CN105110793B - A kind of preparation method of the yttrium with high-heat resistance shock resistant - Google Patents
A kind of preparation method of the yttrium with high-heat resistance shock resistant Download PDFInfo
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Abstract
A kind of preparation method of the yttrium with high-heat resistance shock resistant, is related to a kind of preparation method of yttrium.The present invention is to solve the problem that existing yttrium thermal shock resistance is poor.Method：First, yittrium oxide and intermediate layer powder are granulated；2nd, yttrium blank forming；3rd, sinter, that is, obtain the yttrium with high-heat resistance shock resistant.This method enhances the thermal shock resistance and bending strength of yttrium, while also having consistency higher using the yttrium that the method is obtained.The present invention is used for ceramic material field.
Description
Technical field
The present invention relates to a kind of preparation method of yttrium.
Background technology
Used as a kind of important rare-earth oxidation raw material, yittrium oxide has excellent corrosion resistance, high light transmittance, dielectric high
The features such as constant, it is widely used in the field of functional materials such as transparent ceramic material and infra-red material, and because its fusing point is high, heat-resisting
It is functional, obtained extensively in fields such as refractory material, high performance structures material, nuclear industry, aerospace industries in recent years
Concern.
Titanium alloy is widely used in manufacture aviation aircraft parts as a kind of high performance alloys, and titanium alloy is given birth at present
Product is relatively costly, main reason is that titanium alloy smelting process is caused mostly using Forced water cooling copper crucible as vessel are carried
Energy consumption of reaction is higher, and because volume is restricted, melt is produced component segregation, causes production efficiency relatively low.
To seek the alternate material of carrying melts of titanium alloy, researcher have selected oxide refractories system, generally
For general oxide refractories can carry vessel as high-temperature fusant, but because the fusing point of titanium is higher, and activity compared with
By force, all there is different degrees of chemical reaction with most of refractory materials under high-temperature fusant state, therefore replace copper crucible
Material system does not need only have fusing point higher, while being also required to have relatively low reactivity at high temperature with titanium.
Yttrium oxide material fusing point is (2410 DEG C) higher, is hardly reacted with titanium at high temperature, therefore is a kind of preferable
The refractory material for carrying titanium alloy smelting reaction, usually using other oxides such as zirconium oxide etc. as Crucible body material,
As the defect with alloy melt contact surface material, this kind of method it is that yittrium oxide is evenly distributed on higher-density using yittrium oxide
Contact surface and it is tightly combined relatively difficult, easily occurs the phenomenon that contact surface comes off in use, makes melts of titanium alloy straight
Contact outer oxide thing refractory material, not only can contaminated melt, and with certain danger.And use pure zirconia yttrium system
The high-compactness crucible thermal shock resistance made is poor, during casting of the melt by high temperature → room temperature, easily produces cracking etc. to ask
Topic.To improve its thermal shock resistance, general using the method that crucible consistency increases the porosity is reduced, the defect of this method is to cause
Also the surface roughness of crucible can be increased while density reduction, the partial particulate of rough surface is easily melt in use
Body washes away and comes off, and is mixed into inside alloy, influences its performance.
The content of the invention
The present invention is to solve the problem that existing yttrium thermal shock resistance is poor, there is provided one kind has high-heat resistance shock resistant
Yttrium preparation method.
