CN103193481B - Preparation method of zirconium oxide product - Google Patents
Preparation method of zirconium oxide product Download PDFInfo
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- CN103193481B CN103193481B CN201310128272.5A CN201310128272A CN103193481B CN 103193481 B CN103193481 B CN 103193481B CN 201310128272 A CN201310128272 A CN 201310128272A CN 103193481 B CN103193481 B CN 103193481B
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Abstract
The invention discloses a preparation method of a zirconium oxide product. The preparation method comprises the following steps of: mixing and grinding zirconium oxide, basic magnesium carbonate, iridium oxide and strontium oxide which are taken as raw materials to obtain fine powder, adding glue water, and performing pressure compression in a die to obtain a brick blank; firing the brick blank in a kiln to obtain a primary blank, grinding the primary blank to obtain granules, and deironing and ball-milling the granule to obtain powder; mixing the powder, granules, electrically fused calcium oxide stabilized zirconium oxide and PDA glue water, stirring, sieving, shaking and drying to obtain a mixture; and compression moulding the mixture in a die, drying, loading into the kiln, firing at high temperature, discharging out of the kiln, inspecting and packaging to obtain finished zirconium oxide product. The preparation method disclosed by the invention can be used for greatly improving anti-flushing performance of the product, the strength of the blank and the product yield, guaranteeing the moulding density and controlling the product shrinkage within 6-8%; and the process is not only simple but also easy to operate, and can be used for effectively reducing the firing crack and guaranteeing the product quality.
Description
Technical field
The invention belongs to zirconium product process for processing technical field, be specifically related to a kind of preparation method of zircite product.
Background technology
The zirconium product using is at present all to add a small amount of electric smelting monoclinic zirconia or desiliconization zirconium white, compression moulding, and the poor stability of this method product, and also work-ing life is short.The structure of existing zirconium product is single, although increased titanium dioxide, calcium oxide etc., increase certain stability, but its physical strength is poor, and wear resistance is inadequate, in addition, owing to there is no deimpurity step in technological process, make product foreign matter content high, and easily ftracture, affect the quality of product.
Summary of the invention
Goal of the invention: the object of the invention is to for the deficiencies in the prior art, a kind of preparation method of zircite product, comprises the following steps:
1) taking zirconium white, magnesium basic carbonate, iridium oxide and strontium oxide as raw material mix grinding obtains fine powder, add glue, in mould, be pressed into adobe;
2) adobe is put into cellar for storing things kiln roasting and obtain just base, then first base is carried out to fragmentation and obtain particle, particle is carried out to deironing and ball milling obtains powder;
3) by step 2) in 40 ~ 50 parts, powder, step 2) in 50 ~ 60 parts of particles, add 10 ~ 20 parts of electric smelting calcia-stabilised zirconias, PDA glue is 3 ~ 4 parts, by above-mentioned mass fraction proportioning carry out mixing, sieve, tie tremble, the dry mixture that obtains;
4) mixture compression moulding in mould, dry, dress cellar for storing things, high temperature are burnt till, go out to store, check, are packaged to be finished product zircite product.
The mass fraction of described step 1) Raw is as follows: 87 ~ 90 parts of zirconium whites, magnesium basic carbonate 8 ~ 10,1 ~ 2 part of iridium oxide: strontium oxide 0.5-1 part: glue is 2.2-2.8 part.
Fine powder ratio of grinding media to material 2:1 in described step 1), fineness is 95% by 325 orders.
In order to ensure that zirconium white has certain stability and produces 6-8% volumetric shrinkage, described step 2) in firing temperature be 1280-1320 DEG C, in order to remove impurity iron wherein, deironing is by electromagnetic deironing machine deironing 3-5 time.
Described step 2) in grain diameter be 0.2-0.7mm.
In order to ensure compact density, blank strength, product burns till to shrink and is controlled at 3-8%, by adjusting the add-on capable of regulating contractibility of powder and electric smelting calcia-stabilised zirconia, the batching massfraction in described step 3) is the PDA glue of 10%-20% electric smelting calcia-stabilised zirconia and 3%-4%.
