CN1162580A - Wear resistant sintered zirconium boule composite and manufacture thereof - Google Patents
Wear resistant sintered zirconium boule composite and manufacture thereof Download PDFInfo
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Abstract
A sintered antiwear zirconium-corundum compound material is prepared from Al2O3, ZrSiO4 and additive through proportioning Al2O3 and ZrSiO4 excessively and high-temp in-situ reaction, in which ZrO4 as resultant of decomposing ZrSiO4 is used to toughen the reaction resultant-principal crystalline phase corundum. The material and its preparing process feature that resultant ZrO4 and mullite have high strength and density at ordinary temp, the preparing process has simple technology and low sinter temp (1580 deg.C), and the product has low cost and high antiwear nature.
Description
The invention relates to wear-resistant sintered Al2O3、ZrSiO4Zirconium corundum composite material and its production method, it uses Al2O3、ZrSiO4Is prepared from Al as main raw material, and additive2O3Over-proportioning with ZrSiO4 and high-tempin-situ reaction4Decomposition product ZrO4Toughening the reaction product-main crystal phase corundum to obtain the high wear-resistant zirconia-corundum composite material.
The grinding body is the main material for grinding ceramic slip. At present, the reserves of high-quality natural spherulites are gradually reduced and the exploitation is to be exhausted. The quality of ordinary natural pebbles has clearly failed to meet the demands of increasingly developed ceramic production. The price and quality of artificial marble have become the focus of attention. The high-alumina porcelain ball directly influences popularization and use due to reasons of overhigh price, poor wear resistance and the like. The development of a high wear-resistant and low-cost abrasive body is one of the problems that ceramic technologists strive to find at present.
The invention aims to provide wear-resistant sintered Al2O3、ZrSiO4Zirconium corundum composite material and its production method, it uses Al2O3、ZrSiO4Is prepared from Al as main raw material, and additive2O3And ZrSiO4Over-proportioning and high-temp in-situ reaction, using ZrSiO4Decomposition product ZrO4Toughening the reaction product-main crystal phase corundum to obtain the high wear-resistant zirconia-corundum composite material.
The material and the production process thereof are characterized in that (1) the products of zirconia and mullite have high strength and high density at normal temperature; (2) the zirconium oxide generated is uniformly dispersed in the generated crystalline phase; (3) the sintering method is simple in process and low in product cost, compared with a high-aluminum wear-resistant material, the sintering temperature of the product is 1580 ℃, the sintering temperature is reduced by 70-100 ℃ compared with the temperature of 1650-1680 ℃ of a common 95% aluminum oxide wear-resistant material, but the wear resistance of the product exceeds about 25% of that of the 95% aluminum oxide material.
The wear-resistant sintered Al is2O3、ZrSiO4The formula range of the zirconia-corundum composite material is as follows (by weight):
the main ingredients are as follows: al (Al)2O365-95％ ZrSiO45-35％
Additive (addition): TiO 220-5％ CaO 0-7％ MgO 0-4％
Active SiO20-6％
The sum of the total amount of the additives is 1 to 6 percent
If desired, further auxiliaries may optionally be added: ZrO (ZrO)20-7％ Y2O30-4％
3 to 10 percent of the total amount of the auxiliary agent
The wear-resistant sintered Al is2O3、ZrSiO4The production method of the corundum-zirconia composite material comprises the following steps:
(1) raw material ratio
The formula range is as follows (by weight):
the main raw materials are as follows: al (Al)2O365-95％ ZrSiO45-35％
Raw materials of the additive (additional): TiO 220-5％ CaO 0-7％ MgO 0-4％
Active SiO20-6％
The sum of the total amount of the additives is 1 to 6 percent
If desired, further auxiliaries may optionally be added: ZrO (ZrO)20-7％ Y2O30-4％
3 to 10 percent of the total amount of the auxiliary agent
(2) Ultra-fine grinding
Carrying out wet or dry ultrafine grinding on the raw materials, wherein the grinding particle size is less than 5 mu m;
(3) spraying and granulating
Performing pressure spray granulation on the powder, wherein secondary granules are 40-80 meshes, and the water content is controlled to be 2-8%;
(4) semi-dry pressing or dry pressing
Semi-dry pressing or dry pressing the granulated powder, wherein the forming equipment is a press or an isostatic press, the forming pressure is more than 40MPa, and the forming density is more than 2.2g/cm3；
(5) Fettling and drying
Carrying out manual or automatic blank finishing repair on the molded blank, wherein the drying temperature is 40-80 ℃, and the drying moisture of the blank is controlled to be less than 1%;
(6) firing into
Putting the dried green body into a high-temperature pushed slab kiln or a high-temperature shuttle kiln, wherein the heating rate is 150-200 ℃/h, the firing temperature is 1550-1590 ℃, the highest temperature is kept for 2-4 hours, and the average cooling speed is less than 300 ℃/h;
(7) examination of
And (5) carrying out finished product inspection.
