CN101890752A - Die for slip casting, using method thereof and green-ware and ITO target prepared by die - Google Patents
Die for slip casting, using method thereof and green-ware and ITO target prepared by die Download PDFInfo
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- CN101890752A CN101890752A CN2009101433555A CN200910143355A CN101890752A CN 101890752 A CN101890752 A CN 101890752A CN 2009101433555 A CN2009101433555 A CN 2009101433555A CN 200910143355 A CN200910143355 A CN 200910143355A CN 101890752 A CN101890752 A CN 101890752A
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Abstract
The invention relates to a die for slip casting, a using method thereof and a green-ware and an ITO target prepared by the die. The die for the slip casting comprises a bottom part, a side wall and an accommodation space surrounded by the bottom part and the side wall, wherein only the bottom part is made of a water absorbent porous material and the side wall cannot adsorb water. Only the bottom part is made of the water adsorbent material, and thus, the die for the slip casting completes slip casting operation in one step by utilizing a mode of adsorbing water from a single direction without continuously adding slurry so as to promote the accumulation uniformity of powder and the compactness of the green-ware and make a sintered body difficult to crack and deform; and the die is more suitable for producing the large-sized platy targets.
Description
Technical field
The present invention is the mould that a kind of injection forming is used, and especially a kind ofly is used for moulding and has the livings embryo that improves compactness, makes it be applicable to the mould of making large-size target.
Background technology
Nesa coating tin indium oxide (Indium Tin Oxide) abbreviates ITO as, owing to have the characteristic of low electrical conductivity and high transmission rate simultaneously, has been widely used in the aspects such as electro-conductive glass, solar cell and ELECTROMAGNETIC OBSCURANT glass of display at present.Along with display picture size trend maximizes, high-accuracyization, the flatness on film formation at low temp, low resistance characteristic, high transmission rate and film surface all is emphasis of ITO technical development.
The mainstream technology of preparation ito thin film is a magnetron sputtering technique, be characterized in to make film under low temperature depositing, to obtain good optics and electric property, have the sedimentation rate height in addition, substrate temperature is low, the film forming tack is good, easy to control, cost is low, can large-area coating film etc. advantages, thereby become a most widely used film technique.
The preparation method of ITO target generally from the selection of material powder, is then mixed powder, moulding, sintering, processing and joint.Wherein the method for moulding comprises compression moulding or slip casting.The processing procedure of compression moulding is short, operation is easy, but is difficult for making large-area thin plate, and in order to make living embryo density even, powder must pass through granulation usually.And the operation of slip casting is complicated, and required drying time is long, but is fit to the complicated shape of moulding.Usually has relatively low density with the living embryo after compression moulding or the slip casting moulding, this life embryo can carry out sintering earlier again after all the embryo relative density is given birth in the raising of pressure equipment, yet all press apparatus expensive and be difficult for the production large assemblies, so application can't enlarge.
In the molding process, usually need to add the dispersant of strengthening the powder dispersiveness, in order to the adhesive that improves living embryo intensity, will give birth to the releasing agent that embryo takes out from mould, the lubricant that reduces the mutual friction of powder phase etc. easily.But concerning the ITO target that high-quality requires, the dosage of additive is few more good more, the fringe cost when its reason is produced except reducing, also can improve the purity of target.
Therefore the target material moulding technological development focus on improve living embryo density, the dosage that reduces additive, size maximizes and reduce cost.Especially in the demand side that reduces cost, injection forming becomes the focus of technological development in recent years.Make tabular living embryo with traditional slip casting, system uses the gypsum mold more than two to carry out comprehensively or the absorption of the moisture content on two sides usually, though the liquid that can quicken in the mud is absorbed, shortens molding time, can cause a lot of defective of product.No matter mud in any direction injects the flow liner that mould all can cause living embryo, and then influence the uniformity of sintered density, and the liquid in the mud is pullled by multidirectional suction, and the cohesiveness that makes large-scale living embryo middle level powder easily is relatively poor and produce the phenomenon of delamination; In addition, if the absorption speed of gypsum mold causes giving birth to the degree of drying difference of embryo ectonexine easily, and forms emptying aperture or depression in inside, even working pressure slip casting also can't solve fully inconsistent.