For the mixture making mixes, and prevent conglomeration, reduce pug moisture, increase the intensity of moulding, spice 35-45 minute in described step 3), the sieve aperture sieving is 8 orders, and bundle is trembled more than 8 hours, and in open container, 80 DEG C are dried 12 hours.
In described step 4), be dried and realize as follows: temperature rise rate is 10-15 DEG C/h, is incubated 5-6 hour 130-140 DEG C time, and rate of weight loss is 1.8%-2.4%.
In order to improve kiln temperature homogeneity (upper and lower ± 20 DEG C), to prevent from burning till cracking, high temperature in described step 4) burns till as follows to be realized: temperature rise rate 40-50 DEG C/h, and 1650-1680 DEG C is burnt till, and is incubated 8 hours, firing time 60-70 hour, cooling 80-90 hour.
Prevent the too fast cracking of speed of cooling, the temperature that goes out Jiao Men in described step 4) is 600 DEG C, and the temperature that is used for filling the cellar for storing things car pull-out of zirconium product is 200 DEG C
The density of the finished product zircite product obtaining in described step 4) is 4.85-5.0g/cm
3, normal temperature is withstand voltage at 200-350Mpa.
Beneficial effect: even compared with existing, the present invention has the following advantages: in preparation method of the present invention by adding magnesium oxide as stablizer, add iridium oxide and strontium oxide and can further strengthen zirconic stability, greatly improve the scour resistance of product, the intensity of base substrate, effectively improve conforming product rate, the electric smelting calcia-stabilised zirconia and the PDA glue that add have ensured compact density, product shrinks and is controlled at 6-8%, by adjusting the add-on capable of regulating contractibility of powder and electric smelting calcia-stabilised zirconia, and utilize electromagnetic deironing machine to remove impurity iron wherein, this process is simple but also easy handling not only, effectively reduce and burn till cracking, ensure the quality of product.
Embodiment
Embodiment 1:
A preparation method for zircite product, comprises the following steps:
1) by mass fraction be 87 parts of zirconium whites, 10 parts of magnesium basic carbonates, 2 parts of iridium oxides, 1 part of strontium oxide is for raw material mix grinding obtains ratio of grinding media to material 2:1, and fineness is 95% by 325 object fine powders, adds 2.2 parts, 108 glue, is pressed into adobe in mould;
2) adobe is put into 1280 DEG C, cellar for storing things stove and be fired into just base, then first base is carried out to fragmentation and obtain 0.2mm-0.7mm particle and the following particle of 0.2mm, all particles are carried out to 3 times deironing of electromagnetic deironing machine deironing, fine particle ball milling obtains powder;
3) be step 2 by mass fraction) in add in 50 parts of 40 parts, powder and particles 17 parts of electric smelting calcia-stabilised zirconias and 3 parts, PDA glue mix, spice 35 minutes, the sieve aperture sieving is 8 orders, and bundle is trembled more than 8 hours, 80 DEG C of dry mixtures that obtain for 12 hours in open container;
4) by mixture compression moulding in mould, dry, dress cellar for storing things, go out cellar for storing things, inspection, be packaged to be finished product zirconium white steel teeming ladle slide plate and inlay zirconium plate, wherein dry step is as follows: temperature rise rate is 10 DEG C/h, 130 DEG C time, be incubated 5 hours, rate of weight loss is 1.8%, high temperature burns till as follows and realizes: 40 DEG C/h of temperature rise rates, 1650 DEG C are burnt till, be incubated 8 hours, firing time 60 hours, cooling 80 hours, the temperature that goes out Jiao Men is 600 DEG C, the temperature of the cellar for storing things car pull-out of dress zirconium product is 200 DEG C, the density that the zirconium white steel teeming ladle slide plate obtaining is inlayed zirconium plate is 4.85g/cm
3, normal temperature is withstand voltage at 200Mpa.
