CN101982435A - Method for preparing low-temperature lead-free near zero expansion microcrystalline ceramic coating - Google Patents
Method for preparing low-temperature lead-free near zero expansion microcrystalline ceramic coating Download PDFInfo
- Publication number
- CN101982435A CN101982435A CN 201010533239 CN201010533239A CN101982435A CN 101982435 A CN101982435 A CN 101982435A CN 201010533239 CN201010533239 CN 201010533239 CN 201010533239 A CN201010533239 A CN 201010533239A CN 101982435 A CN101982435 A CN 101982435A
- Authority
- CN
- China
- Prior art keywords
- preparation
- dried
- weight ratio
- temperature
- insulation
- 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.)
- Granted
Links
Abstract
The invention relates to a method for preparing a low-temperature lead-free near zero expansion microcrystalline ceramic coating, belonging to the technical field of specific and functional ceramic. The method comprises the following steps: uniformly performing dry mixing on one or two of low temperature clinker 2, spodumene melt or eucryptite melt in an arbitrary proportion, one or two or three of low temperature clinker I, zirconium tungstate powder, an additive I or an additive 2 in an arbitrary proportion and a nucleating agent; melting the mixture in a Muffle furnace, and preserving the temperature of between 950 and 1,200 DEG C for 0.5 to 1h; pouring the molten glass fluid on a preheated stainless steel plate; continuously heating the molten glass fluid to 750 DEG C in the Muffle furnace at the temperature of between 560 and 650 DEG C, and preserving the temperature for 1 to 4h; naturally cooling the glass fluid to room temperature, crushing to obtain composite ceramic powder; adding a plasticizing agent and deionized water into the composite ceramic powder to prepare slurry; and coating the slurry on the surface of a matrix to sinter at the temperature of between 600 and 650 DEG C to obtain a composite inorganic microcrystalline ceramic coating. The method is scientific and reasonable, simple and practicable, and is convenient to implement; and the prepared coating material is water proof, is lead free, can be used at low temperature, and has near zero linear expansion coefficient.
Description
Technical field
The present invention relates to the preparation method of a kind of low temperature, unleaded, near-zero thermal expansion micro-crystalline ceramic coating, belong to extraordinary, technical field of functional ceramics.
Background technology
The continuous development of aeronautical and space technology has also proposed more and more higher requirement to the performance of electromagnetic wave transparent material, the stupalith of one-component can't satisfy working conditions because of itself inherent shortcoming (low as toughness, fragility is big etc.), so the fabric composite study has become a kind of inevitable trend.Fiber as reinforced fabric mainly contains silica fiber, sapphire whisker and boron nitride fibre etc. at present, and their matrix material successively is used widely in multinomial Aeronautics and Astronautics engineering parts such as nose cone, heat-protection layer, antenna windows, radome.
Silica fiber strengthens the fragility that silica-base composite material has overcome the simple substance pottery, has high toughness, has a wide range of applications in field of aerospace.But goods in use inevitably will bear washing away of weathering and air-flow, thereby cause surface erosion, make the surface become coarse, cause material to peel off or damage.Because this matrix material is the meeting moisture absorption in the prolonged preservation process, causes wave penetrate capability to degenerate.Simultaneously, during greater than 700 ℃, degenerate serious by fibre strength in envrionment temperature for the silica fiber matrix material, and the toughness of matrix material falls sharply.It is organic materials substantially that traditional silica fiber strengthens the silica-base composite material coating, and its temperature tolerance is relatively poor and influence the ripple effect, therefore, must develop a kind of inorganic materials and make it to have under the low temperature that 1. is lower than 650 ℃ and can form dense coating; 2. have the near-zero thermal expansion coefficient close with quartzy matrix material; 3. physicals such as moistureproofness is good.
At present, therefore the most melt temperature height of near-zero thermal expansion stupalith is developed the entry of low temperature near-zero thermal expansion ceramic coating and will be started with from fusing assistant.Plumbous oxide has been used for a long time at ceramic glaze as a kind of low temperature main fluxing, and containing lead glaze, to have a melting behaviour good, and firing temperature is low, premium propertiess such as glaze glossiness height, but very big to the wave penetrate capability influence.In use, lead is stripping very easily, and HUMAN HEALTH is brought certain harm, both at home and abroad to the requirement of lead release also increasingly stringent, has unleadedly become a kind of inevitable trend and bright development prospect is arranged.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of low temperature, unleaded, near-zero thermal expansion micro-crystalline ceramic coating, but the coating waterproof low temperature of preparation uses, unleaded and linear expansivity is near zero.