Pertinent literature can be with reference to JP2007-055055, and it relates to arc design improvement demoulding yield that utilizes the slip casting porch; JP1997-272109, it relates to and utilizes the design that loam cake do not absorb water to solve the defective of formed body inside, produces slight crack when avoiding sintering, but its sidewall is still had an absorbent function, so can cause the defective of living embryo; TW548256, it is to utilize the mode moulding of filtering type film with the decompression draining.
Summary of the invention
The present invention is in order to improve comprehensively or the two sides suction problems such as product defects that mould caused, therefore through continuous research with make great efforts after, invent out the mould that this injection forming is used finally.
The present invention seeks to be to provide a kind of can be used to produce have the mould that good living embryo density is used with the injection forming of the living embryo that is used to make large-size target.
For reaching above-mentioned purpose, the mould that a kind of injection forming of the present invention is used, it comprises bottom, sidewall and a spatial accommodation that is surrounded by this bottom and sidewall, it is the material of water imbibition porous matter that the material of this bottom is wherein only arranged, and this sidewall can't absorb water.
Wherein, the material of this water imbibition porous matter comprises but the material that is not limited in gypsum, resin, macromolecule pellicle and has the water imbibition porous matter of knowing the knowledgeable usually and being familiar with in affiliated technical field.Preferably, the material of this water imbibition porous matter is a gypsum.
Wherein, this sidewall is formed with non-water imbibition material, is formed with waterproof material.
Wherein, this sidewall is being formed with this identical material in bottom, and is provided with the dividing plate that non-water imbibition material is formed in this inside sidewalls, and this dividing plate is formed with waterproof material furthermore.
This non-water imbibition material comprises but is not limited in plastic sheet, sheet metal, sheet glass and has the waterproof material of knowing the knowledgeable usually and being familiar with in affiliated technical field.
The present invention is again about a kind of living embryo, and the mould moulding person that it is to use above-mentioned injection forming to use wherein should give birth to the relative density of embryo greater than 50%.
The present invention also has relevant for a kind of method of making the ITO target, its comprise size mixing, the step of injection forming, demoulding drying and sintering, to obtain this ITO target, wherein the injection forming step comprises that the mould that uses above-mentioned injection forming to use gives birth to embryo with moulding.
Wherein, this relative density of giving birth to embryo is greater than 50%.
Wherein, this sintering step comprises at least low temperature presintering knot and at least high temperature sintering.
Preferably, described high temperature sintering is to carry out in oxygen concentration is atmosphere more than 95%.
The present invention is also about a kind of ITO target, and it is with the prepared product of said method.
The present invention only is made up of with the suction material the bottom, therefore utilize the mode that absorbs moisture content by single direction, once finish the slip casting action, needn't add slurry successively, so can promote the uniformity of powder accumulation and the compactness of giving birth to embryo, make the not easily broken distortion of sintered body, and more can be applied to make large-sized tabular target.
Description of drawings
The three-dimensional view of the described embodiment of mould that Fig. 1 uses for injection forming of the present invention;
The side sectional view of described another embodiment of mould that Fig. 2 uses for injection forming of the present invention.
In the accompanying drawing, the list of parts of each label representative is as follows:
(10) bottom
(20) (20 ') sidewall
(21) dividing plate
The specific embodiment
Please referring to shown in Figure 1, it is an embodiment of the mould used of injection forming of the present invention, it is to be made of a bottom (10) and sidewall (20), the material of this bottom (10) is the material of water imbibition porous matter, in order to the liquid in the absorbent slurry, and this sidewall (20) is formed with non-water-absorbing material, and it is only in order to form living embryo external form, and is non-in order to the liquid in the absorbent slurry.
