CN109384390A - A kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method - Google Patents
A kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method Download PDFInfo
- Publication number
- CN109384390A CN109384390A CN201710661741.8A CN201710661741A CN109384390A CN 109384390 A CN109384390 A CN 109384390A CN 201710661741 A CN201710661741 A CN 201710661741A CN 109384390 A CN109384390 A CN 109384390A
- Authority
- CN
- China
- Prior art keywords
- borosilicate glass
- particle size
- different particle
- size distribution
- material preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Glass Compositions (AREA)
Abstract
A kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method, the material that this method obtains include 1. lower low close and higher compression strength；2. lower thermal conductivity and preferable durothermic feature.The preparation method simple process of this material, it tests easy to operate, and prepared material has the characteristics that different particle diameter distributions, in conjunction with the features such as higher mechanical performance and higher temperature tolerance, the material can potential application in terms of buoyant material with temperature tolerance demand.
Description
Technical field
The invention belongs to structural material preparation technical field, in particular to a kind of different particle size distribution hollow microsphere/borosilicate
Silicate glass material preparation method.
Background technique
The world today is continued to develop with economy, and the mankind continually develop natural resources, and land resources are used as to be divided in the world
Cloth is 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, contain abundant mineral resources, Ocean energy resource is the long-range hair in the world
Exhibition provides a reliable material guarantee, and construction and Development of Marine become the inexorable trend of current social development.Currently, deep-sea
Exploitation is observed in deep-sea field mainly based on deep submergence technology, using benthoscope, measures, samples, installing necessity
Instrument etc. carry out underwater operation.When the mankind can not reach deep-sea, various Exploratory behaviors will then lean on underwater robot auxiliary
It completes.Judging from the current situation, benthoscope, especially deep sea manned submersible, be ocean development foreword and commanding elevation it
One.
Firstly, during exploration, the mankind will also be faced with huge difficult and challenge, in addition to will be by from depth
Outside marine 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.Material is answered with higher incompressible by force to cope with the immense pressure in deep-sea at this time.Secondly, material property is also possible to meeting
It is influenced by particular surroundings, such as when carrying out the transmitting of some equipment in deep-sea, such as torpedo, anti-warship guided missle is emitting
In the process, be often related to huge temperature change, from tens degree to several Baidu even thousands of degree.Material should have good at this time
Good temperature tolerance is to cope with temperature great variety brought by external environment, so that other performances of material are unaffected.Therefore,
Based on above-mentioned both sides problem, preparation highly resistance compressive strength and preferable durothermic solid buoyancy material are proposed huge
Challenge.
Summary of the invention
For the application in terms of the problem of solid buoyancy material temperature tolerance difference at this stage, especially following deep-sea field, originally
Invention is prepared for hollow glass microballoon/borosilicate glass inoganic solids buoyancy with good durothermic different particle size distribution
Material, the material also have good temperature tolerance in addition to having the characteristics that low-density and advantages of higher compressive strength, furthermore the material
The features such as preparation method has controllability, simple process well, does not generate pollution.
A kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method of the present invention, includes the following steps:
(1) preparation of borosilicate glass mixed liquor
With the tert-butyl alcohol for (TBA) solvent, acrylamide (AM) and N, N '-methylene-bisacrylamide (MBAM) be respectively monomer and
Crosslinking agent tests required premixed liquid to prepare；A certain amount of borosilicate glass is added in premixed liquid, it is planetary through high speed
After ball mill ball milling, the mixed liquor containing borosilicate glass is obtained；
(2) hollow glass microballoon/borosilicate glass material preparation
A certain amount of hollow glass microballoon is added in the mixed liquor of above-mentioned (1), and is that it is mixed under the action of magnetic agitation
It closes uniformly, obtains hollow glass microballoon/pyrex slurry, it is molten that initiator ammonium persulfate is added in the slurry in (4)
Liquid 2 ~ 3ml, it is to be mixed uniformly after, slurry is poured into mold and constantly oscillation is to remove the bubble in slurry, then by band
There is the mold of slurry to be placed in 40 ~ 50 DEG C of baking ovens, demoulding to be formed obtains half-dried green body；By green body half-dried after demoulding through dry
Hollow glass microballoon/pyrex material is obtained after dry, sintering.
10 ~ 50 wt.% of additional amount of the hollow glass.
The particle diameter distribution of the hollow glass microballoon is 0 ~ 100 μm.
The mass ratio of the hollow glass microballoon and borosilicate glass is 0.3:1 ~ 2:1.
Proportion in the premixed liquid between TBA:AM:MBAM three is (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 8 ~ 10 wt.%.
Described cube of six gang moulds tool is having a size of 20 ~ 30mm.
A kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method of the present 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, guarantee is provided to prepare good durothermic buoyant material.
(4) in experiment hollow glass microballoon/borosilicate glass material for preparing hold one's breath the aperture in hole can be by adding
Enter the method for the hollow glass microballoon with different particle size distribution and different sintering temperatures to adjust；
(5) can by adjust hollow glass microballoon obtain from the mass ratio of borosilicate glass having different mechanical performances,
Hollow glass microballoon/borosilicate glass material of hot property and physical property.