The preparation method of low temperature of the present invention (being lower than 650 ℃), unleaded, near-zero thermal expansion micro-crystalline ceramic coating, the batching preparation is as follows respectively:
(1) preparation low temperature frit 1(abbreviation LBA-1):
Raw materials used is Quilonum Retard, boric acid, aluminium hydroxide, quartz and magnesium oxide, and according to (7-15): (65-80): (1-4): (5-10): weight ratio (1-5) is dried to be mixed evenly, places retort furnace 850-1100 ℃ to found, insulation 0.5-2h, shrend, ball mill pulverizing, standby;
(2) preparation low temperature frit 2(abbreviation BL168):
Raw materials used is Quilonum Retard, boric acid, aluminium hydroxide, quartz and magnesium oxide, and according to (5-15): (70-85): (9-17): (1-5): weight ratio (0.3-1.5) is dried to be mixed evenly, places retort furnace to found for 950 ℃, insulation 0.5-2h, shrend, ball mill pulverizing, standby;
(3) preparation of triphane melt (being called for short ABA-1):
Raw materials used is Quilonum Retard, aluminium hydroxide and quartz, and according to (12-18): (25-40): weight ratio (40-62) is dried to be mixed evenly, places retort furnace 1300-1500 ℃ to found, insulation 0.5-2h, and ball mill pulverizing, standby;
(4) preparation of eucryptite melt (being called for short ABA-2):
Raw materials used is Quilonum Retard, aluminium hydroxide and quartz, and according to (15-23): (35-50): weight ratio (30-45) is dried to be mixed evenly, place under retort furnace 1300-1500 ℃ and found, and insulation 0.5-2h, ball mill pulverizing, standby;
(5) preparation of wolframic acid zirconium powder body (being called for short ZW-2):
Raw materials used is zirconium white and wolframic acid, according to (17-26): weight ratio (74-90) is dried to be mixed even back and dehydrated alcohol, zirconia ball with weight ratio (0.5-1.5): (0.5-1): ratio ball milling 20-30h (1.5-2.5), again that slip is dry in 60-90 ℃ of loft drier, calcining makes ceramic powder then, calcining temperature 1100-1300 ℃, soaking time 1-3 hour, pulverize, standby;
(6) preparation additive 1(abbreviation ZB-1):
Raw materials used is zinc oxide and boric acid, according to (35-50): dried even being placed in the alumina crucible that be mixed of weight ratio (45-60), calcining makes ceramic powder then, and calcining temperature 900-1200 ℃, soaking time 0.5-1.5 hour, shrend, it is standby to pulverize the back;
(7) preparation additive 2(abbreviation LZS-10):
Raw materials used is Quilonum Retard, quartz, 85% phosphoric acid, Strontium carbonate powder and lithium fluoride, according to (15-30): (25-45): (1-10): (20-45): dried even being placed in the alumina crucible that be mixed of weight ratio (7-20), calcining makes ceramic powder then, calcining temperature 1100-1300 ℃, soaking time 0.5-1.5 hour, shrend, standby after pulverizing;
Preparation process is as follows:
With one or both or three kinds of arbitrary proportions in one or both arbitrary proportions in low temperature frit 2, triphane melt or the eucryptite melt and low temperature frit 1, wolframic acid zirconium powder body, additive 1 or the additive 2 and nucleator dried be mixed even, place under retort furnace 950-1200 ℃ and found, insulation 0.5-1h; The glass metal that melts is cast on the stainless steel plate of prior preheating, places then that 560-650 ℃ retort furnace relaying is continuous to be warming up to 750 ℃, and insulation 1-4h naturally cools to room temperature, after the pulverizing composite ceramic;
With composite ceramic add plastic agent, deionized water is made into slip, is coated in matrix surface, obtains composite inorganic micro-crystalline ceramic coating through 600-650 ℃ of following sintering.
With composite ceramic add plastic agent, deionized water is made into slip, is coated in matrix surface, obtains composite inorganic micro-crystalline ceramic coating through 600-650 ℃ of following sintering.
Used ingredient requirement is as follows:
Quilonum Retard content 〉=99.0%; The weight content of boric acid 〉=99.5%; The aluminium hydroxide analytical reagent; Magnesium oxide is lightweight, its weight content 〉=98.5%; Zirconic weight content 〉=99%; H in the wolframic acid
2WO
4Weight content 〉=99.9%; The weight content of zinc oxide 〉=99.5%; The weight content of Strontium carbonate powder 〉=99.5%; The weight content of lithium fluoride 〉=99%; H in the phosphoric acid
3PO
4Content 〉=85%.Quartz is an amorphous state, silica weight content 〉=99.98%;
Plastic agent is methylcellulose gum or cmc soln, and mass concentration is 0.3～1%, and consumption is 0.2～1% of a powder quality.
Nucleator is zirconium dioxide or titanium oxide, and consumption is 0.5～2% of a powder quality.
The present invention utilizes Quilonum Retard, aluminium hydroxide and silicon-dioxide three under high-temperature calcination solid state reaction to take place, by controlling triphane and the eucryptite diphase ceramic material powder that triangular ratio prepares low bulk even negative expansion, introduce self-control low temperature fusing assistant simultaneously to reduce melt temperature, liquid phase formation temperature and the viscosity of material monolithic.Utilize ZW-2 to finely tune the coefficient of expansion of inorganic coating simultaneously.