The main technical indexes of the product obtained by the invention are as follows:
the water absorption rate is less than 0.15 percent
Density>3.6g/cm3
Hardness (HRA)>80
Flexural strength>200MPa
The fracture toughness Kic is more than 8 MPa.m1/2
The color is white or beige
α-Al2O3Is Al2O3One of the stable crystals belongs to the trigonal system, and has a compact structure and a density of 3.96-4.01 g/cm3The Mohs hardness is 9, the fired product has high strength and high hardness, the defects are poor plastic deformation capability and low wear resistance, and ZrSiO is utilized4High temperature decomposition product ZrO2Toughening the aluminum oxide ceramic is one of the main ways to improve the aluminum oxide ceramic.
The reaction principle is as follows:
the method is characterized in that:
1) the zirconia and the mullite have high strength and high density at normal temperature.
2) The adopted sintering method has simple process and low product cost.
Based on the principle, the invention finds Al through a large number of experiments2O3And ZrSiO4The proper proportion between the components, thereby obtaining more ideal hardness and toughness,
based on the feasibility of the reaction, the method adopts the excess Al2O3On the one hand, excess of Al2O3The formation of a portion of the corundum crystalline phase ensures sufficient hardness of the product, while on the other hand an excess of Al2O3The influence of mullite puffing reaction on preventing density increase is also weakened.
The invention will now be further described with reference to specific embodiments, which are not intended to limit the invention in any way.
Example 1
1. Range of ingredients
The components: al (Al)2O380％ ZrSiO417％ TiO20.4％
CaO 0.3% active SiO20.3 MgO 2％
2. Ultra-fine grinding
The ingredients are put into a wet stirring mill for ultrafine grinding, and the grinding particle size is less than 3 mu m.
3. Spray granulation
And (4) carrying out spray granulation on the ultrafine grinding slurry, and sieving secondary particles with a 40-mesh sieve to obtain the ultrafine grinding slurry with the water content of 6%.
4. Press forming
Molding the ball with the diameter of 40mm on an isostatic press under the pressure of 150 MPa.
5. Fettling and drying
Removing burrs in the middle of the blank, polishing, wherein the drying temperature is 55-65 ℃, and the drying water is less than 1%.
6. Firing into
The grinding balls are put into a high-temperature shuttle kiln, the heating rate is 170 ℃/h, the cooling rate is 200 ℃/h, and the high-sintering temperature is 1580 ℃ multiplied by 2 h.
7. Examination of
And (5) carrying out product detection.
The main technical indexes of the product obtained by the invention are as follows:
the water absorption rate is less than 0.10 percent
Density>3.7g/cm3
Hardness (HRA)>83
Flexural strength>200MPa
The fracture toughness Kic is more than 9.5 MPa.m1/2
The color is white
The composition of its crystalline phase is corundum 62%, zircon 13% and mullite 25%.
The relative and bulk densities and abrasion resistance were 94, 3.60 and 0.154, respectively.
Wherein: 1. relative density ═ bulk density/theoretical density × 100% (the same applies below)
2. Abrasion resistance is the weight loss of the abrasive body/initial weight of the abrasive body × 100% (1 kg of force was applied to a polishing machine-grinder, grinding was carried out for 40 minutes, and the abrasive grains to which SiC of 100 mesh and 200g were added 4 times on average) (the same applies hereinafter).
Example 2
The same procedure as in example 1 above was followed, except that the following ingredients were used and the sintering was carried out at 1550 ℃ for 2 hours:
the components: al (Al)2O365％ ZrSiO435 percent of additive MgO 2.5 percent and TiO20.5％，CaO 0.2％
The main technical indexes of the product obtained by the invention are as follows:
the water absorption rate is less than 0.15 percent
Density>3.63g/cm3
Hardness (HRA)>80
Flexural strength>200MPa
The fracture toughness Kic is more than 8.5 MPa.m1/2
The color is beige
The composition of its crystal phase is corundum 34%, zircon 23% and mullite 43%.
