CN100506747C - Method for preparing yttrium oxide transparent ceramic substrate and film-rolling forming machine - Google Patents
Method for preparing yttrium oxide transparent ceramic substrate and film-rolling forming machine Download PDFInfo
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- CN100506747C CN100506747C CNB2005100441058A CN200510044105A CN100506747C CN 100506747 C CN100506747 C CN 100506747C CN B2005100441058 A CNB2005100441058 A CN B2005100441058A CN 200510044105 A CN200510044105 A CN 200510044105A CN 100506747 C CN100506747 C CN 100506747C
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Abstract
The invention provides a method and a roll forming machine for manufacturing yttria transparent ceramic substrate chips, the processes show as follow: Sythensizing the yttria ceramic slurry, vacuumizing, forming, demoulding, drying and sintering. The composition and weight ratio of yttria ceramic slurry show as follow: composite yttria ceramic powders 30-90wt%, organic solvents 9.5-45wt%, dispersants 0-15wt%, PH adjustment agent 0-5wt%, initiator 0.5-5wt% and catalyst 0-5wt%, injecting the vacuumized yttria ceramic slurry into the roll forming machine to be rolled and solidified in the forming process. There are two horizontal forming belts supported by the two drive wheels in the shell of roll forming machine, a gap between the two belts is located on the lower belt, there is a heater between the two driving wheels, a hopper is installed on the shell, a material discharger locates at the end point of the gap between the two belts.
Description
Affiliated technical field
The present invention relates to a kind of method for preparing yttrium oxide transparent ceramic substrate and film-rolling forming machine, belong to special cermacis fabricating technology field.
Background technology
Yttrium oxide is a kind of transparent, saturating ripple, high temperature ceramic material, the general forming methods such as slip casting, dry-pressing or flow casting molding that adopt, the size that adopts above-mentioned forming method to prepare its shape of products of yttrium material and goods is subjected to certain limitation, as: adopt slip casting, dry-pressing formed, because blank strength is low, the suitable goods that molding thickness (greater than 2mm) is thicker, area is less, and the inner density gradient that produces of base substrate reduce the microstructure of products homogeneity; Adopt flow casting molding can prepare the flaky pottery goods of thin (less than 2mm), but in this technology, use organism to make solvent, cost height not only, and environment caused severe contamination, in technology, the solids content of slurry is lower, shrink when goods burn till greatly, yield rate reduces, and is not suitable for producing in enormous quantities.
Summary of the invention
The purpose of this invention is to provide a kind of can overcome above-mentioned defective, easy to operate, with short production cycle, the work workload is little, production efficiency is high, the rate that manufactures a finished product height and measured method for preparing yttrium oxide transparent ceramic substrate of matter and film-rolling forming machine.Its technical scheme is:
A kind of method for preparing yttrium oxide transparent ceramic substrate, technical process be followed successively by the yttrium slurry preparation, vacuum-treat, moulding, drying, burn till, it is characterized in that: the component of yttrium slurry and weight proportion are: yttrium powder 30-90wt%, organic solution 9.5-45wt%, dispersion agent 0-15wt%, pH value are adjusted agent 0-5wt%, initiator 0.5-5wt% and are mixed, molding procedure is that the yttrium slurry after the vacuum-treat is injected film-rolling forming machine, rolling coagulation forming.
Described method for preparing yttrium oxide transparent ceramic substrate, the component of yttrium powder and weight proportion are: granularity is the yttrium powder 95-100wt% of 50-500nm, and granularity is the additive 0-5wt% of 50-500nm.
Described method for preparing yttrium oxide transparent ceramic substrate, additive is a kind of in Thorotrast, lanthanum trioxide, the lithium fluoride or wherein several, when additive is above-mentioned several compound tense, its component and weight proportion are: Thorotrast 1-59wt%, lanthanum trioxide 40-50wt%, lithium fluoride 1-49wt%.
