CN110015892A - A kind of quartz-ceramics densification maceration extract and preparation method thereof, application method - Google Patents
A kind of quartz-ceramics densification maceration extract and preparation method thereof, application method Download PDFInfo
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- CN110015892A CN110015892A CN201910303125.4A CN201910303125A CN110015892A CN 110015892 A CN110015892 A CN 110015892A CN 201910303125 A CN201910303125 A CN 201910303125A CN 110015892 A CN110015892 A CN 110015892A
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Abstract
The present invention relates to a kind of quartz-ceramics densification maceration extracts and preparation method thereof, application method, the quartz-ceramics densification maceration extract is made by following methods: being weighed high containing hydrogen silicone oil, ethyl orthosilicate respectively and is stirred, then chloroplatinic acid is added to stir under heating condition, it stands after stirring and is precipitated to bottom, supernatant is taken to densify maceration extract up to quartz-ceramics.Under chloroplatinic acid effect, the macromolecular compound of crosslinking is converted to small molecule compound, reduces dipping fluid viscosity, maceration extract increases the bulk density of quartz-ceramics to the duct of quartz-ceramics, the filling rate in gap when can be improved dipping.
Description
Technical field
The present invention relates to photocuring 3D printing quartz-ceramics densification field more particularly to a kind of densification leachings of quartz-ceramics
Stain liquid and preparation method thereof, application method.
Background technique
Ceramic 3D printing technique includes photocuring 3D printing, inkjet printing, fusion sediment, selective laser sintering, lamination reality
Body manufacture etc., ceramic photocuring 3D printing is that wherein formed precision is highest, and this method is using ultraviolet light to containing photosensitive tree
The ceramic slurry of rouge is scanned solidification, and successively accumulation forms the process of ceramic.
According to ceramic slurry type classification used, photocuring 3D printing can be divided into water base and two class of resin base, with resin base
Quartzy slurry is compared, and water base quartz slurry takes water as a solvent, ingredient safety and environmental protection, from the angle of environmental protection, water base stone
The development of English slurry is advocated energetically.
For the quartzy ceramic research of water base photocuring 3D printing by the Michelle of Michigan university, the U.S.
L.Griffith and John W.Halloran is proposed first.The country, Xi'an Communications University Zhou Wei are called together etc. to water base quartz-ceramics
Series of studies has been done in photocuring 3D printing: including quartz-ceramics powder particle size, dispersant and dosage, scanning speed, monomer
Concentration and aqueous solvent preferably etc., research obtains optimal quartz-ceramics bulk density 1.65g/cm3, lead to quartzy pottery
Porcelain mechanical property is poor, experiment shows to reach certain application requests (bending strength >=50MPa), then quartz-ceramics
Bulk density need to be greater than 1.90g/cm3, it is therefore necessary to subsequent densification is carried out to the quartz-ceramics of photocuring 3D printing preparation,
To improve bulk density and bending strength to adapt to practical application.
Summary of the invention
In order to solve the above-mentioned technical problem, the purpose of the present invention is to provide a kind of quartz-ceramics densification maceration extract and its
Preparation method, application method.
According to an aspect of the invention, there is provided a kind of preparation method of quartz-ceramics densification maceration extract, by following
Method is made:
Step 1: weighing high containing hydrogen silicone oil, ethyl orthosilicate and be stirred to obtain mixed liquor；
Step 2: chloroplatinic acid being added in Xiang Suoshu mixed liquor and is stirred under heating condition, is stood after stirring
It is precipitated to bottom；
Step 3: step 2 gained supernatant being taken to densify maceration extract up to quartz-ceramics.
It further, further include that magnesia or calcium oxide is added into the mixed liquor in step 1 or step 2.
Further, in step 1 by weight, 10~30 parts of the high containing hydrogen silicone oil is weighed, ethyl orthosilicate is not more than 2
Part, 0.01~0.1 part of chloroplatinic acid.
Further, in step 1 by weight, 20 parts of the high containing hydrogen silicone oil, 0.5 part of ethyl orthosilicate, chlorine platinum are weighed
0.08 part of acid.