The relative and bulk densities and abrasion resistance were 92, 3.39 and 0.205, respectively.
Example 3
The procedure was as in example 1, except that the following ingredients were used and the sintering was carried out at 1590 ℃ for 2.5 hours:
the components: al (Al)2O390％ ZrSiO4The total amount of the 10 percent of the additive is 2.5 percent
The main technical indexes of the product obtained by the invention are as follows:
the water absorption rate is less than 0.10 percent
Density>3.75g/cm3
Hardness (HRA)>85
Flexural strength>220MPa
The fracture toughness Kic is more than 8.0 MPa.m1/2
The color is white
The crystal phase composition of the corundum-mullite brick comprises 81 percent of corundum, 6.5 percent of zircon and 12.5 percent of mullite.
The results of the above 3 examples show that the relative density, the bulk density and the wear resistance are regularly changed along with the change of the crystal phase composition, and the wear resistance and the density are in an increasing trend.
This indicates that the composition of the corundum crystal phase in excess will reduce the adverse factor of mullite puffing, and the appropriate amount of ZrO2The volume fraction will serve asa toughening effect. Too high ZrO2The content will also lead to coalescence of microcracks, reducing the toughening effect. An excess of corundum crystal phase, i.e. too little ZrO2It will not have toughening effect.
Obtaining compact product pair Al by complete solid phase diffusion2O3And ZrSiO4Ceramic materials are difficult. If appropriate additives are added to form a glassy phase and other liquid phases, a dense product can be obtained and the sintering temperature can be reduced due to the rearrangement and viscous flow of the particles in the liquid phase.
One of the typical results of a certain Al/Zr comparative experiment (in this case 65% for alumina and 35% for zirconium silicate) is given in the following table:
external dosage property 01% 3% 6% abrasion resistance 0.1810.1330.1420.143 relative density 82888990
The typical data statistics show that the density and the wear resistance of the corundum zirconium material can be obviously improved by a proper amount of the additive, and meanwhile, the density of the corundum zirconium material cannot be highly compact by means of adding the additive only.
The method has the advantages of reducing the powder granularity, increasing the solid-phase reaction area, being an important measure for promoting sintering and reducing the sintering temperature of the current special ceramics, being economical and economical, changing the product performance, being beneficial to generating fine and uniform crystals, and improving the densification speed and the wear resistance. The zirconia corundum material is mainly subjected to solid-phase reaction, and the powder granularity and activity are particularly important. Experiments show that the ultrafine grinding is favorable for promoting the density of the corundum-zirconia material to beimproved, and the influence degree of the ultrafine grinding exceeds the use effect of the additive.
The following table shows the usage of the ultrafine grinding (in this case, 80% of alumina, 20% of zirconium silicate, and 3% of additive):
relative density of powder particle size%
88<5 μm
94<3 μm
96<2 μm
The zirconia-corundum material is mainly divided into two parts in the heat treatment process, and the densification process is carried out at 1370-1450 ℃. The mullite puffing reaction and sintering stage is at about 1550 ℃, the chemical reaction is the puffing reaction and sintering stage on one hand, the chemical reaction is the puffing process on the other hand, secondary air holes are easily generated, the end point sintering process on the other hand, the contradiction between the two results in that the end point sintering temperature is important, the reaction cannot be fully performed due to too low temperature, the primary air holes cannot be exhausted, the temperature is too high, crystals grow up, and the generation of the secondary air holes influences the densification degree of the mullite.
By combining the X-diffraction result and the electron microscope picture of the product, the invention can be seen that the zirconite is completely decomposed to generate the products of crystalline corundum, mullite and baddeleyite, the crystal structure takes round grains or cylindrical corundum as the main crystal phase, the baddeleyite and the mullite are embedded in the crystal structure in a pinning mode, and most of the baddeleyite and the mullite are in solid solution in a grain boundary. Baddeleyite is in the form of round particles or clusters with significant microcracks around the baddeleyite. Fracture analysis shows that ZrO2Has a pullout effect with mullite, i.e. belongs to intergranular fracture, and the fracture mode is effectiveThe strength and the wear resistance of the material are improved.
