CN109467314A - A kind of floating bead/hollow microsphere/borosilicate glass buoyant material preparation method - Google Patents
A kind of floating bead/hollow microsphere/borosilicate glass buoyant material preparation method Download PDFInfo
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- CN109467314A CN109467314A CN201710801676.4A CN201710801676A CN109467314A CN 109467314 A CN109467314 A CN 109467314A CN 201710801676 A CN201710801676 A CN 201710801676A CN 109467314 A CN109467314 A CN 109467314A
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- borosilicate glass
- material preparation
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- buoyant material
- floating bead
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C11/00—Multi-cellular glass ; Porous or hollow glass or glass particles
- C03C11/007—Foam glass, e.g. obtained by incorporating a blowing agent and heating
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/002—Use of waste materials, e.g. slags
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Geochemistry & Mineralogy (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
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Abstract
A kind of floating bead/hollow microsphere/borosilicate glass buoyant material preparation method, the material include 1. lower low close and higher compression strength;2. the characteristics of good temperature tolerance and higher high temperature compression strength;3. preparation process is simple, test it is easy to operate, prepared by material there is relatively high low temperature compression intensity and high temperature compression strength, provide possibility in durothermic deep-sea buoyant material for potential demand.
Description
Technical field
The invention belongs to structural material preparation technical field, in particular to a kind of floating bead/hollow microsphere/borosilicate glass
Buoyant material preparation method.
Background technique
With economic continuous development, the mankind constantly excessively develop natural resources, and land resources are used as to be distributed in the world
Most wide, the maximum resource of quantity, has been far from satisfying the growing material requisite of the mankind.Ocean as the mankind or
The direction that emphasis in future is explored, contains abundant mineral resources, and Ocean energy resource is the long term growth in the world
A reliable material guarantee is provided, construction and Development of Marine become the inexorable trend of current social development.Currently, deep-sea is opened
Hair can be observed in deep-sea field using benthoscope, be measured, being sampled, install must mainly based on deep submergence technology
Instrument wanted etc. carries out underwater operation.It can not be reached in deep-sea in the mankind, various detected events will then be assisted by underwater robot
To complete.Judging from the current situation, benthoscope, especially deep sea manned submersible are the emphasis of ocean development.
During exploration, the mankind will also be faced with huge difficult and challenge, in addition to will be by deep-sea
Outside huge pressure, i.e., every depth for increasing 100m, the pressure that object is subject to just will increase about 10 atmospheric pressure, i.e. 1MPa.This
Outside, material property is also possible to will receive the influence of particular surroundings.It is past when launching a guided missile in deep-sea as torpedo, anti-warship guided missle etc.
Toward that can face high temperature, the temperature is often in the range of tens degree to several Baidu even thousands of degree.In order to cope with by
The variation of the performance of material caused by the variation of external environment, the buoyant material should have good temperature tolerance.It is asked based on above-mentioned
Topic, preparing has the research emphasis for becoming today's society compared with the solid buoyancy material of high temperature tolerance.
Summary of the invention
It is solid especially for the temperature tolerance that can be used for deep-sea for the problem that solid buoyancy material temperature tolerance at this stage is poor
The demand of body buoyant material, the present invention are prepared for having a kind of good durothermic floating bead/hollow microsphere/borosilicate glass floating
Dead-wood material, the material also have good temperature tolerance, the preparation of material in addition to having the characteristics that low-density and advantages of higher compressive strength
The features such as method and process is simple, and experiment is easy to operate, and contamination-free generates in experimentation.
