CN105110793A - Preparation method of yttrium oxide ceramic with high thermal shock resistance - Google Patents
Preparation method of yttrium oxide ceramic with high thermal shock resistance Download PDFInfo
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Abstract
The invention relates to a preparation method of yttrium oxide ceramic, particularly to a preparation method of yttrium oxide ceramic with high thermal shock resistance, and aims to solve the problem of poorer thermal shock resistance of existing yttrium oxide ceramic. The method comprises steps as follows: 1, granulation is performed on yttrium oxide and interlayer powder; 2, yttrium oxide ceramic blanks are molded; 3, sintering is performed and then the yttrium oxide ceramic with the high thermal shock resistance is obtained. With the adoption of the method, the thermal shock resistance and the bending strength of the yttrium oxide ceramic are enhanced, and meanwhile, the yttrium oxide ceramic obtained with the method has the higher density. The preparation method is applied to the field of ceramic materials.
Description
Technical field
The present invention relates to a kind of preparation method of yttrium.
Background technology
As a kind of important rare-earth oxidation raw material, yttrium oxide has the excellent feature such as erosion resistance, high light transmittance, high-k, be widely used in the field of functional materials such as transparent ceramic material and infra-red material, again because its fusing point is high, resistance toheat good, all obtain extensive concern in fields such as refractory materials, high performance structures material, nuclear industry, aerospace industries in recent years.
Titanium alloy has been widely used in as a kind of high performance alloys and has manufactured aviation aircraft component, and titanium alloy production cost is higher at present, major cause is that titanium alloy melting process adopts Forced water cooling copper crucible as carrying vessel mostly, cause energy consumption of reaction higher, and because volume is restricted, very easily make melt produce component segregation, cause production efficiency lower.
For seeking the replacement material carrying melts of titanium alloy, researchist have selected oxide refractories system, typically general oxide refractories all can be used as high-temperature fusant carrying vessel, but because the fusing point of titanium is higher, and activity is stronger, chemical reaction in various degree all occurs with most of refractory materials under high-temperature fusant state, and the material system therefore replacing copper crucible not only needs to have higher fusing point, also needs at high temperature there is lower reactive behavior with titanium simultaneously.
Yttrium oxide material fusing point higher (2410 DEG C), at high temperature react hardly with titanium, therefore be the refractory materials of a kind of desirable carrying titanium alloy melting reaction, other oxide compounds of usual use are if zirconium white etc. is as Crucible body material, using yttrium oxide as with alloy melt contact surface material, the defect of this kind of method is that yttrium oxide is evenly distributed on contact surface with higher-density and combines closely more difficult, in use easily there is the phenomenon that contact surface comes off, melts of titanium alloy is made directly to contact outer oxide thing refractory materials, not only can contaminated melt, and there is certain danger.And the high-compactness crucible heat-shock resistance using pure zirconia yttrium to manufacture is poor, in the foundry goods process of melt by high temperature → room temperature, easily produce problems of crack.For improving its heat-shock resistance, general employing reduces the method that crucible density increases void content, the defect of this method also can increase the surfaceness of crucible while of being density reduction, in use the partial particulate of uneven surface is easily washed away by melt and comes off, be mixed into alloy inside, affect its use properties.
Summary of the invention
The present invention will solve the poor problem of existing yttrium heat-shock resistance, provides a kind of preparation method with the yttrium of high-heat resistance shock resistant.
