CN1120819C - Process for preparing non-crack ceramic blank - Google Patents
Process for preparing non-crack ceramic blank Download PDFInfo
- Publication number
- CN1120819C CN1120819C CN00136867A CN00136867A CN1120819C CN 1120819 C CN1120819 C CN 1120819C CN 00136867 A CN00136867 A CN 00136867A CN 00136867 A CN00136867 A CN 00136867A CN 1120819 C CN1120819 C CN 1120819C
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- China
- Prior art keywords
- ceramic
- suspension
- suspensoid
- add
- ball milling
- 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.)
- Expired - Fee Related
Links
- 239000000919 ceramic Substances 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title 1
- 239000000725 suspension Substances 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 16
- 108090000790 Enzymes Proteins 0.000 claims abstract description 14
- 102000004190 Enzymes Human genes 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000012141 concentrate Substances 0.000 claims description 14
- 229940088598 enzyme Drugs 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 7
- 210000002700 urine Anatomy 0.000 claims description 6
- 108010015776 Glucose oxidase Proteins 0.000 claims description 4
- 239000004366 Glucose oxidase Substances 0.000 claims description 4
- 101000693619 Starmerella bombicola Lactone esterase Proteins 0.000 claims description 4
- 229940116332 glucose oxidase Drugs 0.000 claims description 4
- 235000019420 glucose oxidase Nutrition 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 150000002596 lactones Chemical class 0.000 claims description 2
- 238000012423 maintenance Methods 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- -1 methane amide Chemical class 0.000 claims description 2
- 230000001687 destabilization Effects 0.000 abstract 1
- 238000007711 solidification Methods 0.000 abstract 1
- 230000008023 solidification Effects 0.000 abstract 1
- 239000002002 slurry Substances 0.000 description 11
- 208000037656 Respiratory Sounds Diseases 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 230000008602 contraction Effects 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 206010011376 Crepitations Diseases 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 229940095686 granule product Drugs 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention relates to a preparation method for a ceramic body without cracks. Firstly, substrates are added to deionized water and thoroughly dissolved, and then, a thick ceramic suspension is added to a solution, the solution and the thick ceramic suspension are put in a ball milling tank, and the ball milling of the solution and the thick ceramic suspension is carried out; the vacuum defoaming of the solution and the thick ceramic suspension is carried out, and then, organism enzymes corresponding to the substrates are added to the thick ceramic suspension; after the suspension is shaken up, the pouring of the suspension is carried out, and the ceramic body without cracks of the present invention is obtained. In the method of the present invention, the syneresis in the process of the destabilization of the suspension is overcome through the control of the critical delay time before the pouring, and crack generation in the solidification of the ceramic body is avoided.
Description
The present invention relates to a kind of preparation method of non-crack ceramic blank, belong to by the stupalith of the different purposes of various colloidal formation prepared and the category of component.
By ceramic by colloidal molding method prepared ceramic component is one of main method of present forming ceramic.The preparation ceramic concentrate suspension be the gordian technique of all colloidal formation technologies, such as the solid load that directly solidifies injection molding and forming technology requirement suspensoid greater than 50vol.%.The solid load of suspensoid is high more, and the density of molding blank and degree of uniformity are high more.It not only can reduce sintering temperature, and the various defectives of may command molding blank.Forming base substrate by the ceramic concentrate suspension unstability has two kinds of approach, and a kind of is that the pH value of suspensoid is adjusted to iso-electric point, thereby forms ceramic body; Another kind method is to pass through to increase the ionic strength of suspensoid in concentrated suspension, makes the suspensoid curing molding.A kind of method in back is the category that the present invention relates to, and this method can produce a large amount of crackles in ceramic body.
Usually directly solidifying in the injection molding and forming technology, increasing ionic strength unstability ceramic concentrate suspension is a kind of main forming method, people are in order to obtain even flawless ceramic body, generally select for use high purity deionized water as suspension medium, and the suspensoid that rapidly unstability is begun after suspensoid begins unstability inject mould.But this method causes solidifying in the base substrate of back and contains in a large number vertically, laminar cracks.
