CN110511021A - A kind of novel zirconia ceramics forming method - Google Patents
A kind of novel zirconia ceramics forming method Download PDFInfo
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Abstract
The invention discloses a kind of novel zirconia ceramics forming methods and drying process, belong to function ceramics field.Gel-casting method prepares that zirconium oxide is higher compared to traditional injection forming zirconium oxide intensity, compact density is bigger, and the ceramic for preparation large scale and complicated shape provides effective technological approaches.With very big development space.Zirconium powder uses superfine zirconia powder, granularity d50=0.5μm.It is characterized in that, reaching the wet base of rapid draing using different drying modes, so as to shorten process time.
Description
Technical field
The invention belongs to inorganic non-metallic materials and function ceramics field, are related to a kind of forming method of zirconia ceramics
And drying process.
Background technique
Currently, the forming method of ceramics can be divided into two major classes, dry-press process and wet forming.Dry-press process is obtained
Zirconia green body compactness is poor, generally can only be used to make the ceramic product of some simple shapes.Wet forming compared with dry method at
Type improves the compactness of zirconia ceramics after molding, and substantially increases intensity after zirconia ceramics green compact and sintering.
The 1990s develops a kind of completely new colloidal state rapid shaping skill by U.S. Janeey and professor Omatete
Art, abbreviation gel casting forming.Gel casting forming is that one kind fully utilizes polymer chemistry, colloid chemistry, polymer
The novel forming technology of the multi-disciplinary theory such as reason and traditional ceramics moulding process.The technology is excellent in processability and shape
Extremely there is advantage when the ceramic part of complexity, because the mobility of its slurry is preferable, can be very good to fill full mold, and
Powder lot dispersing is uniform in ceramic slurry, and the higher product of intensity can be formed after sintering.
Zirconia ceramics Problems in gel casting forming are as follows:
Currently, Zirconium powder used in 1. gel injection-mouldings is mostly sub-micron or Nano grade ceramic powder, due to ceramic powder compared with
Carefully, large specific surface area, ceramic powder are easy to reunite.The key of gel casting forming zirconia ceramics is that preparing high solid phase contains
The slurry of amount, low viscosity, selects suitable dispersing agent that can reduce the viscosity of slurry to improve the solid content of slurry, to can be improved
The compactness and intensity of zirconia ceramics.2. wet base deforms in the drying process in order to prevent, wet base usually require as
Air drying 2 ~ 4 days, it is then placed in drying 5 ~ 7 days in electric air dry oven again, entire process time is relatively long.
Summary of the invention
Goal of the invention;The forming method for providing a kind of ceramics prepares base to overcome the shortcomings of traditional ceramics forming method
Body intensity high, relatively denser, complicated shape near net-shape precise ceramic component, the different drying mode of simultaneous selection contract
The short processes time.
Technical solution: it in order to solve the above problem, is implemented with the following technical solutions:
A, using deionized water as solvent, monomer, crosslinking agent and anti-foaming agent is added, is fitted into ball grinder ball milling 5 minutes or use
It is configured within blender strong stirring 15 minutes premixed liquid, adjusting pH is 10.5.
B, Zirconium powder (volume content 44% ~ 50%) is added in configured premixed liquid, 4.5 hours configuration slurries of ball milling add
Enter injection molding after defoaming agent, initiator and catalyst stir, is placed in 70 DEG C of vacuum oven solidifications.
C, the wet base after solidification is 1. placed in air drying 3 days, is then placed in electric air dry oven and is dried gradually again
Heating is 6 days dry.2. the wet base after solidification is placed in 8h in PEG10000 solution, be subsequently placed in electric air dry oven dry by
The temperature that edges up is 6 days dry.3. the wet base after solidification is placed in climatic chamber dry 12h, humidity is gradually decreased, finally as electricity
It dries in air dry oven to constant weight.
D, the zirconium oxide green compact after drying are sintered according to the DTA curve of xerogel to 1520 DEG C and keep the temperature 2 hours.
Such as above-mentioned method, it is preferred that monomer is Methacrylamide (MAM).
Such as above-mentioned method, it is preferred that crosslinking agent N, N- methylene-bisacrylamide (MBAM).
Such as above-mentioned method, it is preferred that catalyst is tetramethylethylenediamine.
Such as above-mentioned method, it is preferred that initiator is ammonium persulfate (APS).
Such as above-mentioned method, it is preferred that dispersing agent is 2- phosphonobutane -1,2,4- tricarboxylic acids.
Such as above-mentioned method, it is preferred that Zirconium powder content is 50%.