Described method for preparing yttrium oxide transparent ceramic substrate, the component of organic solution and weight proportion are organic monomer 1-70wt%, distilled water 30-99wt%, and wherein organic monomer is by N, N-methylene radical acrylamide and acrylamide are that the mixed of 1:1-99 is made according to weight ratio.
It is the polyacrylic acid ammonium solution of 20-60wt% that described method for preparing yttrium oxide transparent ceramic substrate, dispersion agent adopt concentration, and pH value is adjusted agent and adopted one or more of ammoniacal liquor, lactic acid, hydrochloric acid, pH value span of control 9~11.
Described method for preparing yttrium oxide transparent ceramic substrate, it is the ammonium persulfate solution of 1-5wt% that initiator adopts concentration.
Described method for preparing yttrium oxide transparent ceramic substrate, primary oxidation yttrium ceramic size vacuum-treat to the vacuum tightness that will not comprise initiator in the vacuum-treat operation reaches-do not have bubble to overflow among the 0.1Mpa, slurry till, adding initiator final vacuum fully stirs and makes the yttrium slurry, and the time was controlled in 3 minutes.
Described method for preparing yttrium oxide transparent ceramic substrate, dried base substrate burn till transparent polycrystal in high temperature more than 1100-2000 ℃ in oxyhydrogen flame, perhaps at 1100~1800 ℃ and 0~100MPa vacuum under pressure hot pressed sintering.
For realizing goal of the invention, the rolling formation equipment that this preparation method is used, be provided with upper and lower two groups of levels in the casing and hang over formed strip on the power wheel, the formed strip that is positioned at the below is than the moulding belt length that is positioned at the top, between adjacent two formed strip certain clearance is arranged, casing is provided with between upper and lower two groups of power wheels all heating element, be provided with a plurality of supporting-point roller in the inboard that is positioned at adjacent formed strip, the both sides of formed strip are provided with baffle plate below being positioned in pressing close to adjacent two formed strip, hopper is installed on the casing, and its discharge end is positioned at the front end of adjacent two formed strip to rolling.
Its principle of work is: the slurry after the vacuum-treat is poured in the hopper, fall on the formed strip that is positioned at the below by discharge port, and be positioned at the front end of adjacent two formed strip to rolling, along with the transmission of the rotation of power wheel, formed strip enters in the gap between adjacent two formed strip, by adjacent two formed strip to rolling into sheet, a plurality of supporting-point roller that the formed strip inboard is provided be for guarantee adjacent two formed strip to roll compacting power evenly, the baffle plate that is provided with of formed strip both sides is in order to prevent leaking outside of slurry.To rolling into flaky ceramic matrix coagulation forming, form by a firing after demoulding, the drying.
The present invention compared with prior art adopts organism in-situ polymerization moulding in the slurry, in the slurry each composition when polymerization not occurrence positions change, make the composition and the density uniformity at each position of goods, burn till the uniform microstructure of back goods.Because this method adopts water base moulding, organic content is little, can not exert an influence to environment, be fit to produce in enormous quantities, and the yield rate height, production cost is low, and the yttrium oxide transparent ceramic substrate grain size that makes is evenly suitable, and light transmission and wave are preferable.
Description of drawings
Fig. 1 is the structural representation of the used rolling formation apparatus embodiments of the present invention.
Among the figure: 1, hopper 2, formed strip 3, heating element 4, casing 5, slurry 6, supporting-point roller 7, power wheel 8, baffle plate
Embodiment
Be provided with upper and lower two groups of levels in the casing 4 and hang over formed strip 2 on the power wheel 7, the formed strip 2 that is positioned at the below is longer than the formed strip 2 that is positioned at the top, between adjacent two formed strip 2 certain clearance is arranged, casing 4 is provided with between upper and lower two groups of power wheels 7 all heating element 3, be provided with a plurality of supporting-point roller 6 in the inboard that is positioned at adjacent formed strip 2, the both sides of formed strip 2 are provided with baffle plate 8 below being positioned in pressing close to adjacent two formed strip 2, hopper 1 is installed on the casing 4, and its discharge end is positioned at 2 pairs of front ends that roll of adjacent two formed strip.
