CN110183215A - A kind of sintering preparation method of translucent alumina ceramics - Google Patents
A kind of sintering preparation method of translucent alumina ceramics Download PDFInfo
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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Abstract
The invention discloses a kind of sintering preparation method of translucent alumina ceramics, include the following steps: (1) die cast, (2) pre-sintering processing, the preparation of (3) impregnated porcelain idiosome, (4) drying process, (5) sintering processes.Preparation method integrated artistic of the present invention is simple, and each step collocation is reasonable, easy to promote and utilize, the mechanical characteristic of translucent alumina ceramics obtained, good optical properties, excellent combination property, the great market competitiveness.
Description
Technical field
The present invention relates to a kind of sintering technology fields of ceramics, and in particular to a kind of sintering system of translucent alumina ceramics
Preparation Method.
Background technique
Aluminium oxide ceramics refers to the pottery using aluminium oxide as substrate and using ceramic process preparation with certain translucency
Porcelain.Aluminium oxide ceramics not only has the characteristics such as high temperature resistant, corrosion-resistant, high insulation, the high intensity of ceramics itself, has been also equipped with glass
Optical property and the incomparable advantage such as conductivity of many other materials institute it is low etc., so aluminium oxide ceramics is gradually in extraordinary instrument
Device manufacture, lighting engineering, wireless electron technology, the fields such as optics and high-temperature technology obtain increasingly extensive application.
The birefringence difference of alpha-alumina crystals is small, and the maximum feature of aluminium oxide ceramics is the transparency and to visible light and red
The good permeability of outer light, furthermore aluminium oxide ceramics also has and is electrically insulated, the high advantage of thermal conductivity.Therefore aluminium oxide ceramics exists
High intensity discharge lamps pipe, the application in the fields such as high-temperature infrared detection window are also increasingly wider.
In process of production, high temperature will lead to increasing rapidly for alpha-alumina crystals to aluminium oxide ceramics, this result will lead to
Gas inside ceramics has little time to be discharged and be closed in formation bubble in ceramics, and influences the translucent effect of aluminium oxide ceramics.
It in order to inhibit the generation of bubble in aluminium oxide ceramics, needs to introduce auxiliary agent to inhibit the rapid growth of alumina grain, allows ceramics
Interior gas having time evolution.Now common inhibitor master is containing the oxide for having Mg, Zr, La, Ca plasma.It introduces and inhibits
The Conventional processing methods of agent mainly have ball milling mixing method to be exactly mixed into inhibitor in solid form in the form of the oxide, chemistry
Method is existing mainly co-precipitation or sol-gal process incorporation inhibitor, or directly using the alumina powder etc. for being impregnated with inhibitor.
These traditional process complex process do time long in advance and need to be added colloid or granulation liquid in premix
Equal organic materials, dumping or degreasing again after shaping, but cannot be guaranteed the thorough of dumping or degreasing, this is aluminium oxide ceramics
The predominant gas source of interior bubble.In traditional handicraft, the usage amount of granulation liquid or colloid the 5%-10% of alumina weight it
Between, although these granulation liquids or colloid can carry out 5 times or so reuses, this substance has production environment certain
Pollution, simultaneously as can not be thoroughly removed in the intracorporal colloid of base or granulation liquid, the remaining part when carrying out high temperature sintering
Colloid or granulation liquid, which generate carbon black there are also part in addition to generating carbon dioxide or water vapour, influences the light transmittance of aluminium oxide ceramics.
Different improvement processing have been carried out to this prior art, such as application No. is: CN201210189159.3 discloses one
The method that kind passes through infiltration body preparation aluminium oxide ceramics, by the way that molding blank pre-burning to be placed in inhibitor deionized water solution
To realize the introducing of inhibitor, above-mentioned bad phenomenon is improved, but bubble still can not preferably be discharged during sintering processes,
The mechanics and optical property for leading to material still have the space that is greatly improved.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of sintering preparation side of translucent alumina ceramics is provided
Method.