The preparation method of yttrium of the present invention with high-heat resistance shock resistant, is carried out according to the following steps：
First, yittrium oxide and intermediate layer powder are granulated
A. 85%~90% yttrium oxide powder, 7%~12% silicon-dioxide powdery and remaining are weighed by mass percentage
The calcium oxide powder of amount；
B. yttrium oxide powder is put into polyurethane ball-milling pot, adds deionized water, obtain yittrium oxide slurry, be subsequently adding lemon
Lemon acid ammonium and gum arabic, 6~10h of ball milling on rolling rods type ball mill is placed on after sealing ball grinder；Wherein yttrium oxide powder with
The mass ratio of deionized water is 1~2:1, ammonium citrate is the 2%~4% of yittrium oxide stock quality, and gum arabic is oxidation
The 2%~4% of yttrium stock quality；
C. silicon-dioxide powdery and calcium oxide powder are mixed and is put into polyurethane ball-milling pot, add deionized water, obtain mixed
Slurry is closed, ammonium citrate and gum arabic is subsequently adding, 6~10h of ball milling on rolling rods type ball mill is placed on after sealing ball grinder；
Wherein mixed powder and the mass ratio of deionized water is 1~2:1, ammonium citrate is the 2%~4% of mixed slurry quality, I
Uncle's natural gum is the 2%~4% of mixed slurry quality；
D. two kinds of good slurries of ball milling are transferred in clean container respectively, by constant flow pump by a kind of slurry at the uniform velocity defeated
It is sent in Spray Grain-make Drier, 170~200 DEG C of dryer temperature setting range；
E. after a kind of slurry granulation is finished, change another slurry and start granulation, before changing slurry, need to be dry to mist projection granulating
Dry machine is cleaned, and cleaning method is 10~15min of deionized water rinsing, finally prepared yittrium oxide pelletizing and mixing granulation
Powder；
2nd, yttrium blank forming
Yittrium oxide pelletizing obtained in step one is poured into mould, is molded using one-way shaft pressure mode, shaping pressure
Power is 20~26MPa, suppresses circular yittrium oxide green compact；
Then mixing granulation powder obtained in step one is poured into mould, is molded using one-way shaft pressure mode, be molded
Pressure is 20~26MPa, suppresses circular mixed powder green compact,
Yittrium oxide green compact are placed on bottom, mixed powder green compact are placed on yittrium oxide green compact, the two center alignment is stacked
In mould, mixed powder green compact upper surface covering yittrium oxide pelletizing, the quality of yittrium oxide pelletizing is bottom oxide yttrium green compact
115%~130%, then cold isostatic compaction is carried out after secondary axes are molded, it is cold that to wait pressure be 100~120MPa；
3rd, sinter
After base substrate takes out, it is sintered using gas pressure sintering stove, sintering temperature is 1700~1750 DEG C, during sintered heat insulating
Between 2~4h, sintering overall process using argon gas atmosphere protect.
Mechanical milling process uses zirconium oxide balls wherein in step one, and ratio of grinding media to material is 2~3:1, rotational speed of ball-mill is set as 600~
900r/min。
Gum arabic described in step one c be by the advance heating for dissolving of the gum arabic of solid in deionized water,
It is configured to the colloidal sol that mass concentration is 40%；Yttrium oxide powder described in step one is bought from Yu Ying Refractory Co., ltds；
Mist projection granulating process need to control temperature, be such as less than or more than setting range, need to open or close auxiliary heater switch；
The 75%~90% of a diameter of yittrium oxide green compact of mixed powder green compact in step 2,
The accuracy of powder addition need to be ensured in step 2 in the molded process of one-way shaft, powder weight error is no more than
1%；The molded base substrate for obtaining of one-way shaft need to carry out Vacuum Package in isostatic cool pressing before processing.
By the way of burning is buried, burying burning powder need to calcine 1h to sintering before in 1300 DEG C, and sieve in step 3.
Beneficial effects of the present invention：
On the basis of yttrium is prepared, addition one is mixed by silica and calcium oxide powder the present invention
Intermediate layer, used as buffer structure, the structure softens in high temperature, when room temperature is transferred to by high temperature absorb outer oxide yttrium due to
The internal stress that temperature shock is produced, while the external heat release during cooling and solidifying, the oxidized yttrium ceramics absorption of this partial heat
Afterwards, influence of the extraneous degree of supercooling to it can be alleviated, yttrium is played a protective role, so as to strengthen the anti-of yttrium
Thermal shock ability.Simultaneously because calcium oxide can play promoter effect to the sintering of yittrium oxide, the yittrium oxide obtained using the technology is made pottery
Porcelain also has consistency higher, and its performance is significantly improved.
(1) present invention can obtain thermal shock resistance suitable for the preparation of the yttrium material higher to use requirement
By force, consistency yttrium material higher.The yttrium material has stronger thermal shock resistance so that multiple
It is not easily broken during cold cycling, averaging loop can reach 5-6 times, and then can guarantee that the long-term reliability of material.
