CN103992037B - Porous height borosilicate and preparation method thereof - Google Patents
Porous height borosilicate and preparation method thereof Download PDFInfo
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- CN103992037B CN103992037B CN201410239183.2A CN201410239183A CN103992037B CN 103992037 B CN103992037 B CN 103992037B CN 201410239183 A CN201410239183 A CN 201410239183A CN 103992037 B CN103992037 B CN 103992037B
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Abstract
The invention discloses a kind of porous height borosilicate and preparation method thereof, wherein, the preparation method of described porous height borosilicate glass comprises the steps: that S1. provides high boron-silicate powders and Fe3O4Powder, mixes the two, Fe in the mixed-powder of formation3O4The mass percent of powder is 1～6%；S2. the mixed-powder formed in S1 is ground；S3. mixed-powder through milled processed in S2 is made powder base；S4. the powder base in S3 is sintered, after cooling, discharging.The high borosilicate glass of porous can be obtained by the preparation method of the present invention, and above-mentioned preparation method step is simple, with low cost, residuals will not be formed, pollution-free, can preferably carry out environmental protection and cost etc. and control.
Description
Technical field
The present invention relates to cellular glass preparing technical field, particularly relate to a kind of porous height borosilicate and
Its preparation method.
Background technology
High-boron-silicon glass is a kind of low thermal expansion, high temperature resistant, high intensity, high rigidity, high transmission rate and height
The specific glass material of chemical stability, borosilicate glass has low-down thermal coefficient of expansion, is approximately
/ 3rd of simple glass.This impact that minimizing is caused because of thermograde stress, thus have higher
Break resistance.Owing to its form variations is the least, this makes it telescope, must not in reflecting mirror
The material that can lack.It can be additionally used in process high radioactive nucleus waste.
Porous height borosilicate glass in high-boron-silicon glass is in biological activity engineering and Chemical Reaction Engineering etc.
Field has broad application prospects, but its technology of preparing limits it is more widely applied.At present,
It is mainly the most several about porous height borosilicate glass technology of preparing:
(1) Foam dipping method.This technique is to use foam impregnation ceramic size, after drying
Burn organic foam, it is thus achieved that a kind of method of porous ceramics.This method is suitable to prepare high porosity, open pore
Porous ceramics, be generally called foamed ceramics.
(2) sol gel process.This technique uses aluminium-alcohol salt hydrolysis preparation porous from pseudo-thin film, uses
Sol-gal process prepares porous material.
(3) preparation technology of the textile property of fiber is utilized.Mainly utilize the textile property of fiber with very thin
Forms etc. form pore and weave in order, arrange unordered accumulation or filling.Generally fiber is arbitrarily stacked, by
In elasticity and the slim-lined construction of fiber, build bridge mutually and form the three-dimensional net structure that the porosity is the highest, by fibre
Dimension is filled in the mould of definite shape, can be formed relatively uniform, have effigurate air hole structure,
Imposing binding agent, high temperature sintering solidification has just obtained the porosity the most much higher hole pottery, the porosity up to
More than 80%.
(4) etch is utilized to produce micropore, the preparation technology of mesopore.At such as to the activation of mineral wool
Reason, many inorganic non-metallic semipermeable membranes are in this way prepared.
But above method all exists can produce a lot of chemical residual in complicated process of preparation, and preparation process
The problem of thing.These chemical residues have impact on the use of porous height borosilicate glass, and can bring dirt
Dye.
Therefore, for the problems referred to above, it is necessary to propose a kind of further improvement project.
Summary of the invention
In view of this, the invention provides a kind of porous height borosilicate glass, and preparation method thereof.
In order to realize foregoing invention purpose, the preparation method of the porous height borosilicate glass of the present invention, institute
The preparation method stating porous height borosilicate glass comprises the steps:
S1., high boron-silicate powders and Fe are provided3O4Powder, mixes the two, the mixed powder of formation
Fe in end3O4The mass percent of powder is 1～6%；
S2. the mixed-powder formed in S1 is ground；
S3. mixed-powder through milled processed in S2 is made powder base；
S4. the powder base in S3 is sintered, after cooling, discharging.
As a further improvement on the present invention, described high boron-silicate powders and Fe3O4The purity of powder >=
99.5%, the particle size range of the two is 20nm-200nm.