The present invention is achieved by the following technical solutions:
A kind of sintering preparation method of translucent alumina ceramics, includes the following steps:
(1) alumina powder and aluminium nitride powder are mixed, then through die cast, it is spare that ceramic idiosome is made；
(2) ceramic idiosome made from step (1) is put into microwave agglomerating furnace and carries out pre-sintering processing, control the temperature of sintering
For 750 ~ 780 DEG C, duration control be 2 ~ 4h, take out after the completion pre-sintered ceramic idiosome is spare；
(3) pre-sintered ceramic idiosome made from step (2) is put into alternating temperature case and carries out cooling processing, be down to 50 to its temperature
It is taken out after ~ 60 DEG C, is immersed in inhibitor solution infiltration immediately after and handles, when a length of 4 ~ 7h of control infiltration processing is completed
After take out impregnated porcelain idiosome is spare；
(4) impregnated porcelain idiosome made from step (3) is put into thermostatic drying chamber and is dried, taken out after 15 ~ 20h
It is spare；
(5) the impregnated porcelain idiosome after being dried step (4), which is put into sintering furnace, to be sintered, and sintering is controlled
Temperature is 1400 ~ 1450 DEG C, duration control is 1 ~ 3h, is taken out after the completion up to translucent aluminum oxide ceramic material.
Preferably, when alumina powder and aluminium nitride powder as described in step (1) mix corresponding weight ratio be 25 ~
30:1。
Preferably, the preparation method of the aluminium nitride powder is specifically: by aluminum oxide powder, kaolin, carbon black
Powder is corresponding to carry out uniformly mixed according to 18 ~ 22:6 of weight ratio ~ 8:2 ~ 4, and the magnesia for then adding its gross mass 2 ~ 5% is mixed
It closes uniformly, is then put in neon atmosphere high temperature calcination reaction again and handles 2.5 ~ 3.5h, the temperature for during which controlling high-temperature calcination is
It 1500 ~ 1600 DEG C, is drawn off being put into middle 1.5 ~ 2h of carbonization treatment in the hothouse that temperature is 820 ~ 850 DEG C after the completion again,
After finally taking out cooled to room temperature.
Preferably, die cast time control pressing pressure as described in step (1) is 400 ~ 500MPa.
Preferably, inhibitor solution described in step (3) is the calcium hydroxide aqueous solution of saturation.
Preferably, it is infiltrated described in step (3) and remains that the temperature of inhibitor solution is 55 ~ 65 DEG C when processing.
Preferably, it is 90 ~ 95 DEG C that the temperature in thermostatic drying chamber is controlled when drying process described in step (4).
Preferably, sintering furnace described in step (5) is hydrogen furnace.
The present invention has carried out special improvement to the sintering preparation method of translucent alumina ceramics and has handled, wherein to oxidation
Aluminium nitride powder ingredient is added in aluminium powder, this aluminium nitride powder is one kind using aluminum oxide powder as silicon source, magnesia
For catalyst, kaolin is the composite filled powdered ingredients of skeleton structure, this ingredient is used as enhancing and promotes aluminium oxide ceramics, excellent
Change the purpose for improving processing conditions, the present invention selects to utilize microwave treatment when pre-sintering processing first, and composite modified nitridation
Aluminium powder can promote to promote self-friction effect, conducive to heating from inside to outside, thereby reduce the temperature of pre-sintering, reduce
On the one hand the temperature of processing can reduce processing cost, be on the other hand able to ascend γ-Al2O3Content, so as to reduce gas
The yield of bubble, correspondence can promote the quality of aluminium oxide ceramics, and this γ-Al2O3Second can be formed with aluminium nitride powder
Phase substance, the second phase substance can play the role of obstruction during aluminium oxide crystal boundary migration, so that it is different to reduce aluminium oxide
The crystal grain boundary migration rate often grown up, reduces the size of the crystal grain of abnormal growth, to further improve aluminium oxide pottery
The quality of porcelain.
