长沙理工大学 | Method for drying wet gel blank of ceramic precursor and method for preparing ceramic body |
| CN111925217B (en) * | 2020-07-17 | 2022-11-22 | 长沙理工大学 | Method for drying wet gel blank of ceramic precursor and method for preparing ceramic body |
| CN113664970A (en) * | 2021-08-26 | 2021-11-19 | 苏州炻原新材料科技有限公司 | Device for liquid phase drying of gel injection molding blank and using method |
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Application publication date: 20180511 |