(2) present invention uses atomizing granulating technology, and the powder for obtaining has stronger mobility, is conducive to improving base substrate cause
Density, while employing the Interlayer Formulation of also sintering aid, can not only improve the heat endurance of yttrium material, together
When can also improve its sintered density.
(3) the inventive method can improve the bending strength of yttrium material, and its bending strength is higher than 155MPa；
(4) present invention is applicable not only to yttrium material, on the premise of appropriate intermediate layer powder is chosen, to one
As oxide ceramic material be respectively provided with general applicability.
Brief description of the drawings
Fig. 1 is the yttrium structural representation containing interlayer structure；
Fig. 2 is the yttrium oxide powder SEM photograph of spray dryer before processing in embodiment 1；
Fig. 3 is the yttrium oxide powder SEM photograph obtained after being processed through Spray Grain-make Drier in embodiment 1；
Fig. 4 is the sample surfaces XRD test charts after thermal shock resistance test in embodiment 1；
Fig. 5 is the SEM photograph on yttrium surface prepared by embodiment 1.
Specific embodiment
Technical solution of the present invention is not limited to act specific embodiment set forth below, also including between each specific embodiment
Any combination.
Specific embodiment one：Present embodiment has the preparation method of the yttrium of high-heat resistance shock resistant, by following
Step is carried out：
First, yittrium oxide and intermediate layer powder are granulated
A. 85%~90% yttrium oxide powder, 7%~12% silicon-dioxide powdery and remaining are weighed by mass percentage
The calcium oxide powder of amount；
B. yttrium oxide powder is put into polyurethane ball-milling pot, adds deionized water, obtain yittrium oxide slurry, be subsequently adding lemon
Lemon acid ammonium and gum arabic, 6~10h of ball milling on rolling rods type ball mill is placed on after sealing ball grinder；
C. silicon-dioxide powdery and calcium oxide powder are mixed and is put into polyurethane ball-milling pot, add deionized water, obtain mixed
Slurry is closed, ammonium citrate and gum arabic is subsequently adding, 6~10h of ball milling on rolling rods type ball mill is placed on after sealing ball grinder；
D. two kinds of good slurries of ball milling are transferred in clean container respectively, by constant flow pump by a kind of slurry at the uniform velocity defeated
It is sent in Spray Grain-make Drier, 170~200 DEG C of dryer temperature setting range；
E. after a kind of slurry granulation is finished, change another slurry and start granulation, before changing slurry, need to be dry to mist projection granulating
Dry machine is cleaned, finally prepared yittrium oxide pelletizing and mixing granulation powder；
2nd, yttrium blank forming
Yittrium oxide pelletizing obtained in step one is poured into mould, is molded using one-way shaft pressure mode, shaping pressure
Power is 20~26MPa, suppresses circular yittrium oxide green compact；
Then mixing granulation powder obtained in step one is poured into mould, is molded using one-way shaft pressure mode, be molded
Pressure is 20~26MPa, suppresses circular mixed powder green compact,
Yittrium oxide green compact are placed on bottom, mixed powder green compact are placed on yittrium oxide green compact, the two center alignment is stacked
In mould, mixed powder green compact upper surface covering yittrium oxide pelletizing, the quality of yittrium oxide pelletizing is bottom oxide yttrium green compact
115%~130%, then cold isostatic compaction is carried out after secondary axes are molded, it is cold that to wait pressure be 100~120MPa；
3rd, sinter
After base substrate takes out, it is sintered using gas pressure sintering stove, sintering temperature is 1700~1750 DEG C, during sintered heat insulating
Between 2~4h, sintering overall process using argon gas atmosphere protect.
Yttrium oxide powder described in step one is bought from Yu Ying Refractory Co., ltds；Mist projection granulating process need to control temperature
Degree, is such as less than or more than setting range, need to open or close auxiliary heater switch；
The accuracy of powder addition need to be ensured in step 2 in the molded process of one-way shaft, powder weight error is no more than
1%；The molded base substrate for obtaining of one-way shaft need to carry out Vacuum Package in isostatic cool pressing before processing.
Present embodiment increases an intermediate layer by ceramic center region, is not changing yttrium high-compactness
On the premise of, strengthen its resistance to stress ability by high temperature → room temperature, increase yttrium cold cycling number of times so as to play
Effect.Present embodiment is also a kind of thermal shock resistant ceramic material technology of preparing with general applicability simultaneously, it is adaptable to engineering
Using.
