CN108821767A - A kind of preparation method of compound zirconia pottery backboard - Google Patents

A kind of preparation method of compound zirconia pottery backboard Download PDF

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Publication number
CN108821767A
CN108821767A CN201810635869.1A CN201810635869A CN108821767A CN 108821767 A CN108821767 A CN 108821767A CN 201810635869 A CN201810635869 A CN 201810635869A CN 108821767 A CN108821767 A CN 108821767A
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backboard
preparation
compound zirconia
zirconia pottery
gained
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CN108821767B (en
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贾建平
周晖雨
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SUZHOU SHANREN NANO TECHNOLOGY Co.,Ltd.
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Suzhou Mountain Man Nano Technology Co Ltd
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Abstract

The invention discloses a kind of preparation method of compound zirconia pottery backboard, this method pours compound zirconia pelletizing into dry-pressing formed in backboard mold, and backboard sintered body can be prepared after degreasing, high-temperature roasting and flash burning technology in gained model.A kind of preparation method of compound zirconia pottery backboard involved in this patent, combine hot pressed sintering and flash burning technology, the temperature of its high-temperature roasting is 500-700 DEG C lower than hot pressing and sintering technique, and the total time of high-temperature roasting is no more than two minutes, gained backboard sintered body is not only suitable with the mechanical property of hot pressing and sintering technique products obtained therefrom, also has the characteristics that compact structure and without microscopic holes defect；In addition, this method also has the advantages that the simple controllable, preparation of process is efficiently and more energy saving, it is suitble to industrialized production.