The present invention has the preparation method of the yttrium of high-heat resistance shock resistant, carries out according to the following steps:
One, yttrium oxide and middle layer powder granulation
A. the calcium oxide powder of the yttrium oxide powder of 85% ~ 90%, the silicon-dioxide powdery of 7% ~ 12% and surplus is taken by mass percentage;
B. yttrium oxide powder is put into polyurethane ball-milling pot, add deionized water, obtain yttrium oxide slurry, then add ammonium citrate and Sudan Gum-arabic, after ball sealer grinding jar, be placed on ball milling 6 ~ 10h on rolling rods type ball mill; Wherein the mass ratio of yttrium oxide powder and deionized water is 1 ~ 2:1, and ammonium citrate is 2% ~ 4% of yttrium oxide stock quality, and Sudan Gum-arabic is 2% ~ 4% of yttrium oxide stock quality;
C. silicon-dioxide powdery and the mixing of calcium oxide powder are put into polyurethane ball-milling pot, add deionized water, obtain mixed slurry, then add ammonium citrate and Sudan Gum-arabic, after ball sealer grinding jar, be placed on ball milling 6 ~ 10h on rolling rods type ball mill; Wherein the mass ratio of mixed powder and deionized water is 1 ~ 2:1, and ammonium citrate is 2% ~ 4% of mixed slurry quality, and Sudan Gum-arabic is 2% ~ 4% of mixed slurry quality;
D. two kinds of good for ball milling slurries are transferred in clean container respectively, by constant flow pump by a kind of slurry at the uniform velocity be transported in Spray Grain-make Drier, dryer temperature setting range 170 ~ 200 DEG C;
E. after a slurry granulation, change another kind of slurry and start granulation, before changing slurry, need clean Spray Grain-make Drier, purging method is deionized water rinsing 10 ~ 15min, final obtained yttrium oxide pelletizing and mixing granulation powder;
Two, yttrium blank forming
The yttrium oxide pelletizing that step one is obtained is poured in forming mould, and adopt unidirectional axial compression mode shaping, forming pressure is 20 ~ 26MPa, the yttrium oxide green compact that compacting is circular;
Then pour in forming mould by the mixing granulation powder that step one is obtained, adopt unidirectional axial compression mode shaping, forming pressure is 20 ~ 26MPa, the powder mix green compact that compacting is circular,
Yttrium oxide green compact are placed on bottom, yttrium oxide green compact are placed powder mix green compact, the two center alignment overlays in mould, powder mix green compact upper surface capping oxidation yttrium pelletizing, the quality of yttrium oxide pelletizing is 115% ~ 130% of bottom oxide yttrium green compact, again axial compression shaping after carry out cold isostatic compaction, cold equipressure is 100 ~ 120MPa;
Three, sinter
After base substrate takes out, adopt gas pressure sintering stove to sinter, sintering temperature is 1700 ~ 1750 DEG C, sintered heat insulating time 2 ~ 4h, and sintering whole process adopts argon gas atmosphere protection.
Wherein in step one, mechanical milling process adopts zirconium oxide balls, and ratio of grinding media to material is 2 ~ 3:1, and rotational speed of ball-mill is set as 600 ~ 900r/min.
Sudan Gum-arabic described in step one c be by the Sudan Gum-arabic of solid in advance heating for dissolving in deionized water, be mixed with the colloidal sol that mass concentration is 40%; Yttrium oxide powder described in step one is bought from Yu Ying Refractory Co., ltd; Mist projection granulating process needs control temperature, as lower than or exceed setting range, boosting switch need be opened or closed;
In step 2, powder mix green compact diameter is 75% ~ 90% of yttrium oxide green compact,
Need ensure the accuracy of powder addition in step 2 in the molded process of one-way shaft, powder weight error is no more than 1%; The molded base substrate obtained of one-way shaft needs to carry out Vacuum Package before isostatic cool pressing process.
In step 3, sintering adopts the mode of burying burning, buries and burns before powder uses and in 1300 DEG C of calcining 1h, and need sieve.
Beneficial effect of the present invention:
The present invention is on the basis of preparing yttrium; add a middle layer mixed by silicon oxide and calcium oxide powder; as buffer structure; this structure is softening when high temperature; the internal stress that outer oxide yttrium produces due to temperature shock is absorbed when being transferred to room temperature by high temperature; external heat release in cooling curing process simultaneously; after the oxidized yttrium pottery of this part heat absorbs; the impact of extraneous condensate depression on it can be alleviated; yttrium is played a protective role, thus strengthens the thermal shock resistance of yttrium.Simultaneously because calcium oxide can play promoter effect to the sintering of yttrium oxide, the yttrium utilizing this technology to obtain also has higher density, and its use properties significantly improves.
(1) the present invention is applicable to the preparation to the higher yttrium material of service requirements, can obtain the yttrium material that thermal shock resistance is strong, density is higher.This yttrium material has stronger thermal shock resistance, makes not easily to break in repeatedly cold cycling process, and averaging loop can reach 5-6 time, and then can ensure the long-term reliability of material.
(2) the present invention adopts atomizing granulating technology, the powder obtained has stronger mobility, is conducive to improving green density, have employed the Interlayer Formulation of sintering aid in addition simultaneously, not only can improve the thermostability of yttrium material, also can improve its sintered density simultaneously.