The present invention has the advantage that compared with prior art
Preparation method integrated artistic of the present invention is simple, and each step collocation is reasonable, easy to promote and utilize, translucent alumina obtained
The mechanical characteristic of ceramics, good optical properties, excellent combination property, the great market competitiveness.
Specific embodiment
Embodiment 1
A kind of sintering preparation method of translucent alumina ceramics, includes the following steps:
(1) alumina powder and aluminium nitride powder are mixed, then through die cast, it is spare that ceramic idiosome is made；
(2) ceramic idiosome made from step (1) is put into microwave agglomerating furnace and carries out pre-sintering processing, control the temperature of sintering
For 750 DEG C, duration control be 2h, take out after the completion pre-sintered ceramic idiosome is spare；
(3) pre-sintered ceramic idiosome made from step (2) is put into alternating temperature case and carries out cooling processing, be down to 50 to its temperature
It is taken out after DEG C, is immersed in inhibitor solution infiltration immediately after and handles, the when a length of 4h of control infiltration processing takes out after the completion
It is spare to obtain impregnated porcelain idiosome；
(4) impregnated porcelain idiosome made from step (3) is put into thermostatic drying chamber and is dried, taken out after 15h standby
With；
(5) the impregnated porcelain idiosome after being dried step (4), which is put into sintering furnace, to be sintered, and sintering is controlled
Temperature is 1400 DEG C, duration control is 1h, is taken out after the completion up to translucent aluminum oxide ceramic material.
Preferably, corresponding weight ratio is 25:1 when alumina powder and aluminium nitride powder as described in step (1) mix.
Preferably, the preparation method of the aluminium nitride powder is specifically: by aluminum oxide powder, kaolin, carbon black
Powder is corresponding to carry out uniformly mixed according to weight ratio 18:6:2, and the magnesia for then adding its gross mass 2% is uniformly mixed, so
It is put in neon atmosphere high temperature calcination reaction processing 2.5h again afterwards, the temperature for during which controlling high-temperature calcination is 1500 DEG C, after the completion
It is drawn off being put into middle carbonization treatment 1.5h in the hothouse that temperature is 820 DEG C again, after finally taking out cooled to room temperature
?.
Preferably, die cast time control pressing pressure as described in step (1) is 400MPa.
Preferably, inhibitor solution described in step (3) is the calcium hydroxide aqueous solution of saturation.
Preferably, it is infiltrated described in step (3) and remains that the temperature of inhibitor solution is 55 DEG C when processing.
Preferably, it is 90 DEG C that the temperature in thermostatic drying chamber is controlled when drying process described in step (4).
Preferably, sintering furnace described in step (5) is hydrogen furnace.
Embodiment 2
A kind of sintering preparation method of translucent alumina ceramics, includes the following steps:
(1) alumina powder and aluminium nitride powder are mixed, then through die cast, it is spare that ceramic idiosome is made；
(2) ceramic idiosome made from step (1) is put into microwave agglomerating furnace and carries out pre-sintering processing, control the temperature of sintering
For 770 DEG C, duration control be 3h, take out after the completion pre-sintered ceramic idiosome is spare；
(3) pre-sintered ceramic idiosome made from step (2) is put into alternating temperature case and carries out cooling processing, be down to 55 to its temperature
It is taken out after DEG C, is immersed in inhibitor solution infiltration immediately after and handles, the when a length of 6h of control infiltration processing takes out after the completion
It is spare to obtain impregnated porcelain idiosome；
(4) impregnated porcelain idiosome made from step (3) is put into thermostatic drying chamber and is dried, taken out after 18h standby
With；
(5) the impregnated porcelain idiosome after being dried step (4), which is put into sintering furnace, to be sintered, and sintering is controlled
Temperature is 1430 DEG C, duration control is 2h, is taken out after the completion up to translucent aluminum oxide ceramic material.