Description

A kind of preparation method of compound zirconia pottery backboard
Technical field
The invention belongs to pottery backboard technical fields, and in particular to a kind of preparation method of compound zirconia pottery backboard.
Background technique
With the development of mechanics of communication and mobile phone science and technology, 5G and wireless charging epoch, but the two was to cell phone back at hand The material of plate it is more demanding, need it as small as possible to the screen effect of electromagnetic signal, therefore nonmetallic back veneer material will become The inevitable choice of the following mobile phone.
Combined oxidation zircon ceramic possesses the performances such as good hardness, flexural strength, toughness and thermal conductivity, compares plastics and glass The nonmetallic materials such as glass backboard it is with the obvious advantage；In addition, combined oxidation zircon ceramic has beautiful, pro-skin characteristic, it is expected to it Applied to high-end handsets product.The production processing flow of compound zirconia pottery backboard can be divided into material ingredient, molding, sintering, Finish four big links；Wherein, sintering process generally uses high temperature sintering technique, and not only the used time is longer, energy consumption is larger, but also The control of product quality is more difficult and products obtained therefrom yield is lower, higher cost and production so as to cause current pottery backboard Energy is limited, especially three-dimension mobile phone backboard, and due to its design shape complexity, mechanical processing difficulty can be bigger, if can burn Machining allowance is reduced during knot, realizes near-net-shape, it will the production cost of mobile phone backboard is greatly reduced.Therefore, quickly high The combined oxidation zircon ceramic three-dimension mobile phone backboard sintering process of effect is the key point for accelerating its application.
Summary of the invention
In order to solve the above technical problems, the present invention proposes a kind of preparation method of compound zirconia pottery backboard, not only mention The high production efficiency and performance of compound zirconia pottery backboard, also reduces production cost.
In order to achieve the above object, technical scheme is as follows：A kind of preparation side of compound zirconia pottery backboard Method includes the following steps：
(1) compound zirconia pelletizing is poured into dry-pressing formed in backboard mold；
(2) gained model in step (1) is placed in degreasing in air and biscuit is made；
(3) gained biscuit in step (2) is placed in air and is roasted；
(4) electrode is placed in gained biscuit two sides in step (3) and passes to direct current, linearly increasing voltage is until dodge Optical phenomenon, then constant current and it is sintered certain time, backboard sintered body can be obtained by being cooled to room temperature.
Preferably, the backboard is three-dimension mobile phone backboard.
Preferably, compound zirconia pelletizing is composed of the following components in the step (1)：Yttrium oxide 3-12mol%, Zirconium oxide 22-88mol%, aluminum oxide 0-66mol%.
Preferably, pressure dry-pressing formed in the step (1) is 200-250MPa, dwell time 20-40s.
Preferably, the skimming temp of model is 400-500 DEG C in the step (2), degreasing time 2-4h.
Preferably, the maturing temperature of biscuit is 900-1000 DEG C in the step (3), calcining time 30-60s.
Preferably, the electrode in the step (4) is platinum electrode.
Preferably, the voltage increase rate in the step (4) is 20-100V/s.
Preferably, the constant current in the step (4) is 800-1000A.
Preferably, the sintering time in the step (4) under constant current is 20-50s.
Preferably, voltage when phosphere occurring in the step (4) is 60-100V.
Beneficial effects of the present invention：The present invention relates to a kind of preparation method of compound zirconia pottery backboard, this method knots Hot pressed sintering and flash burning technology have been closed, the temperature of high-temperature roasting is 500-700 DEG C lower than hot pressing and sintering technique, and high-temperature roasting Total time is no more than two minutes, and gained backboard sintered body is not only suitable with the mechanical property of hot pressing and sintering technique products obtained therefrom, also Have the characteristics that compact structure, without microscopic holes defect, 99.5% or more of density accessibility theory density, bending strength is higher than 850MPa, fracture toughness are more than 7MPam1/2, and average grain size is less than 1 micron；In addition, this method also has process simple Single advantage controllable, preparation is efficiently and more energy saving, is suitble to industrialized production.
Detailed description of the invention
In order to illustrate more clearly of technical solution of the present invention, attached drawing used in embodiment description will be made below simple It introduces.
Fig. 1 is the SEM figure that embodiment one prepares gained backboard sintered body；
Fig. 2 is the SEM figure that embodiment two prepares gained backboard sintered body；
Fig. 3 is the SEM figure that embodiment three prepares gained backboard sintered body；
Fig. 4 is the SEM figure that example IV prepares gained backboard sintered body.
Specific embodiment
In order to make those skilled in the art more fully understand the technical solution in the application, below in conjunction with embodiment to this Technical solution in application carries out clear, complete description.
Embodiment one
A kind of preparation method of compound zirconia pottery backboard, includes the following steps：
(1) compound zirconia pelletizing is poured into three-dimension mobile phone backboard mold, and pressure maintaining 30s can be done under 200Mpa It is molded, wherein the ingredient of compound zirconia pelletizing is shown in Table 1；
(2) gained model in step (1) is placed in air the degreasing 2.0h at 470 DEG C and biscuit is made；
(3) gained biscuit in step (2) is placed in air and roasts 50s at 930 DEG C；
(4) platinum electrode is placed in gained biscuit two sides in step (3) and passes to direct current, increased with the speed linearity of 60V/s Making alive in 950A and maintains 20s until phosphere occurs, by electric current is constant, then is cooled to room temperature and can obtain backboard sintering Body.
Field emission microscope (SEM) characterization is carried out to gained backboard sintered body, it as a result as shown in Figure 1, can from figure Know, the compact structure of the present embodiment preparation gained backboard sintered body, no Micro porosity defect, even grain size, average crystalline substance Particle size is less than 1 micron.
Embodiment two
A kind of preparation method of compound zirconia pottery backboard, includes the following steps：
(1) compound zirconia pelletizing is poured into three-dimension mobile phone backboard mold, and pressure maintaining 20s can be done under 220Mpa It is molded, wherein the ingredient of compound zirconia pelletizing is shown in Table 1；
(2) gained model in step (1) is placed in air and biscuit is made in 400 DEG C of degreasing 2.5h；
(3) gained biscuit in step (2) is placed in air and roasts 40s at 1000 DEG C；
(4) platinum electrode is placed in gained biscuit two sides in step (3) and passes to direct current, increased with the speed linearity of 20V/s Making alive in 1000A and maintains 30s until phosphere occurs, by electric current is constant, then is cooled to room temperature and can obtain backboard sintering Body.
Field emission microscope (SEM) characterization is carried out to gained backboard sintered body, it as a result as shown in Fig. 2, can from figure Know, the compact structure of the present embodiment preparation gained backboard sintered body, no Micro porosity defect, even grain size, average crystalline substance Particle size is less than 1 micron.
Embodiment three
A kind of preparation method of compound zirconia pottery backboard, includes the following steps：
(1) compound zirconia pelletizing is poured into three-dimension mobile phone backboard mold, and pressure maintaining 40s can be done under 230Mpa It is molded, wherein the ingredient of compound zirconia pelletizing is shown in Table 1；
(2) gained model in step (1) is placed in air and biscuit is made in 500 DEG C of degreasing 3.0h；
(3) gained biscuit in step (2) is placed in air and roasts 30s at 900 DEG C；
(4) platinum electrode is placed in gained biscuit two sides in step (3) and passes to direct current, increased with the speed linearity of 100V/s Making alive in 800A and maintains 40s until phosphere occurs, then by electric current is constant, and backboard sintered body can be obtained by being cooled to room temperature.
Field emission microscope (SEM) characterization is carried out to gained backboard sintered body, it as a result as shown in figure 3, can from figure Know, the compact structure of the present embodiment preparation gained backboard sintered body, no Micro porosity defect, even grain size, average crystalline substance Particle size is less than 1 micron.
Example IV
A kind of preparation method of compound zirconia pottery backboard, includes the following steps：
(1) compound zirconia pelletizing is poured into three-dimension mobile phone backboard mold, and pressure maintaining 35s can be done under 250Mpa It is molded, wherein the ingredient of compound zirconia pelletizing is shown in Table 1；
(2) gained model in step (1) is placed in air and biscuit is made in 450 DEG C of degreasing 4.0h；
(3) gained biscuit in step (2) is placed in air and roasts 60s at 970 DEG C；
(4) platinum electrode is placed in gained biscuit two sides in step (3) and passes to direct current, increased with the speed linearity of 80V/s Making alive in 900A and maintains 50s until phosphere occurs, then by electric current is constant, and backboard sintered body can be obtained by being cooled to room temperature.
Field emission microscope (SEM) characterization is carried out to gained backboard sintered body, it as a result as shown in figure 4, can from figure Know, the compact structure of the present embodiment preparation gained backboard sintered body, no Micro porosity defect, even grain size, average crystalline substance Particle size is less than 1 micron.
Table 1
Comparative example one
Using the raw material proportioning of embodiment one and backboard sintered body is made by traditional hot pressing and sintering technique.
It is tough to the progress of backboard sintered body prepared by embodiment one to four and comparative example one density, bending strength, fracture Property and Mechanics Performance Testing, test result are as shown in table 2.
Wherein, the test method of density is Archimedes method, test temperature：25℃；Bending strength is surveyed using bending strength Instrument is tried, test method is three-point bending method；The test method of fracture toughness is indentation method；
Table 2
As can be seen from Table 2, the mechanical property of the backboard sintered body of doped alumina significantly improves, and side of the present invention Method can obtain the backboard sintered body of compact structure, density accessibility theory density (6.11g/cm3) 99.5% or more, bending strength Higher than 850MPa, fracture toughness is more than 7MPam1/2；In addition, comparative example one and comparative example one are it is found that the method for the present invention institute Product mechanical property it is suitable with hot pressing and sintering technique products obtained therefrom, but the present invention progress high-temperature roasting temperature it is lower, when Between it is shorter, thus preparation cost is lower, simple production process, green and controllable.
Embodiment described above is only presently preferred embodiments of the present invention, and the limitation not to embodiment.It should be pointed out that For those of ordinary skill in the art, without departing from the inventive concept of the premise, can also make it is several deformation and It improves, these are all within the scope of protection of the present invention.