(3) the inventive method can improve the bending strength of yttrium material, and its bending strength is higher than 155MPa;
(4) the present invention is not only applicable to yttrium material, under the prerequisite choosing suitable middle layer powder, all has general applicability to general oxide ceramic material.
Accompanying drawing explanation
Fig. 1 is the yttrium structural representation containing interlayer structure;
Fig. 2 is spray-drier yttrium oxide powder SEM before treatment photo in embodiment 1;
Fig. 3 is the yttrium oxide powder SEM photo obtained after Spray Grain-make Drier process in embodiment 1;
Fig. 4 is the sample surfaces XRD test pattern in embodiment 1 after heat-shock resistance test;
Fig. 5 is the SEM photo on yttrium surface prepared by embodiment 1.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: present embodiment has the preparation method of the yttrium of high-heat resistance shock resistant, carry out according to the following steps:
One, yttrium oxide and middle layer powder granulation
A. the calcium oxide powder of the yttrium oxide powder of 85% ~ 90%, the silicon-dioxide powdery of 7% ~ 12% and surplus is taken by mass percentage;
B. yttrium oxide powder is put into polyurethane ball-milling pot, add deionized water, obtain yttrium oxide slurry, then add ammonium citrate and Sudan Gum-arabic, after ball sealer grinding jar, be placed on ball milling 6 ~ 10h on rolling rods type ball mill;
C. silicon-dioxide powdery and the mixing of calcium oxide powder are put into polyurethane ball-milling pot, add deionized water, obtain mixed slurry, then add ammonium citrate and Sudan Gum-arabic, after ball sealer grinding jar, be placed on ball milling 6 ~ 10h on rolling rods type ball mill;
D. two kinds of good for ball milling slurries are transferred in clean container respectively, by constant flow pump by a kind of slurry at the uniform velocity be transported in Spray Grain-make Drier, dryer temperature setting range 170 ~ 200 DEG C;
E. after a slurry granulation, change another kind of slurry and start granulation, before changing slurry, need clean Spray Grain-make Drier, final obtained yttrium oxide pelletizing and mixing granulation powder;
Two, yttrium blank forming
The yttrium oxide pelletizing that step one is obtained is poured in forming mould, and adopt unidirectional axial compression mode shaping, forming pressure is 20 ~ 26MPa, the yttrium oxide green compact that compacting is circular;
Then pour in forming mould by the mixing granulation powder that step one is obtained, adopt unidirectional axial compression mode shaping, forming pressure is 20 ~ 26MPa, the powder mix green compact that compacting is circular,
Yttrium oxide green compact are placed on bottom, yttrium oxide green compact are placed powder mix green compact, the two center alignment overlays in mould, powder mix green compact upper surface capping oxidation yttrium pelletizing, the quality of yttrium oxide pelletizing is 115% ~ 130% of bottom oxide yttrium green compact, again axial compression shaping after carry out cold isostatic compaction, cold equipressure is 100 ~ 120MPa;
Three, sinter
After base substrate takes out, adopt gas pressure sintering stove to sinter, sintering temperature is 1700 ~ 1750 DEG C, sintered heat insulating time 2 ~ 4h, and sintering whole process adopts argon gas atmosphere protection.
Yttrium oxide powder described in step one is bought from Yu Ying Refractory Co., ltd; Mist projection granulating process needs control temperature, as lower than or exceed setting range, boosting switch need be opened or closed;
Need ensure the accuracy of powder addition in step 2 in the molded process of one-way shaft, powder weight error is no more than 1%; The molded base substrate obtained of one-way shaft needs to carry out Vacuum Package before isostatic cool pressing process.
Present embodiment, by increasing a middle layer in ceramic center region, under the prerequisite not changing yttrium high-compactness, is strengthened its resistance to stress ability by high temperature → room temperature, thus is played the effect increasing yttrium cold cycling number of times.Present embodiment is also a kind of thermal shock resistant ceramic material technology of preparing with general applicability simultaneously, is applicable to engineer applied.