A kind of floating bead/hollow microsphere/borosilicate glass buoyant material preparation method, key step are as follows:
(1) pretreatment of fly ash float:
Raw material is weighed, a certain amount of fly ash float is put into distilled water, is stirred, after standing 5 ~ 10min, by the drift on upper layer
Pearl is taken out, and is placed in surface plate, is dried in 90 ~ 110 DEG C of electric drying oven with forced convection, spare;
(2) pretreatment of hollow glass microballoon:
Raw material is weighed, a certain amount of hollow glass microballoon is put into the beaker for filling distilled water, is stirred, it is quiet after 10 ~ 20min
It sets, after hollow glass microballoon and water are layered completely, upper layer microballoon is taken out, is placed in surface plate, in 80 ~ 100 DEG C of baking oven
Drying, it is spare;
(3) preparation of premixed liquid:
Using distilled water as solvent, acrylamide and N, N '-methylene-bisacrylamide are respectively monomer and crosslinking agent, according to certain
Proportion prepare premixed liquid;
(4) fly ash float-hollow glass microballoon/borosilicate glass slurry preparation:
A certain amount of borosilicate glass is added in the premixed liquid of (3), after a certain period of time through high speed planetary ball mill ball milling,
The mixed liquor containing borosilicate glass is obtained, is then added to hollow glass microballoon and fly ash float according to a certain ratio
In mixed liquor, it is uniformly mixed, it is spare;
(5) fly ash float-hollow glass microballoon/borosilicate glass buoyant material preparation
A certain amount of ammonium persulfate is added in mixed slurry in (4), is stirred continuously, is then poured into slurry in mold simultaneously
Constantly oscillation, mold is placed in 40 ~ 50 DEG C of baking ovens, half-dried green body is obtained after demoulding to be formed, through certain temperature it is dry and
After sintering, fly ash float-hollow glass microballoon/borosilicate glass solid buoyancy material is obtained.
The particle diameter distribution of the fly ash float is 80 ~ 200 mesh.
The particle diameter distribution of the hollow glass microballoon is 0 ~ 100 μm.
In the slurry content of solid (including borosilicate glass, fly ash float and hollow glass microballoon) be 10 ~
50 wt.%。
10 ~ 40 wt.% of additional amount of the pyrex.
The mass ratio of the microballoon (including hollow glass microballoon and fly ash float) and pyrex is 0 ~ 2:1.
Distilled water in the premixed liquid: acrylamide: proportion between N ' N methylene-bisacrylamide three be (80 ~
110) ml:(15~25) g:(1~3) g。
The speed of service of the ball mill is 400 ~ 600rpm, and runing time is 3 ~ 5 hs.
The citric acid of 1.5 ~ 2g is added in every 90 ~ 100ml slurry.
The concentration of the ammonium persulfate is 5 ~ 10 wt.%, and additional amount is that 1 ~ 3ml is added in every 100ml.
Described cube of six gang moulds tool is having a size of 20 ~ 30mm.
For the material from room temperature to 600 DEG C, heating rate is 0.5 ~ 2 DEG C/min, keeps the temperature 1 ~ 2h.
The sintering temperature of the material is 650 ~ 800 DEG C, and soaking time is 1 ~ 3h.
A kind of floating bead/hollow microsphere/borosilicate glass buoyant material preparation method of the invention has the beneficial effect that
(1) using hollow glass microballoon as filler material, can play reduces density and raising pressure resistance to a certain extent for this experiment
The effect of degree.
(2) citric acid being added in experiment, can play good peptizaiton to powder in slurry;
(3) using pyrex as matrix in experiment, for preparation there is good durothermic buoyant material to provide guarantee.
(3) using fly ash float as filler material in experiment, it can play improve the durothermic work of material to a certain extent
With.
(4) it can obtain that there are different mechanicalnesses from the mass ratio of hollow glass microballoon by adjusting fly ash float
Fly ash float-hollow glass microballoon/borosilicate glass material of energy, hot property and physical property.
(5) experimental method is simple, easy to operate, and the hollow glass microballoon/pyrex prepared using this method is floating
Dead-wood material mechanical performance with higher and preferable temperature tolerance.