Specific embodiment two：Present embodiment from unlike specific embodiment one：Yttrium oxide powder in step one b
It is 1~2 with the mass ratio of deionized water:1, ammonium citrate is the 2%~4% of yittrium oxide stock quality, and gum arabic is oxygen
Change the 2%~4% of yttrium stock quality.Other are identical with specific embodiment one.
Specific embodiment three：Present embodiment from unlike specific embodiment one：In step one c mixed powder with
The mass ratio of deionized water is 1~2:1, ammonium citrate is the 2%~4% of mixed slurry quality, and gum arabic is mixing slurry
The 2%~4% of material quality.Other are identical with specific embodiment one.
Specific embodiment four：Present embodiment from unlike specific embodiment one：Cleaning method in step one e
Specially 10~15min of deionized water rinsing.Other are identical with specific embodiment one.
Specific embodiment five：Present embodiment from unlike specific embodiment one：Mechanical milling process is adopted in step one
With zirconium oxide balls, ratio of grinding media to material is 2~3:1, rotational speed of ball-mill is set as 600~900r/min.Other and specific embodiment one
It is identical.
Specific embodiment six：Present embodiment from unlike specific embodiment one：It is Arabic described in step one c
Natural gum be by the advance heating for dissolving of the gum arabic of solid in deionized water, be configured to the colloidal sol that mass concentration is 40%.
Other are identical with specific embodiment one.
Specific embodiment seven：Present embodiment from unlike specific embodiment one：Mixed powder green compact in step 2
The 75%~90% of a diameter of yittrium oxide green compact.Other are identical with specific embodiment one.
Specific embodiment eight：Present embodiment from unlike specific embodiment one：Sinter to use in step 3 and bury
The mode of burning, it is 100~150 μm to bury burning diameter of particle, and burying burning powder need to calcine 1h before in 1300 DEG C, and sieve.Other with
Specific embodiment one is identical.
It is checking beneficial effects of the present invention, carries out tests below：
Embodiment 1：Prepare yttrium samples of the diameter 60mm containing intermediate layer
First, weigh 1000g high-purity yttrium oxide powders to be put into polyurethane ball-milling pot A, 850g silicon-dioxide powderies and 150g
Calcium oxide powder is put into polyurethane ball-milling pot B, respectively to addition 1500g deionized waters, 2000g zirconium oxide balls, 25g in two tanks
Ammonium citrate and 40g gum arabics；
Polyurethane ball-milling pot A and polyurethane ball-milling pot B are placed on rolling rods type ball mill, rotating speed 900r/min, ball are set
Time consuming 8h；
Two kinds of slurries are dried using Spray Grain-make Drier successively, drying temperature is set to 180 DEG C, punching is needed before changing slurry
Wash drying inner wall of tower 15min；Yittrium oxide pelletizing 50g and mixing granulation powder 10g is finally obtained；
Fig. 2 is pattern before this example yttrium oxide powder mist projection granulating, and Fig. 3 is to process rear oxidation yttrium powder body by mist projection granulating
Pattern, understands by contrast, the mixed powder without granulation treatment, and pattern is irregular block, and mostly sheet or tip-angled shape
Grain, and by after granulation treatment, preferably, the powder of preparation is larger in spherical, breadth of particle size distribution for the shape homogeneity of powder, make
The grain size distribution of powder is more reasonable, is conducive to obtaining processability higher.
2nd, yittrium oxide pelletizing obtained in step one is poured into mould, is molded using one-way shaft pressure mode, be molded
Pressure is 26MPa, suppresses circular yittrium oxide green compact；
Then mixing granulation powder obtained in step one is poured into mould, is molded using one-way shaft pressure mode, be molded
Pressure is 26MPa, suppresses circular mixed powder green compact,
Yittrium oxide green compact are placed on bottom, mixed powder green compact are placed on yittrium oxide green compact, the two center alignment is stacked
In mould, mixed powder green compact upper surface covering yittrium oxide pelletizing, the quality of yittrium oxide pelletizing is bottom oxide yttrium green compact
115%~130%, then cold isostatic compaction is carried out after secondary axes are molded, it is cold that to wait pressure be 100MPa；It is obtained as shown in Figure 1
Round ceramic base substrate, blank diameter 60mm；A is the intermediate layer that silica and calcium oxide powder are mixed in Fig. 1, and b is
Yittrium oxide；
3rd, sinter：After base substrate takes out, sintered under an argon atmosphere using air pressure stove, sintering temperature is 1750 DEG C, sintering
Soaking time 2h.