Embodiment two: present embodiment and embodiment one unlike: in step one b, the mass ratio of yttrium oxide powder and deionized water is 1 ~ 2:1, ammonium citrate is 2% ~ 4% of yttrium oxide stock quality, and Sudan Gum-arabic is 2% ~ 4% of yttrium oxide stock quality.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one unlike: in step one c, the mass ratio of mixed powder and deionized water is 1 ~ 2:1, ammonium citrate is 2% ~ 4% of mixed slurry quality, and Sudan Gum-arabic is 2% ~ 4% of mixed slurry quality.Other is identical with embodiment one.
Embodiment four: present embodiment and embodiment one unlike: the purging method in step one e is specially deionized water rinsing 10 ~ 15min.Other is identical with embodiment one.
Embodiment five: present embodiment and embodiment one unlike: in step one, mechanical milling process adopts zirconium oxide balls, and ratio of grinding media to material is 2 ~ 3:1, and rotational speed of ball-mill is set as 600 ~ 900r/min.Other is identical with embodiment one.
Embodiment six: present embodiment and embodiment one unlike: Sudan Gum-arabic described in step one c be by the Sudan Gum-arabic of solid in advance heating for dissolving in deionized water, be mixed with the colloidal sol that mass concentration is 40%.Other is identical with embodiment one.
Embodiment seven: present embodiment and embodiment one unlike: in step 2, powder mix green compact diameter is 75% ~ 90% of yttrium oxide green compact.Other is identical with embodiment one.
Embodiment eight: present embodiment and embodiment one unlike: sinter the mode adopting and bury burning in step 3, bury that to burn diameter of particle be 100 ~ 150 μm, bury and burn before powder uses and in 1300 DEG C of calcining 1h, and need sieve.Other is identical with embodiment one.
For verifying beneficial effect of the present invention, carry out following test:
Embodiment 1: prepare the yttrium sample of diameter 60mm containing middle layer
One, weigh 1000g high-purity yttrium oxide powder and put into polyurethane ball-milling pot A, 850g silicon-dioxide powdery and 150g calcium oxide powder put into polyurethane ball-milling pot B, respectively to adding 1500g deionized water, 2000g zirconium oxide balls, 25g ammonium citrate and 40g Sudan Gum-arabic in two tanks;
Polyurethane ball-milling pot A and polyurethane ball-milling pot B is placed on rolling rods type ball mill, rotating speed 900r/min is set, Ball-milling Time 8h;
Adopt Spray Grain-make Drier to dry two kinds of slurries successively, bake out temperature is set to 180 DEG C, needs to rinse drying tower inwall 15min before changing slurry; Final obtained yttrium oxide pelletizing 50g and mixing granulation powder 10g;
Fig. 2 is pattern before this example yttrium oxide powder mist projection granulating, Fig. 3 is through mist projection granulating process rear oxidation yttrium morphology microstructure, known through contrasting, without the powder mix of granulation process, pattern is irregular bulk, and mostly be the particle of sheet or tip-angled shape, and after granulation process, the shape homogeneity of powder is better, the powder of preparation be spherical, breadth of particle size distribution is larger, make the grain size distribution of powder more reasonable, be conducive to obtaining higher processability.
Two, pour in forming mould by the yttrium oxide pelletizing that step one is obtained, adopt unidirectional axial compression mode shaping, forming pressure is 26MPa, the yttrium oxide green compact that compacting is circular;
Then pour in forming mould by the mixing granulation powder that step one is obtained, adopt unidirectional axial compression mode shaping, forming pressure is 26MPa, the powder mix green compact that compacting is circular,
Yttrium oxide green compact are placed on bottom, yttrium oxide green compact are placed powder mix green compact, the two center alignment overlays in mould, powder mix green compact upper surface capping oxidation yttrium pelletizing, the quality of yttrium oxide pelletizing is 115% ~ 130% of bottom oxide yttrium green compact, again axial compression shaping after carry out cold isostatic compaction, cold equipressure is 100MPa; Obtained round ceramic base substrate as shown in Figure 1, blank diameter 60mm; In Fig. 1, a is the middle layer that silicon-dioxide and calcium oxide powder mix, and b is yttrium oxide;
Three, sinter: after base substrate takes out, adopt air pressure stove to sinter under an argon atmosphere, sintering temperature is 1750 DEG C, sintered heat insulating time 2h.
