CN103992037A - Porous high borosilicate and preparation method thereof - Google Patents
Porous high borosilicate and preparation method thereof Download PDFInfo
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- CN103992037A CN103992037A CN201410239183.2A CN201410239183A CN103992037A CN 103992037 A CN103992037 A CN 103992037A CN 201410239183 A CN201410239183 A CN 201410239183A CN 103992037 A CN103992037 A CN 103992037A
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- powder
- high borosilicate
- preparation
- borosilicate glass
- porous
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Abstract
The invention discloses porous high borosilicate and a preparation method thereof. The preparation method of the porous high borosilicate comprises the following steps: S1, providing high borosilicate powder and Fe3O4 powder, and mixing high borosilicate powder with Fe3O4 powder, wherein the mass percent of the Fe3O4 powder in the formed mixed powder is 1-6%; S2, grinding the mixed powder formed in S1; S3, preparing a powder base from the mixed powder grinded in S2; S4, sintering the powder base in S3, and discharging after cooling. Porous high borosilicate glass can be obtained by the preparation method disclosed by the invention, the preparation method is simple in steps, low in cost, free of residues and free of pollution, control on environmental protection, cost and the like can be better carried out.
Description
Technical field
The present invention relates to sintered glass preparing technical field, particularly relate to high borosilicate of a kind of porous and preparation method thereof.
Background technology
High-boron-silicon glass is the specific glass material of a kind of low thermal expansion, high temperature resistant, high strength, high rigidity, high transmission rate and high chemical stability, and borosilicate glass has low-down thermal expansivity, is approximately 1/3rd of simple glass.This will reduce the impact causing because of thermograde stress, thereby has stronger break resistance.Because its form variations is very little, this makes it become visual telescope, requisite material in speculum.It also can be used for processing high radioactive nucleus waste.
The high borosilicate glass of porous in high-boron-silicon glass has broad application prospects in fields such as biological activity engineering and chemical reaction engineerings, applies more widely but its technology of preparing has limited it.At present, be mainly several as follows about the high borosilicate glass technology of preparing of porous:
(1) foam impregnation technique.This technique is to use foam impregnation ceramic size, after being dried, burns organic foam, obtains a kind of method of porous ceramics.This method is suitable for preparing high porosity, the porous ceramics of ventilate, common name foamed ceramics.
(2) colloidal sol-gel process.This technique is used aluminium-alcohol salt hydrolysis preparation porous from pseudo-film, prepares porous material with sol-gel processing.
(3) utilize the preparation technology of the textile property of fiber.Mainly utilize the formation such as textile property and the very thin form pore of fiber to weave in order, arrange unordered accumulation or filling.Conventionally fiber is arbitrarily stacked, due to elasticity and the slim-lined construction of fiber, build bridge mutually and form the very high three-dimensional net structure of void content, by fiber filled in the mould of definite shape, can form relatively evenly, the effigurate air hole structure of tool, imposes binding agent, high temperature sintering is curing has just obtained the very much higher hole of void content pottery, and void content can reach more than 80%.
(4) utilize etch to produce the preparation technology of micropore, mesopore.The for example activation treatment to mineral wool, many inorganic non-metallic semi-permeable membraness are in this way prepared.
But above method all exists complicated process of preparation, and in preparation process, understand the problem that produces a lot of chemical residues.These chemical residues have affected the use of the high borosilicate glass of porous, and can bring pollution.
Therefore,, for the problems referred to above, be necessary to propose a kind of further improvement project.
Summary of the invention
In view of this, the invention provides the high borosilicate glass of a kind of porous, and preparation method thereof.
In order to realize foregoing invention object, the preparation method of the high borosilicate glass of porous of the present invention, the preparation method of the high borosilicate glass of described porous comprises the steps:
S1., high borosilicate powder and Fe are provided
3o
4powder, mixes the two, Fe in the mixed powder of formation
3o
4the mass percent of powder is 1～6%;
S2. the mixed powder forming in S1 is ground;
S3. the mixed powder through milled processed in S2 is made to powder base;
S4. the powder base in S3 is carried out to sintering, cooling after, discharging.
As a further improvement on the present invention, described high borosilicate powder and Fe
3o
4purity>=99.5% of powder, the size range of the two is 20nm-200nm.
As a further improvement on the present invention, the mixed powder forming in S1 is ground and is specially, mixed powder is put into ball mill and carry out ball milling, described Ball-milling Time is at least 4h.
As a further improvement on the present invention, the mixed powder through milled processed in S2 is made to powder base and be specially, the mixed powder of milled processed is put into pressing machine, at 20MPa at least, at least, under 1min condition, preparing diameter is 10mm, is highly the powder base of 30mm.
