CN102424568B - Method for preparing tungsten-containing alumina ceramic heating substrate - Google Patents
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- CN102424568B CN102424568B CN 201110259241 CN201110259241A CN102424568B CN 102424568 B CN102424568 B CN 102424568B CN 201110259241 CN201110259241 CN 201110259241 CN 201110259241 A CN201110259241 A CN 201110259241A CN 102424568 B CN102424568 B CN 102424568B
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Abstract
The invention provides a method for preparing a tungsten-containing alumina ceramic heating substrate, and relates to a method for preparing a ceramic heating element. The invention is capable of solving the problems of poor wettability on powder by a solvent (water), difficult defoaming on slurry, slow volatilization, long drying time, poor bonding force of ceramic and metal level after sintering during an aqueous tape-casting process. The method for preparing the tungsten-containing alumina ceramic heating substrate can substantially enhance the sintering qualification rate and production efficiency. The method comprises the following steps: preparing a premix compound and tungsten slurry, ball milling, tape-casting, screen printing, sintering and nickel plating.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, relate to a kind of preparation method of ceramic heating element, especially relate to a kind of preparation method of tungsten-containing alumina ceramic heating substrate.
Background technology
Ceramic heating base plate is a new generation's upgrading Heating element product innovation of developing in recent years, have the characteristics such as the feature of environmental protection, high reliability, long lifetime due to it, substituting the PTC heating unit that contains plumbous composition that in the past generally used, the domestic and international application market outlook are wide.Therefore the production technology of researching high-temperature alumina ceramic heating pdm substrate is by people institute pay attention to day by day.
At present, more common production technique is that wherein hot die-casting molding technique is often adopted in compacting with steps such as ceramic raw material process ball milling, compacting, sintering, metallization, double sintering and nickel plating, and the blank of moulding easily is out of shape, yield rate is low.And pottery also often runs into following problem in metallization processes: Metallization strength is on the low side, membranous layer binding force is poor, density is low, metallization face printing opacity, easily oxidation etc.These not only cause yield rate to lower, and affect quality product, and therefore constantly research improves the metallization process level, and is most important for the development of improving the quality of products, promote ceramic heating element.
As everyone knows, flow casting molding is widely used in the preparation of ceramic substrate and sandwich as a kind of important moulding process of thin slice stupalith.It can be divided into non-water system and water system two classes.The casting technique of non-water system is comparative maturity, and the ceramic green sheet even structure of preparation, intensity is high, snappiness good, is convenient to cutting and processing, widespread use in industrial production.But be that non-water system flow casting molding adopts a large amount of organic solvents, serious environment pollution causes the raising of production cost.Therefore, low, nontoxic, water system curtain coating technology environmental protection of research cost has become irreversible trend.
The water system casting molding processes makes water substitute organic solvent as solvent, because water molecules is polar molecule, and binding agent, plastic agent and dispersion agent etc. are organic additives, and there is the problem of consistency between water molecules, therefore in the selection of additive, need to select water-soluble or the organism that can form stabilized emulsion in water to guarantee to obtain the slurry of stable homogeneous.This shows, the suitable slurry of preparation is crucial in the water system casting molding processes.
Chen Hualong (Chen Hualong. the research [J] of water system curtain coating alumina ceramic substrate. Chinese pottery industry, 2009,16 (1): 13-20) point out to adopt compound binding agent more easily to operate than single binding agent, defective still less but can not exert an influence to performance.And experiment adds appropriate PVA when obtaining compound binding agent and being 20wt%PVA+80wt%B-1070 in casting slurry, improved the yield value of slurry, obtains being fit to the slurry of curtain coating.
The people such as Fu Changyi (Fu Changyi, the water system flow casting molding research [J] of the .99 alumina ceramic substrates such as Luo Linghong. Chinese pottery, 2009,45 (9): 7-9) point out the pH value be 9.0 and dispersion agent polyacrylic acid (PAA) consumption be under the condition of 0.5-0.6wt%, can prepare the alumina slurry of high solids content (45vol%), stably dispersing.