Embodiment 1:
Consisting of of yttrium powder: granularity is the yttrium powder 100wt% of 60nm, consisting of of organic solution: organic monomer 5wt%, distilled water 95wt%, wherein organic monomer is N, and N-methylene radical acrylamide 2wt% and acrylamide 98wt% mix; Dispersion agent adopts the polyacrylic acid ammonium solution, and concentration is 30wt%; PH value is adjusted agent and is adopted 40wt% ammoniacal liquor, and pH value is controlled in the scope of 9-11; It is the ammonium persulfate solution of 4wt% that initiator adopts concentration.
Preparation: with above-mentioned organic solution, dispersion agent, pH value is adjusted agent and is made mixed organic solvents according to 89: 10: 1 mixed of weight ratio, again with the yttrium powder with add ballstone after mixed organic solvents mixes according to weight ratio at 80: 20 and grind, make even suspension primary oxidation yttrium ceramic size, vacuum-treat to vacuum tightness reaches-0.1Mpa, till not having bubble to overflow in the slurry, adding initiator 0.01wt% final vacuum more fully stirs, time was controlled in 3 minutes, make the yttrium slurry, this slurry is injected the hopper 1 of rolling formation equipment, fall on the formed strip 2 that is positioned at the below by discharge port, and be positioned at 2 pairs of front ends that roll of adjacent two formed strip, along with the rotation of power wheel 7 and the transmission of formed strip 2, slurry enters in the gap between adjacent two formed strip 2, roll into sheet by 2 pairs of adjacent two formed strip, a plurality of supporting-point roller 6 that formed strip 2 inboards are provided with are in order to guarantee the even of 2 pairs of roll compacting power of adjacent two formed strip, the baffle plate 8 that is provided with of formed strip 2 both sides is in order to prevent leaking outside of slurry, to rolling into flaky ceramic body 90 ℃ of temperature, curing molding under time 10-20 minute the condition, the demoulding then, dry, at last dried base substrate is burnt till in 1700 ℃ temperature range, make yttrium oxide transparent ceramic substrate of the present invention.
Embodiment 2:
Consisting of of yttrium powder: granularity is that yttrium powder and the Thorotrast additive of 60nm made with the mixed of 90:10; Organic solution consist of organic monomer 5wt%, distilled water 95wt%, wherein the composition of organic monomer and proportioning are N, N-methylene radical acrylamide 2wt%, acrylamide 98wt%; Dispersion agent adopts the polyacrylic acid ammonium solution, and concentration is 30wt%; PH value is adjusted agent and is adopted 40wt% ammoniacal liquor, and pH value is controlled in the scope of 9-11; It is the ammonium persulfate solution of 4wt% that initiator adopts concentration.
Preparation: with above-mentioned organic solution, dispersion agent, pH value is adjusted agent and is made mixed organic solvents according to the mixed of weight ratio 89:10:1, then with the yttrium powder with add ballstone after mixed organic solvents mixes according to weight ratio 80:20 and grind, make even suspension primary oxidation yttrium ceramic size, vacuum-treat to vacuum tightness reaches-0.1Mpa, till not having bubble to overflow in the slurry, adding initiator 0.01wt% final vacuum more fully stirs, time was controlled in 3 minutes, make the yttrium slurry, the hopper 1 that this slurry is injected rolling formation equipment rolls into sheet, curing molding, the demoulding then, dry, at last dried base substrate is burnt till in 1700 ℃ temperature range, make yttrium oxide transparent ceramic substrate of the present invention.