Preparation method of the present invention is scientific and reasonable, and is simple, be convenient to implement, but the coated material waterproof of acquisition, the use of unleaded low temperature and linear expansivity is near zero.
Embodiment
The invention will be further described below in conjunction with embodiment.
At first preparation is called for short LBA-1, BL168, ABA-1, ABA-2, ZW-2, ZB-1 and LZS-10, and is as follows respectively:
(1) preparation of LBA-1:
1#, raw materials used be Quilonum Retard, boric acid, aluminium hydroxide, quartz and magnesium oxide, be mixed evenly according to the weight ratio of 10:75:5:6:4 is dried, place retort furnace 900-1050 ℃ to found, insulation 1h, shrend, ball mill pulverizing, standby;
2#, raw materials used be Quilonum Retard, boric acid, aluminium hydroxide, quartz and magnesium oxide, be mixed evenly according to the weight ratio of 13:72:3:7:5 is dried, place retort furnace 850-1100 ℃ to found, insulation 0.5-2h, shrend, ball mill pulverizing, standby;
3#, raw materials used be Quilonum Retard, boric acid, aluminium hydroxide, quartz and magnesium oxide, be mixed evenly according to the weight ratio of 11:80:2:5:2 is dried, place retort furnace 850-1100 ℃ to found, insulation 0.5-2h, shrend, ball mill pulverizing, standby;
(2) preparation of BL168:
1#, raw materials used be Quilonum Retard, boric acid, aluminium hydroxide, quartz and magnesium oxide, be mixed evenly according to the weight ratio of 8:75:11:5:1 is dried, place retort furnace to found for 950 ℃, insulation 0.5-2h, shrend, ball mill pulverizing, standby;
2#, raw materials used be Quilonum Retard, boric acid, aluminium hydroxide, quartz and magnesium oxide, be mixed evenly according to the weight ratio of 10:72:12:4.5:1.5 is dried, place retort furnace to found for 950 ℃, insulation 0.5-2h, shrend, ball mill pulverizing, standby;
3#, raw materials used be Quilonum Retard, boric acid, aluminium hydroxide, quartz and magnesium oxide, be mixed evenly according to the weight ratio of 12:70:15:2:1 is dried, place retort furnace to found for 950 ℃, insulation 0.5-2h, shrend, ball mill pulverizing, standby;
(3) preparation of ABA-1:
1#, raw materials used be Quilonum Retard, aluminium hydroxide and quartz, be mixed evenly according to the weight ratio of 13:28:59 is dried, place retort furnace 1300-1500 ℃ to found, insulation 0.5-2h, ball mill pulverizing, standby;
2#, raw materials used be Quilonum Retard, aluminium hydroxide and quartz, be mixed evenly according to the weight ratio of 15:35:50 is dried, place retort furnace 1300-1500 ℃ to found, insulation 0.5-2h, ball mill pulverizing, standby;
3#, raw materials used be Quilonum Retard, aluminium hydroxide and quartz, be mixed evenly according to the weight ratio of 17:33:50 is dried, place retort furnace 1300-1500 ℃ to found, insulation 0.5-2h, ball mill pulverizing, standby;
(4) preparation of ABA-2:
1#, raw materials used be Quilonum Retard, aluminium hydroxide and quartz, be mixed evenly according to the weight ratio of 17:40:43 is dried, place under retort furnace 1300-1500 ℃ and found, insulation 0.5-2h, ball mill pulverizing, standby;
2#, raw materials used be Quilonum Retard, aluminium hydroxide and quartz, be mixed evenly according to the weight ratio of 20:35:45 is dried, place under retort furnace 1300-1500 ℃ and found, insulation 0.5-2h, ball mill pulverizing, standby;
3#, raw materials used be Quilonum Retard, aluminium hydroxide and quartz, be mixed evenly according to the weight ratio of 22:36:42 is dried, place under retort furnace 1300-1500 ℃ and found, insulation 0.5-2h, ball mill pulverizing, standby;
(5) preparation of ZW-2:
Raw materials used is zirconium white and wolframic acid, according to the weight ratio of 20:80 dried be mixed even back and dehydrated alcohol, zirconia ball with weight ratio (0.5-1.5): (0.5-1): ratio ball milling 20-30h (1.5-2.5), again that slip is dry in 60-90 ℃ of loft drier, calcining makes ceramic powder then, calcining temperature 1100-1300 ℃, soaking time 1-3 hour, pulverize, standby;
(6) preparation of ZB-1:
1#, raw materials used be zinc oxide and boric acid, according to dried even being placed in the alumina crucible that be mixed of the weight ratio of 40:60, calcining makes ceramic powder then, calcining temperature 900-1200 ℃, soaking time 0.5-1.5 hour, shrend, it is standby to pulverize the back;