Although these researchs have all promoted the development of water system casting molding processes, still have some problems to be solveds: (1) solvent (water) is relatively poor to the wettability of powder, volatilization is slow, time of drying is long; (2) removing bubbles from slurry difficulty; (3) after casting film-forming, the ceramic green sheet snappiness is relatively poor, crack defect easily occurs, and intensity is not high etc.
And in the ceramic metallization process, ceramic metallization method commonly used mainly contains chemical Ni-P plating method, electroplating Ni-P alloy method, high temperature sintering by Ag (Ni) method, Mo-Mn sintering process, vacuum evaporatation and vacuum sputtering coating method at present.Although the electroless plating rete is anti-corrosion, wear resistance good, hardness is high, hole is few, and does not need power supply, membranous layer binding force is poor, and tensile strength is low, and the plating solution cost is high, complex technical process.Although the electroplated Ni rete is made a concerted effort by force with ceramic junction, internal stress is little, but the cleaning on the porcelain piece that metallized surface and the impact of the pure degree of plating solution are large, cause the defective of metallization porcelain piece after electroplating more, such as peeling, foaming, pit, stain etc., very easily be subjected to simultaneously the impact of different positions in Electropolating hangers and plating cylinder, cause covering power poor, mutually the blocking between porcelain piece of metallizing in addition also can cause the porcelain piece surface that the phenomenon of male and female face is arranged.High temperature sintering is that the rete that obtains is partially thin, discontinuous, inhomogeneous and Erosion resistance is poor by the present subject matter of Ag (Ni) method.Although vacuum evaporatation is a kind of cleaning procedure, metallic diaphragm is relatively poor with the bonding force of pottery, and the thickness of rete is wayward, uniformity coefficient and consistence is poor, the utilization ratio of material is lower.This shows, the bonding strength that improves metal and pottery in the ceramic metallization process is crucial.
Disclose a kind of method in Japanese Patent JP No.5-238857, it is by adding extremely expensive titanium hydride to make substrate reach enough cohesive strengths in Metal slurry.But this method has obviously increased manufacturing cost.
Publication number is that the Chinese patent of CN 101104567A discloses a kind of recombining process, and it provides a kind of middle temperature metallizing formula and technique to improve tensile strength and the resistance to air loss of metal layer, has obtained average tensile strength value 〉=150MPa, leak rate≤1 * 10
-11Pam
3/ s.But this metallizing formula can only be used for the surface recombination of 95% alumina-ceramic, and its application is limited by very large.
Summary of the invention
Main purpose of the present invention is to provide can solve that water system flow casting molding Solvent (water) is relatively poor to the wettability of powder, removing bubbles from slurry is difficult, volatilization is slow and time of drying is long, and pottery and the problems such as the metal level bonding force is poor after sintering, can significantly improve the preparation method of a kind of tungsten-containing alumina ceramic heating substrate of sintering qualification rate and production efficiency.
The present invention includes following steps:
1) the ceramic Preblend of preparation and tungsten slurry
Distilled water, magnesium oxide, titanium oxide, dispersion agent and fluidizer are mixed, then add alumina powder and with ammoniacal liquor regulation system pH value, make ceramic Preblend; Tungsten powder, Binder Phase, organic carrier are put into the vibromill mix grinding after mixing, make the median size of slurry less than 0.8 μ m, make tungsten slurry;
2) ball milling
With step 1) made ceramic Preblend ball milling, then add the binding agent mix grinding, make the median size of slurry less than 0.3 μ m, add afterwards defoamer, carry out vacuum stripping, make ceramic size;
3) flow casting molding
With step 2) made ceramic size flow casting molding and dry on casting machine, the aluminum oxide ceramic chips is made in section afterwards;
4) silk screen printing
With step 1) made tungsten slurry deposits on the surface of aluminum oxide ceramic chips equably through screen printing technique;
5) sintering
With step 4) in carry out with the aluminum oxide ceramic chips of print film standing, dry, binder removal is processed, sintering, the substrate that obtains sintering;
6) nickel plating
Adopt nickel chemical plating technology, the plating solution of the substrate that sinters being put into sulfur acid nickel keeps, and makes the substrate surface that sinters form one deck nickel dam, namely obtains tungsten-containing alumina ceramic heating substrate.