Further, step 2 persistently stirs 2-10 hours in a heated condition, and heating temperature is 30~50 DEG C.
Further, the viscosity of quartz-ceramics densification maceration extract is 10-20mPa.s.
According to another aspect of the present invention, a kind of quartz-ceramics densification maceration extract is provided, by above-mentioned any one
The preparation method of the quartz-ceramics densification maceration extract is made.
A kind of quartz-ceramics densification maceration extract application method is provided according to another aspect of the present invention, including following
Step:
S1, the processing of quartz-ceramics dumping
Prefabricated 3D printing quartz-ceramics biscuit is kept the temperature 1-4 hours at 400~600 DEG C；
S2, dipping and curing process
3D printing quartz-ceramics biscuit is placed in the quartz-ceramics densification maceration extract under vacuum condition and impregnates 10-
50min, then at 60~80 DEG C baking and curing to constant weight；
S3, densification
By the 3D printing quartz-ceramics green body after curing process 1000~1500 DEG C heat treatment 0.1-2 hours, caused
The quartz ceramic of densification.
Further, the quartz ceramic bulk density of the densification is not less than 1.9g/cm3。
Further, vacuum degree≤- 0.08MPa of the vacuum condition.
Compared with prior art, the invention has the following advantages:
1, the preparation method of the present invention exemplary quartz-ceramics densification maceration extract, under chloroplatinic acid effect, crosslinking it is big
Molecular compound is converted to small molecule compound, reduces dipping fluid viscosity, maceration extract is to quartz-ceramics when can be improved dipping
Duct, gap filling rate, increase the bulk density of quartz-ceramics.
2, the exemplary quartz-ceramics of the present invention densify maceration extract, hole of the maceration extract to quartz-ceramics when can be improved dipping
Road, gap filling rate, increase the bulk density of quartz-ceramics.
3, the exemplary a kind of quartz-ceramics densification maceration extract application method of the present invention, by the molding quartz-ceramics of 3D printing
Biscuit keeps the temperature 2 hours at 400~600 DEG C, and organic principle in quartz-ceramics biscuit is discharged, it is intergranular can to open green body
Channel not only ensure that the unsticking of green body, but also provide dipping passage for subsequent dipping process, and maceration extract is realized in densified processing
Middle silicon atom is to SiO2Conversion be completed at the same time the sintering process of quartz-ceramics green body, maceration extract is to quartz when can be improved dipping
The filling rate in ceramic duct, gap, increases the bulk density of quartz-ceramics, increases quartz-ceramics bending strength.
Detailed description of the invention
Fig. 1 is quartz-ceramics element scanning electron microscope (SEM) photograph before dumping is handled.
Fig. 2 is quartz-ceramics element scanning electron microscope (SEM) photograph after dumping processing.
Fig. 3 is quartz-ceramics green body scanning electron microscope (SEM) photograph before impregnation.
Fig. 4 is quartz ceramic scanning electron microscope (SEM) photograph after densification.
Specific embodiment
In order to be better understood by technical solution of the present invention, combined with specific embodiments below, Figure of description is to the present invention
It is described further.
Embodiment 1:
A kind of preparation method of quartz-ceramics densification maceration extract of the present embodiment, is made by following methods:
Step 1: weighing high containing hydrogen silicone oil, ethyl orthosilicate and be stirred to obtain mixed liquor；The height is weighed by weight
20 parts of containing hydrogen silicone oil, ethyl orthosilicate are not more than 0.5 part, are stirred to obtain mixed liquor.
Step 2: being added 0.08 part of chloroplatinic acid in Xiang Suoshu mixed liquor and persistently stirred under heating condition 4 hours or more, added
Hot temperature is 40 DEG C, stands after stirring to bottom and precipitates；Ethyl orthosilicate issues raw hydrolysis in chloroplatinic acid effect and turns
Turn to SiO2, high containing hydrogen silicone oil occurs dehydrogenation reaction and to precipitate under chloroplatinic acid effect, and macromolecular compound is converted into small
Molecular compound can reduce dipping fluid viscosity, increase the mobility of maceration extract, be conducive to improve maceration extract to quartz-ceramics
The filling rate in duct, gap；By taking chloroplatinic acid as an example: C6H18OSi2+H2Cl6Pt (chloroplatinic acid) → C6H16OSi2+ 2HCl+Pt (platinum black
Precipitating), bottom is stood after stirring will appear black precipitate.