As a further improvement on the present invention, the powder base in S3 is carried out to sintering and be specially, powder base is put into resistance furnace or atmosphere furnace is carried out heat preservation sintering, heat-up rate is 4～30 DEG C/min, at 900 DEG C, be incubated after 100min, continue to be warmed up to 1100 DEG C, insulation 100min～300min.
As a further improvement on the present invention, carry out sintering in atmosphere furnace time, the gas passing into is argon gas.
As a further improvement on the present invention, described high borosilicate powder comprises by mass percentage: 3.7% Na
2o, 3.7% K
2o, 3.0% Al
2o
3, 23% B
2o
3, in described high borosilicate powder, surplus is SiO
2.
The present invention also provides a kind of porous being obtained by above-mentioned preparation method high borosilicate glass.
Compared with prior art, the preparation method of the high borosilicate glass of porous of the present invention by Optimizing Process Parameters, obtained the high borosilicate glass of the porous that certain pore size distributes.Manufacture method of the present invention can be applied to the industry such as biotechnology and chemical reaction engineering, has solved preparation method's complexity of existing in existing preparation method, has easily caused the problem that remains objectionable impurities in environmental pollution, product.Its step is simple, with low cost, can not form residuals, pollution-free, can better carry out the controls such as environmental protection and cost.
Brief description of the drawings
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, to the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described below, apparently, the accompanying drawing the following describes is only some embodiment that record in the present invention, for those of ordinary skill in the art, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is the method flow schematic diagram of the preparation method's of the high borosilicate glass of a porous of the present invention embodiment;
Fig. 2 is the micromorphology figure of the high borosilicate glass of porous of preparation in embodiments of the invention 1;
Fig. 3 is the micromorphology figure of the high borosilicate glass of porous of preparation in embodiments of the invention 2;
Fig. 4 is the micromorphology figure of the high borosilicate glass of porous of preparation in embodiments of the invention 3.
Embodiment
As shown in Figure 1, the preparation method of the high borosilicate glass of a kind of porous of the present invention, this preparation method comprises the steps:
S1., high borosilicate powder and Fe are provided
3o
4powder, mixes the two, Fe in the mixed powder of formation
3o
4the mass percent of powder is 1～6%;
S2. the mixed powder forming in S1 is ground;
S3. the mixed powder through milled processed in S2 is made to powder base;
S4. the powder base in S3 is carried out to sintering, cooling after, discharging.
For realizing above-mentioned steps, described high borosilicate powder and Fe
3o
4the purity grade of powder is analytical pure, particularly, and described high borosilicate powder and Fe
3o
4purity>=99.5% of powder, the size range of the two is 20nm～200nm.
Described high borosilicate powder is mixture, and by mass percentage, it comprises following component: 3.7% Na
2o, 3.7% K
2o, 3.0% Al
2o
3, 23% B
2o
3, in this high borosilicate powder, surplus is SiO
2.
In S2, mixed powder is ground to the mode of preferred employing ball milling, particularly, mixed powder is put into ball mill and carry out ball milling, described Ball-milling Time is at least 4h.
In S3, carry out in pressing machine making powder base through the mixed powder of milled processed, the condition of preparing powder base in pressing machine is: in pressing machine, pressure is at least 20MPa, and the press time is at least 1min.The powder base of preparing is cylindrical, and the diameter of this cylindrical powder base is preferably 10mm, is highly preferably 30mm.
In S4, when powder base is carried out to sintering, powder base is put into and in resistance furnace or atmosphere furnace, carried out heat preservation sintering.When heat preservation sintering, controlling heat-up rate is 4～30 DEG C/min, and in the time being warming up to 900 DEG C, insulation 100min, then continues to be warmed up to 1100 DEG C, insulation 100min～300min.While using atmosphere furnace to carry out heat preservation sintering, the gas passing into is argon gas.
The present invention also discloses the high borosilicate glass of a kind of porous, and the high borosilicate glass of this porous obtains by preparation method as above.
Below in conjunction with specific embodiment, the preparation method of the high borosilicate glass of porous of the present invention is elaborated.
Embodiment 1
By 99% high borosilicate glass powder and 1% Fe
3o
4powder mixes.Wherein, high borosilicate glass powder comprises by mass percentage: 3.7% Na
2o, 3.7% K
2o, 3.0% Al
2o
3, 23% B
2o
3, surplus is SiO
2.High borosilicate glass powder and Fe
3o
4the purity of powder is 99.5%, and granularity is 20nm.