In step 1) in, the content of described distilled water, magnesium oxide, titanium oxide, dispersion agent and fluidizer is respectively 93%～110%, 1%～2.4%, 0.4%～1.2%, 1%～2.4% and 9.7%～12% of described alumina powder quality; Described pH value can be 10～11; Described dispersion agent can be polyacrylic acid etc., and described fluidizer can be polyoxyethylene glycol etc.; The composition of described Binder Phase can be by mass percentage: manganese oxide 5%～10%, magnesium oxide 15%～25%, silicon-dioxide 60%～80%; The composition of described organic carrier can be by mass percentage: Terpineol 350 60%～70%, butylcarbitol 15%～25%, butyl carbitol acetate 5%～15%, ethyl cellulose 2%～8%, Yelkin TTS 0.2%～0.8%; Described organic carrier is ultrasonic agitation 15～20min gained after each component of organic carrier is mixed; The composition of described tungsten slurry can be by mass percentage: tungsten powder 60%～90%, Binder Phase 20%～40%, organic carrier 5%～30%.
In step 2) in, the time of described ball milling can be 23～26h; The time of described mix grinding can be 0.4～0.6h; The composition of described binding agent can be by mass percentage: polyvinyl alcohol 50%～60%, and polyethylene glycol 40%～50%, the add-on of binding agent can be 9.7%～11.5% of described alumina powder quality; Described defoamer can be paraffin series emulsion etc., and the add-on of defoamer can be 0.4%～1.2% of described alumina powder quality; Described vacuum stripping can be adopted the vacuum tank of putting under the 4000Pa residual voltage, stirs 0.5～1h.
In step 4) in, the print film thickness of described tungsten slurry can be 25～40 μ m.
In step 5) in, the described standing time can be 10～20min; The temperature of described drying can be 150～200 ℃, is preferably 160～180 ℃, and the dry time can be 15～20min; Described binder removal is processed can in loft drier, the heat-up rate with 10 ℃/min be warmed up to 370～400 ℃ with being placed on the aluminum oxide ceramic chips of print film after drying, is preferably 380～390 ℃, and is incubated 3～5h; Described sintering can in the stove that contain hydrogen reduction atmosphere, the heat-up rate with 2 ℃/min be warmed up to 1500～1700 ℃ with transferring to the aluminum oxide ceramic chips of print film after the binder removal processing, be preferably 1550～1600 ℃, and be incubated 2～3h, wherein nitrogen atmosphere is wet hydrogen atmosphere, when entering, passes through hydrogen the tank in humidifier, bring a certain amount of steam into, just control the size of vapour quantity by water temperature, water temperature can be 40～55 ℃.
In step 6) in, the temperature of the plating solution of described sulfur acid nickel can be 75～85 ℃, is preferably 78～83 ℃; The thickness of described nickel dam can be 2～5 μ m.
The tungsten-containing alumina ceramic heating substrate that adopts above-mentioned preparation method to produce is tested its density 〉=3.8g/cm with Archimedes's method
3Test its tensile strength 〉=150MPa with electronic universal tester; Resistance to air loss≤1 * 10
-10Pam
3/ s; Record its insulation resistance 〉=5 * 10 with Insulation Resistance Tester
9Ω; Normal temperature resistance 70～200 Ω; Satisfy electron trade fully to the requirement of ceramic metallization product.
Adopt such scheme, have the following advantages:
1, contain titanium oxide in ceramic material formula of the present invention, character constant and the Al of titanium oxide
2O
3The character constant approach, can and Al
2O
3Generate sosoloid; The simultaneous oxidation titanium is the oxide compound that appraises at the current rate, and produces defective because the effect of appraising at the current rate makes the alumina-ceramic microtexture, the activation character, and acceleration of sintering can make sintering temperature reduce by 100～150 ℃.
2, contain defoamer in raw material of the present invention, and added ultrasonic stirring and vacuum degassing process, the ceramic chips pore after moulding is less, resistance to air loss good.
3, the present invention adopts flow casting molding, the simple and process stabilizing of molding device, but operate continuously, and production efficiency is high, and automatization level is high, forming ceramic substrate performance uniformity and be easy to control.