Step 3: step 2 gained supernatant being taken to densify maceration extract, viscosity 10mPa.s up to quartz-ceramics.
Above-mentioned quartz-ceramics densify maceration extract application method, comprising the following steps:
S1, the processing of quartz-ceramics dumping
The heating rate that 0.1-2 DEG C/min is arranged is warming up to 400 DEG C, by prefabricated 3D printing quartz-ceramics biscuit 400
2 hours are kept the temperature at DEG C, as shown in Figure 1 and Figure 2, organic principle in quartz-ceramics biscuit is discharged during quartz-ceramics dumping, is beaten
The intergranular channel of cogging body not only ensure that the unsticking of green body, but also provide dipping passage for subsequent dipping process.
S2, dipping and curing process
3D printing quartz-ceramics biscuit after dumping is placed in the quartz-ceramics densification maceration extract under vacuum condition
Impregnate 10-50min, vacuum degree≤- 0.08MPa of the vacuum condition, then at 60~80 DEG C baking and curing to constant weight；It can
Maceration extract is conducive to the bulk density for increasing quartz-ceramics to the duct of quartz-ceramics, the filling rate in gap when improving dipping.
S3, densification
The heating rate that 0.1-4 DEG C/min is arranged is warming up to 1250 DEG C, by the 3D printing quartz-ceramics base after curing process
Body is heat-treated 1 hour at 1250 DEG C, and high containing hydrogen silicone oil reacts the C generated with chloroplatinic acid6H16OSi2It is converted into densification stage
SiO2, the quartz ceramic densified, densified processing realizes in maceration extract silicon atom to SiO2Conversion simultaneously it is complete
At the sintering process of quartz-ceramics green body.As shown in Figure 3, Figure 4, since the maceration extract macromolecular compound of preparation is converted into small point
Sub- compound reduces viscosity, and quartz-ceramics dumping process opens the intergranular channel of green body, and maceration extract will be stitched
Gap is sufficient filling with, and increases the bulk density of quartz-ceramics, and the quartz ceramic bulk density of densification described in the present embodiment is
1.95g/cm3, bending strength is greater than 50MPa.Optionally, the preparation of maceration extract, to institute in step 1 or step 2
It states and magnesia or 0.5 part of calcium oxide is added in mixed liquor, to reduce the densification temperature of quartz-ceramics green body, prevent at high warm
Green body cracks during reason.
Embodiment 2:
A kind of preparation method of quartz-ceramics densification maceration extract of the present embodiment, is made: by weight by following methods
10 parts of the high containing hydrogen silicone oil, ethyl orthosilicate are weighed no more than 0.1 part, is stirred, 0.01 part of chloroplatinic acid, oxygen is then added
Change magnesium or 1.4 parts of calcium oxide are persistently stirred 5 hours under heating condition, heating temperature is 50 DEG C；Ethyl orthosilicate is in chloroplatinic acid
Effect issues raw hydrolysis and is converted into SiO2, high containing hydrogen silicone oil occurs dehydrogenation reaction and to precipitate under chloroplatinic acid effect,
Macromolecular compound is converted into small molecule compound, reduces dipping fluid viscosity, by taking chloroplatinic acid as an example: C6H18OSi2+H2Cl6Pt
(chloroplatinic acid) → C6H16OSi2+ 2HCl+Pt (platinum black), bottom is stood after stirring will appear black precipitate, take supernatant up to stone
English ceramic densifying maceration extract, viscosity 14mPa.s.