Embodiment 3:
Consisting of of yttrium powder: granularity is the yttrium oxide 90wt% of 500nm, lanthanum trioxide additive 10wt%; Consisting of of organic solution: organic monomer 5wt%, distilled water 95wt%, wherein organic monomer consists of N, N-methylene radical acrylamide 5wt%, acrylamide 95wt%; It is the polyacrylic acid ammonium solution of 30wt% that dispersion agent adopts concentration, and concentration is 30wt%; PH value is adjusted agent and is adopted 40wt% ammoniacal liquor, and pH value is controlled in the scope of 9-11; It is the ammonium persulfate solution of 1wt% that initiator adopts concentration.
Preparation: with above-mentioned organic solution, dispersion agent, pH value is adjusted agent and is made mixed organic solvents according to the mixed of weight ratio 89:10:1, then with the yttrium powder with add ballstone after mixed organic solvents mixes according to weight ratio 80:20 and grind, make even suspension primary oxidation yttrium ceramic size, vacuum-treat to vacuum tightness reaches-0.1Mpa, till not having bubble to overflow in the slurry, adding initiator 0.06wt% final vacuum more fully stirs, time was controlled in 3 minutes, make the yttrium slurry, the hopper 1 that this slurry is injected rolling formation equipment rolls into sheet, curing molding, the demoulding then, dry, at last dried base substrate is burnt till in 1700 ℃ temperature range, make yttrium oxide transparent ceramic substrate of the present invention.
Embodiment 4:
Consisting of of yttrium powder: granularity is that yttrium powder and Thorotrast, the lithium fluoride additive of 60nm made with the mixed of 90:6:4; Organic solution consist of organic monomer 5wt%, distilled water 95wt%, wherein the composition of organic monomer and proportioning are N, N-methylene radical acrylamide 2wt%, acrylamide 98wt%; Dispersion agent adopts the polyacrylic acid ammonium solution, and concentration is 30wt%; PH value is controlled in the scope of 9-11, and pH value is adjusted agent and adopted 40wt% ammoniacal liquor; It is the ammonium persulfate solution of 4wt% that initiator adopts concentration.
Preparation: with above-mentioned organic solution, dispersion agent, pH value is adjusted agent according to weight ratio 89:10:: 1 mixed is made mixed organic solvents, then with the yttrium powder with add ballstone after mixed organic solvents mixes according to weight ratio 40:60 and grind, make even suspension primary oxidation yttrium ceramic size, vacuum-treat to vacuum tightness reaches-0.1Mpa, till not having bubble to overflow in the slurry, adding initiator 0.01wt% final vacuum more fully stirs, time was controlled in 3 minutes, make the yttrium slurry, the hopper 1 that this slurry is injected rolling formation equipment rolls into sheet, curing molding, the demoulding then, dry, at last dried base substrate is burnt till in 1700 ℃ temperature range, make yttrium oxide transparent ceramic substrate of the present invention.
The purity of used proportion material is among the embodiment 1~4: yttrium oxide, Thorotrast, lanthanum trioxide and fluoridize the reason purity be 99.999%, other is analytical pure.
Through check, the technical indicator of the product that makes is: specific inductivity is 12~14, and the transparency is good, 80% the straight line transmitance of still having an appointment in the far infrared region.
Claims (9)
1, a kind of method for preparing yttrium oxide transparent ceramic substrate, technical process be followed successively by the yttrium slurry preparation, vacuum-treat, moulding, the demoulding, drying, burn till, it is characterized in that: the component of yttrium slurry and weight proportion are: yttrium powder 30-90wt%, organic solution 9.5-45wt%, dispersion agent 0-15wt%, pH value are adjusted agent 0-5wt%, initiator 0.5-5wt% and are mixed, molding procedure is that the yttrium slurry after the vacuum-treat is injected film-rolling forming machine, rolling coagulation forming.
2, method for preparing yttrium oxide transparent ceramic substrate as claimed in claim 1, it is characterized in that: the component of yttrium powder and weight proportion are: granularity is the yttrium powder 80-100wt% of 50-500nm, and granularity is the additive 0-20wt% of 50-500nm.