2#, raw materials used be zinc oxide and boric acid, according to dried even being placed in the alumina crucible that be mixed of the weight ratio of 45:55, calcining makes ceramic powder then, calcining temperature 900-1200 ℃, soaking time 0.5-1.5 hour, shrend, it is standby to pulverize the back;
(7) preparation of LZS-10:
1#, raw materials used be Quilonum Retard, quartz, 85% phosphoric acid, Strontium carbonate powder and lithium fluoride, according to dried even being placed in the alumina crucible that be mixed of the weight ratio of 20:30:5:30:15, calcining makes ceramic powder then, calcining temperature 1100-1300 ℃, soaking time 0.5-1.5 hour, shrend, standby after pulverizing;
2#, raw materials used be Quilonum Retard, quartz, 85% phosphoric acid, Strontium carbonate powder and lithium fluoride, according to dried even being placed in the alumina crucible that be mixed of the weight ratio of 15:30:5:40:10, calcining makes ceramic powder then, calcining temperature 1100-1300 ℃, soaking time 0.5-1.5 hour, shrend, standby after pulverizing;
3#, raw materials used be Quilonum Retard, quartz, 85% phosphoric acid, Strontium carbonate powder and lithium fluoride, according to dried even being placed in the alumina crucible that be mixed of the weight ratio of 25:35:10:20:10, calcining makes ceramic powder then, calcining temperature 1100-1300 ℃, soaking time 0.5-1.5 hour, shrend, standby after pulverizing;
Preparation low temperature, unleaded, near-zero thermal expansion micro-crystalline ceramic coating:
Embodiment 1
Take by weighing respectively that 60g2#ABA-1,48g1#LBA-1,12g1#ZB-1,12gZW-2 are dried to be mixed evenly, be contained in the alumina crucible, place under retort furnace 1000-1100 ℃ and found, insulation 0.6h.The glass metal that melts is cast on the stainless steel plate of prior preheating, treats that electric furnace cooling back reheat to 600 ℃ is warming up to 840 ℃, insulation 2h carries out micritization to be handled, and naturally cools to room temperature afterwards.
To pulverize behind the above-mentioned composite ceramic material ball milling 24h.Promptly get 50 gram powders and add 38.5 ml distilled waters and 31.5ml methocel solution, the 100g zirconia balls is as carrying out under the technology of grinding medium.Behind ball milling, be made into ceramic slurry and apply or be sprayed on matrix surface, be incubated 1 hour down at 620 ℃ and found into composite inorganic micro-crystalline ceramic coating.Its coefficient of expansion value is α=0.2068 * 10
-6/ ℃.
Embodiment 2
Take by weighing respectively that 46g1#BL168 and 54g3#ABA-2 are dried to be mixed evenly, be contained in the alumina crucible, place under retort furnace 1100-1200 ℃ and found, insulation 1h.The glass metal that melts is cast on the stainless steel plate of prior preheating, treats that electric furnace cooling back reheat to 600 ℃ is warming up to 840 ℃, insulation 2h carries out micritization to be handled, and naturally cools to room temperature afterwards.
To pulverize behind the above-mentioned composite ceramic material ball milling 24h.Promptly get 50 gram powders and add 38.5 ml distilled waters and 31.5ml methocel solution, the 100g zirconia balls is as carrying out under the technology of grinding medium.Behind ball milling, be made into ceramic slurry and apply or be sprayed on matrix surface, be incubated 1 hour down at 620 ℃ and found into composite inorganic micro-crystalline ceramic coating.Its coefficient of expansion value is α=0.1192 * 10
-6/ ℃.
Embodiment 3
Take by weighing 43.2g2#ABA-2,36.8g1#BL168 and 4.8g3#LZS-10 respectively, driedly be mixed evenly, be contained in the alumina crucible, place under retort furnace 950-1100 ℃ and found, insulation 0.5h.The glass metal that melts is cast on the stainless steel plate of prior preheating, treats that electric furnace cooling back reheat to 600 ℃ is warming up to 860 ℃, insulation 3h carries out micritization to be handled, and naturally cools to room temperature afterwards.
To pulverize behind the above-mentioned composite ceramic material ball milling 24h.Promptly get 50 gram powders and add 38.5 ml distilled waters and 31.5ml methocel solution, the 100g zirconia balls is as carrying out under the technology of grinding medium.Behind ball milling, be made into ceramic slurry and apply or be sprayed on matrix surface, be incubated 1 hour down at 650 ℃ and found into composite inorganic micro-crystalline ceramic coating.Its coefficient of expansion value is α=-0.0258 * 10
-6/ ℃.