The thermal shock resistance of test sintering rear oxidation yttrium ceramics sample, method is circulated for room temperature~1200 ± 10 DEG C, every kind of
Environment stops 3min, stops when there is obvious crackle to sample surfaces；
Result shows that pure zirconia yttrium ceramics sample test result is averaging loop 3 times, is prepared using the present embodiment method
Compound oxidizing yttrium ceramics sample test result is averaging loop 5 times.Sample surfaces after testing thermal shock resistance carry out XRD surveys
Examination, as a result as shown in figure 4, whole characteristic peaks of experimental result correspond to yittrium oxide collection of illustrative plates, it was demonstrated that the present embodiment method not only may be used
The thermal shock resistance of yittrium oxide is improved, and does not produce the mass transfer behavior on surface and inside in use, it is adaptable to oxygen
Change yttrium purity requirement use environment higher.
Repeat sintering experiment made above, and sample to obtaining carries out consistency test, as a result shows compound sample
Compared with pure zirconia yttrium sample consistency lifting about 4.59%, bending strength test is carried out after 5 battens are cut after sample drying, to knot
Fruit is averaged, it is known that pure zirconia yttrium ceramics sample bending strength is 135.7MPa, and uses the compound oxygen of this method preparation
It is 155.3MPa to change yttrium ceramics sample bending strength, illustrates this method to improving consistency and the bending strength tool of yttrium
There is positive role.
Sem analysis are carried out to yttrium surface manufactured in the present embodiment, as a result as shown in figure 5, can substantially observe
The nearly equiaxed grain structures of sintered body, surface compact, almost pore-free, illustrates yttrium surface compact prepared by this method
Change degree is higher, and this is favorably improved yttrium mechanical property and surface smoothness.
Embodiment 2：Prepare the diameter 60mm samples of yttrium containing intermediate layer
First, weigh 1000g high-purity yttrium oxide powders to be put into polyurethane ball-milling pot A, 900g silica and 100g are aoxidized
Calcium powder body is put into polyurethane ball-milling pot B, respectively to addition 1500g deionized waters, 2000g zirconium oxide balls, 25g lemons in two tanks
Sour ammonium and 40g gum arabics；
Polyurethane ball-milling pot A and polyurethane ball-milling pot B are placed on rolling rods type ball mill, rotating speed 900r/min, ball are set
Time consuming 10h；
Two kinds of slurries are dried using Spray Grain-make Drier successively, drying temperature is set to 170 DEG C, punching is needed before changing slurry
Wash drying inner wall of tower 15min；Yittrium oxide pelletizing 50g and mixing granulation powder 10g is finally obtained；
2nd, yittrium oxide pelletizing obtained in step one is poured into mould, is molded using one-way shaft pressure mode, be molded
Pressure is 26MPa, suppresses circular yittrium oxide green compact；
Then mixing granulation powder obtained in step one is poured into mould, is molded using one-way shaft pressure mode, be molded
Pressure is 26MPa, suppresses circular mixed powder green compact,
Yittrium oxide green compact are placed on bottom, mixed powder green compact are placed on yittrium oxide green compact, the two center alignment is stacked
In mould, mixed powder green compact upper surface covering yittrium oxide pelletizing, the quality of yittrium oxide pelletizing is bottom oxide yttrium green compact
115%~130%, then cold isostatic compaction is carried out after secondary axes are molded, it is cold that to wait pressure be 120MPa；It is obtained as shown in Figure 1
Round ceramic base substrate, blank diameter 60mm；
3rd, sinter：After base substrate takes out, sintered under an argon atmosphere using air pressure stove, sintering temperature is 1720 DEG C, sintering
Soaking time 2h.
