CN102260078B - Zirconia ceramic and preparation method thereof - Google Patents
Zirconia ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention, belonging to the technical field of zirconia ceramic, discloses a zirconia ceramic and a preparation method thereof. The ceramic comprises matrix, sintering aid, neodymium oxide and additive, wherein, the matrix is yttria stabilized zirconia, the additive is selected from one or more of zinc oxide, barium carbonate and calcium fluoride, and the diffraction peak of the XRD appears when the 2 theta is 34.8-36.2 degrees. The zirconia ceramic has stable and beautiful purple. The preparation method comprises the following steps: adding neodymium oxide particles in a diethanolamine solution for soaking, then carrying out solid-liquid separation; carrying out ball mill mixing of the matrix, processed neodymium oxide particles, sintering aid and additive, then carrying out die forming and high temperature sintering. The preparation method provided by the present invention is simple and easy, and is suitable for large-scale industrial production.
Description
Technical field
The invention belongs to the zirconia ceramics technical field, relate in particular to a kind of colored zirconia ceramics and preparation method thereof.
Background technology
Zirconia ceramics has the characteristics such as intensity height, hardness height, good toughness, anticorrosive, high temperature resistant, good moldability, is widely used in every field, such as cutter, mould, valve, refractory materials, oxygen sensor, solid fuel cell etc.
In recent years, along with people to the improving constantly of ornament demand, colored zirconia ceramics becomes the new lover of high-grade finishing material, such as mobile phone, watch chain, bangle etc. with its excellent mechanicalness, bright colour, metalluster and without the characteristics of allergy effect.But at present zirconia ceramics is common only has two kinds of colors of black and white.
There is document to point out also to have obtained blue, yellow zirconium oxide ceramic.So the zirconia ceramics of the more colors of exploitation has wide market outlook, particularly the purple zirconia ceramics.
Traditional purple also is not suitable for zirconia ceramics, such as: manganese oxide, chromic oxide, Praseodymium trioxide etc. are raw material, synthetic praseodymium manganese chrome violet ceramic pigment color.But this violet pigment adds in the zirconia ceramics, can not make zirconia ceramics show purple.
Summary of the invention
Technical problem to be solved by this invention is not show the ceramic oxide of purple in the prior art, thereby a kind of purple zirconia ceramics and preparation method thereof is provided.
A kind of purple zirconia ceramics, it comprises body material, sintering aid, Neodymium trioxide, additive; Described body material is yttria stabilized zirconia; Described additive is selected from zinc oxide, barium carbonate and the Calcium Fluoride (Fluorspan) one or more; In using the Alpha-ray X-ray diffraction of Cu-K, be 34.8～36.2 ° at 2 θ and the maximum diffraction peak occurs.
Second purpose of the present invention provided a kind of preparation method of above-mentioned zirconia ceramics.
A kind of preparation method of zirconia ceramics, it comprises the steps:
(1) Neodymium trioxide pre-treatment: the Neodymium trioxide particle joined in the diethanolamine solution soak, then solid-liquid separation;
(2) molding sintering: base material, sintering aid, additive, the pretreated Neodymium trioxide particle of step (1) ball milling are mixed, rear die forming, high temperature sintering forms again.
Zirconia ceramics provided by the present invention shows purple, and color stability, color and luster are pure beautiful.Its preparation method is simple, is applicable to industrial mass production.
Embodiment
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
A kind of purple zirconia ceramics, it comprises body material, sintering aid, Neodymium trioxide, additive; Described body material is yttria stabilized zirconia; Described additive is selected from zinc oxide, barium carbonate and the Calcium Fluoride (Fluorspan) one or more; In using the Alpha-ray X-ray diffraction of Cu-K, be 34.8～36.2 ° at 2 θ and diffraction peak occurs.
Wherein, yttria stabilized zirconia is known in those skilled in the art, and the present invention is preferably semi-stability type yttria stabilized zirconia.
Preferably, the molar fraction of the yttrium oxide in the yttria stabilized zirconia of the present invention is 3～5%.
The effect of sintering aid is the sintering temperature that reduces pottery among the present invention, improves the sintering effect of pottery.Sintering aid commonly used is the higher oxide compound of thermal conductivity.