The objective of the invention is to propose a kind of preparation method of non-crack ceramic blank, by the critical delay time before the control cast, to overcome the synersis in the suspensoid unstability process, avoid in the solidified base substrate, cracking, thus the molding blank q﹠r of raising stupalith.Here be meant that the suspensoid unstability begins to pouring into a mould before during this period of time mentioned time of lag.Critical delay time is meant the time of cast base substrate crackle disappearance afterwards.
The preparation method of a kind of non-crack ceramic blank that the present invention proposes comprises following each step:
1, preparation ceramic concentrate suspension: add the substrate of 0.2～5mol/l in deionized water, and make its thorough dissolving, add ceramic powder then in above-mentioned solution, volume ratio is: pottery: (water+pottery)=40～80: 100.
2, above-mentioned ceramic concentrate suspension is put into ball grinder, ball milling 12-48 hour.
3, the ceramic concentrate suspension behind the maintenance ball milling is 0-40 ℃ of following froth in vacuum.
4, the corresponding biological enzyme of substrate of the adding and the above-mentioned the first step in above-mentioned ceramic concentrate suspension, add-on is to add 1～600 milligram biological enzyme in every kilogram the ceramic powder, after 1-4 hour, suspensoid is shaken up the back cast, promptly get non-crack ceramic blank of the present invention.
The mechanism of action of the inventive method is made up of three phases, is described in detail below:
Fs does not observe the contraction of suspensoid, does not promptly have volume change.This is because suspensoid begins second mnm. that dispersed particles progressively is tending towards attracting each other after the unstability, and initial granuloplastic gel-strength is very weak, is not enough to intergranular moisture content is discharged, and does not therefore observe the volume change of suspension.In subordinate phase, the volume of suspensoid begins contraction and reaches stable until the suspensoid contraction.Therefore in this stage, the granuloplastic gel-strength that attracts each other strengthens gradually, and intergranular moisture content is discharged from gradually, and can observe has the very clear water layer of one deck on the surface of suspensoid.At three phases, the contraction of suspensoid reaches stable, because particle is positioned at second mnm., particle motion is a reversible, will increase in circumgranular ligancy of this stage, causes the intensity of base substrate to increase.
In fact crackle in the ceramic body is formed at second stage, the i.e. stage of suspensoid synersis.In this stage, suspensoid still can flow, so the generation of crackle does not cause owing to internal stress.At this moment therefore the whole gel-strength of the suspensoid contraction that is not enough to resist suspensoid has caused having produced in the suspensoid crackle.After suspensoid began unstability, a large amount of ion of biological enzyme bottom exploded deposits yields that the present invention uses was waited for then to critical delay time, the suspensoid that contains crackle that has formed is shaken up, to destroy established structure, cast can be avoided the generation of crackle again.
Introduce embodiments of the invention below:
Embodiment 1:
α-Al
2O
3Be commercially available high-purity (＞99.99%) raw material, particulate moment of volume mean diameter is 0.5 μ m, and shape is even.The ceramic concentrate suspension of preparation 57vol.% adds the urea of 2.2mol/l as substrate in deionized water during formulated suspension.The suspensoid of process ball milling after 24 hours be froth in vacuum at first, then slurry is cooled to 5 degree, will urinate enzyme again and be added in the refrigerative slurry.The add-on of urine enzyme is to add 20 milligrams urine enzyme in 1 kilogram the aluminum oxide.Wait for after 150 minutes slurry is shaken up cast again, can obtain the intact ceramic body of flawless.
Embodiment 2:
SiC and be commercially available commercial powder, average particle size particle size 0.7 μ m, preparation 62vol.% ceramic concentrate suspension.In deionized water, add the 6mol/l lactone during formulated suspension as substrate.The suspensoid of process ball milling after 24 hours be froth in vacuum at first, and slurry temperature is remained on room temperature, lactonase is added in the slurry again.The add-on of lactonase is to add 230 milligrams lactonase in 1 kilogram the silicon carbide.Cast again after waiting for 90 minutes then with slurry and shaking up can obtain the intact ceramic body of flawless.