The thermal shock resistance of test sintering rear oxidation yttrium ceramics sample, method is room temperature ~ 1200 ± 10 DEG C circulations, and often kind of environment stops 3min, stops when obvious crackle appears in sample surfaces;
Result shows, pure zirconia yttrium ceramics sample test result is averaging loop 3 times, and the compound oxidizing yttrium ceramics sample test result adopting the present embodiment method to prepare is averaging loop 5 times.XRD test is carried out to the sample surfaces after heat-shock resistance test, result as shown in Figure 4, the equal corresponding yttrium oxide collection of illustrative plates of whole characteristic peaks of experimental result, prove that the present embodiment method not only can improve the thermal shock resistance of yttrium oxide, and in use do not produce surface and inner mass transfer behavior, be applicable to the environment for use higher to yttrium oxide purity requirement.
Sintering experiment is prepared more than repeating, and density test is carried out to the sample obtained, result shows the comparatively pure zirconia yttrium sample density lifting about 4.59% of compound sample, after sample is dried, cut 5 battens carry out flexural strength test, to results averaged, known pure zirconia yttrium ceramics sample bending strength is 135.7MPa, and the compound oxidizing yttrium ceramics sample bending strength adopting present method to prepare is 155.3MPa, illustrate that present method has active effect to the density and bending strength that improve yttrium.
Sem analysis is carried out to yttrium surface prepared by the present embodiment, result as shown in Figure 5, obviously can observe the nearly equiaxed grain structures of sintered compact, surface compact, almost pore-free, illustrate that yttrium surface densification degree prepared by present method is higher, this contributes to improving yttrium mechanical property and surface smoothness.
Embodiment 2: prepare diameter 60mm containing middle layer yttrium sample
One, weigh 1000g high-purity yttrium oxide powder and put into polyurethane ball-milling pot A, 900g silicon-dioxide and 100g calcium oxide powder put into polyurethane ball-milling pot B, respectively to adding 1500g deionized water, 2000g zirconium oxide balls, 25g ammonium citrate and 40g Sudan Gum-arabic in two tanks;
Polyurethane ball-milling pot A and polyurethane ball-milling pot B is placed on rolling rods type ball mill, rotating speed 900r/min is set, Ball-milling Time 10h;
Adopt Spray Grain-make Drier to dry two kinds of slurries successively, bake out temperature is set to 170 DEG C, needs to rinse drying tower inwall 15min before changing slurry; Final obtained yttrium oxide pelletizing 50g and mixing granulation powder 10g;
Two, pour in forming mould by the yttrium oxide pelletizing that step one is obtained, adopt unidirectional axial compression mode shaping, forming pressure is 26MPa, the yttrium oxide green compact that compacting is circular;
Then pour in forming mould by the mixing granulation powder that step one is obtained, adopt unidirectional axial compression mode shaping, forming pressure is 26MPa, the powder mix green compact that compacting is circular,
Yttrium oxide green compact are placed on bottom, yttrium oxide green compact are placed powder mix green compact, the two center alignment overlays in mould, powder mix green compact upper surface capping oxidation yttrium pelletizing, the quality of yttrium oxide pelletizing is 115% ~ 130% of bottom oxide yttrium green compact, again axial compression shaping after carry out cold isostatic compaction, cold equipressure is 120MPa; Obtained round ceramic base substrate as shown in Figure 1, blank diameter 60mm;
Three, sinter: after base substrate takes out, adopt air pressure stove to sinter under an argon atmosphere, sintering temperature is 1720 DEG C, sintered heat insulating time 2h.
The thermal shock resistance of test sintering rear oxidation yttrium ceramics sample, method is room temperature ~ 1200 ± 10 DEG C circulations, and often kind of environment stops 3min, stops when obvious crackle appears in sample surfaces;
Result shows, pure zirconia yttrium ceramics sample test result is averaging loop 3 times, the compound oxidizing yttrium ceramics sample test result adopting the present embodiment to prepare is averaging loop 6 times, experimental result shows that the present embodiment method can improve the thermal shock resistance of yttrium, is applicable to the environment for use higher to yttrium oxide purity requirement.
Sintering experiment is prepared more than repeating, and density test is carried out to the sample obtained, result shows the comparatively pure zirconia yttrium sample density lifting about 5.61% of compound sample, after sample is dried, cut 5 battens carry out flexural strength test, to results averaged, known pure zirconia yttrium ceramics sample bending strength is 141.1MPa, and the compound oxidizing yttrium ceramics sample bending strength adopting present method to prepare is 159.7MPa, illustrate that present method has active effect to the density and bending strength that improve yttrium.