Above-mentioned quartz-ceramics densify maceration extract application method, comprising the following steps:
S1, the processing of quartz-ceramics dumping
The heating rate that 0.1-2 DEG C/min is arranged is warming up to 400 DEG C, by prefabricated 3D printing quartz-ceramics biscuit 400
Lower heat preservation 4 hours, organic principle in quartz-ceramics biscuit is discharged in the process for quartz-ceramics dumping, and it is intergranular logical to open green body
Road not only ensure that the unsticking of green body, but also provide dipping passage for subsequent dipping process.
S2, dipping and curing process
3D printing quartz-ceramics biscuit is placed in the quartz-ceramics densification maceration extract under vacuum condition and is impregnated
10min, vacuum degree≤- 0.08MPa of the vacuum condition, then baking and curing is to constant weight at 60 DEG C, and maceration extract will when dipping
The duct of quartz-ceramics, gap filling.
S3, densification
The heating rate that 0.1-4 DEG C/min is arranged is warming up to 1000 DEG C, by the 3D printing quartz-ceramics base after curing process
Body is heat-treated 2 hours at 1000 DEG C, the quartz ceramic densified, and silicon atom in maceration extract is realized in densified processing
To SiO2Conversion be completed at the same time the sintering process of quartz-ceramics green body, the quartz ceramic body of densification described in the present embodiment
Product density is 1.93g/cm3, bending strength is greater than 50MPa.
Embodiment 3:
A kind of preparation method of quartz-ceramics densification maceration extract of the present embodiment, is made: by weight by following methods
Weigh 30 parts of the high containing hydrogen silicone oil, ethyl orthosilicate is stirred no more than 2 parts and magnesia or 1 part of calcium oxide, then plus
Enter 0.1 part of chloroplatinic acid persistently to stir under heating condition 10 hours, heating temperature is 30 DEG C；Ethyl orthosilicate is acted in chloroplatinic acid
It issues raw hydrolysis and is converted into SiO2, high containing hydrogen silicone oil occurs dehydrogenation reaction and is precipitated under chloroplatinic acid effect, big to divide
Sub- compound is converted into small molecule compound, reduces dipping fluid viscosity, by taking chloroplatinic acid as an example: C6H18OSi2+H2Cl6Pt (chlorine platinum
Acid) → C6H16OSi2+ 2HCl+Pt (platinum black), bottom is stood after stirring will appear black precipitate, take supernatant up to quartz-ceramics
Densify maceration extract, viscosity 10mPa.s.
Above-mentioned quartz-ceramics densify maceration extract application method, comprising the following steps:
S1, the processing of quartz-ceramics dumping
The heating rate that 0.1-2 DEG C/min is arranged is warming up to 600 DEG C, by prefabricated 3D printing quartz-ceramics biscuit 600
1 hour is kept the temperature at DEG C；Organic principle in quartz-ceramics biscuit is discharged, the intergranular channel of green body can be opened, both ensure that
The unsticking of green body, and provide dipping passage for subsequent dipping process, when dipping be conducive to maceration extract by the duct of quartz-ceramics,
Gap is sufficient filling with, and increases the bulk density of quartz-ceramics.
S2, dipping and curing process
3D printing quartz-ceramics biscuit is placed in the quartz-ceramics densification maceration extract under vacuum condition and is impregnated
50min, vacuum degree≤- 0.08MPa of the vacuum condition, then at 80 DEG C baking and curing to constant weight；
S3, densification
The heating rate that 0.1-4 DEG C/min is arranged is warming up to 1500 DEG C, by the 3D printing quartz-ceramics base after curing process
Body is heat-treated 2 hours at 1500 DEG C, the quartz ceramic densified, and silicon atom in maceration extract is realized in densified processing
To SiO2Conversion be completed at the same time the sintering process of quartz-ceramics green body, the quartz ceramic body of densification described in the present embodiment
Product density is 1.91g/cm3, bending strength is greater than 50MPa.