Embodiment 4
Take by weighing 21.6g3#ABA-2,18.4g2#BL168,2.4g1#LZS-10 and 0.24g titanium dioxide respectively, driedly be mixed evenly, be contained in the alumina crucible, place under retort furnace 950-1050 ℃ and found, insulation 1h.The glass metal that melts is cast on the stainless steel plate of prior preheating, treats that electric furnace cooling back reheat to 640 is warming up to 890 ℃, insulation 4h carries out micritization to be handled, and naturally cools to room temperature.
To pulverize behind the above-mentioned composite ceramic material ball milling 24h.Promptly get the cmc soln that 11.45 gram powders add 8.8ml distilled water and 7.2ml0.5%, the 23g zirconia balls is to carry out under the technology of grinding medium.Behind ball milling, be made into ceramic slurry and apply or be sprayed on matrix surface, be incubated 1 hour down at 650 ℃ and found into composite ceramic coat.Its coefficient of expansion value is α=-0.0179 * 10
-6/ ℃.
Embodiment 5
Take by weighing 21.6g1#ABA-2,18.4g3#BL168,2.4g1#LZS-10 and 0.4g zirconium dioxide respectively, driedly be mixed evenly, be contained in the alumina crucible, place under retort furnace 950-1100 ℃ and found, insulation 1h.The glass metal that melts is cast on the stainless steel plate of prior preheating, treat electric furnace cooling after, be warming up to 890 ℃ being heated to 640 ℃, insulation 4h carries out micritization to be handled, and naturally cools to room temperature.
To pulverize behind the above-mentioned composite ceramic material ball milling 24h.Promptly get 11.57 gram powders and add 8.9ml distilled water and 7.2ml cmc solns, the 23g zirconia balls is to carry out under the technology of grinding medium., behind ball milling, be made into ceramic slurry and apply or be sprayed on matrix surface, be incubated 1 hour down at 650 ℃ and found into composite inorganic micro-crystalline ceramic coating.Its coefficient of expansion value is α=-0.0387 * 10
-6/ ℃.
Embodiment 6
Take by weighing respectively that 60g1#ABA-1,48g1#LBA-1,12g2#ZB-1,12gZW-2 are dried to be mixed evenly, be contained in the alumina crucible, place under retort furnace 1000-1150 ℃ and found, insulation 1h.The glass metal that melts is cast on the stainless steel plate of prior preheating, treats that electric furnace cooling back reheat to 600 ℃ is warming up to 840 ℃, insulation 2h carries out micritization to be handled, and naturally cools to room temperature afterwards.
To pulverize behind the above-mentioned composite ceramic material ball milling 24h.Promptly get 50 gram powders and add 38.5 ml distilled waters and 31.5ml methocel solution, the 100g zirconia balls is as carrying out under the technology of grinding medium.Behind ball milling, be made into ceramic slurry and apply or be sprayed on matrix surface, be incubated 1 hour down at 620 ℃ and found into composite inorganic micro-crystalline ceramic coating.Its coefficient of expansion value is α=0.0373 * 10
-6/ ℃.
Embodiment 7
Take by weighing respectively that 46g2#BL168 and 54g2#ABA-2 are dried to be mixed evenly, be contained in the alumina crucible, place under retort furnace 1100-1200 ℃ and found, insulation 1h.The glass metal that melts is cast on the stainless steel plate of prior preheating, treats that electric furnace cooling back reheat to 600 ℃ is warming up to 840 ℃, insulation 2h carries out micritization to be handled, and naturally cools to room temperature afterwards.
To pulverize behind the above-mentioned composite ceramic material ball milling 24h.Promptly get 50 gram powders and add 38.5 ml distilled waters and 31.5ml methocel solution, the 100g zirconia balls is as carrying out under the technology of grinding medium.Behind ball milling, be made into ceramic slurry and apply or be sprayed on matrix surface, be incubated 1 hour down at 620 ℃ and found into composite inorganic micro-crystalline ceramic coating.Its coefficient of expansion value is α=0.1028 * 10
-6/ ℃.
Embodiment 8
Take by weighing 43.2g1#ABA-2,36.8g3#BL168 and 4.8g2#LZS-10 respectively, driedly be mixed evenly, be contained in the alumina crucible, place under retort furnace 1100-1200 ℃ and found, insulation 0.5h.The glass metal that melts is cast on the stainless steel plate of prior preheating, treats that electric furnace cooling back reheat to 600 ℃ is warming up to 860 ℃, insulation 3h carries out micritization to be handled, and naturally cools to room temperature afterwards.
To pulverize behind the above-mentioned composite ceramic material ball milling 24h.Promptly get 50 gram powders and add 38.5 ml distilled waters and 31.5ml methocel solution, the 100g zirconia balls is as carrying out under the technology of grinding medium.Behind ball milling, be made into ceramic slurry and apply or be sprayed on matrix surface, be incubated 1 hour down at 650 ℃ and found into composite inorganic micro-crystalline ceramic coating.Its coefficient of expansion value is α=-0.0374 * 10
-6/ ℃.