Claims (10)

1. a kind of preparation method of compound zirconia pottery backboard, which is characterized in that include the following steps：
(1) compound zirconia pelletizing is poured into dry-pressing formed in backboard mold；
(2) gained model in step (1) is placed in degreasing in air and biscuit is made；
(3) gained biscuit in step (2) is placed in air and is roasted；
(4) electrode is placed in gained biscuit two sides in step (3) and passes to direct current, linearly increasing voltage is until occur to glisten existing As, then constant current and it being sintered certain time, backboard sintered body can be obtained by being cooled to room temperature.
2. a kind of preparation method of compound zirconia pottery backboard according to claim 1, which is characterized in that the back Plate is three-dimension mobile phone backboard.
3. a kind of preparation method of compound zirconia pottery backboard according to claim 1, which is characterized in that the step (1) compound zirconia pelletizing is composed of the following components in：Yttrium oxide 3-12mol%, zirconium oxide 22-88mol%, three oxidations two Aluminium 0-66mol%.
4. a kind of preparation method of compound zirconia pottery backboard according to claim 1, which is characterized in that the step (1) dry-pressing formed pressure is 200-250MPa, dwell time 20-40s in.
5. a kind of preparation method of compound zirconia pottery backboard according to claim 1, which is characterized in that the step (2) skimming temp of model is 400-500 DEG C in, degreasing time 2-4h.
6. a kind of preparation method of compound zirconia pottery backboard according to claim 1, which is characterized in that the step (3) maturing temperature of biscuit is 900-1000 DEG C in, calcining time 30-60s.
7. a kind of preparation method of compound zirconia pottery backboard according to claim 1, which is characterized in that the step (4) electrode in is platinum electrode.
8. according to claim 1 or a kind of preparation method of compound zirconia pottery backboard described in 7, which is characterized in that institute Stating the voltage increase rate in step (4) is 20-100V/s.
9. a kind of preparation method of compound zirconia pottery backboard according to claim 1, which is characterized in that the step (4) constant current in is 800-1000A.
10. according to claim 1 or a kind of preparation method of compound zirconia pottery backboard described in 9, which is characterized in that institute Stating the sintering time in step (4) under constant current is 20-50s.
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CN109734445A (en) * 2019-03-06 2019-05-10 武汉理工大学 A kind of electric field-assisted flash sintering method of Ultra-fine Grained hafnium oxide ceramics
CN114222724A (en) * 2019-07-29 2022-03-22 国立大学法人东海国立大学机构 Method and apparatus for manufacturing sintered body
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CN113307624A (en) * 2021-05-13 2021-08-27 佛山华骏特瓷科技有限公司 Method for sintering ceramic at room temperature
CN113754435A (en) * 2021-09-08 2021-12-07 郑州航空工业管理学院 Y2O3Preparation method of-MgO infrared transparent ceramic
CN113754435B (en) * 2021-09-08 2023-12-22 郑州航空工业管理学院 Y (Y) 2 O 3 Method for preparing MgO infrared transparent ceramic

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