The present invention is preferably selected from two or more in magnesium oxide, aluminum oxide, silicon oxide, calcium oxide and the cerium oxide.More than several oxide compound thermal conductivitys high, and join in the zirconia ceramics and can not exert an adverse impact to zirconia ceramics.
More preferably in the situation, take the gross weight of sintering aid as benchmark, each component and the content thereof of sintering aid are: magnesium oxide 5～50wt%, aluminum oxide 10～50wt%, silicon oxide 10～50wt%, calcium oxide 5～50wt%, cerium oxide 5～50wt%.
Preferably, the median size of Neodymium trioxide is 0.1～20 μ m among the present invention, more preferably 1～10 μ m.
Additive among the present invention is the colour stability that strengthens zirconia ceramics, and the brightness of color.
The median size of additive is preferably 1～20 μ m.
Preferably, take the gross weight of pottery as benchmark, the content of body material is 80～95wt%, and the content of sintering aid is 0.1～5wt%, and the content of Neodymium trioxide is 3～10wt%, and the content of additive is 1～5wt%.
More preferably, the content of body material is 87～90wt%, and the content of sintering aid is 1～4wt%, and the content of Neodymium trioxide is 6～10wt%, and the content of additive is 1.5～3wt%.
The preparation method of purple zirconia ceramics of the present invention, it comprises the steps:
(1) Neodymium trioxide pre-treatment: the Neodymium trioxide particle joined in the diethanolamine solution soak, then solid-liquid separation;
(2) molding sintering: base material, sintering aid, additive, the pretreated Neodymium trioxide particle of step (1) ball milling are mixed, rear die forming, high temperature sintering forms again.
The median size of Neodymium trioxide particle of the present invention is preferably 0.1～20 μ m, more preferably 1～10 μ m.
Wherein, the present invention can get final product the Neodymium trioxide submergence fully to the not too many restriction of the consumption of diethanolamine solution.The consumption of the diethanolamine solution of the preferred every gram Neodymium trioxide of the present invention is 10～40mL.
Preferably, the concentration of diethanolamine solution is 1.5～4mol/L.
Under the preferable case, immersion is to carry out under whipped state.More preferably under 100～250rad/min, soak 0.5～2h.
Then solid-liquid separation is about to the Neodymium trioxide particle and separates from solution.Can adopt the solid-liquid separating method commonly used such as filtration, suction filtration, centrifugation.
Again with isolated Neodymium trioxide particle drying.
Step (2) is mixed the Neodymium trioxide particle ball milling after substrate material, sintering aid, additive, step (1) processing.
The present invention preferably mixes the Neodymium trioxide particle first with the additive ball milling, then add the body material ball milling and mix, and adds at last the sintering aid ball milling and mixes.
Wherein, die forming is known in those skilled in the art, does not do at this and gives unnecessary details.
High temperature sintering also is known in those skilled in the art, and the present invention is preferably at 1400～1650 ℃ of lower sintering 1～10h, more preferably 1450～1600 ℃ of lower sintering 3～8h.
The present invention is sintering under inert atmosphere preferably, because under oxidizing atmosphere, has a small amount of trivalent neodymium ion during sintering and is oxidized to high price, thereby cause purple more shallow.And under inert atmosphere, the colour developing efficient of neodymium ion is high, and ceramic color is darker.Inert atmosphere of the present invention refers to atmosphere or its mixed atmospheres such as 0 family's gas atmosphere or nitrogen.
As everyone knows, the colorant of chromatic ceramics will evenly be formed in the stupalith through high temperature sintering.And the relative general ceramic material of the sintering temperature of zirconia ceramics will exceed a lot, generally is higher than 1400 ℃.Under high temperature so, general ceramic pigment or tinting material can occur to decompose or volatilization, and be difficult to reach color developing effect, thereby be difficult to make the bright-coloured colored zirconia ceramics of colour generation, let alone the purple zirconium white.