Detailed description of the invention
Fig. 1 is the floating bead/hollow microsphere/borosilicate glass buoyant material prepared in embodiment 1, respectively through 650 DEG C,
700 DEG C, 750 DEG C of sintered scanning electron microscope diagrams.
Specific embodiment
Prepare premixed liquid using distilled water, acrylamide, N ' N methylene-bisacrylamide and citric acid as raw material, then to
A certain amount of borosilicate glass is added in premix, a certain amount of fly ash float is added after ball milling mixing is uniform in
Empty glass microsphere is added a certain amount of ammonium persulfate, is poured into mold after being uniformly mixed, through molding, drying and sintering
Etc. obtain floating bead/hollow microsphere/borosilicate glass buoyant material after technical process, with reference to the accompanying drawings and examples to this hair
It is bright to be described further:
Embodiment 1
A kind of floating bead/hollow microsphere/borosilicate glass buoyant material preparation method, its step are as follows:
(1) preparation of premixed liquid
With distilled water, acrylamide in this embodiment, N ' N methylene-bisacrylamide and citric acid prepare premixed liquid, and three kinds
Ratio be 100ml:15g:1.5g:1.4g, it is spare;
(2) fly ash float-hollow glass microballoon/pyrex green body preparation
A certain amount of borosilicate glass is added into premixed liquid, after revolving speed is the planetary ball mill ball milling 4h of 600rpm,
A certain amount of fly ash float and hollow glass microballoon are added into mixed liquor, wherein the solid content in slurry is 40 wt.%,
The particle diameter distribution of hollow glass microballoon is 0 ~ 75 μm, and average grain diameter is 40 μm, and the additional amount of borosilicate glass is 20 wt.%,
The quality of microballoon and borosilicate glass is 1:1, the uniformly rear solution (0 that the ammonium persulfate that concentration is 10 wt.% is added to be mixed
~ 2ml), it stirs evenly, then by six gang mould of slurry cast to 20mm × 20mm × 20mm tool, through 50 DEG C of curing moldings, dries
After sintering, fly ash float-hollow glass microballoon/borosilicate glass buoyant material is obtained.
By the green body of material respectively after being sintered under the conditions of 650 DEG C, 700 DEG C and 750 DEG C, in obtained fly ash float-
The density of empty glass microsphere/borosilicate glass material is respectively 0.356,0.685 and 0.855g/cm3.
From fly ash float-hollow glass microballoon/borosilicate glass buoyant material through 700 DEG C of sintered scanning electron microscope
As can be seen that the material has the characteristics that porous pore structure of holding one's breath in figure.
Claims (9)
1. a kind of floating bead/hollow microsphere/borosilicate glass buoyant material preparation method, it is characterised in that: the material preparation side
Steps are as follows for method,
(1) pretreatment of fly ash float:
Raw material is weighed, a certain amount of fly ash float is put into distilled water, is stirred, after standing 5 ~ 10min, by the drift on upper layer
Pearl is taken out, and is placed in surface plate, is dried in 90 ~ 110 DEG C of electric drying oven with forced convection, spare;
(2) pretreatment of hollow glass microballoon:
Raw material is weighed, a certain amount of hollow glass microballoon is put into the beaker for filling distilled water, is stirred, it is quiet after 10 ~ 20min
It sets, after hollow glass microballoon and water are layered completely, upper layer microballoon is taken out, is placed in surface plate, in 80 ~ 100 DEG C of baking oven
Drying, it is spare;
(3) preparation of premixed liquid:
Using distilled water as solvent, acrylamide and N, N '-methylene-bisacrylamide are respectively that monomer and crosslinking agent are pre- to prepare
Mixed liquid, citric acid is as dispersing agent;
(4) preparation of slurry:
A certain amount of borosilicate glass is added in the premixed liquid of (3), after a certain period of time through high speed planetary ball mill ball milling,
The mixed liquor containing borosilicate glass is obtained, is then added to hollow glass microballoon and fly ash float according to a certain ratio
It in mixed liquor, is stirred continuously, is uniformly mixed, it is spare;
(5) fly ash float-hollow glass microballoon/borosilicate glass buoyant material preparation:
Be added a certain amount of ammonium persulfate in slurry in (4), it is to be mixed uniformly after, slurry is poured into mold and constantly
Mold, is then placed in 40 ~ 50 DEG C of baking ovens, half-dried green body is obtained after demoulding to be formed, after drying and sintering, obtain by oscillation
To fly ash float-hollow glass microballoon/borosilicate glass solid buoyancy material.