3, method for preparing yttrium oxide transparent ceramic substrate as claimed in claim 2, it is characterized in that: additive is a kind of in Thorotrast, lanthanum trioxide, the lithium fluoride or wherein several, when additive is above-mentioned several compound tense, its component and weight proportion are: Thorotrast 1-59wt%, lanthanum trioxide 40-50wt%, lithium fluoride 1-49wt%.
4, method for preparing yttrium oxide transparent ceramic substrate as claimed in claim 1, it is characterized in that: the component of organic solution and weight proportion are organic monomer 1-70wt%, distilled water 30-99wt%, wherein organic monomer is by N, N-methylene radical acrylamide and acrylamide are that the mixed of 1:1-99 is made according to weight ratio.
5, method for preparing yttrium oxide transparent ceramic substrate as claimed in claim 1, it is characterized in that: it is the polyacrylic acid ammonium solution of 20-60wt% that dispersion agent adopts concentration, pH value is adjusted agent and is adopted one or more of ammoniacal liquor, lactic acid, hydrochloric acid, pH value span of control 9~11.
6, method for preparing yttrium oxide transparent ceramic substrate as claimed in claim 1 is characterized in that: it is the ammonium persulfate solution of 1-5wt% that initiator adopts concentration.
7, method for preparing yttrium oxide transparent ceramic substrate as claimed in claim 1, it is characterized in that: primary oxidation yttrium ceramic size vacuum-treat to the vacuum tightness that will not comprise initiator in the vacuum-treat operation reaches-do not have bubble to overflow among the 0.1Mpa, slurry till, adding initiator final vacuum fully stirs and makes the yttrium slurry, and the time was controlled in 3 minutes.
8, method for preparing yttrium oxide transparent ceramic substrate as claimed in claim 1, it is characterized in that: dried base substrate burns till transparent polycrystal in high temperature more than 1100-2000 ℃ in oxyhydrogen flame, perhaps at 1100~1800 ℃ and 0~100MPa vacuum under pressure hot pressed sintering.
9, the rolling formation equipment that the described preparation method of a kind of claim 1 is used, it is characterized in that: comprise casing (4), casing is provided with in (4), following two groups of levels hang over the formed strip (2) on the power wheel (7), the formed strip (2) that is positioned at the below is longer than the formed strip (2) that is positioned at the top, between adjacent two formed strip (2) certain clearance is arranged, casing (4) is last, being provided with between following two groups of power wheels (7) all has heating element (3), be provided with a plurality of supporting-point roller (6) in the inboard that is positioned at adjacent formed strip (2), the both sides that are positioned at below formed strip (2) in pressing close to adjacent two formed strip (2) are provided with baffle plate (8), hopper (1) is installed on the casing (4), and its discharge end is positioned at the front end of adjacent two formed strip (2) to rolling.
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CNB2005100441058A CN100506747C (en) | 2005-07-08 | 2005-07-08 | Method for preparing yttrium oxide transparent ceramic substrate and film-rolling forming machine |
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CNB2005100441058A CN100506747C (en) | 2005-07-08 | 2005-07-08 | Method for preparing yttrium oxide transparent ceramic substrate and film-rolling forming machine |
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CN100506747C true CN100506747C (en) | 2009-07-01 |
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CN101591170B (en) * | 2008-05-30 | 2011-11-30 | 山东理工大学 | Preparation method for boride porous ceramic |
CN102951903A (en) * | 2011-08-19 | 2013-03-06 | 深圳富泰宏精密工业有限公司 | Ceramic body and preparation method thereof, and electronic device adopting the ceramic body |
CN114571580B (en) * | 2022-03-31 | 2023-02-03 | 江苏国盛新材料有限公司 | Film rolling forming machine for small-granularity yttrium oxide substrate and preparation process of film rolling forming machine |
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