The thermal shock resistance of test sintering rear oxidation yttrium ceramics sample, method is circulated for room temperature~1200 ± 10 DEG C, every kind of
Environment stops 3min, stops when there is obvious crackle to sample surfaces；
Result shows that pure zirconia yttrium ceramics sample test result is averaging loop 3 times, using manufactured in the present embodiment compound
Type yttrium sample tests are averaging loop 6 times, test result indicate that the present embodiment method can improve yittrium oxide pottery
The thermal shock resistance of porcelain, it is adaptable to the use environment higher to yittrium oxide purity requirement.
Repeat sintering experiment made above, and sample to obtaining carries out consistency test, as a result shows compound sample
Compared with pure zirconia yttrium sample consistency lifting about 5.61%, bending strength test is carried out after 5 battens are cut after sample drying, to knot
Fruit is averaged, it is known that pure zirconia yttrium ceramics sample bending strength is 141.1MPa, and uses the compound oxygen of this method preparation
It is 159.7MPa to change yttrium ceramics sample bending strength, illustrates this method to improving consistency and the bending strength tool of yttrium
There is positive role.
Embodiment 3：Prepare the diameter 80mm samples of yttrium containing intermediate layer
First, 1000g high-purity yttrium oxide powders are weighed and is put into polyurethane ball-milling pot A, 850g silica and 150g calcium oxide
Powder is put into polyurethane ball-milling pot B, respectively to addition 1500g deionized waters, 2000g zirconium oxide balls, 25g citric acids in two tanks
Ammonium and 40g gum arabics；
Polyurethane ball-milling pot A and polyurethane ball-milling pot B are placed on rolling rods type ball mill, rotating speed 900r/min, ball are set
Time consuming 8h；
Two kinds of slurries are dried using Spray Grain-make Drier successively, drying temperature is set to 190 DEG C, punching is needed before changing slurry
Wash drying inner wall of tower 15min；Yittrium oxide pelletizing 70g and mixing granulation powder 15g is finally obtained；
2nd, yittrium oxide pelletizing obtained in step one is poured into mould, is molded using one-way shaft pressure mode, be molded
Pressure is 25MPa, suppresses circular yittrium oxide green compact；
Then mixing granulation powder obtained in step one is poured into mould, is molded using one-way shaft pressure mode, be molded
Pressure is 25MPa, suppresses circular mixed powder green compact,
Yittrium oxide green compact are placed on bottom, mixed powder green compact are placed on yittrium oxide green compact, the two center alignment is stacked
In mould, mixed powder green compact upper surface covering yittrium oxide pelletizing, the quality of yittrium oxide pelletizing is bottom oxide yttrium green compact
115%~130%, then cold isostatic compaction is carried out after secondary axes are molded, it is cold that to wait pressure be 120MPa；Obtained round ceramic
Blank diameter is 80mm；
3rd, sinter：After base substrate takes out, sintered under an argon atmosphere using air pressure stove, sintering temperature is 1750 DEG C, sintering
Soaking time 2h.
The thermal shock resistance of test sintering rear oxidation yttrium ceramics sample, method is circulated for room temperature~1200 ± 10 DEG C, every kind of
Environment stops 3min, stops when there is obvious crackle to sample surfaces；
Result shows that pure zirconia yttrium ceramics sample test result is averaging loop 3 times, using manufactured in the present embodiment compound
Type yttrium sample tests are averaging loop 5 times, test result indicate that the present embodiment method can improve yittrium oxide pottery
The thermal shock resistance of porcelain, it is adaptable to the use environment higher to yittrium oxide purity requirement.
Repeat sintering experiment made above, and sample to obtaining carries out consistency test, as a result shows compound sample
Compared with pure zirconia yttrium sample consistency lifting about 4.96%, bending strength test is carried out after 5 battens are cut after sample drying, to knot
Fruit is averaged, it is known that pure zirconia yttrium ceramics sample bending strength is 139.6MPa, and uses the compound oxygen of this method preparation
It is 157.5MPa to change yttrium ceramics sample bending strength, illustrates this method to improving consistency and the bending strength tool of yttrium
There is positive role.