2. a kind of floating bead/hollow microsphere/borosilicate glass buoyant material preparation method according to claim 1, special
Sign is: the particle diameter distribution of fly ash float is 80 ~ 200 mesh;The particle diameter distribution of hollow glass microballoon is 0 ~ 100 μm.
3. a kind of floating bead/hollow microsphere/borosilicate glass buoyant material preparation method according to claim 1, special
Sign is: the content of the solid in slurry is 10 ~ 50 wt.%;10 ~ 40 wt.% of additional amount of pyrex.
4. a kind of floating bead/hollow microsphere/borosilicate glass buoyant material preparation method according to claim 1, special
Sign is: the mass ratio of microballoon (including hollow glass microballoon and fly ash float) and pyrex is 0 ~ 2:1;Distilled water:
Acrylamide: the proportion between N ' N methylene-bisacrylamide three is (80 ~ 110) ml:(15 ~ 25) g:(1 ~ 3) g.
5. a kind of floating bead/hollow microsphere/borosilicate glass buoyant material preparation method according to claim 1, special
Sign is: ball mill is when preparing mixed slurry with 400 ~ 600rpm high speed ball milling, 3 ~ 5 hs.
6. a kind of floating bead/hollow microsphere/borosilicate glass buoyant material preparation method according to claim 1, special
Sign is: the citric acid of 1.5 ~ 2g is added in slurry in every 90 ~ 100ml.
7. a kind of floating bead/hollow microsphere/borosilicate glass buoyant material preparation method according to claim 1, special
Sign is: the concentration of ammonium persulfate solution is 5 ~ 10 wt.%, and the middle additional amount of every 100ml slurry is 1 ~ 3ml.
8. a kind of floating bead/hollow microsphere/borosilicate glass buoyant material preparation method according to claim 1, special
Sign is: used cube of six gang moulds tool is having a size of (20 ~ 30) mm × (20 ~ 30) mm × (20 ~ 30) mm.
9. a kind of floating bead/hollow microsphere/borosilicate glass buoyant material preparation method according to claim 1, special
Sign is: when being sintered to green body, from room temperature to 600 DEG C, heating rate is 0.5 ~ 2 DEG C/min, keeps the temperature 1 ~ 2h;
Sintering temperature is 650 ~ 800 DEG C, and soaking time is 1 ~ 3h.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112897897A (en) * | 2020-05-10 | 2021-06-04 | 中国科学院理化技术研究所 | Method for improving durability of hollow glass microspheres and hollow glass microspheres obtained by same |
WO2023076138A1 (en) * | 2021-10-29 | 2023-05-04 | Corning Incorporated | Composition and methods for making glass ceramic porous structures |
Citations (1)
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CN102674662A (en) * | 2012-05-28 | 2012-09-19 | 中国海洋大学 | Process for preparing hollow glass-ceramics microballoon sphere |
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2017
- 2017-09-07 CN CN201710801676.4A patent/CN109467314A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102674662A (en) * | 2012-05-28 | 2012-09-19 | 中国海洋大学 | Process for preparing hollow glass-ceramics microballoon sphere |
Non-Patent Citations (2)
Title |
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SUE REN等: "Mechanical properties and thermal conductivity of a temperature resistance hollow glass microspheres/borosilicate glass buoyance material", 《MATERIALS SCIENCE & ENGINEERING A》 * |
郑斌: "低铝高硼硅固体浮力材料的制备及研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112897897A (en) * | 2020-05-10 | 2021-06-04 | 中国科学院理化技术研究所 | Method for improving durability of hollow glass microspheres and hollow glass microspheres obtained by same |
WO2023076138A1 (en) * | 2021-10-29 | 2023-05-04 | Corning Incorporated | Composition and methods for making glass ceramic porous structures |
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