Embodiment 9
Take by weighing 21.6g2#ABA-2,18.4g1#BL168,2.4g3#LZS-10 and 0.24g titanium dioxide respectively, driedly be mixed evenly, be contained in the alumina crucible, place under retort furnace 950-1100 ℃ and found, insulation 1h.The glass metal that melts is cast on the stainless steel plate of prior preheating, treats that electric furnace cooling back reheat to 640 is warming up to 890 ℃, insulation 4h carries out micritization to be handled, and naturally cools to room temperature.
To pulverize behind the above-mentioned composite ceramic material ball milling 24h.Promptly get the cmc soln that 11.45 gram powders add 8.8ml distilled water and 7.2ml0.5%, the 23g zirconia balls is to carry out under the technology of grinding medium.Behind ball milling, be made into ceramic slurry and apply or be sprayed on matrix surface, be incubated 1 hour down at 650 ℃ and found into composite ceramic coat.Its coefficient of expansion value is α=-0.0162 * 10
-6/ ℃.
Embodiment 10
Take by weighing 21.6g3#ABA-2,18.4g3#BL168,2.4g2#LZS-10 and 0.4g zirconium dioxide respectively, driedly be mixed evenly, be contained in the alumina crucible, place under retort furnace 1100-1200 ℃ and found, insulation 0.5h.The glass metal that melts is cast on the stainless steel plate of prior preheating, treat electric furnace cooling after, be warming up to 890 ℃ being heated to 640 ℃, insulation 4h carries out micritization to be handled, and naturally cools to room temperature.
To pulverize behind the above-mentioned composite ceramic material ball milling 24h.Promptly get 11.57 gram powders and add 8.9ml distilled water and 7.2ml cmc solns, the 23g zirconia balls is to carry out under the technology of grinding medium., behind ball milling, be made into ceramic slurry and apply or be sprayed on matrix surface, be incubated 1 hour down at 650 ℃ and found into composite inorganic micro-crystalline ceramic coating.Its coefficient of expansion value is α=-0.0421 * 10
-6/ ℃.
Claims (3)
1. the preparation method of a low temperature, unleaded, near-zero thermal expansion micro-crystalline ceramic coating is characterized in that the batching preparation is as follows respectively:
(1) preparation of low temperature frit 1:
Raw materials used is Quilonum Retard, boric acid, aluminium hydroxide, quartz and magnesium oxide, and according to (7-15): (65-80): (1-4): (5-10): weight ratio (1-5) is dried to be mixed evenly, places retort furnace 850-1100 ℃ to found, insulation 0.5-2h, shrend, ball mill pulverizing, standby;
(2) preparation of low temperature frit 2:
Raw materials used is Quilonum Retard, boric acid, aluminium hydroxide, quartz and magnesium oxide, and according to (5-15): (70-85): (9-17): (1-5): weight ratio (0.3-1.5) is dried to be mixed evenly, places retort furnace to found for 950 ℃, insulation 0.5-2h, shrend, ball mill pulverizing, standby;
(3) preparation of triphane melt:
Raw materials used is Quilonum Retard, aluminium hydroxide and quartz, and according to (12-18): (25-40): weight ratio (40-62) is dried to be mixed evenly, places retort furnace 1300-1500 ℃ to found, insulation 0.5-2h, and ball mill pulverizing, standby;
(4) preparation of eucryptite melt:
Raw materials used is Quilonum Retard, aluminium hydroxide and quartz, and according to (15-23): (35-50): weight ratio (30-45) is dried to be mixed evenly, place under retort furnace 1300-1500 ℃ and found, and insulation 0.5-2h, ball mill pulverizing, standby;
(5) preparation of wolframic acid zirconium powder body:
Raw materials used is zirconium white and wolframic acid, according to (17-26): weight ratio (74-90) is dried to be mixed even back and dehydrated alcohol, zirconia ball with weight ratio (0.5-1.5): (0.5-1): ratio ball milling 20-30h (1.5-2.5), again that slip is dry in 60-90 ℃ of loft drier, calcining makes ceramic powder then, calcining temperature 1100-1300 ℃, soaking time 1-3 hour, pulverize, standby;
(6) preparation of additive 1:
Raw materials used is zinc oxide and boric acid, according to (35-50): dried even being placed in the alumina crucible that be mixed of weight ratio (45-60), calcining makes ceramic powder then, and calcining temperature 900-1200 ℃, soaking time 0.5-1.5 hour, shrend, it is standby to pulverize the back;
(7) preparation of additive 2:
Raw materials used is Quilonum Retard, quartz, 85% phosphoric acid, Strontium carbonate powder and lithium fluoride, according to (15-30): (25-45): (1-10): (20-45): dried even being placed in the alumina crucible that be mixed of weight ratio (7-20), calcining makes ceramic powder then, calcining temperature 1100-1300 ℃, soaking time 0.5-1.5 hour, shrend, standby after pulverizing;
Preparation process is as follows:
With one or both or three kinds of arbitrary proportions in one or both arbitrary proportions in low temperature frit 2, triphane melt or the eucryptite melt and low temperature frit 1, wolframic acid zirconium powder body, additive 1 or the additive 2 and nucleator dried be mixed even, place under retort furnace 950-1200 ℃ and found, insulation 0.5-1h; The glass metal that melts is cast on the stainless steel plate of prior preheating, places then that 560-650 ℃ retort furnace relaying is continuous to be warming up to 750 ℃, and insulation 1-4h naturally cools to room temperature, after the pulverizing composite ceramic;
With composite ceramic add plastic agent, deionized water is made into slip, is coated in matrix surface, obtains composite inorganic micro-crystalline ceramic coating through 600-650 ℃ of following sintering.