As a further improvement on the present invention, the mixed-powder formed in S1 is ground specifically, incite somebody to action
Mixed-powder is put into and is carried out ball milling in ball mill, and described Ball-milling Time is at least 4h.
As a further improvement on the present invention, mixed-powder through milled processed in S2 is made powder base tool
Body is, puts in forcing press by the mixed-powder of milled processed, at least 20MPa, and at least 1min condition
Under, prepare a diameter of 10mm, height is the powder base of 30mm.
As a further improvement on the present invention, the powder base in S3 is sintered specifically, put into by powder base
Carrying out heat preservation sintering in resistance furnace or atmosphere furnace, programming rate is 4～30 DEG C/min, is incubated at 900 DEG C
After 100min, continue to be warmed up to 1100 DEG C, be incubated 100min～300min.
As a further improvement on the present invention, when being sintered in atmosphere furnace, the gas being passed through is argon
Gas.
As a further improvement on the present invention, described high boron-silicate powders includes by mass percentage:
The Na of 3.7%2O, the K of 3.7%2O, the Al of 3.0%2O3, the B of 23%2O3, described high borosilicic acid salt fines
In end, surplus is SiO2。
The present invention also provides for a kind of porous height borosilicate glass obtained by above-mentioned preparation method.
Compared with prior art, the preparation method of the porous height borosilicate glass of the present invention is by optimizing work
Skill parameter, obtain the high borosilicate glass of porous of certain pore size distribution.The manufacture method of the present invention
Can apply to the industry such as biological engineering and Chemical Reaction Engineering, solve in existing preparation method and exist
Preparation method complicated, easily cause the problem remaining harmful substance in environmental pollution, product.Its step
Simply, with low cost, residuals will not be formed, pollution-free, can preferably carry out environmental protection and cost etc.
Control.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to reality
Execute the required accompanying drawing used in example or description of the prior art to be briefly described, it should be apparent that below,
Accompanying drawing in description is only some embodiments described in the present invention, for those of ordinary skill in the art
From the point of view of, on the premise of not paying creative work, it is also possible to obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the side of a detailed description of the invention of the preparation method of the porous height borosilicate glass of the present invention
Method schematic flow sheet；
Fig. 2 is the micromorphology of the porous height borosilicate glass of preparation in embodiments of the invention 1
Figure；
Fig. 3 is the micromorphology of the porous height borosilicate glass of preparation in embodiments of the invention 2
Figure；
Fig. 4 is the micromorphology of the porous height borosilicate glass of preparation in embodiments of the invention 3
Figure.
Detailed description of the invention
As it is shown in figure 1, the preparation method of a kind of porous height borosilicate glass of the present invention, this preparation side
Method comprises the steps:
S1., high boron-silicate powders and Fe are provided3O4Powder, mixes the two, the mixed powder of formation
Fe in end3O4The mass percent of powder is 1～6%；
S2. the mixed-powder formed in S1 is ground；
S3. mixed-powder through milled processed in S2 is made powder base；
S4. the powder base in S3 is sintered, after cooling, discharging.
For realizing above-mentioned steps, described high boron-silicate powders and Fe3O4The purity grade of powder is point
Analyse pure, specifically, described high boron-silicate powders and Fe3O4Purity >=99.5% of powder, the grain of the two
Degree scope is 20nm～200nm.
Described high boron-silicate powders is mixture, and by mass percentage, it includes following component:
The Na of 3.7%2O, the K of 3.7%2O, the Al of 3.0%2O3, the B of 23%2O3, this high boron-silicate powders
Middle surplus is SiO2。
In S2, mixed-powder is ground preferably employing the mode of ball milling, specifically, by mixed-powder
Putting into and carry out ball milling in ball mill, described Ball-milling Time is at least 4h.
In S3, the mixed-powder through milled processed is made powder base and carries out in a press, in pressure
The condition preparing powder base in power machine is: in forcing press, pressure is at least 20MPa, and the press time is at least
1min.The powder base prepared is cylinder, and the diameter of this cylinder powder base is preferably 10mm, the most excellent
Elect 30mm as.