The present inventor is unexpected to be found, the Neodymium trioxide particle is immersed in the diethanolamine solution, then prepares together with matrix, sintering aid and additive, and the zirconia ceramics of preparing shows stable purple.The reason that the present invention infers is, the Neodymium trioxide particle is under the immersion of diethanolamine, and the outstanding key of Neodymium trioxide particle surface has been eliminated in the surface reaction of diethanolamine and Neodymium trioxide particle, has reduced the surface energy of Neodymium trioxide, and the activity of neodymium ion is improved.When sintering, fusing assistant melts first, in liquid environment, promotes neodymium to replace zirconium, forms stable crystalline network.2 θ are 34.8～36.2 ° and diffraction peak occurs in its XRD figure, are exactly that zirconium and neodymium are in conjunction with the diffraction peak that produces; Thereby make zirconia ceramics manifest stable purple.The trivalent neodymium ion is more at the absorption peak of visible light part, and color is complicated.Zirconium and neodymium combination make the spectrum of trivalent neodymium ion produce skew, present stable purple.
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1
Matrix: 88g semi-stability type yttria stabilized zirconia, wherein the molar fraction of yttrium oxide is 3%.
Sintering aid: 0.6g magnesium oxide, 0.8g silicon oxide, 0.6g aluminum oxide
Neodymium trioxide: the 8g median size is the Neodymium trioxide of 5 μ m
Additive: 0.4g zinc oxide, 0.8g barium carbonate, 0.8g Calcium Fluoride (Fluorspan)
(1) pre-treatment: first the Neodymium trioxide particle is joined in the diethanolamine solution of 240ml 3mol/L, under the 200rad/min rotating speed, stir 1h.Then the Neodymium trioxide particle is filtered out from diethanolamine solution, at 100 ℃ of dry 0.5h.
(2) molding sintering: Neodymium trioxide and additive that matrix, sintering aid, step (1) are obtained join in the 200mL dehydrated alcohol, then ball milling mixing 6h.Taking-up is placed in 100 ℃ the baking oven and dries 6h.With porcelain mortar the powder that obtains is pulverized rear mistake 200 mesh sieves.Powder after will sieving with four post press-down type oil presses is with 25kN/cm
2Pressure compacting 1min, be pressed into 5*2*1 centimetre base substrate.With the compacting after base substrate in cabinet-type electric furnace (Shandong is the KS S-17XB of method testing furnace factory forever, 1700 ℃) with 1500 ℃ of sintering 5h, namely make the purple zirconia ceramics, be denoted as Al.
Embodiment 2
Matrix: 94g semi-stability type yttria stabilized zirconia, wherein the molar fraction of yttrium oxide is 3.5%.
Sintering aid: 0.5g magnesium oxide, 0.5g calcium oxide
Neodymium trioxide: the 3g median size is the Neodymium trioxide of 1 μ m
Additive: 0.4g zinc oxide, 0.8g barium carbonate, 0.8g Calcium Fluoride (Fluorspan)
(1) pre-treatment: first the Neodymium trioxide particle is joined in the diethanolamine solution of 90ml 3mol/L, under the 200rad/min rotating speed, stir 1h.Then the Neodymium trioxide particle is filtered out from diethanolamine solution, at 100 ℃ of dry 0.5h.
(2) molding sintering: Neodymium trioxide and additive that matrix, sintering aid, step (1) are obtained add in the 200mL dehydrated alcohol, then ball milling mixing 6h.Taking-up is placed in 100 ℃ the baking oven and dries 6h.With porcelain mortar the powder that obtains is pulverized rear mistake 200 mesh sieves.Powder after will sieving with four post press-down type oil presses is with 25kN/cm
2Pressure compacting 1min be pressed into 5*2*1 centimetre base substrate.With the compacting after base substrate in cabinet-type electric furnace (Shandong is the KS S-17XB of method testing furnace factory forever) with 1450 ℃ of sintering 5h, can make the purple zirconia ceramics, be denoted as A2.
Embodiment 3
Matrix: 83g semi-stability type yttria stabilized zirconia, wherein the molar fraction of yttrium oxide is 3%.
Sintering aid: 1g magnesium oxide, 1g aluminum oxide, 2g silicon oxide, 1g cerium oxide
Neodymium trioxide: the 10g median size is the Neodymium trioxide of 20 μ m
Additive: 0.4g zinc oxide, 0.8g barium carbonate, 0.8g Calcium Fluoride (Fluorspan)
(1) pre-treatment: first the Neodymium trioxide particle is joined in the diethanolamine solution of 300ml 3mol/L, under the 200rad/min rotating speed, stir 1h.Then the Neodymium trioxide particle is filtered out from diethanolamine solution, at 100 ℃ of dry 0.5h.
