CN1262243A - Refractory vagcor product and its preparing process - Google Patents
Refractory vagcor product and its preparing process Download PDFInfo
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- CN1262243A CN1262243A CN 00111493 CN00111493A CN1262243A CN 1262243 A CN1262243 A CN 1262243A CN 00111493 CN00111493 CN 00111493 CN 00111493 A CN00111493 A CN 00111493A CN 1262243 A CN1262243 A CN 1262243A
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Abstract
A process for preparing the high-accuracy large shaped or profiled refractory products from porous high-siloxy glass by special ceramic injection technology, especially for preparing high-siloxy glass bowl, is disclosed. Said products feature excellent performance.
Description
The invention belongs to the field shaping technique of inorganic materials, relate to a kind of preparation technology of refractory product, relate in particular to the high silica porous glass preparation technology of large-scale, special-shaped, the high-precision refractory product that is material.
" vagcor " is that nineteen thirty-nine is just sold related products with the Vycor name by Corning Incorporated's at first invention in 1934.Vagcor is at first to make high silica porous glass through phase-splitting, acid treatment by borosilicate glass, forms through sintering again.Its SiO
2Content is about 96%, and has the plurality of advantages that is similar to fused silica glass, and as heat resisting temperature height (can use repeatedly below 800 ℃), the coefficient of expansion is little by (＜8 * 10
-7/ ℃), heatproof acute degeneration good (can stand the thermal shocking more than 1000 ℃) etc.Be mainly used in and make that some are heat-resisting, the glasswork of printing opacity, thin-walled, as high-power fluorescent tube, burn device etc.High silica porous glass then can be used for materials such as catalyst base, liquid filtering, gas absorption and doping treatment.Because material can produce bigger swelling effect in the acid treatment process, bigger volumetric shrinkage appears in sintering process, so be very easy to cracking even broken, this has just limited the size and dimension of vagcor goods, maximum ga(u)ge is no more than 10mm usually.
Many patents, document disclose or have reported the technology relevant with high silica porous glass, as: [1] " manufacturing of micropore glass " silicate journal [1] (1989) 38～44[2] " Method of Making High Silica Glass " USP 2355746 (1944) [3] " Properties of Some Vycor-Brand Glass " J.Am.Ceram.Soc.27[10] (1944) 299～305[4] " Method of Making Ulatraviolet Transmitting High Silica Glass " USP 2505001 (1950) [5] " Method of Leaching High Silica Glass Having 0.5～2.0%P2O
5" USP3785793 (1974) [6] " Effect of Heat-treatment on the Density and Constitution of High-silica Glasses of the Borosilicate Type " J.Am.Ceram.Soc.31[7] (1948) 177～86[7] " Scanning Electron Micrographs of Phase-separated Glasses in TheSystem Na
2O-B
2O
3-SiO
2" J.Am.Ceram.Soc.53[1] (1970) 64[8] " HCl Leaching Rate and Microstructuer of Phase-SeparatedBorosilicate Glasses " and J.Am.Ceram.Soc.61[11～12] (1978) 509～12.
The content that above-mentioned patent or document relate to is mainly: the compositing range of borosilicate glass, parvafacies mechanism, the preparation technology of high silica porous glass, the sintering process of vagcor, the performance of vagcor and possible application or the like.And be that the technology of large-scale, the special-shaped refractory product of feedstock production aspect is not reported with the high silica porous glass.
The ceramic grout moulding is a kind of traditional technology of producing pottery or fire resistive material product, is about to ceramic raw material and makes slip, is cast in moulding in the plaster mold, and demoulding after drying is agglomerating technology again.The large-scale refractory product of applying mechanically ceramic grout moulding and sintering process production simply and with the high silica porous glass be raw material obviously is impossible, must adopt special complete processing.Because the refractory product of vagcor material has and the visibly different excellent properties of other refractory materialss, as: SiO
2Content height (＞95%) can not produce pollution to the silicate glass melt; Apparent porosity little (＜1%) is difficult for introducing bubble in the glass melt, and strengthens the resistance to fouling of goods; The coefficient of expansion is little by (＜8 * 10
-7/ ℃), temperature resistance acute degeneration good (can stand the thermal shocking more than 1000 ℃), refractory product can directly be put into high temperature (＞1000 ℃) and use, and can not burst.Therefore, developing as early as possible with the high silica porous glass is that the preparation technology of high-precision refractory product of material has become pressing for of especially colored and black and white kinescope glass bulb manufacturing enterprise of branch of industry.
The object of the present invention is to provide a kind of is the preparation technology of the high-precision refractory product of material, the especially preparation technology of vagcor orifice ring with the high silica porous glass, to satisfy the needs of relevant department.