4, adopt manganese oxide, magnesium oxide and silicon-dioxide to make binding agent in Metal slurry of the present invention, and by rationally adjusting three's ratio, make that the bonding strength of metal level and pottery improves greatly after moulding.
5, the present invention adopts screen printing technique, and the even and thickness of print film is easily regulated, and stereoscopic sensation is strong, and the screen printing apparatus cost is low in addition, easily forms large-scale production.
6, the present invention adopts two-step sintering method and has selected suitable intensification route, has improved sintering qualification rate, greatly reduces production cost.
In sum, the present invention has the bonding force that can significantly improve metal layer and pottery after sintering, makes that the ceramic heating base plate yield rate is high, the preparation method of the measured tungsten-containing alumina ceramic heating substrate of matter.The ceramic heating base plate performance of being produced by the method is good, quality is good, yield rate is high, and production cost is low; The method improves overall performance and the sintering qualification rate of ceramic heating base plate by rational slurry preparation and suitable operational path.And this preparation method is simple, and is easy to operate, is suitable for large-scale production.Products obtained therefrom can satisfy electron trade fully to the requirement of ceramic metallization product.Ceramic heating base plate of the present invention can be widely used in the fields such as household electrical appliance, medical disinfecting, electric heating equipment.
Description of drawings
Fig. 1 is the preparation flow figure of the embodiment of the present invention.
Fig. 2 is the sintering heating curve figure in the sintering step of the embodiment of the present invention.In Fig. 2, X-coordinate is time/min, ordinate zou be temperature/℃; Fig. 2 has provided step 5) drying, binder removal in (sintering) process and the heating curve figure of final high temperature sintering, embodied corresponding time and temperature relation.
Embodiment
Embodiment 1
1. the preparation of ceramic Preblend
Distilled water, magnesium oxide, titanium oxide, dispersion agent and fluidizer are mixed, stir 15min with ultrasonic stirrer, then add 96% alumina powder and with ammoniacal liquor regulation system pH value to 11, make ceramic Preblend.Wherein the add-on of distilled water, magnesium oxide, titanium oxide, dispersion agent and fluidizer is respectively 101%, 1.8%, 0.7%, 1.6%, 10.7% of described alumina powder quality.
2. the preparation of tungsten slurry
The composition of tungsten slurry is by mass percentage: tungsten powder 70%, Binder Phase 20%, organic carrier 10%; Tungsten powder, Binder Phase, organic carrier are put into the vibromill mix grinding after mixing, and make the tungsten slurry median size less than 0.8 μ m.Wherein the composition of Binder Phase is by mass percentage: manganese oxide 5%, magnesium oxide 20%, silicon-dioxide 75%; The composition of organic carrier is by mass percentage: Terpineol 350 65.5%, and butylcarbitol 20%, butyl carbitol acetate 10%, ethyl cellulose 4%, Yelkin TTS 0.5% stirs 18min with ultrasonic stirrer after each composition of organic carrier mixes.
2) vibromill ball milling 24h is put in above-mentioned ceramic Preblend, then (composition of binding agent is by mass percentage: polyvinyl alcohol 60% to add 10.5% binding agent, polyethylene glycol 40%) mix grinding 0.5h, make the median size of slurry less than 0.3 μ m, add afterwards 0.9% defoamer and stir 10min with ultrasonic stirrer, the vacuum tank stirring 0.8h that then slurry is put under the 4000Pa residual voltage carries out vacuum stripping, stir 10min with ultrasonic stirrer more at last, make ceramic size.
3) with ceramic size flow casting molding and dry on casting machine, the aluminum oxide ceramic chips is made in section afterwards.
4) silk screen printing.The tungsten slurry for preparing is deposited on the surface of aluminum oxide ceramic chips equably through screen printing technique, and wherein the print film thickness of tungsten slurry is 30 μ m.
5) will carry out with the aluminum oxide ceramic chips of print film standingly, time of repose is 20min, more standing rear aluminum oxide ceramic chips with print film is put into infrared drying oven carry out drying treatment.Wherein drying temperature is 160 ℃, and the time is 20min.Then the heat-up rate with 10 ℃/min is warmed up to 380 ℃, and insulation 4h carries out binder removal to be processed.Transfer to afterwards in the stove that contains hydrogen reduction atmosphere under the condition that heat-up rate with 2 ℃/min is raised to 1570 ℃ and insulation 2h and carry out high temperature sintering, the substrate that obtains sintering.