2. the preparation method of low temperature according to claim 1, unleaded, near-zero thermal expansion micro-crystalline ceramic coating, it is characterized in that: plastic agent is methocel solution or cmc soln, mass concentration is 0.3-1%, and consumption is 0.2～1% of a powder quality.
3. the preparation method of low temperature according to claim 1, unleaded, near-zero thermal expansion micro-crystalline ceramic coating is characterized in that nucleator is zirconium dioxide or titanium oxide, and consumption is 0.5～2% of a powder quality.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010533239 CN101982435B (en) | 2010-11-05 | 2010-11-05 | Method for preparing low-temperature lead-free near zero expansion microcrystalline ceramic coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010533239 CN101982435B (en) | 2010-11-05 | 2010-11-05 | Method for preparing low-temperature lead-free near zero expansion microcrystalline ceramic coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101982435A true CN101982435A (en) | 2011-03-02 |
| CN101982435B CN101982435B (en) | 2012-02-01 |
Family
ID=43619349
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010533239 Active CN101982435B (en) | 2010-11-05 | 2010-11-05 | Method for preparing low-temperature lead-free near zero expansion microcrystalline ceramic coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101982435B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276278A (en) * | 2011-05-26 | 2011-12-14 | 中材高新材料股份有限公司 | Preparation method of inorganic composite coating on surface of silica fiber-reinforced silica-based composite material |
| CN103102078A (en) * | 2013-01-08 | 2013-05-15 | 广东伟邦微晶科技有限公司 | Preparation method of microcrystal dry grains, microlite ceramic tile and production method of microlite ceramic tile |
| CN106116700A (en) * | 2016-06-30 | 2016-11-16 | 山东工业陶瓷研究设计院有限公司 | Nitride ceramics high-temperature wear resistant coating and preparation method thereof |
| CN108706878A (en) * | 2018-07-02 | 2018-10-26 | 福建省德化祥裕陶瓷文化有限责任公司 | A kind of near-zero thermal expansion glaze water and preparation method thereof |
| CN108793752A (en) * | 2018-07-02 | 2018-11-13 | 福建省德化祥裕陶瓷文化有限责任公司 | A kind of microwave-medium glaze water and preparation method thereof |
| CN111718121A (en) * | 2019-03-20 | 2020-09-29 | 山东工业陶瓷研究设计院有限公司 | Low-melting-point borate material with wave-transmitting performance and preparation method thereof |
| CN113604112A (en) * | 2021-08-31 | 2021-11-05 | 深圳清研皓隆科技有限公司 | Electrothermal coating and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5082810A (en) * | 1990-02-28 | 1992-01-21 | E. I. Du Pont De Nemours And Company | Ceramic dielectric composition and method for preparation |
| JP2005139030A (en) * | 2003-11-06 | 2005-06-02 | Hojun:Kk | Gel-like clay containing no water, method of manufacturing gel-like clay, and polar organic solvent prepared using gel-like clay and gel-like clay composition dispersed and thickened in polar organic solvent |
| CN1854105A (en) * | 2004-12-31 | 2006-11-01 | 电子科技大学 | Nanometer ceramic-material doping agent, ceramic capacitor media material and production thereof |
| CN101045609A (en) * | 2007-03-29 | 2007-10-03 | 复旦大学 | Preparation process of lithium-doped glass film suitable for ion exchange |
-
2010
- 2010-11-05 CN CN 201010533239 patent/CN101982435B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5082810A (en) * | 1990-02-28 | 1992-01-21 | E. I. Du Pont De Nemours And Company | Ceramic dielectric composition and method for preparation |
| JP2005139030A (en) * | 2003-11-06 | 2005-06-02 | Hojun:Kk | Gel-like clay containing no water, method of manufacturing gel-like clay, and polar organic solvent prepared using gel-like clay and gel-like clay composition dispersed and thickened in polar organic solvent |
| CN1854105A (en) * | 2004-12-31 | 2006-11-01 | 电子科技大学 | Nanometer ceramic-material doping agent, ceramic capacitor media material and production thereof |
| CN101045609A (en) * | 2007-03-29 | 2007-10-03 | 复旦大学 | Preparation process of lithium-doped glass film suitable for ion exchange |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276278A (en) * | 2011-05-26 | 2011-12-14 | 中材高新材料股份有限公司 | Preparation method of inorganic composite coating on surface of silica fiber-reinforced silica-based composite material |