Design of the present invention is such:
With the high silica porous glass is raw material, under specific processing condition, adopts the moulding of ceramic grout method, drying, sintering again, and cold working prepares the refractory product of all kinds of large-scale, special-shaped, high-compactness.According to above-mentioned design, the present invention proposes technical scheme as described below:
1. at first adopt a kind of SiO of prior art for preparing
2Content is about 96%, and the glass porosity reaches 30～40%, the porous borosilicate glass of aperture＜100nm, and preparation process is summarized as follows:
The selection borosilicate glass consists of: SiO
260～65%, B
2O
325～30%, Na
2O 5～10%, add a small amount of Al again
2O
3The phase-splitting of (＜3%) feed glass.High temperature melting under 1400 ℃～1450 ℃ conditions reaches discharging after clarification, the homogenizing.The borosilicate ternary phase diagrams can provide this system glass at broad temperature and compositing range in have the branch phase behaviour, promptly be divided into high silicon mutually with sodium boron mutually.When form and the thermal treatment temp selection proper, can obtain the communicate-type phase-splitting, help the leaching of sodium boron phase.Phase separation temperature is controlled at 550 ℃～650 ℃ for well, 10～30 hours phase-splitting time.Handle with 1～3N hydrochloric acid or sulfuric acid leaching, treat the stripping fully mutually of sodium boron, washing oven dry again obtains a kind of SiO
2Content is about 96%, and the glass porosity reaches 30～40%, the porous borosilicate glass of aperture＜100nm;
2. adopt the ceramic grout moulding again the agglomerating prepared be the high-precision refractory product of material, especially vagcor orifice ring with the high silica porous glass.
Because the porosity characteristic of high silica porous glass material must strictly be controlled its every processing parameter in slip preparation, injection forming, drying and sintering process, in order to avoid the goods generation is inhomogeneous, form pore, even occurs significantly being out of shape or ftractureing.This process mainly may further comprise the steps:
(1) moulding of refractory vagcor product:
High silica porous glass behind the cleaning-drying, at material-water ratio is 1: ball milling slurrying under the condition of (0.4～0.6) (weight ratio), obtaining median size is the slip of 5～15 μ m, casting in plaster mold, suction time generally was controlled at 12～24 hours according to products thickness and difference is the goods of 30～50mm for maximum ga(u)ge, inhale the slurry temperature and must be higher than 10 ℃, be preferably 15 ℃～25 ℃;
(2) demoulding drying:
Demoulding drying after waiting to inhale slurry and finishing, necessary strict controlled temperature of drying process and humidity, usually (temperature: 30～50 ℃ under the high humidity constant temperature, humidity: greater than 90%) continue 2～3 days, the dehumidification that progressively heats up again is warming up to 110 ℃～130 ℃ gradually in 3～4 days, heat up about 20～30 ℃ every day, humidity is reduced to below 20%, makes goods reach constant weight.Thorough drying is to make the prerequisite of qualified product;
(3) sintering of refractory vagcor product:
Because these goods are to be raw material with the porous borosilicate glass, biscuit after the cryodrying still contains a certain amount of moisture content in nanometer level microporous, only in sintering process, could further remove, for preventing the goods cracking, must strict control temperature rise rate before moisture content removes fully.Micropore will produce contraction in the goods between 800～1200 ℃, if temperature distributing disproportionation in heat up too fast or the stove can produce bigger string stress, so that destroy goods, so suitably insulation in this temperature range.The micron order hole that the mud particle cast forms needs higher temperature to get rid of, this also is the key of densification sintering, usually sintering under near the softening temperature condition, but must prevent crystallization, otherwise cracking can appear in the goods cooling or the back step course of processing;
Sintering process is divided into three phases:
Fs is the thorough drying stage: room temperature to 780 ℃～820 ℃, 10 ℃/min of temperature rise rate～30 ℃/min;
Subordinate phase is the nanometer level microporous contraction phase: temperature is risen to 1100 ℃～1200 ℃, every 100 ℃ of insulation 40min～60min;
Phase III is a particle packing pore elimination phase: temperature is risen to 1450～1500 ℃, and temperature rise rate is 80～100 ℃/min;
(4) cold working of refractory vagcor product:
Refractory vagcor product, especially vagcor orifice ring in use must with good combination such as feed basin, heating collar, the size of discharge port also because of load is different must strict control, the smooth finish requirement that each surface, position is different because of the contactant difference has.The conventional cold working method of glass material can be adopted,, said refractory vagcor product can be obtained as hard abrasion wheel grindings such as diamonds etc.
Below will relevant details of the present invention be further described by embodiment.
Embodiment 1
Before address, orifice ring be colored and the black and white kinescope glass bulb produce in the expendable parts of key, Fig. 1 is the synoptic diagram of said orifice ring.Fig. 2 is the vertical view of Fig. 1.Maximum thickness δ is 30mm, and the goods blank thickness is 40mm, and its preparation process is as follows:
(1) preparation of high silica porous glass: borosilicate glass is formed: SiO
260%, B
2O
330%, Na
2O 7.5%, Al
2O
32.5%, glass melting temperature: 1440 ℃, phase separation temperature: 600 ℃ of phase-splittings 20 hours, acid treatment: 3N sulfuric acid was handled 48 hours for 95 ℃, promptly obtained said high silica porous glass.