By the high borosilicate glass powder and the Fe that mix
3o
4powder is put into ball mill and is carried out ball milling, and Ball-milling Time is 4h.After ball milling, by high borosilicate glass powder and Fe through ball-milling processing
3o
4powder is put into pressing machine and is suppressed, under 20MPa, and compacting 1min, making diameter is 10mm, is highly the cylindrical powder base of 30mm.Take out powder base, put it in the atmosphere furnace of argon gas atmosphere and carry out heat preservation sintering, controlling heat-up rate is 4 DEG C/min, is warming up to 900 DEG C of insulation 100min, then continues to be warmed up to 1100 DEG C, insulation 100min.After heat preservation sintering, cooling, discharging, obtains the high borosilicate glass of porous of the present invention.
As shown in Figure 2, be the micromorphology figure of the high borosilicate glass of porous prepared in the present embodiment, in figure, black part is divided into the hole of formation, shows thus to have preparation method of the present invention can obtain the high borosilicate glass of porous.
Embodiment 2
By 97% high borosilicate glass powder and 3% Fe
3o
4powder mixes.Wherein, high borosilicate glass powder comprises by mass percentage: 3.7% Na
2o, 3.7% K
2o, 3.0% Al
2o
3, 23% B
2o
3, surplus is SiO
2.High borosilicate glass powder and Fe
3o
4the purity of powder is 99.5%, and granularity is 110nm.
By the high borosilicate glass powder and the Fe that mix
3o
4powder is put into ball mill and is carried out ball milling, and Ball-milling Time is 4h.After ball milling, by high borosilicate glass powder and Fe through ball-milling processing
3o
4powder is put into pressing machine and is suppressed, under 20MPa, and compacting 1min, making diameter is 10mm, is highly the cylindrical powder base of 30mm.Take out powder base, put it in resistance furnace and carry out heat preservation sintering, controlling heat-up rate is 17 DEG C/min, is warming up to 900 DEG C of insulation 100min, then continues to be warmed up to 1100 DEG C, insulation 200min.After heat preservation sintering, cooling, discharging, obtains the high borosilicate glass of porous of the present invention.
As shown in Figure 3, be the micromorphology figure of the high borosilicate glass of porous prepared in the present embodiment.In figure, black and white border circular areas is the hole of formation, shows thus to have preparation method of the present invention can obtain the high borosilicate glass of porous.
Embodiment 3
By 94% high borosilicate glass powder and 6% Fe
3o
4powder mixes.Wherein, high borosilicate glass powder comprises by mass percentage: 3.7% Na
2o, 3.7% K
2o, 3.0% Al
2o
3, 23% B
2o
3, surplus is SiO
2.High borosilicate glass powder and Fe
3o
4the purity of powder is 99.5%, and granularity is 200nm.
By the high borosilicate glass powder and the Fe that mix
3o
4powder is put into ball mill and is carried out ball milling, and Ball-milling Time is 4h.After ball milling, by high borosilicate glass powder and Fe through ball-milling processing
3o
4powder is put into pressing machine and is suppressed, under 20MPa, and compacting 1min, making diameter is 10mm, is highly the cylindrical powder base of 30mm.Take out powder base, put it in resistance furnace and carry out heat preservation sintering, controlling heat-up rate is 30 DEG C/min, is warming up to 900 DEG C of insulation 100min, then continues to be warmed up to 1100 DEG C, insulation 300min.After heat preservation sintering, cooling, discharging, obtains the high borosilicate glass of porous of the present invention.
As shown in Figure 4, be the micromorphology figure of the high borosilicate glass of porous prepared in the present embodiment.In figure, black and white border circular areas is the hole of formation, shows thus to have preparation method of the present invention can obtain the high borosilicate glass of porous.
In sum, the preparation method of the high borosilicate glass of porous of the present invention by Optimizing Process Parameters, obtained the high borosilicate glass of the porous that certain pore size distributes.Manufacture method of the present invention can be applied to the industry such as biotechnology and chemical reaction engineering, has solved preparation method's complexity of existing in existing preparation method, has easily caused the problem that remains objectionable impurities in environmental pollution, product.Its step is simple, with low cost, can not form residuals, pollution-free, can better carry out the controls such as environmental protection and cost.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned example embodiment, and in the situation that not deviating from spirit of the present invention or essential characteristic, can realize the present invention with other specific form.Therefore, no matter from which point, all should regard embodiment as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, is therefore intended to all changes that drop in the implication and the scope that are equal to important document of claim to include in the present invention.Any Reference numeral in claim should be considered as limiting related claim.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but be not that each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should make specification sheets as a whole, and the technical scheme in each embodiment also can, through appropriately combined, form other embodiments that it will be appreciated by those skilled in the art that.