According to the general grinding ball abrasion test method provided by the national building institute, the abrasion test is carried out on the corundum zirconium grinding ball obtained by the method, and the abrasion rate is 3.4%. (provided by national building institute, the best 95 percent of alumina in China currently has the wear rate of 3-4 percent)
The test conditions are as follows: 1L alumina pot
20 balls with diameter of 20
400ml of water
Running time 24h
The rotational speed is 140 rpm
In addition, in the quick grinding process, the ball stones of different manufacturers are added, the comparison experiment is carried out, and the experimental results are shown in the following table
95 percent of alumina 2.12 percent of a building material yard
From Tangshan manufacturer, 95% of alumina 1.78%
The zirconia corundum grinding body of the invention is 1.42 percent
Obviously, the above embodiments are only examples of the present invention, and do not limit the scope of the present invention, including wear liners, nozzles, textile wire loops, etc., and the thermal shock properties specific to the products of the present invention, and the applications of spark plugs, etc., on heat engines, can be produced according to the process provided by the present invention, and the application prospects are very broad.
Claims (3)
1. Wear-resistant sintered Al2O3、ZrSiO4The formula range of the zirconia-corundum composite material is as follows (by weight):
the main ingredients are as follows: al (Al)2O365-95％ ZrSiO45-35％
Additive (addition): TiO 220-5％ CaO 0-7％ MgO 0-4％
Active SiO20-6％
The sum of the total amount of the additives is 1 to 6 percent
If desired, further auxiliaries may optionally be added: ZrO (ZrO)20-7％ Y2O30-4％
3 to 10 percent of the total amount of the auxiliary agent
2. The material of claim 1, useful as a wear liner, a nozzle, a textile wire loop, and for use in heat engines, spark plugs.
3. Wear-resistant sintered Al2O3、ZrSiO4The production method of the corundum-zirconia composite material comprises the following steps:
(1) raw material ratio
The formula range is as follows (by weight):
the main raw materials are as follows: al (Al)2O365-95％ ZrSiO45-35％
Raw materials of the additive (additional): TiO 220-5％ CaO 0-7％ MgO 0-4％
Active SiO20-6％
The sum of the total amount of the additives is 1 to 6 percent
If desired, further auxiliaries may optionally be added: ZrO (ZrO)20-7％ Y2O30-4％
3 to 10 percent of the total amount of the auxiliary agent
(2) Ultra-fine grinding
Carrying out wet or dry ultrafine grinding on the raw materials, wherein the grinding particle size is less than 5 mu m;
(3) spraying and granulating
Performing pressure spray granulation on the powder, wherein secondary granules are 40-80 meshes, and the water content is controlled to be 2-8%;
(4) semi-dry pressing or dry pressing
Granulating the powderSemi-dry pressing or dry pressing, the forming equipment is a press or isostatic pressingThe molding pressure is more than 40MPa, and the molding density is more than 2.2g/cm3；
(5) Fettling and drying
Carrying out manual or automatic blank finishing repair on the molded blank, wherein the drying temperature is 40-80 ℃, and the drying moisture of the blank is controlled to be less than 1%;
(6) firing into
Putting the dried green body into a high-temperature pushed slab kiln or a high-temperature shuttle kiln, wherein the heating rate is 150-200 ℃/h, the firing temperature is 1550-1590 ℃, the highest temperature is kept for 2-4 hours, and the average cooling speed is less than 300 ℃/h;
(7) examination of
And (5) carrying out finished product inspection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96114109A CN1061330C (en) | 1996-12-23 | 1996-12-23 | Wear resistant sintered zirconium boule composite and manufacture thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96114109A CN1061330C (en) | 1996-12-23 | 1996-12-23 | Wear resistant sintered zirconium boule composite and manufacture thereof |
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| Publication Number | Publication Date |
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| CN1162580A true CN1162580A (en) | 1997-10-22 |
| CN1061330C CN1061330C (en) | 2001-01-31 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN96114109A Expired - Fee Related CN1061330C (en) | 1996-12-23 | 1996-12-23 | Wear resistant sintered zirconium boule composite and manufacture thereof |