Please referring to shown in Figure 2, it is another embodiment of the present invention, it is roughly same as the previously described embodiments, its difference is that sidewall (20 ') is to utilize with bottom (10) identical materials to form in this embodiment, and be provided with non-absorptive dividing plate (21) in this sidewall (20 ') inboard, absorb with the moisture content of avoiding sidewall (20 ') direction, this dividing plate (21) more has the function of the auxiliary demoulding except the function that isolated moisture content absorption is arranged.
In further embodiment of this invention, this sidewall can be made up of non-water-absorbing material, and is provided with non-absorptive dividing plate again in this inside sidewalls, definitely to avoid the liquid in the sidewall absorbent slurry, can help demoulding again.
The present invention is the moulding of carrying out the living embryo of target with the mould of unidirectional suction thus, the dispersant that only need add trace in the slurry helps powder to disperse, do not need additionally to add the equipment of adhesive or other slip casing by pressure, even must not pass through any journey of all suppressing, the living embryo relative density of gained can reach more than 50%.Therefore utilize the present invention except promoting target purity, more can significantly reduce production costs.
Living embryo after the moulding can obtain the target of relative density more than 99% through high temperature sintering.In the sintering process, when the temperature of ITO sintered body during greater than 750 ℃, for example Chang Yong In2O3 can be decomposed into In2O and O2, In2O can further be decomposed into In and O2 again again under higher temperature, this decomposition behavior meeting influences the compactness and the electric conductivity of target, for the generation that suppresses to decompose, the present invention will give birth to embryo and carry out interim low temperature presintering knot in the environment of logical oxygen, and carry out high temperature sintering in the high atmosphere of oxygen concentration.
Embodiment:
Make the mould that injection forming is used
Make 5 centimeters gypsum template and housings that (cm) is thick with calcium plaster, this gypsum template is the bottom as mould, and housing system is located at for thirty years of age on this gypsum template to cross a spatial accommodation as the sidewall of mould, this housing is to make according to giving birth to the embryo size requirements, the spatial accommodation that is crossed is to be used for splendid attire mud, lives mud with frame above the gypsum template and leaks to prevent mud; Place side within the housing with plastic tab before the grouting, blocking the liquid in the housing absorbent slurry, and be convenient to the demoulding.
Size mixing
Use tin indium oxide (ITO) powder to size mixing, the mixing ratio of powder and water is 5: 1, adds the dispersant of 0.3wt% afterwards, there is no and adds any adhesive, carries out ball milling 20 hours, to mix ITO mud.
Injection forming
The ITO mud that has mixed up is injected above-mentioned mould, and the gravity of mud produces the pressure of injection forming, and the bubble of mud inside is floated, and therefore ingress of air and disappearing can not need add defoamer.
Demoulding drying
ITO mud is left standstill, carry out the demoulding and give birth to the embryo drying after the liquid in ITO mud is absorbed by gypsum mold, measure living embryo density with Ah a fews' Mead method this moment and reach 4g/cm
3, its relative density that converts can reach more than 55%.
Sintering
With giving birth to embryo carries out 900 ℃ of pre-burnings in the stove of logical oxygen after, in the atmosphere of oxygen concentration more than 95%, carry out 1600 ℃ of high temperature sinterings again, can obtain the ITO target, its relative density can reach more than 99.5%.Wherein, the ITO particle diameter is controlled in the 0.5um, and the viscosity and the flowability of control slurry, be to use normal pressure to lead to the oxygen sintering furnace in the present embodiment, to save investment cost of equipment.
Comparative example 1:
Make the mould that injection forming is used
Make 5 centimeters gypsum template and housings that (cm) is thick as embodiment with calcium plaster, this gypsum template is the bottom as mould, and being sidewall as mould, housing is located at for thirty years of age on this gypsum template to cross a spatial accommodation, this housing is to make according to giving birth to the embryo size requirements, the spatial accommodation that is crossed is to be used for splendid attire mud, lives mud with frame above the gypsum template and leaks to prevent mud.
Size mixing
Use tin indium oxide (ITO) mud identical with embodiment.