Embodiment 3: prepare diameter 80mm containing middle layer yttrium sample
One, weigh 1000g high-purity yttrium oxide powder and put into polyurethane ball-milling pot A, 850g silicon-dioxide and 150g calcium oxide powder put into polyurethane ball-milling pot B, respectively to adding 1500g deionized water, 2000g zirconium oxide balls, 25g ammonium citrate and 40g Sudan Gum-arabic in two tanks;
Polyurethane ball-milling pot A and polyurethane ball-milling pot B is placed on rolling rods type ball mill, rotating speed 900r/min is set, Ball-milling Time 8h;
Adopt Spray Grain-make Drier to dry two kinds of slurries successively, bake out temperature is set to 190 DEG C, needs to rinse drying tower inwall 15min before changing slurry; Final obtained yttrium oxide pelletizing 70g and mixing granulation powder 15g;
Two, pour in forming mould by the yttrium oxide pelletizing that step one is obtained, adopt unidirectional axial compression mode shaping, forming pressure is 25MPa, the yttrium oxide green compact that compacting is circular;
Then pour in forming mould by the mixing granulation powder that step one is obtained, adopt unidirectional axial compression mode shaping, forming pressure is 25MPa, the powder mix green compact that compacting is circular,
Yttrium oxide green compact are placed on bottom, yttrium oxide green compact are placed powder mix green compact, the two center alignment overlays in mould, powder mix green compact upper surface capping oxidation yttrium pelletizing, the quality of yttrium oxide pelletizing is 115% ~ 130% of bottom oxide yttrium green compact, again axial compression shaping after carry out cold isostatic compaction, cold equipressure is 120MPa; Obtained round ceramic blank diameter is 80mm;
Three, sinter: after base substrate takes out, adopt air pressure stove to sinter under an argon atmosphere, sintering temperature is 1750 DEG C, sintered heat insulating time 2h.
The thermal shock resistance of test sintering rear oxidation yttrium ceramics sample, method is room temperature ~ 1200 ± 10 DEG C circulations, and often kind of environment stops 3min, stops when obvious crackle appears in sample surfaces;
Result shows, pure zirconia yttrium ceramics sample test result is averaging loop 3 times, the compound oxidizing yttrium ceramics sample test result adopting the present embodiment to prepare is averaging loop 5 times, experimental result shows that the present embodiment method can improve the thermal shock resistance of yttrium, is applicable to the environment for use higher to yttrium oxide purity requirement.
Sintering experiment is prepared more than repeating, and density test is carried out to the sample obtained, result shows the comparatively pure zirconia yttrium sample density lifting about 4.96% of compound sample, after sample is dried, cut 5 battens carry out flexural strength test, to results averaged, known pure zirconia yttrium ceramics sample bending strength is 139.6MPa, and the compound oxidizing yttrium ceramics sample bending strength adopting present method to prepare is 157.5MPa, illustrate that present method has active effect to the density and bending strength that improve yttrium.