6) nickel plating.Adopt nickel chemical plating technology, the plating solution of the substrate that sinters being put into 80 ℃ of sulfur acid nickel keeps 40min, makes the substrate surface that sinters form one deck 3 thick nickel dams of μ m, can obtain tungsten-containing alumina ceramic heating substrate of the present invention.
The tungsten-containing alumina ceramic heating substrate that obtains is tested, and test result sees Table 1.
Embodiment 2
The preparation method is with embodiment 1, difference is, step 1) 1. described in the add-on of distilled water, magnesium oxide, titanium oxide, dispersion agent and fluidizer of ceramic Preblend be respectively 103%, 1.4%, 0.9%, 1.8%, 10.6% of described alumina powder quality.Described pH value is 10.The add-on of defoamer step 2) is 0.7% of described alumina powder quality, and the add-on of binding agent is 11% of described alumina powder quality, and the composition of binding agent is by mass percentage: polyvinyl alcohol 55%, polyethylene glycol 45%.
The tungsten-containing alumina ceramic heating substrate that obtains is tested, and test result sees Table 1.
Embodiment 3
The preparation method is with embodiment 1, difference is, in the pottery premix formulation, the add-on of distilled water, magnesium oxide, titanium oxide, dispersion agent and fluidizer is respectively 99%, 1.5%, 1.0%, 2.0%, 10% of described alumina powder quality, and described pH value is 10.5.The add-on of defoamer is 1.0% of described alumina powder quality, and the add-on of binding agent is 10% of described alumina powder quality, and the composition of binding agent is by mass percentage: polyvinyl alcohol 50%, polyethylene glycol 50%.
The ceramic heating substrate that obtains is tested, and test result sees Table 1.
Embodiment 4
The preparation method is with embodiment 1, and difference is, the composition of tungsten slurry is by mass percentage: tungsten powder 65%, Binder Phase 23%, organic carrier 12%.Wherein the composition of Binder Phase is by mass percentage: manganese oxide 8%, magnesium oxide 22%, silicon-dioxide 70%; The composition of organic carrier is by mass percentage: the content of Terpineol 350 is 68.4%, and the content of butylcarbitol is 18%, and the content of butyl carbitol acetate is 8%, and the content of ethyl cellulose is 5%, and the content of Yelkin TTS is 0.6%.
The ceramic heating substrate that obtains is tested, and test result sees Table 1.
Embodiment 5
The preparation method is with embodiment 1, and difference is, the composition of tungsten slurry is by mass percentage: tungsten powder 75%, Binder Phase 17%, organic carrier 8%.Wherein the composition of Binder Phase is by mass percentage: manganese oxide 7%, magnesium oxide 17%, silicon-dioxide 76%; The composition of organic carrier is by mass percentage: the content of Terpineol 350 is 67%, and the content of butylcarbitol is 16%, and the content of butyl carbitol acetate is 11%, and the content of ethyl cellulose is 5.5%, and the content of Yelkin TTS is 0.5%.
The ceramic heating substrate that obtains is tested, and test result sees Table 1.
Embodiment 6
The preparation method is with embodiment 1, and difference is, in step 5) in time of repose be 12min, the temperature of infrared drying is 170 ℃, the time is 18min.Then the speed with 10 ℃/min is warmed up to 385 ℃, and insulation 3.5h carries out binder removal to be processed.The speed with 2 ℃/min transferred to afterwards in the stove that contains hydrogen reduction atmosphere is raised under the condition of 1600 ℃ and insulation 2.5h carries out high temperature sintering.
The ceramic heating substrate that obtains is tested, and test result sees Table 1.
Embodiment 7
The preparation method is with embodiment 1, and difference is, in step 5) in time of repose be 15min, the temperature of infrared drying is 190 ℃, the time is 15min.Then the speed with 10 ℃/min is warmed up to 390 ℃, and insulation 4h carries out binder removal to be processed.The speed with 2 ℃/min transferred to afterwards in the stove that contains hydrogen reduction atmosphere is raised under the condition of 1580 ℃ and insulation 2.5h carries out high temperature sintering.