The utility model has the advantages that
1. gel casting forming zirconia ceramics is opposite compared with traditional shaping method of ceramics, green compact are obtained with sinter intensity
It improves, zirconia ceramics compact density is high, and internal particle is fine and close.
2. the dry wet base time can be greatly reduced using wet-drying or using the drying of constant temperature and humidity drying case.
Detailed description of the invention
Fig. 1 is zirconium oxide green compact SEM figure, and Fig. 2 is that zirconia ceramics is sintered SEM figure.
Specific embodiment
The invention specific implementation step is as follows:
Embodiment 1:
Take 20ml deionized water that 3g Methacrylamide, 0.56g polyvinylpyrrolidone, 0.2g methylene bisacrylamide acyl is added
Amine, ball milling 5min configures premixed liquid in the ball mill, and adjusting premixed liquid pH using ammonium hydroxide is 10.5, and it is 50% that volume content, which is added,
Part yttrium stable zirconium oxide powder mass percent seperated with 2wt%(zirconium oxide) 2- phosphoric acid butane -1,2,4 tricarboxylic acids, and
Ball milling 5h prepares slurry.
The slurry prepared is poured into beaker and is vacuumized 5min, sequentially add n-octyl alcohol (the 0.1% of stock quality),
Ammonium persulfate (the 2.5% of monomer mass) and tetramethylethylenediamine (drop) inject in 50 × 10 × 10 molds after mixing evenly, put
Enter solidification 30min or so in 70 DEG C of vacuum ovens (not vacuumizing).It demoulds after the completion of solidification, first does wet base in air
Dry 3 days, wet base is then put into the curve in electric air dry oven according to setting and is gradually warmed up drying, final temperature is set as
100 DEG C, finally green compact are burnt according to TG-DTA curve setting to 1520 DEG C of heat preservation 2h.
Zirconia ceramics green compact bending strength reaches 18.7MPa, green density 3.08g/cm after drying3, green compact it is dry
Dry shrinking percentage is 2.5%, and zirconia ceramics bending strength reaches 502.3MPa, bulk density 5.87g/cm after sintering3。
Embodiment 2:
Take 20ml deionized water that 3g Methacrylamide, 0.56g polyvinylpyrrolidone, 0.2g methylene bisacrylamide acyl is added
Amine, ball milling 5min configures premixed liquid in the ball mill, and adjusting premixed liquid pH using ammonium hydroxide is 10.5, and it is 50% that volume content, which is added,
Part yttrium stable zirconium oxide powder mass percent seperated with 2wt%(zirconium oxide) 2- phosphoric acid butane -1,2,4 tricarboxylic acids, and
Ball milling 5h prepares slurry.
The slurry prepared is poured into beaker and is vacuumized 5min, sequentially add n-octyl alcohol (the 0.1% of stock quality),
Ammonium persulfate (the 2.5% of monomer mass) and tetramethylethylenediamine (drop) inject in 50 × 10 × 10 molds after mixing evenly, put
Enter solidification 30min or so in 70 DEG C of vacuum ovens (not vacuumizing).It is demoulded after the completion of solidification, wet base is put into and has configured concentration
For 8h in 20% PEG10000 solution, then wet base is dried according to 1 drying mode of example, final temperature is set as 100
DEG C, green compact are finally fired into 1520 DEG C of heat preservation 2h according to TG-DTA curve setting.
Zirconia ceramics green compact bending strength reaches 12.3MPa, green density 2.97g/cm after drying3, green compact it is dry
Dry shrinking percentage is 2%, and zirconia ceramics bending strength reaches 263.4MPa, bulk density 5.73g/cm after sintering3。
Embodiment 3:
Take 20ml deionized water that 3g Methacrylamide, 0.56g polyvinylpyrrolidone, 0.2g methylene bisacrylamide acyl is added
Amine, ball milling 5min configures premixed liquid in the ball mill, and adjusting premixed liquid pH using ammonium hydroxide is 10.5, and it is 50% that volume content, which is added,
Part yttrium stable zirconium oxide powder mass percent seperated with 2wt%(zirconium oxide) 2- phosphoric acid butane -1,2,4 tricarboxylic acids, and
Ball milling 5h prepares slurry.
The slurry prepared is poured into beaker and is vacuumized 5min, sequentially add n-octyl alcohol (the 0.1% of stock quality),
Ammonium persulfate (the 2.5% of monomer mass) and tetramethylethylenediamine (drop) inject in 50 × 10 × 10 molds after mixing evenly, put
Enter solidification 30min or so in 70 DEG C of vacuum ovens (not vacuumizing).It is demoulded after the completion of solidification, wet base is put into climatic chamber
In, dry 2h, then increases the temperature to 80 DEG C of dry 2h, then humidity is reduced to first in 40 DEG C, the environment of 98%RH
40%RH and temperature is increased to 100 DEG C of dry 3h, finally green body is put into 80 DEG C of baking oven and is dried to constant weight.Finally will
Green compact fire 1520 DEG C of heat preservation 2h according to TG-DTA curve setting.