Embodiment 3:
Si
3N
4Be commercially available commercial powder, granule product moment mean diameter is 0.6 μ m.In deionized water, add a certain amount of methane amide during formulated suspension as substrate.The ceramic suspension body of preparation 64vol.%.Slurry at room temperature adds a certain amount of urine enzyme through after 48 hours the ball milling.The add-on of urine enzyme is to add 100 milligrams urine enzyme in 1 kilogram the silicon carbide.Cast again after waiting for 90 minutes then with slurry and shaking up can obtain flawless ceramic body.
Embodiment 4:
ZrO2 is commercially available commercial powder, average particle size particle size 0.2 μ m, preparation 52vol.% ceramic concentrate suspension.In deionized water, add the glucose of 3mol/l during formulated suspension as substrate.The suspensoid of process ball milling after 24 hours be froth in vacuum at first, and slurry temperature is remained on 10 degree, glucose oxidase is added in the slurry again.The add-on of glucose oxidase is to add 10 milligrams glucose oxidase in 1 kilogram the zirconium white.Cast again after waiting for 120 minutes then with slurry and shaking up can obtain the intact ceramic body of flawless.
Claims (1)
1, a kind of preparation method of non-crack ceramic blank is characterized in that, this method comprises following each step:
(1) preparation ceramic concentrate suspension: the substrate that in deionized water, adds 0.2～5mol/l, and make its thorough dissolving, in above-mentioned solution, add ceramic powder then, volume ratio is: pottery: (water+pottery)=40～80: 100, and substrate wherein is any in urea, lactone, methane amide or the glucose;
(2) above-mentioned ceramic concentrate suspension is put into ball grinder, ball milling 12-48 hour;
(3) ceramic concentrate suspension behind the maintenance ball milling is 0-40 ℃ of following froth in vacuum;
(4) the corresponding biological enzyme of substrate of the adding and the above-mentioned the first step in above-mentioned ceramic concentrate suspension, biological enzyme is urine any in enzyme, lactonase or the glucose oxidase, add-on is to add 1～600 milligram biological enzyme in every kilogram the ceramic powder, after 1-4 hour, suspensoid is shaken up the back cast, promptly get non-crack ceramic blank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00136867A CN1120819C (en) | 2000-12-29 | 2000-12-29 | Process for preparing non-crack ceramic blank |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00136867A CN1120819C (en) | 2000-12-29 | 2000-12-29 | Process for preparing non-crack ceramic blank |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1304909A CN1304909A (en) | 2001-07-25 |
| CN1120819C true CN1120819C (en) | 2003-09-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN00136867A Expired - Fee Related CN1120819C (en) | 2000-12-29 | 2000-12-29 | Process for preparing non-crack ceramic blank |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100560536C (en) * | 2006-03-10 | 2009-11-18 | 中国科学院上海硅酸盐研究所 | The method of water-soluble epoxy resin in situ solidification for preparing ceramic blank |
| CN109485432B (en) * | 2018-11-22 | 2021-01-26 | 北京科技大学 | High-purity alpha-Si3N4Preparation method of nano powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1236761A (en) * | 1999-06-18 | 1999-12-01 | 清华大学 | Enzyme-catalytic high-molecular in-situ solidification process for shaping ceramic parts |
| CN1237564A (en) * | 1998-05-28 | 1999-12-08 | 中国科学技术大学 | Extrusion forming method of porous ceramics solidified by adopting high molecular polymerization crosslinking process |
| CN1257851A (en) * | 1999-12-22 | 2000-06-28 | 中国科学院上海硅酸盐研究所 | Process for preparing biscuit of ceramics by reaction induced gelatination |
-
2000
- 2000-12-29 CN CN00136867A patent/CN1120819C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1237564A (en) * | 1998-05-28 | 1999-12-08 | 中国科学技术大学 | Extrusion forming method of porous ceramics solidified by adopting high molecular polymerization crosslinking process |
| CN1236761A (en) * | 1999-06-18 | 1999-12-01 | 清华大学 | Enzyme-catalytic high-molecular in-situ solidification process for shaping ceramic parts |
| CN1257851A (en) * | 1999-12-22 | 2000-06-28 | 中国科学院上海硅酸盐研究所 | Process for preparing biscuit of ceramics by reaction induced gelatination |
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| Publication number | Publication date |
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| CN1304909A (en) | 2001-07-25 |
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