Claims (7)
1. a kind of preparation method of the yttrium with high-heat resistance shock resistant, it is characterised in that the method is entered according to the following steps
OK：
First, yittrium oxide and intermediate layer powder are granulated
A. 85%~90% yttrium oxide powder, 7%~12% silicon-dioxide powdery and surplus are weighed by mass percentage
Calcium oxide powder；
B. yttrium oxide powder is put into polyurethane ball-milling pot, adds deionized water, obtain yittrium oxide slurry, be subsequently adding citric acid
Ammonium and gum arabic, 6~10h of ball milling on rolling rods type ball mill is placed on after sealing ball grinder；
C. silicon-dioxide powdery and calcium oxide powder are mixed and is put into polyurethane ball-milling pot, add deionized water, obtain mixing slurry
Material, is subsequently adding ammonium citrate and gum arabic, and 6~10h of ball milling on rolling rods type ball mill is placed on after sealing ball grinder；
D. two kinds of good slurries of ball milling are transferred in clean container respectively, by constant flow pump by a kind of slurry being transported at the uniform velocity
In Spray Grain-make Drier, 170~200 DEG C of dryer temperature setting range；
E. after a kind of slurry granulation is finished, change another slurry and start granulation, before changing slurry, need to be to Spray Grain-make Drier
Cleaned, finally prepared yittrium oxide pelletizing and mixing granulation powder；
2nd, yttrium blank forming
Yittrium oxide pelletizing obtained in step one is poured into mould, is molded using one-way shaft pressure mode, briquetting pressure is
20~26MPa, suppresses circular yittrium oxide green compact；
Then mixing granulation powder obtained in step one is poured into mould, is molded using one-way shaft pressure mode, briquetting pressure
It is 20~26MPa, suppresses circular mixed powder green compact,
Yittrium oxide green compact are placed on bottom, mixed powder green compact are placed on yittrium oxide green compact, the two center alignment overlays mould
In tool, mixed powder green compact upper surface covering yittrium oxide pelletizing, the quality of yittrium oxide pelletizing is bottom oxide yttrium green compact
115%~130%, then cold isostatic compaction is carried out after secondary axes are molded, cold to wait pressure be 100~120MPa；
3rd, sinter
After base substrate takes out, it is sintered using gas pressure sintering stove, sintering temperature is 1700~1750 DEG C, sintered heat insulating time 2
~4h, sintering overall process is protected using argon gas atmosphere, that is, obtain the yttrium with high-heat resistance shock resistant；
The 75%~90% of a diameter of yittrium oxide green compact of mixed powder green compact in step 2.
2. the preparation method of a kind of yttrium with high-heat resistance shock resistant according to claim 1, it is characterised in that
Yttrium oxide powder and the mass ratio of deionized water are 1~2 in step one b:1, ammonium citrate for yittrium oxide stock quality 2%~
4%, gum arabic is the 2%~4% of yittrium oxide stock quality.
3. the preparation method of a kind of yttrium with high-heat resistance shock resistant according to claim 1, it is characterised in that
Mixed powder and the mass ratio of deionized water are 1~2 in step one c:1, ammonium citrate is the 2%~4% of mixed slurry quality,
Gum arabic is the 2%~4% of mixed slurry quality.
4. the preparation method of a kind of yttrium with high-heat resistance shock resistant according to claim 1, it is characterised in that
Cleaning method in step one e is specially 10~15min of deionized water rinsing.
5. the preparation method of a kind of yttrium with high-heat resistance shock resistant according to claim 1, it is characterised in that
Mechanical milling process uses zirconium oxide balls in step one, and ratio of grinding media to material is 2~3:1, rotational speed of ball-mill is set as 600~900r/min.
6. the preparation method of a kind of yttrium with high-heat resistance shock resistant according to claim 1, it is characterised in that
Gum arabic described in step one c be by the advance heating for dissolving of the gum arabic of solid in deionized water, be configured to matter
Amount concentration is 40% colloidal sol.
7. the preparation method of a kind of yttrium with high-heat resistance shock resistant according to claim 1, it is characterised in that
By the way of burning is buried, it is 100~150 μm to bury burning diameter of particle to sintering in step 3, and burying burning powder need to forge before in 1300 DEG C
1h is burnt, and is sieved.
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