Zirconia ceramics green compact bending strength reaches 15.7MPa, green density 2.92g/cm after drying3, green compact are dry
Dry shrinking percentage is 3%, and zirconia ceramics bending strength reaches 274.6MPa, bulk density 5.86g/cm after sintering3。
Sem analysis is carried out to zirconium oxide green compact prepared by embodiment 1 and zirconia ceramics, as shown in Figure 1 and Figure 2, from figure
1 zirconium oxide green compact are observed, and are contacted between zirconia particles more closely, with the presence of a small number of stomatas, generally, zirconium oxide green compact
Inside distribution is more uniform.
Claims (10)
1. technological principle: a kind of method of gel casting forming high intensity zirconia ceramics using deionized water as solvent, is added
Monomer and crosslinking agent form tridimensional network and wrap up Zirconium powder under the action of catalyst and initiator, so as to
Reach in-situ solidifying molding, the zirconia ceramics green body of high-compactness can be obtained.
2. according to forming method described in right 1, which is characterized in that used Zirconium powder is that part yttrium stablizes superfine powder
Body, partial size is at 0.5 μm, yttria levels 5.25wt%.
3. according to forming method described in right 1, it is characterised in that: telling Zirconium powder additional amount is 44% ~ 50%.
4. according to forming method described in right 1, it is characterised in that: the monomer is Methacrylamide (MAM).
5. according to forming method described in right 1, it is characterised in that: the crosslinking agent is N, N- methylene-bisacrylamide
(MBAM).
6. according to forming method described in right 1, it is characterised in that: the initiator is ammonium persulfate (APS).
7. according to forming method described in right 1, it is characterised in that: the catalyst is tetramethylethylenediamine (TEMED).
8. according to forming method described in right 1, it is characterised in that: the dispersing agent is 2- phosphonobutane -1,2,4- tricarboxylic acids
Or calgon or ammonium citrate or tetramethyl second ammonium hydroxide.
9. according to forming method described in right 1, which is characterized in that affiliated zirconium oxide gel-casting method following steps:
1. configuring premixed liquid: deionized water, crosslinking agent, defoaming agent, monomer being configured to premixed liquid and adjust pH, zirconium oxide is added
Powder ball milling prepares slurry;
2. wet base is dry: initiator and catalyst is added in the slurry prepared, then injection molding, solidified, dry, sintering obtains
Zirconium oxide green compact and sinter;Using three kinds of drying modes: 1. dry in air first, and wet base is then placed in electric air blast and is done
In dry case;2. wet base is placed in PEG solution first, then wet base is placed in electric air dry oven again;3. permanent using constant temperature
The dry wet base of wet tank;
3. sintering: doing TG-DTA analysis to xerogel, sintering curre is arranged according to TG-DTA tracing analysis, final sintering temperature is
1520 DEG C, and keep the temperature 2 hours.
10. according to right 9, it is characterised in that: according to step, 2. made zirconium oxide green compact bending strength is 10 ~ 20MPa, raw
Base compact density is 2.7 ~ 3.1g/cm3;Zirconia ceramics bending strength is 200 ~ 500MPa, firing after being 3. burnt into according to step
Zirconium oxide compact density is 5.6 ~ 6g/cm afterwards3。
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111848157A (en) * | 2020-06-11 | 2020-10-30 | 深圳美鸣科技有限公司 | Zirconia ceramic block prepared by gel film-injection process and preparation method thereof |
CN113800906A (en) * | 2021-09-30 | 2021-12-17 | 河南工业大学 | Method for modifying nano zirconium oxide powder by wet method |
CN116375467A (en) * | 2023-02-13 | 2023-07-04 | 三祥新材股份有限公司 | Preparation method of zirconia ceramic backboard of wearable equipment |
-
2019
- 2019-09-10 CN CN201910855097.7A patent/CN110511021A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111848157A (en) * | 2020-06-11 | 2020-10-30 | 深圳美鸣科技有限公司 | Zirconia ceramic block prepared by gel film-injection process and preparation method thereof |
CN113800906A (en) * | 2021-09-30 | 2021-12-17 | 河南工业大学 | Method for modifying nano zirconium oxide powder by wet method |
CN116375467A (en) * | 2023-02-13 | 2023-07-04 | 三祥新材股份有限公司 | Preparation method of zirconia ceramic backboard of wearable equipment |
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