Claims (8)
1. there is a preparation method for the yttrium of high-heat resistance shock resistant, it is characterized in that the method is carried out according to the following steps:
One, yttrium oxide and middle layer powder granulation
A. the calcium oxide powder of the yttrium oxide powder of 85% ~ 90%, the silicon-dioxide powdery of 7% ~ 12% and surplus is taken by mass percentage;
B. yttrium oxide powder is put into polyurethane ball-milling pot, add deionized water, obtain yttrium oxide slurry, then add ammonium citrate and Sudan Gum-arabic, after ball sealer grinding jar, be placed on ball milling 6 ~ 10h on rolling rods type ball mill;
C. silicon-dioxide powdery and the mixing of calcium oxide powder are put into polyurethane ball-milling pot, add deionized water, obtain mixed slurry, then add ammonium citrate and Sudan Gum-arabic, after ball sealer grinding jar, be placed on ball milling 6 ~ 10h on rolling rods type ball mill;
D. two kinds of good for ball milling slurries are transferred in clean container respectively, by constant flow pump by a kind of slurry at the uniform velocity be transported in Spray Grain-make Drier, dryer temperature setting range 170 ~ 200 DEG C;
E. after a slurry granulation, change another kind of slurry and start granulation, before changing slurry, need clean Spray Grain-make Drier, final obtained yttrium oxide pelletizing and mixing granulation powder;
Two, yttrium blank forming
The yttrium oxide pelletizing that step one is obtained is poured in forming mould, and adopt unidirectional axial compression mode shaping, forming pressure is 20 ~ 26MPa, the yttrium oxide green compact that compacting is circular;
Then pour in forming mould by the mixing granulation powder that step one is obtained, adopt unidirectional axial compression mode shaping, forming pressure is 20 ~ 26MPa, the powder mix green compact that compacting is circular,
Yttrium oxide green compact are placed on bottom, yttrium oxide green compact are placed powder mix green compact, the two center alignment overlays in mould, powder mix green compact upper surface capping oxidation yttrium pelletizing, the quality of yttrium oxide pelletizing is 115% ~ 130% of bottom oxide yttrium green compact, again axial compression shaping after carry out cold isostatic compaction, cold equipressure is 100 ~ 120MPa;
Three, sinter
After base substrate takes out, adopt gas pressure sintering stove to sinter, sintering temperature is 1700 ~ 1750 DEG C, sintered heat insulating time 2 ~ 4h, and sintering whole process adopts argon gas atmosphere protection, namely obtains the yttrium with high-heat resistance shock resistant.
2. a kind of preparation method with the yttrium of high-heat resistance shock resistant according to claim 1, it is characterized in that the mass ratio of yttrium oxide powder and deionized water in step one b is 1 ~ 2:1, ammonium citrate is 2% ~ 4% of yttrium oxide stock quality, and Sudan Gum-arabic is 2% ~ 4% of yttrium oxide stock quality.
3. a kind of preparation method with the yttrium of high-heat resistance shock resistant according to claim 1, it is characterized in that the mass ratio of mixed powder and deionized water in step one c is 1 ~ 2:1, ammonium citrate is 2% ~ 4% of mixed slurry quality, and Sudan Gum-arabic is 2% ~ 4% of mixed slurry quality.
4. a kind of preparation method with the yttrium of high-heat resistance shock resistant according to claim 1, is characterized in that the purging method in step one e is specially deionized water rinsing 10 ~ 15min.
5. a kind of preparation method with the yttrium of high-heat resistance shock resistant according to claim 1, it is characterized in that in step one, mechanical milling process adopts zirconium oxide balls, ratio of grinding media to material is 2 ~ 3:1, and rotational speed of ball-mill is set as 600 ~ 900r/min.
6. a kind of preparation method with the yttrium of high-heat resistance shock resistant according to claim 1, it is characterized in that Sudan Gum-arabic described in step one c be by the Sudan Gum-arabic of solid in advance heating for dissolving in deionized water, be mixed with the colloidal sol that mass concentration is 40%.
7. a kind of preparation method with the yttrium of high-heat resistance shock resistant according to claim 1, is characterized in that in step 2, powder mix green compact diameter is 75% ~ 90% of yttrium oxide green compact.
8. a kind of preparation method with the yttrium of high-heat resistance shock resistant according to claim 1, it is characterized in that in step 3, sintering adopts the mode of burying burning, burying burning diameter of particle is 100 ~ 150 μm, buries and burns before powder uses and in 1300 DEG C of calcining 1h, and need sieve.
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| CN102000458A (en) * | 2010-10-19 | 2011-04-06 | 北京航空航天大学 | Yttria foamed ceramic filter and preparation method thereof |
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| CN101628812A (en) * | 2008-07-14 | 2010-01-20 | 东北大学 | Method for preparing compact yttria ceramics |
| CN101462760A (en) * | 2009-01-15 | 2009-06-24 | 东北大学 | Method for preparing high performance yttrium oxide material |
| CN101875091A (en) * | 2009-11-30 | 2010-11-03 | 北京航空航天大学 | Yttrium sol bonded yttrium oxide formwork and preparation method thereof |
| CN102000458A (en) * | 2010-10-19 | 2011-04-06 | 北京航空航天大学 | Yttria foamed ceramic filter and preparation method thereof |
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| CN113620694A (en) * | 2021-09-03 | 2021-11-09 | 湖南昕昱科技有限公司 | Crucible for smelting alloy containing active elements and preparation method thereof |
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