Preferably, corresponding weight ratio is 28:1 when alumina powder and aluminium nitride powder as described in step (1) mix.
Preferably, the preparation method of the aluminium nitride powder is specifically: by aluminum oxide powder, kaolin, carbon black
Powder is corresponding to carry out uniformly mixed according to weight ratio 20:7:3, and the magnesia for then adding its gross mass 4% is uniformly mixed, so
It is put in neon atmosphere high temperature calcination reaction processing 3h again afterwards, the temperature for during which controlling high-temperature calcination is 1550 DEG C, after the completion again
It is drawn off being put into middle carbonization treatment 1.7h in the hothouse that temperature is 840 DEG C, is after finally taking out cooled to room temperature
It can.
Preferably, die cast time control pressing pressure as described in step (1) is 450MPa.
Preferably, inhibitor solution described in step (3) is the calcium hydroxide aqueous solution of saturation.
Preferably, it is infiltrated described in step (3) and remains that the temperature of inhibitor solution is 60 DEG C when processing.
Preferably, it is 93 DEG C that the temperature in thermostatic drying chamber is controlled when drying process described in step (4).
Preferably, sintering furnace described in step (5) is hydrogen furnace.
Embodiment 3
A kind of sintering preparation method of translucent alumina ceramics, includes the following steps:
(1) alumina powder and aluminium nitride powder are mixed, then through die cast, it is spare that ceramic idiosome is made；
(2) ceramic idiosome made from step (1) is put into microwave agglomerating furnace and carries out pre-sintering processing, control the temperature of sintering
For 780 DEG C, duration control be 4h, take out after the completion pre-sintered ceramic idiosome is spare；
(3) pre-sintered ceramic idiosome made from step (2) is put into alternating temperature case and carries out cooling processing, be down to 60 to its temperature
It is taken out after DEG C, is immersed in inhibitor solution infiltration immediately after and handles, the when a length of 7h of control infiltration processing takes out after the completion
It is spare to obtain impregnated porcelain idiosome；
(4) impregnated porcelain idiosome made from step (3) is put into thermostatic drying chamber and is dried, taken out after 20h standby
With；
(5) the impregnated porcelain idiosome after being dried step (4), which is put into sintering furnace, to be sintered, and sintering is controlled
Temperature is 1450 DEG C, duration control is 3h, is taken out after the completion up to translucent aluminum oxide ceramic material.
Preferably, corresponding weight ratio is 30:1 when alumina powder and aluminium nitride powder as described in step (1) mix.
Preferably, the preparation method of the aluminium nitride powder is specifically: by aluminum oxide powder, kaolin, carbon black
Powder is corresponding to carry out uniformly mixed according to weight ratio 22:8:4, and the magnesia for then adding its gross mass 5% is uniformly mixed, so
It is put in neon atmosphere high temperature calcination reaction processing 3.5h again afterwards, the temperature for during which controlling high-temperature calcination is 1600 DEG C, after the completion
It is drawn off being put into middle carbonization treatment 2h in the hothouse that temperature is 850 DEG C again, is after finally taking out cooled to room temperature
It can.
Preferably, die cast time control pressing pressure as described in step (1) is 500MPa.
Preferably, inhibitor solution described in step (3) is the calcium hydroxide aqueous solution of saturation.
Preferably, it is infiltrated described in step (3) and remains that the temperature of inhibitor solution is 65 DEG C when processing.
Preferably, it is 95 DEG C that the temperature in thermostatic drying chamber is controlled when drying process described in step (4).
Preferably, sintering furnace described in step (5) is hydrogen furnace.