Injection forming
The ITO mud that has mixed up is injected above-mentioned mould, and the gravity of mud produces the pressure of injection forming, and the bubble of mud inside is floated, and therefore ingress of air and disappearing can not need add defoamer.But, in drainage procedure, must mend slurry again because the draining simultaneously of sidewall and bottom causes slurry surface to form concave surface.
Demoulding drying
ITO mud is left standstill, carry out the demoulding and give birth to the embryo drying after the liquid in ITO mud is absorbed by gypsum mold, measure living embryo density with Ah a fews' Mead method this moment and reach 3.5g/cm
3, its relative density about 49% converts.
Sintering
Carry out sintering with giving birth to embryo under the condition identical with embodiment, it is about 94.5% to obtain the relative density of ITO target, and target material surface can be observed obvious slight crack, and target can be found slip casting for the first time and mended the non-uniform phenomenon that slurry causes after disrumpent feelings.
Comparative example 2:
Make the mould that injection forming is used
Make 5 centimeters gypsum template and housings that (cm) is thick as embodiment with calcium plaster, this gypsum template is the bottom as mould, and being sidewall as mould, housing is located at for thirty years of age on this gypsum template to cross a spatial accommodation, this housing is to make according to giving birth to the embryo size requirements, the spatial accommodation that is crossed is to be used for splendid attire mud, live mud with frame above the gypsum template and leak to prevent mud, in addition with a slice plasterboard as loam cake.
Size mixing
Use tin indium oxide (ITO) mud identical with embodiment.
Injection forming
The ITO mud that has mixed up is injected above-mentioned mould, cover the gypsum loam cake.Sidewall, bottom and loam cake draining simultaneously at this moment.
Demoulding drying
ITO mud is left standstill, carry out the demoulding and give birth to the embryo drying after the liquid in ITO mud is absorbed by gypsum mold, it is loose to find to give birth to the embryonic knob structure this moment, gives birth to embryo density with the measurement of Ah a fews' Mead method and reaches 3.3g/cm
3, its relative density about 46% converts.
Sintering
Carry out sintering with giving birth to embryo under the condition identical with embodiment, it is about 92% to obtain the relative density of ITO target, and target material surface can be observed obvious slight crack and distortion, and target can be found that there is the many places hole target inside after disrumpent feelings.
Use the mould molding that can absorb water more than the two sides relative density in the comparative example, feasiblely utilize the relative density of the made ito substrate of this life embryo less than 95% less than 50% livings embryo; And can molding relative density, mould provided by the present invention thus reaches 55% living embryo, and make the cost of successive process reduce, can allow the relative density of made ITO target up to more than 99.5% again, therefore solve existing existence problem for a long time, and can supply the related industry utilization, to promote industry development.
Claims (10)
1. mould that injection forming is used is characterized in that: comprise bottom, sidewall and a spatial accommodation that is surrounded by this bottom and sidewall, it is the material of water imbibition porous matter that the material of described bottom is wherein only arranged, and this sidewall can't absorb water.
2. the mould used of injection forming according to claim 1, it is characterized in that: the material of described water imbibition porous matter is gypsum, resin or macromolecule pellicle, described sidewall is formed with non-water imbibition material.
3. the mould of using as injection forming as described in the claim 2, it is characterized in that: described non-water imbibition material is plastic sheet, sheet metal or sheet glass.
4. the mould used of injection forming according to claim 1 is characterized in that: described sidewall is being formed with this identical material in bottom, and is provided with the dividing plate that non-water imbibition material is formed in this inside sidewalls.
5. the mould of using as injection forming as described in the claim 4, it is characterized in that: described non-water imbibition material is plastic sheet, sheet metal or sheet glass.
6. living embryo is characterized in that: be to use the product as the mould institute moulding that injection forming is used as described in each in the claim 1 to 5, the relative density of wherein said living embryo is greater than 50%.