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Cited By (16)
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| CN1092163C (en) * | 2000-09-19 | 2002-10-09 | 中国科学院上海硅酸盐研究所 | Heterogeneous zirconia-mullite refractory material with sintered bound phase and its preparation |
| CN100387546C (en) * | 2003-05-09 | 2008-05-14 | 郑州大学 | Method for preparing alumine base electric fused zirconium corundum |
| CN101805197A (en) * | 2010-04-22 | 2010-08-18 | 上海海事大学 | Production method of corundum-mullite-zirconia |
| CN101906663A (en) * | 2010-08-09 | 2010-12-08 | 西峡县正弘单晶刚玉有限责任公司 | Blue ssuperindividual corundum and preparation method thereof |
| CN101952220A (en) * | 2008-02-18 | 2011-01-19 | 耐火材料知识产权有限两合公司 | Refractory slag band |
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| CN101691296B (en) * | 2009-09-24 | 2012-09-05 | 中山市华山特种陶瓷有限公司 | Zircon corundum ceramics |
| CN102701735A (en) * | 2012-06-08 | 2012-10-03 | 武汉工程大学 | Method for preparing stable zirconia/mullite ceramic material |
| WO2013011436A1 (en) * | 2011-07-20 | 2013-01-24 | Saint-Gobain Centre De Recherches Et D'etudes Europeen | Sintered zircon particle |
| FR2978143A1 (en) * | 2011-07-20 | 2013-01-25 | Saint Gobain Ct Recherches | Sintered particle in the form of ball, useful for treating surface of bottles, comprises composition of e.g. zirconium oxide and hafnium oxide, silicon oxide and aluminum oxide, and crystallized phases of e.g. zircon, mullite and corundum |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US3775164A (en) * | 1971-05-10 | 1973-11-27 | Sybron Corp | Method of controlling crystallization of glass |
| US4489022A (en) * | 1981-11-25 | 1984-12-18 | Glaverbel | Forming coherent refractory masses |
| CN1093072A (en) * | 1993-04-01 | 1994-10-05 | 山东省硅酸盐研究设计院 | Corundum ceramic material and method for making thereof and purposes |
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- 1996-12-23 CN CN96114109A patent/CN1061330C/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1092163C (en) * | 2000-09-19 | 2002-10-09 | 中国科学院上海硅酸盐研究所 | Heterogeneous zirconia-mullite refractory material with sintered bound phase and its preparation |
| CN100387546C (en) * | 2003-05-09 | 2008-05-14 | 郑州大学 | Method for preparing alumine base electric fused zirconium corundum |
| CN101952220A (en) * | 2008-02-18 | 2011-01-19 | 耐火材料知识产权有限两合公司 | Refractory slag band |
| CN101952220B (en) * | 2008-02-18 | 2013-01-30 | 耐火材料知识产权有限两合公司 | Refractory slag band |
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| CN101691296B (en) * | 2009-09-24 | 2012-09-05 | 中山市华山特种陶瓷有限公司 | Zircon corundum ceramics |
| CN101671179B (en) * | 2009-10-15 | 2012-05-02 | 湖南泰鑫瓷业有限公司 | High strength and high wear-resistance zirconium-aluminum-silicon composite self-release glazed ceramic material and manufacture method thereof |
| CN101805197A (en) * | 2010-04-22 | 2010-08-18 | 上海海事大学 | Production method of corundum-mullite-zirconia |
| CN101906663A (en) * | 2010-08-09 | 2010-12-08 | 西峡县正弘单晶刚玉有限责任公司 | Blue ssuperindividual corundum and preparation method thereof |
| FR2978143A1 (en) * | 2011-07-20 | 2013-01-25 | Saint Gobain Ct Recherches | Sintered particle in the form of ball, useful for treating surface of bottles, comprises composition of e.g. zirconium oxide and hafnium oxide, silicon oxide and aluminum oxide, and crystallized phases of e.g. zircon, mullite and corundum |
| WO2013011436A1 (en) * | 2011-07-20 | 2013-01-24 | Saint-Gobain Centre De Recherches Et D'etudes Europeen | Sintered zircon particle |
| CN102701735A (en) * | 2012-06-08 | 2012-10-03 | 武汉工程大学 | Method for preparing stable zirconia/mullite ceramic material |
| CN104478415A (en) * | 2014-12-23 | 2015-04-01 | 山东万乔集团有限公司 | Alumina-basedcomplex-phasewear-resisting plate and preparation method thereof |
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| CN104844168A (en) * | 2015-04-27 | 2015-08-19 | 安徽省含山县顺天纺织有限公司 | High wear resistant alumina ceramic eyelet containing yttrium oxide |
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| Publication number | Publication date |
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| CN1061330C (en) | 2001-01-31 |
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