Comparative experiments example 1
A kind of sintering preparation method of translucent alumina ceramics, includes the following steps:
(1) alumina powder and aluminium nitride powder are mixed, then through die cast, it is spare that ceramic idiosome is made；
(2) ceramic idiosome made from step (1) is put into microwave agglomerating furnace and carries out pre-sintering processing, control the temperature of sintering
For 770 DEG C, duration control be 3h, take out after the completion pre-sintered ceramic idiosome is spare；
(3) pre-sintered ceramic idiosome made from step (2) is put into alternating temperature case and carries out cooling processing, be down to 55 to its temperature
It is taken out after DEG C, is immersed in inhibitor solution infiltration immediately after and handles, the when a length of 6h of control infiltration processing takes out after the completion
It is spare to obtain impregnated porcelain idiosome；
(4) impregnated porcelain idiosome made from step (3) is put into thermostatic drying chamber and is dried, taken out after 18h standby
With；
(5) the impregnated porcelain idiosome after being dried step (4), which is put into sintering furnace, to be sintered, and sintering is controlled
Temperature is 1430 DEG C, duration control is 2h, is taken out after the completion up to translucent aluminum oxide ceramic material.
Preferably, the preparation method of the aluminium nitride powder is specifically: aluminum oxide powder, hydrocarbon black powder is corresponding
Carried out according to weight ratio 20:3 it is uniformly mixed, then add its gross mass 4% magnesia be uniformly mixed, be then put in neon again
Gas atmosphere high temperature calcination reaction handles 3h, and the temperature for during which controlling high-temperature calcination is 1550 DEG C, is drawn off putting after the completion again
Enter middle carbonization treatment 1.7h in the hothouse for being 840 DEG C to temperature, after finally taking out cooled to room temperature.
Compared with Example 2, difference is only that in the preparation of aluminium nitride powder this comparative experiments example 1, eliminates kaolinite
The addition and use of soil, method and step in addition to this are all the same.Kaolinic addition using effect is characterized with this.
Comparative experiments example 2
A kind of sintering preparation method of translucent alumina ceramics, includes the following steps:
(1) it is spare that ceramic idiosome is made through die cast in alumina powder；
(2) ceramic idiosome made from step (1) is put into microwave agglomerating furnace and carries out pre-sintering processing, control the temperature of sintering
For 770 DEG C, duration control be 3h, take out after the completion pre-sintered ceramic idiosome is spare；
(3) pre-sintered ceramic idiosome made from step (2) is put into alternating temperature case and carries out cooling processing, be down to 55 to its temperature
It is taken out after DEG C, is immersed in inhibitor solution infiltration immediately after and handles, the when a length of 6h of control infiltration processing takes out after the completion
It is spare to obtain impregnated porcelain idiosome；
(4) impregnated porcelain idiosome made from step (3) is put into thermostatic drying chamber and is dried, taken out after 18h standby
With；
(5) the impregnated porcelain idiosome after being dried step (4), which is put into sintering furnace, to be sintered, and sintering is controlled
Temperature is 1430 DEG C, duration control is 2h, is taken out after the completion up to translucent aluminum oxide ceramic material.
Compared with Example 2, difference is only that the addition for eliminating aluminium nitride powder uses to this comparative experiments example 2, removes this
Outer method and step is all the same.The addition using effect of aluminium nitride powder is characterized with this.
Comparative experiments example 3
Application No. is: a kind of method by infiltrating body preparation aluminium oxide ceramics disclosed in CN201210189159.3.
In order to compare effect of the present invention, to above-described embodiment 2, comparative experiments example 1, comparative experiments example 2, comparative experiments example 3
Corresponding aluminium oxide ceramics obtained is tested for the property, and specific correlation data is as shown in table 1 below:
Table 1
Note: each performance parameter described in upper table 1 is measured according to this field professional standard.
The synthesis that the method for the present invention can be obviously improved translucent alumina ceramics it can be seen from upper table 1 uses product
Matter, great application value.