In S4, when powder base is sintered, powder base is put in resistance furnace or atmosphere furnace and carry out insulation burning
Knot.During heat preservation sintering, controlling programming rate is 4～30 DEG C/min, when being warming up to 900 DEG C, and insulation
100min, then proceedes to be warmed up to 1100 DEG C, is incubated 100min～300min.Atmosphere furnace is used to protect
During temperature sintering, the gas being passed through is argon.
Invention additionally discloses a kind of porous height borosilicate glass, this porous height borosilicate glass is by such as
Upper described preparation method obtains.
Below in conjunction with specific embodiment, the preparation method of the porous height borosilicate glass of the present invention is carried out
Describe in detail.
Embodiment 1
High borosilicate glass powder by 99% and the Fe of 1%3O4Powder mixes.Wherein, high borosilicic acid
Salt glass powder includes by mass percentage: the Na of 3.7%2O, the K of 3.7%2O, the Al of 3.0%2O3,
The B of 23%2O3, surplus is SiO2.High borosilicate glass powder and Fe3O4The purity of powder is
99.5%, granularity is 20nm.
By the high borosilicate glass powder mixed and Fe3O4Powder is put into and is carried out ball in ball mill
Mill, Ball-milling Time is 4h.After ball milling, by through ball-milling treatment high borosilicate glass powder with
Fe3O4Powder is put in forcing press and is suppressed, and under 20MPa, suppresses 1min, makes a diameter of
10mm, height is the cylindrical powder base of 30mm.Take out powder base, put it into the atmosphere furnace of argon gas atmosphere
In carry out heat preservation sintering, controlling programming rate is 4 DEG C/min, is warming up to 900 DEG C of insulation 100min, then
Continue to be warmed up to 1100 DEG C, be incubated 100min.After heat preservation sintering, cooling, discharging, it is thus achieved that the present invention's
Porous height borosilicate glass.
As in figure 2 it is shown, be the micromorphology of the porous height borosilicate glass of preparation in the present embodiment
Figure, in figure, black part is divided into the hole of formation, and the preparation method being indicated above the present invention can obtain porous
High borosilicate glass.
Embodiment 2
High borosilicate glass powder by 97% and the Fe of 3%3O4Powder mixes.Wherein, high borosilicic acid
Salt glass powder includes by mass percentage: the Na of 3.7%2O, the K of 3.7%2O, the Al of 3.0%2O3,
The B of 23%2O3, surplus is SiO2.High borosilicate glass powder and Fe3O4The purity of powder is
99.5%, granularity is 110nm.
By the high borosilicate glass powder mixed and Fe3O4Powder is put into and is carried out ball in ball mill
Mill, Ball-milling Time is 4h.After ball milling, by through ball-milling treatment high borosilicate glass powder with
Fe3O4Powder is put in forcing press and is suppressed, and under 20MPa, suppresses 1min, makes a diameter of
10mm, height is the cylindrical powder base of 30mm.Take out powder base, put it in resistance furnace and be incubated
Sintering, controlling programming rate is 17 DEG C/min, is warming up to 900 DEG C of insulation 100min, then proceedes to heat up
To 1100 DEG C, it is incubated 200min.After heat preservation sintering, cooling, discharging, it is thus achieved that the porous height boron of the present invention
Silicate glass.
As it is shown on figure 3, be the micromorphology of the porous height borosilicate glass of preparation in the present embodiment
Figure.In figure, black and white border circular areas is the hole of formation, is indicated above the preparation side of the present invention
Method can obtain the high borosilicate glass of porous.
Embodiment 3
High borosilicate glass powder by 94% and the Fe of 6%3O4Powder mixes.Wherein, high borosilicic acid
Salt glass powder includes by mass percentage: the Na of 3.7%2O, the K of 3.7%2O, the Al of 3.0%2O3,
The B of 23%2O3, surplus is SiO2.High borosilicate glass powder and Fe3O4The purity of powder is
99.5%, granularity is 200nm.