Embodiment 2:
A preparation method for zircite product, comprises the following steps:
1) by mass fraction be 90 parts of zirconium whites, 8 parts of magnesium basic carbonates, 1 part of iridium oxide, 0.5 part of strontium oxide is for raw material mix grinding obtains ratio of grinding media to material 2:1, and fineness is 95% by 325 object fine powders, adds 2.8 parts, 108 glue, is pressed into adobe in mould;
2) adobe is put into 1320 DEG C, cellar for storing things stove and be fired into just base, then first base is carried out to fragmentation and obtain 0.2mm-0.7mm particle and the following particle of 0.2mm, all particles are carried out to 5 times deironing of electromagnetic deironing machine deironing, fine particle ball milling obtains powder;
3) be step 2 by mass fraction) in 45 parts, powder and 60 parts of particles, add 4 parts, 10 parts of electric smelting calcia-stabilised zirconias and PDA glue to mix, spice 35-45 minute, the sieve aperture sieving is 8 orders, bundle is trembled more than 8 hours, 80 DEG C of dry mixtures that obtain for 12 hours in open container;
4) by mixture compression moulding in mould, dry, dress cellar for storing things, go out to store, check, be packaged to be zircite product, wherein dry step is as follows: temperature rise rate is 15 DEG C/h, 140 DEG C time, be incubated 6 hours, rate of weight loss is 2.4%, high temperature burns till as follows and realizes: 50 DEG C/h of temperature rise rates, 1680 DEG C are burnt till, be incubated 8 hours, firing time 70 hours, cooling 90 hours, the temperature that goes out Jiao Men is 600 DEG C, and the temperature of the cellar for storing things car pull-out of dress zirconium product is 200 DEG C, and the density of the zircite product obtaining is 5.0g/cm
3, normal temperature is withstand voltage at 350Mpa.
Embodiment 3:
A preparation method for zircite product, comprises the following steps:
1) be 88 parts taking mass fraction as zirconium white, magnesium basic carbonate is 10 parts, and iridium oxide is 1.5 parts, strontium oxide is 0.5 part and obtains ratio of grinding media to material 2:1 for raw material mix grinding, fineness is 95% by 325 object fine powders, adds 2.6 parts, 108 glue, is pressed into adobe in mould;
2) adobe is put into 1300 DEG C, cellar for storing things stove and be fired into just base, then first base is carried out to fragmentation and obtain 0.2mm-0.7mm particle and the following particle of 0.2mm, all particles are carried out to 4 times deironing of electromagnetic deironing machine deironing, fine particle ball milling obtains powder;
3) be step 2 by mass fraction) in 50 parts, powder and 55 parts of particles, add 3 parts, 15 parts of electric smelting calcia-stabilised zirconias and PDA glue to mix, spice 40 minutes, the sieve aperture sieving is 8 orders, bundle is trembled more than 8 hours, 80 DEG C of dry mixtures that obtain for 12 hours in open container;
4) by mixture compression moulding in mould, dry, dress cellar for storing things, go out to store, check, be packaged to be zircite product, wherein dry step is as follows: temperature rise rate is 12 DEG C/h, 135 DEG C time, be incubated 5 hours, rate of weight loss is 2 %, high temperature burns till as follows and realizes: 45 DEG C/h of temperature rise rates, 1660 DEG C are burnt till, be incubated 8 hours, firing time 65 hours, cooling 85 hours, the temperature that goes out Jiao Men is 600 DEG C, and the temperature of the cellar for storing things car pull-out of dress zirconium product is 200 DEG C, and the density that the zirconium white steel teeming ladle slide plate obtaining is inlayed zirconium plate is 4.9g/cm
3, normal temperature is withstand voltage at 300Mpa.