(2) molding sintering: Neodymium trioxide and additive that matrix, sintering aid, step (1) are obtained add in the 200mL dehydrated alcohol, then ball milling mixing 6h.Taking-up is placed in 100 ℃ the baking oven and dries 6h.With porcelain mortar the powder that obtains is pulverized rear mistake 200 mesh sieves.Powder after will sieving with four post press-down type oil presses is with 25kN/cm
2Pressure compacting 1min be pressed into 5*2*1 centimetre base substrate.With the compacting after base substrate in cabinet-type electric furnace (Shandong is the KS S-17XB of method testing furnace factory forever) with 1600 ℃ of sintering 5h, can make the purple zirconia ceramics, be denoted as A3.
Embodiment 4
Matrix: 88g semi-stability type yttria stabilized zirconia, wherein the molar fraction of yttrium oxide is 5%.
Sintering aid: 0.6g magnesium oxide, 0.8g silicon oxide, 0.6g aluminum oxide
Neodymium trioxide: the 8g median size is the Neodymium trioxide of 5 μ m
Additive: 0.4g zinc oxide, 0.8g barium carbonate, 0.8g Calcium Fluoride (Fluorspan)
(1) pre-treatment: first the Neodymium trioxide particle is joined in the diethanolamine solution of 240ml 1.5mol/L, under the 250rad/min rotating speed, stir 2h.Then the Neodymium trioxide particle is filtered out from diethanolamine solution, at 100 ℃ of dry 0.5h.
(2) molding sintering: Neodymium trioxide and additive that matrix, sintering aid, step (1) are obtained add in the 200mL dehydrated alcohol, then ball milling mixing 6h.Taking-up is placed in 100 ℃ the baking oven and dries 6h.With porcelain mortar the powder that obtains is pulverized rear mistake 200 mesh sieves.Powder after will sieving with four post press-down type oil presses is with 25kN/cm
2Pressure compacting 1min be pressed into 5*2*1 centimetre base substrate.With the compacting after base substrate in cabinet-type electric furnace (Shandong is the KS S-17XB of method testing furnace factory forever) with 1500 ℃ of sintering 5h, can make the purple zirconia ceramics, be denoted as A4.
Embodiment 5
Matrix: 85g semi-stability type yttria stabilized zirconia, wherein the molar fraction of yttrium oxide is 5%.
Sintering aid: 0.6g magnesium oxide, 0.8g silicon oxide, 0.6g aluminum oxide
Neodymium trioxide: the 8g median size is the Neodymium trioxide of 5 μ m
Additive: 1.5g zinc oxide, 1.5g barium carbonate, 2g Calcium Fluoride (Fluorspan)
(1) pre-treatment: first the Neodymium trioxide particle is joined in the diethanolamine solution of 240ml 1.5mol/L, under the 250rad/min rotating speed, stir 2h.Then the Neodymium trioxide particle is filtered out from diethanolamine solution, at 100 ℃ of dry 0.5h.
(2) molding sintering: Neodymium trioxide and additive that matrix, sintering aid, step (1) are obtained add in the 200mL dehydrated alcohol, then ball milling mixing 6h.Taking-up is placed in 100 ℃ the baking oven and dries 6h.With porcelain mortar the powder that obtains is pulverized rear mistake 200 mesh sieves.Powder after will sieving with four post press-down type oil presses is with 25kN/cm
2Pressure compacting 1min be pressed into 5*2*1 centimetre base substrate.With the compacting after base substrate in cabinet-type electric furnace (Shandong is the KS S-17XB of method testing furnace factory forever) with 1500 ℃ of sintering 5h, can make zirconia ceramics of the present invention, be denoted as A5.
Comparative Examples 1
At present, manganese oxide, chromic oxide, Praseodymium trioxide etc. are raw material, adopt even coprecipitation method at 1100 ℃ of lower insulation 2h, have synthesized praseodymium manganese chrome violet ceramic pigment color.
Replace Neodymium trioxide with praseodymium manganese chrome violet ceramic pigment color, other are denoted as AC1 with embodiment 1 preparation zirconia ceramics.
Performance test
The XRD test: adopt the D/MAX2200PC type XRD tester of Rigaku company, test voltage is 40KV; Test current is 20mA.