Claims (8)
1. a kind of sintering preparation method of translucent alumina ceramics, which comprises the steps of:
(1) alumina powder and aluminium nitride powder are mixed, then through die cast, it is spare that ceramic idiosome is made；
(2) ceramic idiosome made from step (1) is put into microwave agglomerating furnace and carries out pre-sintering processing, control the temperature of sintering
For 750 ~ 780 DEG C, duration control be 2 ~ 4h, take out after the completion pre-sintered ceramic idiosome is spare；
(3) pre-sintered ceramic idiosome made from step (2) is put into alternating temperature case and carries out cooling processing, be down to 50 to its temperature
It is taken out after ~ 60 DEG C, is immersed in inhibitor solution infiltration immediately after and handles, when a length of 4 ~ 7h of control infiltration processing is completed
After take out impregnated porcelain idiosome is spare；
(4) impregnated porcelain idiosome made from step (3) is put into thermostatic drying chamber and is dried, taken out after 15 ~ 20h
It is spare；
(5) the impregnated porcelain idiosome after being dried step (4), which is put into sintering furnace, to be sintered, and sintering is controlled
Temperature is 1400 ~ 1450 DEG C, duration control is 1 ~ 3h, is taken out after the completion up to translucent aluminum oxide ceramic material.
2. a kind of sintering preparation method of translucent alumina ceramics according to claim 1, which is characterized in that step
(1) alumina powder described in and aluminium nitride powder when mixing corresponding weight ratio be 25 ~ 30:1.
3. a kind of sintering preparation method of translucent alumina ceramics according to claim 2, which is characterized in that described
The preparation method of aluminium nitride powder is specifically: by aluminum oxide powder, kaolin, hydrocarbon black powder it is corresponding according to weight ratio 18 ~
22:6 ~ 8:2 ~ 4 carry out it is uniformly mixed, then add its gross mass 2 ~ 5% magnesia be uniformly mixed, be then put in neon again
Atmosphere high temperature calcination reaction handles 2.5 ~ 3.5h, and the temperature for during which controlling high-temperature calcination is 1500 ~ 1600 DEG C, again will after the completion
It, which takes out, is put into middle 1.5 ~ 2h of carbonization treatment in the hothouse that temperature is 820 ~ 850 DEG C, finally takes out cooled to room temperature
Afterwards.
4. a kind of sintering preparation method of translucent alumina ceramics according to claim 1, which is characterized in that step
(1) the die cast time control pressing pressure described in is 400 ~ 500MPa.
5. a kind of sintering preparation method of translucent alumina ceramics according to claim 1, which is characterized in that step
(3) inhibitor solution described in is the calcium hydroxide aqueous solution of saturation.
6. a kind of sintering preparation method of translucent alumina ceramics according to claim 1, which is characterized in that step
(3) infiltration described in remains that the temperature of inhibitor solution is 55 ~ 65 DEG C when handling.
7. a kind of sintering preparation method of translucent alumina ceramics according to claim 1, which is characterized in that step
(4) temperature when drying process described in control thermostatic drying chamber is 90 ~ 95 DEG C.
8. a kind of sintering preparation method of translucent alumina ceramics according to claim 1, which is characterized in that step
(5) sintering furnace described in is hydrogen furnace.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111153688A (en) * | 2020-02-17 | 2020-05-15 | 中国工程物理研究院材料研究所 | Preparation method of high-strength semitransparent alumina ceramic |
| CN111730732A (en) * | 2020-06-23 | 2020-10-02 | 姜家吉 | Process for improving advanced ceramic sintering yield |
-
2019
- 2019-05-28 CN CN201910449711.XA patent/CN110183215A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111153688A (en) * | 2020-02-17 | 2020-05-15 | 中国工程物理研究院材料研究所 | Preparation method of high-strength semitransparent alumina ceramic |
| CN111730732A (en) * | 2020-06-23 | 2020-10-02 | 姜家吉 | Process for improving advanced ceramic sintering yield |
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Application publication date: 20190830 |