Embodiment 4:
A kind of preparation method of quartz-ceramics densification maceration extract of the present embodiment, is made: by weight by following methods
20 parts of the high containing hydrogen silicone oil, ethyl orthosilicate are weighed no more than 1 part, is stirred, 0.05 part of chloroplatinic acid is then added in adding
It is persistently stirred under heat condition 8 hours, heating temperature is 40 DEG C；Ethyl orthosilicate issues raw hydrolysis conversion in chloroplatinic acid effect
For SiO2, high containing hydrogen silicone oil occurs dehydrogenation reaction and to precipitate under chloroplatinic acid effect, and macromolecular compound is converted into small point
Sub- compound reduces dipping fluid viscosity, by taking chloroplatinic acid as an example: C6H18OSi2+H2Cl6Pt (chloroplatinic acid) → C6H16OSi2+2HCl
+ Pt (platinum black), bottom is stood after stirring will appear black precipitate, and supernatant is taken to densify maceration extract, viscosity up to quartz-ceramics
For 18mPa.s.
Above-mentioned quartz-ceramics densify maceration extract application method, comprising the following steps:
S1, the processing of quartz-ceramics dumping
The heating rate that 0.1-2 DEG C/min is arranged is warming up to 500 DEG C, by prefabricated 3D printing quartz-ceramics biscuit 500
2 hours are kept the temperature at DEG C；Organic principle in quartz-ceramics biscuit is discharged, the intergranular channel of green body can be opened, both ensure that
The unsticking of green body, and provide dipping passage for subsequent dipping process, when dipping be conducive to maceration extract by the duct of quartz-ceramics,
Gap is sufficient filling with, and increases the bulk density of quartz-ceramics.
S2, dipping and curing process
3D printing quartz-ceramics biscuit is placed in the quartz-ceramics densification maceration extract under vacuum condition and is impregnated
30min, vacuum degree≤- 0.08MPa of the vacuum condition, then at 70 DEG C baking and curing to constant weight；
S3, densification
The heating rate that 0.1-4 DEG C/min is arranged is warming up to 1400 DEG C, by the 3D printing quartz-ceramics base after curing process
Body is heat-treated 1 hour at 1400 DEG C, the quartz ceramic densified, and silicon atom in maceration extract is realized in densified processing
To SiO2Conversion be completed at the same time the sintering process of quartz-ceramics green body, the quartz ceramic body of densification described in the present embodiment
Product density is 1.92g/cm3, bending strength is greater than 50MPa.Optionally, the preparation of maceration extract, in step 1 or step
Magnesia or 1.2 parts of calcium oxide are added in 2 into the mixed liquor, to reduce the densification temperature of quartz-ceramics green body, prevent
Green body cracks in high-temperature heat treatment process.
Embodiment 5
A kind of densifying method of 3D printing quartz-ceramics, comprising the following steps:
(1) preparation of maceration extract
25 parts of the high containing hydrogen silicone oil, ethyl orthosilicate are weighed by weight no more than 1.5 parts, is stirred, then plus
Enter 0.06 part of chloroplatinic acid persistently to stir under heating condition 7 hours, heating temperature is 45 DEG C；Ethyl orthosilicate is acted in chloroplatinic acid
It issues raw hydrolysis and is converted into SiO2, high containing hydrogen silicone oil occurs dehydrogenation reaction and is precipitated under chloroplatinic acid effect, big to divide
Sub- compound is converted into small molecule compound, reduces dipping fluid viscosity, by taking chloroplatinic acid as an example: C6H18OSi2+H2Cl6Pt (chlorine platinum
Acid) → C6H16OSi2+ 2HCl+Pt (platinum black), bottom is stood after stirring will appear black precipitate, take supernatant up to quartz-ceramics
Densify maceration extract, viscosity 19.5mPa.s.
(2) quartz-ceramics dumping is handled
The heating rate that 0.1-2 DEG C/min is arranged is warming up to 550 DEG C, by prefabricated 3D printing quartz-ceramics biscuit 550
1.8 hours are kept the temperature at DEG C；Organic principle in quartz-ceramics biscuit is discharged, the intergranular channel of green body can be opened, both guaranteed
The unsticking of green body, and provide dipping passage for subsequent dipping process, when dipping, are conducive to hole of the maceration extract by quartz-ceramics
Road, gap are sufficient filling with, and increase the bulk density of quartz-ceramics.