(6) 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 hollow glass microballoon/borosilicate glass buoyant material prepared in embodiment 1, after 650 DEG C of sintering,
Its scanning electron microscope diagram and hole graph of pore diameter distribution of holding one's breath accordingly.
Fig. 2 is the hollow glass microballoon/borosilicate glass buoyant material prepared in embodiment 1, after 700 DEG C of sintering,
Its scanning electron microscope diagram and hole graph of pore diameter distribution of holding one's breath accordingly.
Fig. 3 is the hollow glass microballoon/borosilicate glass buoyant material prepared in embodiment 1, after 750 DEG C of sintering,
Its scanning electron microscope diagram and hole graph of pore diameter distribution of holding one's breath accordingly.
Specific embodiment
Premixed liquid is prepared using distilled water, acrylamide, N ' N methylene-bisacrylamide and citric acid as raw material, then in advance
A certain amount of hollow glass microballoon and borosilicate glass are added in mixed liquor, by evenly mixing after, be then poured into mold,
Under the action of initiator ammonium persulfate, hollow glass microballoon/borosilicate is obtained after the processes such as overmolding, drying and sintering
The buoyant material of glass,
Present invention will be further explained below with reference to the attached drawings and examples:
Embodiment 1
A kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method, its step are as follows:
(1) preparation being pre-mixed
Premixed liquid is configured with distilled water, acrylamide and N ' N methylene-bisacrylamide in this embodiment, three kinds of ratio is
100ml:15g:1.5g；
(2) hollow glass microballoon/pyrex green body preparation
A certain amount of hollow glass microballoon and borosilicate glass are added into premixed liquid, wherein the solid concentration of slurry is 45
The mass ratio of wt.%, hollow glass microballoon and borosilicate glass is 6:4, under the action of magnetic agitation, is uniformly mixed, will be dense
Degree is in the slurry that the solution (0 ~ 2ml) of the ammonium persulfate of 10 wt.% is added dropwise to, then by the slurry cast mixed to 20mm
In six gang mould of × 20mm × 20mm tool, through 50 DEG C of curing moldings, after dry and sintering, hollow glass microballoon/borosilicate is obtained
The buoyant material of glass.
The hollow glass microballoon prepared in experiment/borosilicate glass buoyant material is in 650 DEG C, 700 DEG C and 750 DEG C conditions
Under density be respectively 0.356,0.685 and 0.855g/cm3。
Fig. 1, Fig. 2, Fig. 3 are that the hollow glass microballoon/borosilicate glass buoyant material prepared in embodiment 1 passes through respectively
650 DEG C, 700 DEG C and 750 DEG C sintered scanning electron microscope (SEM) photographs, as can be seen from the figure after different temperatures is sintered, material tool
There is the characteristics of different particle diameter distributions.
Claims (9)
1. a kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method, it is characterised in that: preparation method step
It is rapid as follows
(1) pretreatment of HGMs:
The HGMs is the abbreviation of hollow glass microballoon, weighs raw material, a certain amount of HGMs is put into the beaker for filling water,
It stirs, is stood after 10min ~ 20min, after microballoon and water are layered completely, upper layer microballoon is taken out, is placed in surface plate, 80 DEG C ~
It is dried in 100 DEG C of baking oven, it is spare；
(2) preparation of premixed liquid:
With the tert-butyl alcohol for (TBA) solvent, acrylamide (AM) and N, N '-methylene-bisacrylamide (MBAM) be respectively monomer and
Crosslinking agent prepares premixed liquid；
(3) preparation of mixed liquor:
A certain amount of borosilicate glass is added in the premixed liquid of (2), after high speed planetary ball mill ball milling, is contained
The mixed liquor of borosilicate glass；
(4) preparation of slurry:
After a certain amount of HGMs is added in mixed liquor in (3), it is uniformly mixed under the action of magnetic agitation, it is spare；
(5) it forms:
In slurry in (4) be added 2 ~ 3ml of initiator ammonium persulfate solution, it is to be mixed uniformly after, slurry is poured into mold
In and constantly oscillation to remove the bubble in slurry, then will be placed in 40 ~ 50 DEG C of baking ovens with the mold of slurry, it is to be formed de-
Mould obtains half-dried green body；
(6) dry:
After green body half-dried after demoulding is dried 1 ~ 2d in air, it is then placed into 50 ~ 60 DEG C of air dry oven and dries
12h；
(7) dumping:
Green body obtained in (6) is risen to 600 DEG C from room temperature with the heating rate of 1 ~ 2 DEG C/min, keeps the temperature 1 ~ 2h；
(8) it calcines:
Green body in (7) after dumping is sintered respectively at 650 DEG C ~ 800 DEG C, heating rate is 1 ~ 2 DEG C/min, when heat preservation
Between be 2 ~ 3h, finally obtain the hollow glass microballoon with different particle size distribution/borosilicate glass inoganic solids buoyancy material
Material.