Claims (8)
1. a preparation method for the high borosilicate glass of porous, is characterized in that, the preparation method of the high borosilicate glass of described porous comprises the steps:
S1., high borosilicate powder and Fe are provided
3o
4powder, mixes the two, Fe in the mixed powder of formation
3o
4the mass percent of powder is 1～6%;
S2. the mixed powder forming in S1 is ground;
S3. the mixed powder through milled processed in S2 is made to powder base;
S4. the powder base in S3 is carried out to sintering, cooling after, discharging.
2. the preparation method of the high borosilicate glass of porous according to claim 1, is characterized in that, described high borosilicate powder and Fe
3o
4purity>=99.5% of powder, the size range of the two is 20nm-200nm.
3. the preparation method of the high borosilicate glass of porous according to claim 1, is characterized in that, the mixed powder forming in S1 is ground and is specially, and mixed powder is put into ball mill and carry out ball milling, and described Ball-milling Time is at least 4h.
4. the preparation method of the high borosilicate glass of porous according to claim 1, it is characterized in that, mixed powder through milled processed in S2 is made to powder base to be specially, the mixed powder of milled processed is put into pressing machine, at 20MPa at least, at least, under 1min condition, preparing diameter is 10mm, is highly the powder base of 30mm.
5. the preparation method of the high borosilicate glass of porous according to claim 1, it is characterized in that, powder base in S3 is carried out to sintering to be specially, powder base is put into resistance furnace or atmosphere furnace is carried out heat preservation sintering, heat-up rate is 4～30 DEG C/min, at 900 DEG C, be incubated after 100min, continue to be warmed up to 1100 DEG C, insulation 100min～300min.
6. the preparation method of the high borosilicate glass of porous according to claim 5, is characterized in that, carry out sintering in atmosphere furnace time, the gas passing into is argon gas.
7. the preparation method of the high borosilicate glass of porous according to claim 1, is characterized in that, described high borosilicate powder comprises by mass percentage: 3.7% Na
2o, 3.7% K
2o, 3.0% Al
2o
3, 23% B
2o
3, in described high borosilicate powder, surplus is SiO
2.
8. the high borosilicate glass of porous, is characterized in that, the high borosilicate glass of described porous obtains according to the preparation method described in claim 1～7 any one.
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|---|---|---|---|
| CN201410239183.2A CN103992037B (en) | 2014-05-30 | 2014-05-30 | Porous height borosilicate and preparation method thereof |
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|---|---|---|---|
| CN201410239183.2A CN103992037B (en) | 2014-05-30 | 2014-05-30 | Porous height borosilicate and preparation method thereof |
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| CN103992037A true CN103992037A (en) | 2014-08-20 |
| CN103992037B CN103992037B (en) | 2016-08-24 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105084759A (en) * | 2015-09-06 | 2015-11-25 | 东南大学 | High-temperature-resistant transparent phosphate glass and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060251737A1 (en) * | 2003-02-20 | 2006-11-09 | Edgar Dutra Zanotto | Process and compositions for preparing particulate, bioactive or resorbable biosilicates for use in the treatment of oral ailments |
| CN101288780A (en) * | 2008-06-10 | 2008-10-22 | 浙江大学 | Degradable dynamics enhancement type bioglass radical porous composite material and preparation method thereof |
| CN101531462A (en) * | 2009-04-10 | 2009-09-16 | 北京工业大学 | Method for preparing borosilicate foam glass |
| CN102795783A (en) * | 2012-08-31 | 2012-11-28 | 哈尔滨工业大学 | Preparation method of porous glass material |
-
2014
- 2014-05-30 CN CN201410239183.2A patent/CN103992037B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060251737A1 (en) * | 2003-02-20 | 2006-11-09 | Edgar Dutra Zanotto | Process and compositions for preparing particulate, bioactive or resorbable biosilicates for use in the treatment of oral ailments |
| CN101288780A (en) * | 2008-06-10 | 2008-10-22 | 浙江大学 | Degradable dynamics enhancement type bioglass radical porous composite material and preparation method thereof |
| CN101531462A (en) * | 2009-04-10 | 2009-09-16 | 北京工业大学 | Method for preparing borosilicate foam glass |
| CN102795783A (en) * | 2012-08-31 | 2012-11-28 | 哈尔滨工业大学 | Preparation method of porous glass material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105084759A (en) * | 2015-09-06 | 2015-11-25 | 东南大学 | High-temperature-resistant transparent phosphate glass and preparation method thereof |
| CN105084759B (en) * | 2015-09-06 | 2017-06-09 | 东南大学 | The preparation method of high temperature resistant phosphate clear glass |
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|---|---|
| CN103992037B (en) | 2016-08-24 |
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