By the high borosilicate glass powder mixed and Fe3O4Powder is put into and is carried out ball in ball mill
Mill, Ball-milling Time is 4h.After ball milling, by through ball-milling treatment high borosilicate glass powder with
Fe3O4Powder is put in forcing press and is suppressed, and under 20MPa, suppresses 1min, makes a diameter of
10mm, height is the cylindrical powder base of 30mm.Take out powder base, put it in resistance furnace and be incubated
Sintering, controlling programming rate is 30 DEG C/min, is warming up to 900 DEG C of insulation 100min, then proceedes to heat up
To 1100 DEG C, it is incubated 300min.After heat preservation sintering, cooling, discharging, it is thus achieved that the porous height boron of the present invention
Silicate glass.
As shown in Figure 4, for the micromorphology of the porous height borosilicate glass of preparation in the present embodiment
Figure.In figure, black and white border circular areas is the hole of formation, is indicated above the preparation side of the present invention
Method can obtain the high borosilicate glass of porous.
In sum, the preparation method of the porous height borosilicate glass of the present invention by Optimizing Process Parameters,
Obtain the high borosilicate glass of the porous of certain pore size distribution.The manufacture method of the present invention can be applied
In the industry such as biological engineering and Chemical Reaction Engineering, solve preparation side present in existing preparation method
Method is complicated, easily cause the problem remaining harmful substance in environmental pollution, product.Its step is simple, becomes
This is cheap, will not form residuals, pollution-free, can preferably carry out environmental protection and cost etc. and control.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment,
And without departing from the spirit or essential characteristics of the present invention, it is possible to real in other specific forms
The existing present invention.Therefore, no matter from the point of view of which point, embodiment all should be regarded as exemplary, and
Being nonrestrictive, the scope of the present invention is limited by claims rather than described above, therefore purport
All changes in falling in the implication of equivalency and scope of claim are included in the present invention.
Should not be considered as limiting involved claim by any reference in claim.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, but the most each reality
Mode of executing only comprises an independent technical scheme, and this narrating mode of description is only for understand
Seeing, those skilled in the art should be using description as an entirety, and the technical scheme in each embodiment is also
Other embodiments that it will be appreciated by those skilled in the art that can be formed through appropriately combined.
Claims (7)
1. the preparation method of a porous height borosilicate glass, it is characterised in that described porous height boron
The preparation method of silicate glass comprises the steps:
S1., high boron-silicate powders and Fe are provided3O4Powder, mixes the two, the mixed powder of formation
Fe in end3O4The mass percent of powder is 1～6%；
S2. the mixed-powder formed in S1 is ground；
S3. mixed-powder through milled processed in S2 is made powder base；
S4. the powder base in S3 is sintered, after cooling, discharging；
Wherein, the powder base in S3 is sintered specifically, put in resistance furnace or atmosphere furnace by powder base
Row heat preservation sintering, programming rate is 4～30 DEG C/min, after being incubated 100min, continues to heat up at 900 DEG C
To 1100 DEG C, it is incubated 100min～300min.
The preparation method of porous height borosilicate glass the most according to claim 1, its feature exists
In, described high boron-silicate powders and Fe3O4Purity >=99.5% of powder, the particle size range of the two is
20nm-200nm。
The preparation method of porous height borosilicate glass the most according to claim 1, its feature exists
In, the mixed-powder formed in S1 is ground specifically, mixed-powder is put in ball mill and carries out
Ball milling, described Ball-milling Time is at least 4h.
The preparation method of porous height borosilicate glass the most according to claim 1, its feature exists
In, mixed-powder through milled processed in S2 is made powder base specifically, by the mixed powder of milled processed
End is put in forcing press, under the conditions of at least 20MPa, at least 1min, prepares a diameter of 10mm,
It it is highly the powder base of 30mm.
The preparation method of porous height borosilicate glass the most according to claim 1, its feature exists
In, when being sintered in atmosphere furnace, the gas being passed through is argon.
The preparation method of porous height borosilicate glass the most according to claim 1, its feature exists
In, described high boron-silicate powders includes by mass percentage: the Na of 3.7%2O, the K of 3.7%2O,
The Al of 3.0%2O3, the B of 23%2O3, in described high boron-silicate powders, surplus is SiO2。
7. a porous height borosilicate glass, it is characterised in that described porous height borosilicate glass
Obtain according to the preparation method described in any one of claim 1～6.
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| CN101288780B (en) * | 2008-06-10 | 2011-05-25 | 浙江大学 | Degradable dynamics enhancement type bioglass base porous composite material and preparation method thereof |
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