| CN102276278B (en) * | 2011-05-26 | 2012-12-12 | 中材高新材料股份有限公司 | Preparation method of inorganic composite coating on surface of silica fiber-reinforced silica-based composite material |
| CN103102078A (en) * | 2013-01-08 | 2013-05-15 | 广东伟邦微晶科技有限公司 | Preparation method of microcrystal dry grains, microlite ceramic tile and production method of microlite ceramic tile |
| CN103102078B (en) * | 2013-01-08 | 2015-08-05 | 广东伟邦微晶科技有限公司 | A kind of preparation method of crystallite dry granular, microlite ceramic tile and production method thereof |
| CN106116700A (en) * | 2016-06-30 | 2016-11-16 | 山东工业陶瓷研究设计院有限公司 | Nitride ceramics high-temperature wear resistant coating and preparation method thereof |
| CN108706878A (en) * | 2018-07-02 | 2018-10-26 | 福建省德化祥裕陶瓷文化有限责任公司 | A kind of near-zero thermal expansion glaze water and preparation method thereof |
| CN108793752A (en) * | 2018-07-02 | 2018-11-13 | 福建省德化祥裕陶瓷文化有限责任公司 | A kind of microwave-medium glaze water and preparation method thereof |
| CN108793752B (en) * | 2018-07-02 | 2021-09-24 | 福建省德化祥裕陶瓷文化有限责任公司 | Microwave medium glaze water and preparation method thereof |
| CN111718121A (en) * | 2019-03-20 | 2020-09-29 | 山东工业陶瓷研究设计院有限公司 | Low-melting-point borate material with wave-transmitting performance and preparation method thereof |
| CN113604112A (en) * | 2021-08-31 | 2021-11-05 | 深圳清研皓隆科技有限公司 | Electrothermal coating and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101982435B (en) | 2012-02-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101982435B (en) | Method for preparing low-temperature lead-free near zero expansion microcrystalline ceramic coating | |
| CN102276278B (en) | Preparation method of inorganic composite coating on surface of silica fiber-reinforced silica-based composite material | |
| CN102797042B (en) | Crucible for melting crystalline silicon, method for producing crucible and spray coating liquid | |
| CN102527594A (en) | Quartz crucible for ingot casting and manufacturing method thereof | |
| CN106187289A (en) | A kind of method utilizing nickel slag and biomass powder to prepare light foamed ceramic | |
| CN110117457A (en) | A kind of high temperature resistant anti-infrared attenuation energy-saving coatings | |
| CN108911778A (en) | A kind of production method of lithium tailing light ceramic plate | |
| CN106116700A (en) | Nitride ceramics high-temperature wear resistant coating and preparation method thereof | |
| CN102786300B (en) | Radiant heat reinforced absorbent and preparation method thereof | |
| CN103305039A (en) | Infrared radiation coating, preparation method thereof and infrared radiation coating | |
| CN102765950B (en) | Cordierite light fire brick and preparation method of cordierite light fire brick | |
| CN106336117B (en) | A kind of preparation method of the waterproof coating of fused quartz ceramic | |
| CN106316134B (en) | A kind of diopside and feldspar principal crystalline phase devitrified glass and preparation method thereof | |
| CN106431370B (en) | Using aluminium chromium slag as mullite synthesizing raw material of major ingredient and preparation method thereof | |
| Lu et al. | PREPARATION AND PERFORMANCE STUDY OF GLASS-CERAMIC GLAZES DERIVED FROM BLAST FURNACE SLAG AND FLY ASH | |
| CN113698211B (en) | Coating for smelting aluminum lithium alloy crucible and preparation and coating methods thereof | |
| CN102167512A (en) | Silicon carbide-doped glass-ceramic coating for titanium alloy | |
| CN105801141B (en) | Ausmelt furnace furnace bottom macro hole Corundum-spinel brick and preparation method thereof | |
| CN102560321B (en) | Yttrium silicate hot-spray composite powder and preparation method thereof | |
| CN102030535B (en) | Preparation method of zirconium-nitride enhanced aluminum-oxynitride composite ceramic material | |
| WO2024032163A1 (en) | Method for preparing high-temperature- and wear-resistant ceramic coating | |
| CN109081687B (en) | High thermal shock resistance ceramic crucible suitable for calcining lithium battery anode material and preparation method thereof | |
| CN110066598A (en) | A kind of high temperature anti-dropout infrared radiative energy-saving coating | |
| CN105860611A (en) | Infrared radiation paint and preparation method thereof | |
| CN105272315A (en) | Porous calcium zirconium aluminate and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |