CN109608191A - A kind of high intensity gray oxide zircon ceramic and preparation method thereof - Google Patents
A kind of high intensity gray oxide zircon ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of high-intensitive gray oxide zircon ceramics and preparation method thereof, by carrying out high-energy ball milling processing to the mixed slurry comprising zirconium oxide, yttrium oxide, dispersing agent and deionized water；Then the slurry after high-energy ball milling is dried, obtains nm-class powder of zirconium oxide；Nm-class powder of zirconium oxide is formed again, high temperature sintering, obtains white oxide zircon ceramic；White oxide zircon ceramic is finally placed in atmosphere furnace under hydrogen reducing atmosphere high temperature sintering to get to gray oxide zircon ceramic；Preparation process is simple and convenient, energy consumption and at low cost；Simultaneously, during this technique prepares gray oxide zircon ceramic, it does not need to introduce and there is the transition metal colorants such as volatile Cr, Co, Mn, it solves the problems, such as the easy pyrolytic volatilization of colorant and ceramic color is caused to be unevenly distributed, and avoid the toxic action of colored parts ion pair human body and the doping of section transitions metallochrome to reduce the defect of Mechanical Property of Ceramics.
Description
Technical field
The present invention relates to ceramic technology fields more particularly to a kind of high-intensitive gray oxide zircon ceramic and preparation method thereof.
Background technique
Zirconia ceramics is widely used in because having many advantages, such as excellent thermal property, mechanical property and chemical stability
Aviation and wide, biomaterial, refractory material and ornament materials, the fields such as marine settings, especially field of marine equipment, than
The screw of carrier-borne aircraft, ship Large-Scale Equipment is such as prepared, it is higher to intensity requirement.
In recent years, the requirements such as the color of colored zirconia ceramics, brightness, performance are continuously improved, wherein have excellent performance
The preparation of gray oxide zircon ceramic has become hot and difficult issue.Currently, industrial mainly by being added in white oxide zirconium powder body
Transition metal oxide or rare earth oxide prepare colored zirconia ceramics, and mostly use chemical coprecipitation.
Prepare blue ceramic application No. is CN201710357961.1 and application number CN201710358402.2 prepare it is black
The method of color ceramics is mingled with the transition metal colorant such as Cr, Co, Mn with volatility, the easy pyrolytic of colorant wherein
It volatilizees and ceramic color is caused to be unevenly distributed, and colored parts ion pair human body toxic action, the transition metal such as iron oxide
The doping of colorant can also reduce ceramics mechanical property, especially for it is ornamental directly contact human body ceramics (watch chain,
Button, mobile phone backboard etc.) it is the coloured ceramics for not being available this method preparation；In addition, present some coloured ceramic systems are standby
Method, intensity can only achieve between 850-1000Mpa, and the use in the fields such as marine settings, aeronautical material is far not achieved in performance
It is required that.In addition to this, for chemical coprecipitation preparation process, chemical coprecipitation preparation process can introduce a large amount of acid
Radical ion not only results in the harm to environment, also adds consumption and the preparation cost of the energy, be not inconsistent when washing acid ion
Close the demand for development of the following new material preparation process.
Summary of the invention
The purpose of the present invention is to provide a kind of high-intensitive gray oxide zircon ceramics and preparation method thereof, and the present invention is prepared into
The gray oxide zircon ceramic COLOR COMPOSITION THROUGH DISTRIBUTION arrived is uniform, and effect nontoxic to the human body, good mechanical performance, intensity is big, can satisfy ship
The marine settings materials'use such as oceangoing ship, carrier-borne aircraft, and preparation process safety non-pollution, low energy consumption, high production efficiency.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of preparation methods of high-intensitive gray oxide zircon ceramic, comprising the following steps:
Step 1: to the mixed slurry comprising oxide, dispersing agent and deionized water in sand mill carry out high-energy ball milling processing,
Wherein the quality of oxide is the 35%-55% of the gross mass of oxide dispersing agent and deionized water；The oxide is zirconium oxide
And yttrium oxide；
Step 2: the slurry after high-energy ball milling being dried, nm-class powder of zirconium oxide is obtained；
Step 3: nm-class powder of zirconium oxide is pressed by dry pressuring forming process by required ceramic idiosome, and through high-temperature roasting,
Obtain white oxide zircon ceramic；The maturing temperature is 1350-1500 DEG C；
Step 4: white oxide zircon ceramic being placed under the conditions of high-purity hydrogen high-temperature roasting to get being 1600-1700Mpa to intensity
Gray oxide zircon ceramic, the maturing temperature be 1300-1500 DEG C, wherein high-purity hydrogen be passed through flow be 40-200ml/
The gray scale of min, the gray oxide zircon ceramic restored under the conditions of high-purity hydrogen can reach requirement gray scale, and intensity is big, and
Nontoxic, modes, the intensity of the zirconia ceramics restored such as other restoring method, such as the reduction of carbon monoxide, carbon far reach not
To domain requirements such as ocean, space flight, and reduction is not thorough, and can go out hickie in ceramic surface, ceramic core will appear Bai Xin.
Preferably, the mass ratio of zirconium oxide and yttrium oxide is (942-952): (48-58) in the step 1.
Preferably, the dispersing agent in the step 1 is independently ammonium polyacrylate, sodium tripolyphosphate, calgon, gathers
One or more of methacrylic acid ammonia and polyethylene glycol, the addition quality and zirconium oxide, yttrium oxide and aluminium oxide of dispersing agent
Total mass ratio be (0.2-1.0): 100.
Preferably, Process During High Energy Ball Milling carries out in sand mill in the step 1, and high-energy ball milling revolving speed is 2000-
2500r/min, processing time are 2-6h, and abrasive media is the zirconium oxide bead of 0.1-0.8mm.
Preferably, in the step 2 be dried mode include spray drying, Electric heat oven drying, evaporator dry, from
One or more of heart dehydration, filter-press dehydration.
Preferably, suppressing in the step 3 successively includes the compacting of preforming and isostatic cool pressing, wherein preforming pressure is
5-15MPa；The pressure of isostatic cool pressing compacting is 150-250MPa.
Preferably, the time roasted in the step 3 is 2-5h.
Preferably, the high-temperature roasting time is 2-5h under reducing atmosphere condition in the step 4.
The present invention also provides the gray oxide zircon ceramic that preparation method described in a kind of above-mentioned technical proposal obtains, packets
Include: gray oxide zircon ceramic is single tetragonal phase structure；The density of gray oxide zircon ceramic is 6.06g/cm3More than, hardness is
14.70Gpa or more, intensity are higher than 1000Mpa, and toughness is higher than 9MPam1/2, good mechanical performance.
The beneficial effects of the present invention are provide a kind of preparation method of gray oxide zircon ceramic: the present invention is to comprising oxygen
Change zirconium, yttrium oxide, dispersing agent and deionized water solid content be 35%-55% mixed slurry in being carried out at high-energy ball milling in sand mill
Reason；Then the slurry after high-energy ball milling is dried, obtains nm-class powder of zirconium oxide；By dry pressuring forming process by oxygen
Change zirconium nano-powder and be pressed into required ceramic idiosome, and through 1350-1500 DEG C of high-temperature roasting, obtains white oxide zircon ceramic；
Then through 1300-1500 DEG C of high-temperature roasting under high-purity hydrogen atmospheric condition, i.e., white oxide zircon ceramic is placed in atmosphere furnace
Obtain gray oxide zircon ceramic.The present invention is roasted based on white oxide zircon ceramic using high temperature under high-purity hydrogen atmospheric condition
The technique of burning obtains gray oxide zircon ceramic, and not needing to introduce has the transition metal colorants such as volatile Cr, Co, Mn, solution
The problem of easy pyrolytic of colorant of having determined volatilizees and ceramic color is caused to be unevenly distributed, and avoid colored parts ion
The doping of toxic action and section transitions metallochrome to human body can reduce the defect of Mechanical Property of Ceramics；Meanwhile this system
Standby technique green non-pollution, low energy consumption meet the demand for development of the following new material preparation process.In addition, the present invention provides
Gray oxide zircon ceramic density be 6.06g/cm3More than, hardness is 14.70Gpa or more, and intensity is higher than 1000Mpa, toughness
Higher than 9MPam1/2, good mechanical performance.
Detailed description of the invention
Fig. 1 is that the zirconia nanopowder ceramic powder Flied emission scanning electron that 1 high-energy ball milling of the embodiment of the present invention obtains is aobvious
Micro mirror picture.
Fig. 2 is the XRD diagram of white and gray oxide zircon ceramic in the embodiment of the present invention 2.
Specific embodiment
Gray oxide zircon ceramic provided by the invention and preparation method thereof is described in detail below with reference to embodiment,
But they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
It is 1000 parts of calculating with zirconium oxide and yttrium oxide gross mass, accurately weighs 942 parts of zirconium oxide, 58 parts of yttrium oxide, dispersing agent
2 parts of polymethylacrylic acid ammonia, deionized water is added, adjusting slurry content is 35%, material is imported high energy ball mill, with partial size
For 0.6-0.8mm zirconium oxide bead as abrasive body, high-energy ball milling 6h, rotational speed of ball-mill is 2000 r/min；
Slurry after high-energy ball milling is subjected to spraying drying, adjusting atomization frequency is 45Hz, 240 DEG C of inlet air temperature, leaving air temp
90 DEG C, obtaining partial size is 100nm nano-ceramic powder below；Flied emission scanning electricity is carried out to the nano-ceramic powder being prepared
The detection of sub- microscope, testing result is as shown in Figure 1, as shown in Figure 1, the ceramic powder uniform particle sizes that the present embodiment is prepared,
Less than 100nm.
Zirconia ceramics powder is preforming under 5MPa then further cold etc. through 150MPa by two-way ceramic hydraulic press
Static pressure suppression roasts 5h at 1350 DEG C at ceramic idiosome, and by it, obtains white oxide zircon ceramic.
White oxide zircon ceramic is placed in atmosphere furnace, in 1300 DEG C of roasting 5h under high-purity hydrogen atmospheric condition, wherein
The flow that is passed through of high-purity hydrogen is 40ml/min to get the gray oxide zircon ceramic for being 1675Mpa to intensity.
Embodiment 2
It is 1000 parts of calculating with zirconium oxide and yttrium oxide gross mass, accurately weighs 945 parts of zirconium oxide, 55 parts of yttrium oxide, dispersing agent
4 parts of ammonium polyacrylate, deionized water is added, adjusting slurry content is 40%, and material is imported high energy ball mill, is with partial size
The zirconium oxide bead of 0.5-0.6mm is 2100 r/min as abrasive body, high-energy ball milling 5h, rotational speed of ball-mill；
By the slurry after high-energy ball milling directly through Electric heat oven in 90 DEG C of dry 12h, obtaining partial size is 100nm nanometer pottery below
Porcelain powder.
Zirconia ceramics powder is preforming under 8MPa then further cold etc. through 180MPa by two-way ceramic hydraulic press
Static pressure suppression roasts 4h at 1400 DEG C at ceramic idiosome, and by it, obtains white oxide zircon ceramic.
White oxide zircon ceramic is placed in atmosphere furnace, in 1350 DEG C of roasting 4h under high-purity hydrogen atmospheric condition, wherein
The flow that is passed through of high-purity hydrogen is 80ml/min to get the gray oxide zircon ceramic for being 1655Mpa to intensity.
XRD detection is carried out to the white and gray oxide zircon ceramic being prepared, XRD result is as shown in Fig. 2, from XRD diagram
It can be defined in spectrum, the phase structure of obtained white and gray oxide zircon ceramic is single tetragonal phase structure, miscellaneous without other
Mutually exist.
Embodiment 3
It is 1000 parts of calculating with zirconium oxide and yttrium oxide gross mass, accurately weighs 948 parts of zirconium oxide, 52 parts of yttrium oxide, dispersing agent
6 parts of sodium tripolyphosphate, deionized water is added, adjusting slurry content is 45%, and material is imported high energy ball mill, is with partial size
The zirconium oxide bead of 0.4-0.5mm is 2200 r/min as abrasive body, high-energy ball milling 4h, rotational speed of ball-mill；
Slurry after high-energy ball milling is obtained into the nano-ceramic powder that partial size is less than 100nm in 80 DEG C of dry 8h through evaporator.
Zirconia ceramics powder is preforming under 10MPa then further cold through 200MPa by two-way ceramic hydraulic press
Etc. static pressure suppressions roast 3h at 1450 DEG C at ceramic idiosome, and by it, obtain white oxide zircon ceramic.
White oxide zircon ceramic is placed in atmosphere furnace, in 1400 DEG C of roasting 3h under high-purity hydrogen atmospheric condition, wherein
The flow that is passed through of high-purity hydrogen is 120ml/min to get the gray oxide zircon ceramic for being 1684Mpa to intensity.
Embodiment 4
It is 1000 parts of calculating with zirconium oxide and yttrium oxide gross mass, accurately weighs 950 parts of zirconium oxide, 50 parts of yttrium oxide, dispersing agent
8 parts of calgon, deionized water is added, adjusting slurry solid content is 50%, and material is imported high energy ball mill, is with partial size
The zirconium oxide bead of 0.3-0.4mm is 2300 r/min as abrasive body, high-energy ball milling 3h, rotational speed of ball-mill；
Slurry after high-energy ball milling is subjected to filter-press dehydration first, then through Electric heat oven in 90 DEG C of dry 5h, obtaining partial size is
100nm nano-ceramic powder below.
Zirconia ceramics powder is preforming under 12MPa then further cold through 220MPa by two-way ceramic hydraulic press
Etc. static pressure suppressions roast 2.5h at 1480 DEG C at ceramic idiosome, and by it, obtain white oxide zircon ceramic.
White oxide zircon ceramic is placed in atmosphere furnace, in 1450 DEG C of roasting 2.5h under high-purity hydrogen atmospheric condition,
The flow that is passed through of middle high-purity hydrogen is 160ml/min to get the gray oxide zircon ceramic for being 1679Mpa to intensity.
Embodiment 5
It is 1000 parts of calculating with zirconium oxide and yttrium oxide gross mass, accurately weighs 952 parts of zirconium oxide, 48 parts of yttrium oxide, dispersing agent
10 parts of polyethylene glycol, deionized water is added, adjusting slurry content is 55%, and material is imported high energy ball mill, is 0.1- with partial size
The zirconium oxide bead of 0.2mm is 2500 r/min as abrasive body, high-energy ball milling 2h, rotational speed of ball-mill；
Slurry after high-energy ball milling is subjected to centrifugal dehydration first, then through Electric heat oven in 90 DEG C of dry 5h, obtaining partial size is
100nm nano-ceramic powder below.
Zirconia ceramics powder is preforming under 15MPa then further cold through 250MPa by two-way ceramic hydraulic press
Etc. static pressure suppressions roast 2h at 1500 DEG C at ceramic idiosome, and by it, obtain white oxide zircon ceramic.
White oxide zircon ceramic is placed in atmosphere furnace, in 1500 DEG C of roasting 2h under high-purity hydrogen atmospheric condition, wherein
The flow that is passed through of high-purity hydrogen is 200ml/min to get the gray oxide zircon ceramic for being 1688Mpa to intensity.
The present invention detects the physical property of the obtained gray oxide zircon ceramic of embodiment 1-5, before reduction
White oxide zircon ceramic carry out performance evaluation comparison.
The physical property of white oxide zircon ceramic before 1 embodiment 1-5 of table is restored
The physical property of the obtained gray oxide zircon ceramic of 2 embodiment 1-5 of table
As can be seen from Table 2, the gray oxide zircon ceramic that the present invention is prepared is fine and close, and density reaches 6.06g/cm3More than,
Vickers hardness is higher than 14.70Gpa, and intensity is higher than 1600Mpa, and toughness has been more than 9MPa m1/2, technical solution through the invention
The excellent in mechanical performance of the gray oxide zircon ceramic of preparation, especially intensity, much higher than the ceramics strength before reduction.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (7)
1. a kind of preparation method of high intensity gray oxide zircon ceramic, it is characterised in that: prepare the use of gray oxide zircon ceramic
Raw material are as follows: oxycompound, dispersing agent, deionized water and high-purity hydrogen are as reducing agent, and wherein oxycompound is zirconium oxide and oxygen
Change yttrium, the quality of oxide is the 35%-55% of the gross mass of dispersing agent and deionized water；The quality of the zirconium oxide and yttrium oxide
Than for (942-952): (48-58)；The preparation of zirconia ceramics the following steps are included:
Step 1: to the mixed slurry comprising oxide, dispersing agent and deionized water in sand mill carry out high-energy ball milling processing,
Form slurry；
Step 2: the slurry after high-energy ball milling being dried, nm-class powder of zirconium oxide is obtained；
Step 3: nm-class powder of zirconium oxide described in step 2 is pressed by dry pressuring forming process by required ceramic idiosome,
And through high-temperature roasting, white oxide zircon ceramic is obtained；The maturing temperature is 1350-1500 DEG C, and the time of roasting is 2-5h；
Step 4: white oxide zircon ceramic, which is placed under high-purity hydrogen reducing atmosphere condition high-temperature roasting to get to intensity, is
The gray oxide zircon ceramic of 1600-1700Mpa, the maturing temperature are 1300-1500 DEG C, calcining time 2-5h.
2. a kind of preparation method of high-intensitive gray oxide zircon ceramic according to claim 1, it is characterised in that: the step
Dispersing agent in rapid 1 is independently ammonium polyacrylate, sodium tripolyphosphate, calgon, polymethylacrylic acid ammonia and poly- second two
One or more of alcohol, the addition quality of dispersing agent and the total mass ratio of zirconium oxide, yttrium oxide and aluminium oxide are (0.2-
1.0): 100.
3. a kind of preparation method of high-intensitive gray oxide zircon ceramic according to claim 1, it is characterised in that: the step
The process of high-energy ball milling carries out in sand mill in rapid 1, and high-energy ball milling revolving speed is 2000-2500r/min, and the processing time is 2-
6h, abrasive media are the zirconium oxide bead of 0.1-0.8mm.
4. a kind of preparation method of high-intensitive gray oxide zircon ceramic according to claim 1, it is characterised in that: the step
It includes spray drying, Electric heat oven drying, evaporator dry, centrifugal dehydration, one in filter-press dehydration that mode is dried in rapid 2
Kind is several.
5. a kind of preparation method of high-intensitive gray oxide zircon ceramic according to claim 1, it is characterised in that: the step
Suppressing in rapid 3 successively includes the compacting of preforming and isostatic cool pressing, wherein preforming pressure is 5-15MPa；Isostatic cool pressing compacting
Pressure be 150-250MPa.
6. a kind of preparation method of high-intensitive gray oxide zircon ceramic according to claim 1, it is characterised in that: the height
The flow that is passed through of pure hydrogen is 40-200ml/min.
7. the high-intensitive gray oxide zircon ceramic that preparation method described in -6 any one obtains according to claim 1, feature
Be: the gray oxide zircon ceramic is single tetragonal phase structure；The density of the gray oxide zircon ceramic is 6.06g/cm3With
On, hardness is 14.70Gpa or more, and intensity is higher than 1000Mpa, and toughness is higher than 9MPam1/2。
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| CN113563070A (en) * | 2021-08-16 | 2021-10-29 | 内蒙古科技大学 | Toughened purple ceramic and preparation method thereof |
| CN113582688A (en) * | 2021-09-01 | 2021-11-02 | 内蒙古科技大学 | High-toughness haze gray ceramic and preparation method thereof |
| CN115093217A (en) * | 2022-06-20 | 2022-09-23 | 深圳陶陶科技有限公司 | Preparation method of gray zirconia ceramic and gray zirconia ceramic |
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| CN113563070A (en) * | 2021-08-16 | 2021-10-29 | 内蒙古科技大学 | Toughened purple ceramic and preparation method thereof |
| CN113563070B (en) * | 2021-08-16 | 2022-10-11 | 内蒙古科技大学 | Toughened purple ceramic and preparation method thereof |
| CN113582688A (en) * | 2021-09-01 | 2021-11-02 | 内蒙古科技大学 | High-toughness haze gray ceramic and preparation method thereof |
| CN113582688B (en) * | 2021-09-01 | 2022-10-14 | 内蒙古科技大学 | High-toughness haze gray ceramic and preparation method thereof |
| CN115093217A (en) * | 2022-06-20 | 2022-09-23 | 深圳陶陶科技有限公司 | Preparation method of gray zirconia ceramic and gray zirconia ceramic |
| CN115093217B (en) * | 2022-06-20 | 2023-07-14 | 深圳陶陶科技有限公司 | Preparation method of gray zirconia ceramic and gray zirconia ceramic |
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