7. method of making the ITO target, it is characterized in that: comprise size mixing, the step of injection forming, demoulding drying and sintering, to obtain described ITO target, wherein said injection forming step comprises that use gives birth to embryo as the mould that injection forming is used as described in each in the claim 1 to 5 with moulding, and the relative density of wherein said living embryo is greater than 50%.
8. as claim 7 a described method, it is characterized in that: described sintering step comprises at least low temperature presintering knot and at least high temperature sintering.
9. method as claimed in claim 8 is characterized in that: described high temperature sintering is to carry out in oxygen concentration is atmosphere more than 95%.
10. an ITO target is characterized in that: be the product that makes with claim 7,8 or 9 described methods.
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CN2009101433555A CN101890752A (en) | 2009-05-22 | 2009-05-22 | Die for slip casting, using method thereof and green-ware and ITO target prepared by die |
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CN2009101433555A CN101890752A (en) | 2009-05-22 | 2009-05-22 | Die for slip casting, using method thereof and green-ware and ITO target prepared by die |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104308952A (en) * | 2014-10-22 | 2015-01-28 | 福建省诺希新材料科技有限公司 | Device and method for manufacturing plaster mold |
CN108640674A (en) * | 2018-06-22 | 2018-10-12 | 广东凯盛光伏技术研究院有限公司 | A kind of method of constant temperature and humidity rapid draing ITO target green body |
CN108863343A (en) * | 2018-06-22 | 2018-11-23 | 广东凯盛光伏技术研究院有限公司 | A kind of method of the sintering integrated formula production ITO target of degreasing- |
CN109176828A (en) * | 2018-08-16 | 2019-01-11 | 中国船舶重工集团公司第七二五研究所 | Prevent the big specification plane ceramic green body gel-casting method of buckling deformation |
CN109624025A (en) * | 2018-12-28 | 2019-04-16 | 广西晶联光电材料有限责任公司 | A kind of the injection forming mold and method of oxide target material |
CN112062584A (en) * | 2020-09-18 | 2020-12-11 | 山东鲁阳浩特高技术纤维有限公司 | Composite refractory material and preparation method thereof |
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2009
- 2009-05-22 CN CN2009101433555A patent/CN101890752A/en active Pending
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104308952A (en) * | 2014-10-22 | 2015-01-28 | 福建省诺希新材料科技有限公司 | Device and method for manufacturing plaster mold |
CN108640674A (en) * | 2018-06-22 | 2018-10-12 | 广东凯盛光伏技术研究院有限公司 | A kind of method of constant temperature and humidity rapid draing ITO target green body |
CN108863343A (en) * | 2018-06-22 | 2018-11-23 | 广东凯盛光伏技术研究院有限公司 | A kind of method of the sintering integrated formula production ITO target of degreasing- |
CN108863343B (en) * | 2018-06-22 | 2021-06-08 | 广东凯盛光伏技术研究院有限公司 | Method for producing ITO target material through integrated degreasing and sintering |
CN109176828A (en) * | 2018-08-16 | 2019-01-11 | 中国船舶重工集团公司第七二五研究所 | Prevent the big specification plane ceramic green body gel-casting method of buckling deformation |
CN109176828B (en) * | 2018-08-16 | 2021-02-05 | 中国船舶重工集团公司第七二五研究所 | Gel injection molding method for large-size planar ceramic blank capable of preventing warping deformation |
CN109624025A (en) * | 2018-12-28 | 2019-04-16 | 广西晶联光电材料有限责任公司 | A kind of the injection forming mold and method of oxide target material |
CN109624025B (en) * | 2018-12-28 | 2024-07-19 | 广西晶联光电材料有限责任公司 | Grouting forming die and method for oxide target |
CN112062584A (en) * | 2020-09-18 | 2020-12-11 | 山东鲁阳浩特高技术纤维有限公司 | Composite refractory material and preparation method thereof |
CN112062584B (en) * | 2020-09-18 | 2022-06-10 | 山东鲁阳浩特高技术纤维有限公司 | Composite refractory material and preparation method thereof |
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Application publication date: 20101124 |