Zirconia ceramics sample A1-A5 and AC1 that above-described embodiment and Comparative Examples are made put into polishing machine (letter electronic system equipment company limited of Hunan section, the accurate single side polishing machine of PW-1000CE-JY) in, import first 5 microns green silicon carbides of meso-position radius (gold east, Nantong City silicon carbide factory, W5) powder corase grind, use again 1.5 microns green silicon carbides of meso-position radius (gold east, Nantong City silicon carbide factory, W1.5) powder fine grinding, use at last meso-position radius 0.5 micron diamond (Changshu diamond powder factory, W0.5) powder polishing, wash the test sample after obtaining polishing.
The color measurement of pottery
Adopt spectrophotometer O030007 (Shanghai precision instrumentation company limited, model 723A) and vancometer O070002 (Beijing Tai Yasai Foucault skill Development Co., Ltd, the MN type) the zirconia ceramics sample A 1-A5 after the polishing and glossiness and the colourity of AC1 are detected, the result is as shown in table 1.
The performance test of pottery
Adopt Rockwell Hardness meter (sclerometer subsidiary factory of Shanghai Yanrun Ray Machine Technology Co., Ltd., MC010-HR-150A) and universal testing machine (the favourable electric furnace in sky, Tianjin company limited, high low temperature universal testing machine WSM-20KB) detects the zirconia ceramics sample A1-A5 after the polishing and hardness and the bending strength of AC1; Adopting linear wear resistant instrument (U.S. Taber5750) test condition is 1 inch of loading 600g, stroke, the rub resistance of test zirconia ceramics sample A1-A5 and AC1, and the result is as shown in table 1.
Table 1
As can be seen from Table 1, adopt ceramics sample A1-A5 that the method among the present invention makes on performance all than the height of Comparative Examples sample AC1.In the test result of colourity, the R value represents red, and the G value represents green, and the B value represents blue, can find out that by Data Comparison A1-A5 is in the purple scope, and AC1 does not demonstrate purple fully, but presents white.Embodiment compares ratio simultaneously, and its wear resistance has had significantly raising.
The above only is preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. zirconia ceramics, it comprises matrix, sintering aid, Neodymium trioxide, additive; Described matrix is yttria stabilized zirconia; Described additive is selected from zinc oxide, barium carbonate and the Calcium Fluoride (Fluorspan) one or more; In using the Alpha-ray X-ray diffraction of Cu-K, be 34.8～36.2 ° at 2 θ and diffraction peak occurs,
Wherein, the molar fraction of yttrium oxide is 3%～5% in the described matrix,
Take the gross weight of pottery as benchmark, the content of described body material is 80～95wt%, and the content of described sintering aid is 0.1～5wt%, and the content of described Neodymium trioxide is 3～10wt%, and the content of described additive is 1～5wt%.
2. zirconia ceramics according to claim 1, it is characterized in that: described sintering aid is two or more in magnesium oxide, aluminum oxide, silicon oxide, calcium oxide and the cerium oxide.
3. zirconia ceramics according to claim 1, it is characterized in that: take the gross weight of pottery as benchmark, the content of described body material is 87～90wt%, the content of described sintering aid is 1～4wt%, the content of described Neodymium trioxide is 6～10wt%, and the content of described additive is 1.5～3wt%.
4. the preparation method of a zirconia ceramics claimed in claim 1, it comprises the steps:
(1) Neodymium trioxide pre-treatment: the Neodymium trioxide particle joined in the diethanolamine solution soak, then solid-liquid separation;
(2) molding sintering: Neodymium trioxide particle, sintering aid, additive ball milling after base material, step (1) processing are mixed, rear die forming, high temperature sintering forms again.
5. the preparation method of zirconia ceramics according to claim 4, it is characterized in that: the median size of described Neodymium trioxide particle is 0.1～20 μ m; The median size of described additive is 1～20 μ m.
6. the preparation method of zirconia ceramics according to claim 4, it is characterized in that: the concentration of described diethanolamine solution is 1.5～4mol/L.
7. the preparation method of zirconia ceramics according to claim 5, it is characterized in that: the time of described immersion is 1～5h.
8. the preparation method of zirconia ceramics according to claim 5, it is characterized in that: the temperature of described high temperature sintering is 1400～1650 ℃, the time is 1～10h.
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| CN102260078A (en) | 2011-11-30 |
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