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (8)
1. a preparation method for zircite product, is characterized in that comprising the following steps:
1) taking zirconium white, magnesium basic carbonate, iridium oxide and strontium oxide as raw material mix grinding obtains fine powder, add glue, in mould, be pressed into adobe; The mass fraction of described raw material is as follows: 87 ~ 90 parts of zirconium whites, and 8 ~ 10 parts of magnesium basic carbonates, 1 ~ 2 part of iridium oxide, strontium oxide 0.5-1 part, glue is 2.2-2.8 part;
2) adobe is put into cellar for storing things kiln roasting and obtain just base, then first base is carried out to fragmentation and obtain 0.2mm-0.7mm particle and the following particle of 0.2mm, all particles are carried out to deironing, fine particle ball milling obtains powder;
3) by step 2) in 40 ~ 50 parts, powder, step 2) in 50 ~ 60 parts of particles, add 10 ~ 20 parts of electric smelting calcia-stabilised zirconias, PDA glue is 3 ~ 4 parts, by above-mentioned mass fraction proportioning carry out mixing, sieve, tie tremble, the dry mixture that obtains;
4) mixture compression moulding in mould, dry, dress cellar for storing things, high temperature are burnt till, go out to store, check, are packaged to be finished product zircite product.
2. the preparation method of a kind of zircite product according to claim 1, is characterized in that: the ratio of grinding media to material 2:1 of ball milling in described step 1), fineness is 95% by 325 orders.
3. the preparation method of a kind of zircite product according to claim 1, is characterized in that: described step 2) in firing temperature be 1280-1320 DEG C, deironing is by electromagnetic deironing machine deironing 3-5 time.
4. the preparation method of a kind of zircite product according to claim 1, is characterized in that: spice 35-45 minute in described step 3), and the sieve aperture sieving is 8 orders, and bundle is trembled more than 8 hours, and in open container, 80 DEG C are dried 12 hours.
5. the preparation method of a kind of zircite product according to claim 1, it is characterized in that: in described step 4), be dried and realize as follows: temperature rise rate is 10-15 DEG C/h, 130-140 DEG C time, be incubated 5-6 hour, rate of weight loss is 1.8%-2.4%.
6. the preparation method of a kind of zircite product according to claim 1, it is characterized in that: the high temperature in described step 4) burns till as follows to be realized: temperature rise rate 40-50 DEG C/h, 1650-1680 DEG C is burnt till, be incubated 8 hours, firing time 60-70 hour, cooling 80-90 hour.
7. the preparation method of a kind of zircite product according to claim 1, is characterized in that: the temperature that goes out Jiao Men in described step 4) is 600 DEG C, and the temperature of the cellar for storing things car pull-out of dress zircite product is 200 DEG C.
8. the preparation method of a kind of zircite product according to claim 1, is characterized in that: the density of the finished product zircite product obtaining in described step 4) is 4.85-5.0g/cm
3, normal temperature is withstand voltage is 200-350MPa.
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| CN105601275A (en) * | 2016-01-13 | 2016-05-25 | 太仓宏达俊盟新材料有限公司 | Manufacture process of immersive elongated-nozzle zirconia flow control |
| CN106396675A (en) * | 2016-08-31 | 2017-02-15 | 太仓宏达俊盟新材料有限公司 | Preparation method and application of low energy consumption partially-stable zirconia |
| CN112142478B (en) * | 2019-06-28 | 2022-06-10 | 比亚迪股份有限公司 | Zirconia ceramic powder, zirconia ceramic, preparation method of zirconia ceramic and electronic equipment shell |
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| WO2001041660A1 (en) * | 1999-12-07 | 2001-06-14 | Vorobiev, Alexandr Sergeevich | Zirconium dioxide based material, surgical cutting tools made of zirconium dioxide based material, tools made of zirconium dioxide based material |
| CN101108775B (en) * | 2007-08-27 | 2010-10-13 | 中钢集团洛阳耐火材料研究院有限公司 | Method for manufacturing zirconium oxide product |
| JP5270913B2 (en) * | 2007-12-26 | 2013-08-21 | サンゴバン・ティーエム株式会社 | High electrical resistance high zirconia cast refractory |
| CN101503304B (en) * | 2009-03-26 | 2012-02-15 | 中钢集团洛阳耐火材料研究院有限公司 | Low temperature method for manufacturing high thermal shock superhigh temperature zircite product |
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Denomination of invention: Preparation method of zirconium oxide product Effective date of registration: 20171220 Granted publication date: 20140806 Pledgee: Bank of Jiangsu Limited by Share Ltd Taicang branch Pledgor: Taicang Hongda Junmeng New Material Co., Ltd. Registration number: 2017320010091 |