2. a kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method according to claim 1,
It is characterized in that: 10 ~ 50 wt.% of additional amount of hollow glass.
3. a kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method according to claim 1,
Be characterized in that: the particle diameter distribution of hollow glass microballoon is 0 ~ 100 μm.
4. a kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method according to claim 1,
Be characterized in that: the mass ratio of hollow glass microballoon and borosilicate glass is 0.3:1 ~ 2:1.
5. a kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method according to claim 1,
Be characterized in that: the proportion between TBA:AM:MBAM three is (80 ~ 110) ml:(15 ~ 25) g:(1 ~ 3) g.
6. a kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method according to claim 1,
Be characterized in that: when preparing mixed liquor, ball mill is with 400 ~ 600rpm speed ball milling, 3 ~ 5 hs.
7. a kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method according to claim 1,
Be characterized in that: the citric acid of 1.5 ~ 2g is added in every 90 ~ 100ml slurry.
8. a kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method according to claim 1,
Be characterized in that: the concentration of ammonium persulfate is 8 ~ 10 wt.%.
9. a kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method according to claim 1,
Be characterized in that: used cube of six gang moulds tool is having a size of 20 ~ 30mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710661741.8A CN109384390A (en) | 2017-08-04 | 2017-08-04 | A kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710661741.8A CN109384390A (en) | 2017-08-04 | 2017-08-04 | A kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109384390A true CN109384390A (en) | 2019-02-26 |
Family
ID=65412323
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710661741.8A Pending CN109384390A (en) | 2017-08-04 | 2017-08-04 | A kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109384390A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109836048A (en) * | 2019-04-04 | 2019-06-04 | 周勇 | A kind of hollow glass microballoon composite inorganic solid buoyancy material and preparation method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674662A (en) * | 2012-05-28 | 2012-09-19 | 中国海洋大学 | Process for preparing hollow glass-ceramics microballoon sphere |
-
2017
- 2017-08-04 CN CN201710661741.8A patent/CN109384390A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 (3)
| Title |
|---|
| HAI XU等: "Preparation of porous silica ceramics with relatively high strength by a TBA-based gel-casting method", 《CHEMICAL ENGINEERING JOURNAL》 * |
| 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 (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109836048A (en) * | 2019-04-04 | 2019-06-04 | 周勇 | A kind of hollow glass microballoon composite inorganic solid buoyancy material and preparation method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103979938B (en) | The withstand voltage alumina-ceramic hollow float in a kind of deep-sea | |
| CN103113123B (en) | Preparation method of SiCf/SiC ceramic matrix composite turbine blades | |
| CN103665615B (en) | For the fiber bead and preparation method thereof of solid buoyancy material | |
| CN102702679B (en) | Preparation method for high-strength solid buoyancy material for deep submergence | |
| CN103496999B (en) | A kind of method adopting ceramic hollow ball to prepare porous ceramics | |
| AU2020102229A4 (en) | A preparation method of buoyancy material of floating beads/hollow microspheres/borosilicate glass | |
| CN105924225B (en) | A kind of preparation method of mullite bonded carborundum porous ceramics | |
| WO2018233449A1 (en) | High-strength polymer hollow microsphere, preparation method therefor, and phase transition energy storage microsphere | |
| CN104402446A (en) | Method for preparing porous silicon carbide ceramic | |
| CN104403261A (en) | Inorganic material-modified phenolic foam insulation material with low water absorption and preparation method thereof | |
| CN104942269B (en) | Device for improving foaming uniformity of foamed aluminum and foaming technology | |
| CN104003732A (en) | Ceramic mold vacuum degreasing method for gel-casting turbine blades | |
| CN103588482A (en) | Manufacture method of high porosity and high strength yttrium-silicon-oxygen porous ceramics | |
| CN103910520B (en) | Preparation method for aluminium oxide porous ceramic | |
| CN105294111A (en) | Gelcasting forming method of Si3N4 porous ceramic | |
| CN104446203A (en) | Inorganic non-metallic solid buoyancy material and producing method thereof | |
| CN109384390A (en) | A kind of different particle size distribution hollow microsphere/borosilicate glass material preparation method | |
| CN109467314A (en) | A kind of floating bead/hollow microsphere/borosilicate glass buoyant material preparation method | |
| CN105271177A (en) | Preparation method of graphene multilayer foam carbon material | |
| CN106083205B (en) | A kind of method that integral alumina base ceramic-mould elevated temperature strength is improved by chemical vapor infiltration | |
| CN104448719B (en) | Organic and inorganic hollow microsphere compounded deepwater buoyancy material and preparation method thereof | |
| CN105234344B (en) | A kind of lost foam casting special cooling coating and preparation method thereof | |
| CN109694240A (en) | A kind of preparation method of high temperature resistant floating bead/mullite solid buoyancy material | |
| CN113979746A (en) | Preparation method of oxide structure ceramic-based hollow floating ball | |
| CN109437946A (en) | A kind of method that aqueous gel casting prepares YSZ fiber-based porous ceramic |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190226 |
|
| WD01 | Invention patent application deemed withdrawn after publication |