(2) vagcor orifice ring moulding:
Above-mentioned high silica porous glass is put into ball mill slurrying, and material-water ratio is 1: 0.5, and the median size of slip is 10 μ m, and above-mentioned slip is injected the plaster mould moulding, and suction time is 18 hours, and inhaling the slurry temperature is 20 ℃, demoulding drying after 20 hours;
It is 40 ℃ that biscuit is placed on temperature, and humidity is under 95% the condition dry 2 days, with every day 20 ℃ of temperature rise rates be warming up to 120 ℃, make goods reach constant weight;
(3) vagcor orifice ring sintering
Dried product is placed sintering oven, rise to 800 ℃ with 20 ℃/hour temperature rise rates, respectively be incubated 50 minutes at 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃ then, rise to 1500 ℃ of insulations with 80 ℃ of/hour temperature rise rates then and close the stove cooling after 10 minutes, can obtain said vagcor orifice ring blank, finish preparation through cold working again.
After tested, the performance of high silica porous glass orifice ring is as follows: (1) material is the vagcor body, SiO
2Content is greater than 95%.(2) coefficient of expansion is less than 8 * 10
-7/ ℃.(3) volume density is greater than 2.1g/cm
3(4) void content is less than 1%.(5) product surface is bright and clean, pore-free, flawless.(6) thermal shock resistance is good, and high temperature (1100 ℃) is changed orifice ring and do not ftractureed.
By above-mentioned disclosed technical scheme and embodiment as seen, the product properties excellence that said method is prepared can satisfy the needs of explained hereafter fully.Obviously, according to technology disclosed by the invention, the relevant personnel can lift one and turn over the vagcor goods that three ground are used to make other types.This also within the scope of the invention.
Claims (5)
1. the preparation technology of a refractory vagcor product is characterized in that, mainly comprises the steps:
1. the moulding of refractory vagcor product:
With the high silica porous glass behind the cleaning-drying, ball milling slurrying is at plaster mould
Casting in the type;
2. demoulding drying:
Demoulding drying after waiting to inhale slurry and finishing is 30 ℃～50 ℃ in temperature, high humidity
Under 90% condition, continue 2～3 days; Heat up 20 ℃～30 ℃ then every day,
Be warming up to 110 ℃～130 ℃;
3. the sintering of refractory vagcor product:
Fs is by room temperature to 780 ℃～820 ℃;
Subordinate phase rises to 1100 ℃～1200 ℃ with temperature;
Phase III rises to 1450 ℃～1500 ℃ with temperature, can obtain said
Refractory vagcor product.
2. preparation technology as claimed in claim 1 is characterized in that, ball milling slurrying is 1 at material-water ratio: carry out under the condition of (0.4～0.6) weight ratio.
3. preparation technology as claimed in claim 1 is characterized in that, the refractory vagcor product that 3. step is obtained adopts conventional glass material cold working method to process.
4. preparation technology as claimed in claim 1 is characterized in that, step 3. fs temperature rise rate is 10 ℃/min～30 ℃/min; Subordinate phase is every 100 ℃ of insulation 40min～60min; The phase III temperature rise rate is 80～100 ℃/min.
5. preparation technology as claimed in claim 1 is characterized in that: can be used to prepare the vagcor orifice ring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00111493A CN1098219C (en) | 2000-01-25 | 2000-01-25 | Refractory vagcor product and its preparing process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00111493A CN1098219C (en) | 2000-01-25 | 2000-01-25 | Refractory vagcor product and its preparing process |
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| Publication Number | Publication Date |
|---|---|
| CN1262243A true CN1262243A (en) | 2000-08-09 |
| CN1098219C CN1098219C (en) | 2003-01-08 |
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167500A (en) * | 2011-01-10 | 2011-08-31 | 圣戈班石英（锦州）有限公司 | Preparation method of non-transparent quartz labware |
| CN102167499A (en) * | 2011-01-10 | 2011-08-31 | 圣戈班石英（锦州）有限公司 | Manufacturing method of quartz ceramic container |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2719674C1 (en) * | 2019-10-09 | 2020-04-21 | Общество с ограниченной ответственностью "ЛЕТО" | Method of making a glass article and an article made by such method |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2514876B2 (en) * | 1991-08-31 | 1996-07-10 | 信越石英株式会社 | Method for producing synthetic quartz glass molded body for optics |
| JPH05201736A (en) * | 1991-10-25 | 1993-08-10 | Furukawa Electric Co Ltd:The | Production of porous parent material for quartz glass |
| US5248638A (en) * | 1992-04-06 | 1993-09-28 | Corning Incorporated | Yellow high silica glass |
-
2000
- 2000-01-25 CN CN00111493A patent/CN1098219C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167500A (en) * | 2011-01-10 | 2011-08-31 | 圣戈班石英（锦州）有限公司 | Preparation method of non-transparent quartz labware |
| CN102167499A (en) * | 2011-01-10 | 2011-08-31 | 圣戈班石英（锦州）有限公司 | Manufacturing method of quartz ceramic container |
| CN102167500B (en) * | 2011-01-10 | 2013-01-09 | 圣戈班石英（锦州）有限公司 | Preparation method of non-transparent quartz labware |
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| Publication number | Publication date |
|---|---|
| CN1098219C (en) | 2003-01-08 |
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