(3) dipping and curing process
3D printing quartz-ceramics biscuit is placed in the quartz-ceramics densification maceration extract under vacuum condition and is impregnated
45min, vacuum degree≤- 0.08MPa of the vacuum condition, then at 75 DEG C baking and curing to constant weight；
(4) densification
The heating rate that 0.1-4 DEG C/min is arranged is warming up to 1230 DEG C, by the 3D printing quartz-ceramics base after curing process
Body is heat-treated 1.5 hours at 1230 DEG C, the quartz ceramic densified, and densified processing realizes that silicon is former in maceration extract
Son is to SiO2Conversion be completed at the same time the sintering process of quartz-ceramics green body, the quartz ceramic of densification described in the present embodiment
Bulk density is 1.96g/cm3, bending strength is greater than 50MPa.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.Those skilled in the art
Member is it should be appreciated that invention scope involved in the application, however it is not limited to technology made of the specific combination of above-mentioned technical characteristic
Scheme, while should also cover in the case where not departing from the inventive concept, it is carried out by above-mentioned technical characteristic or its equivalent feature
Any combination and the other technical solutions formed.Such as features described above has similar function with (but being not limited to) disclosed herein
Energy.
Claims (10)
1. a kind of preparation method of quartz-ceramics densification maceration extract, which is characterized in that be made by following methods:
Step 1: weighing high containing hydrogen silicone oil, ethyl orthosilicate and be stirred to obtain mixed liquor；
Step 2: chloroplatinic acid being added in Xiang Suoshu mixed liquor and is stirred under heating condition, stands after stirring to bottom and precipitates；
Step 3: step 2 gained supernatant being taken to densify maceration extract up to quartz-ceramics.
2. the preparation method of quartz-ceramics densification maceration extract according to claim 1, which is characterized in that further include in step
Rapid 1 or step 2 in magnesia or calcium oxide are added into the mixed liquor.
3. the preparation method of quartz-ceramics densification maceration extract according to claim 2, which is characterized in that pressed in step 1
Parts by weight weigh 10~30 parts of the high containing hydrogen silicone oil, ethyl orthosilicate no more than 2 parts, 0.01~0.1 part of chloroplatinic acid, oxidation
Magnesium or 0.5-1.4 parts of calcium oxide.
4. the preparation method of quartz-ceramics densification maceration extract according to claim 1 or 3, which is characterized in that in step 1
By weight, weighing 20 parts of the high containing hydrogen silicone oil, 0.5 part of ethyl orthosilicate, 0.08 part of chloroplatinic acid.
5. the preparation method of quartz-ceramics densification maceration extract according to claim 1 or 2, which is characterized in that step 2 exists
It is persistently stirred under heating condition 2-10 hours, heating temperature is 30~50 DEG C.
6. the preparation method of quartz-ceramics densification maceration extract according to claim 1, which is characterized in that quartz-ceramics cause
The viscosity of densification maceration extract is 10-20mPa.s.
7. a kind of quartz-ceramics densify maceration extract, which is characterized in that by quartz-ceramics as claimed in any one of claims 1 to 6
The preparation method for densifying maceration extract is made.
8. a kind of quartz-ceramics densify maceration extract application method, which comprises the following steps:
S1, the processing of quartz-ceramics dumping
Prefabricated 3D printing quartz-ceramics biscuit is kept the temperature 1-4 hours at 400~600 DEG C；
S2, dipping and curing process
3D printing quartz-ceramics biscuit is placed in the quartz-ceramics densification maceration extract under vacuum condition and impregnates 10-50min,
Then at 60~80 DEG C baking and curing to constant weight；
S3, densification
By the 3D printing quartz-ceramics green body after curing process 1000~1500 DEG C heat treatment 0.1-2 hours, densified
Quartz ceramic.
9. quartz-ceramics according to claim 8 densify maceration extract application method, which is characterized in that the densification
Quartz ceramic bulk density is not less than 1.9g/cm3。
10. quartz-ceramics according to claim 8 densify maceration extract application method, which is characterized in that the vacuum item
Vacuum degree≤- 0.08MPa of part.
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