The ceramic heating substrate that obtains is tested, and the test result of each embodiment gained ceramic heating substrate sees Table 1.
Table 1
| Embodiment | Density (g/cm 3) | Tensile strength (MPa) | Insulation resistance (1 * 10 9Ω) | Normal temperature resistance (Ω) |
| 1 | 3.85 | 160 | 5.2 | 150 |
| 2 | 3.84 | 150 | 5.2 | 145 |
| 3 | 3.83 | 155 | 5.3 | 155 |
| 4 | 3.83 | 150 | 5.3 | 165 |
| 5 | 3.84 | 155 | 5.2 | 140 |
| 6 | 3.82 | 160 | 5.2 | 150 |
| 7 | 3.84 | 155 | 5.2 | 145 |
At present, common alumina ceramic heating substrate density is about 3.72g/cm
3, insulation resistance 〉=5 * 10
7Ω; As can be seen from Table 1, adopt tungsten-containing alumina ceramic heating substrate that preparation method of the present invention produces with Archimedes's method test its density equal 〉=3.8g/cm
3With electronic universal tester test its tensile strength all 〉=150MPa; Resistance to air loss≤1 * 10
-10Pam
3/ s; Record its insulation resistance all 〉=5.2 * 10 with Insulation Resistance Tester
9Ω; Normal temperature resistance all 〉=140 Ω (between 70～200 Ω); Satisfy electron trade fully to the requirement of ceramic metallization product.This shows, the tungsten-containing alumina ceramic heating substrate density that adopts preparation method of the present invention to produce is large, resistance to air loss good, and insulation resistance is large, and pottery is high with the bonding strength of metal, and market outlook will be very wide.
Claims (9)
1. the preparation method of a tungsten-containing alumina ceramic heating substrate is characterized in that comprising the following steps:
1) the ceramic Preblend of preparation and tungsten slurry
Distilled water, magnesium oxide, titanium oxide, dispersion agent and fluidizer are mixed, then add alumina powder and with ammoniacal liquor regulation system pH value, make ceramic Preblend; Tungsten powder, Binder Phase, organic carrier are put into the vibromill mix grinding after mixing, make the median size of slurry less than 0.8 μ m, make tungsten slurry;
The content of described distilled water, magnesium oxide, titanium oxide, dispersion agent and fluidizer is respectively 93%～110%, 1%～2.4%, 0.4%～1.2%, 1%～2.4% and 9.7%～12% of described alumina powder quality, and the content summation of each component is 100%;
Described dispersion agent is polyacrylic acid, and described fluidizer is polyoxyethylene glycol; The composition of described Binder Phase is by mass percentage: manganese oxide 5%～10%, and magnesium oxide 15%～25%, silicon-dioxide 70%～80%, the content summation of each component is 100%; The composition of described organic carrier is by mass percentage: Terpineol 350 60%～70%, and butylcarbitol 15%～25%, butyl carbitol acetate 5%～15%, ethyl cellulose 2%～8%, Yelkin TTS 0.2%～0.8%, the content summation of each component is 100%;
The composition of described tungsten slurry is by mass percentage: tungsten powder 60%～75%, and Binder Phase 20%～40%, organic carrier 5%～30%, the content summation of each component is 100%;
2) ball milling
With step 1) made ceramic Preblend ball milling, then add the binding agent mix grinding, make the median size of slurry less than 0.3 μ m, add afterwards defoamer, carry out vacuum stripping, make ceramic size;
3) flow casting molding
With step 2) made ceramic size flow casting molding and dry on casting machine, the aluminum oxide ceramic chips is made in section afterwards;
4) silk screen printing
With step 1) made tungsten slurry deposits on the surface of aluminum oxide ceramic chips equably through screen printing technique;
5) sintering
With step 4) in carry out with the aluminum oxide ceramic chips of print film standing, dry, binder removal is processed, sintering, the substrate that obtains sintering; The described standing time is 10～20min; The temperature of described drying is 150～200 ℃, and described binder removal processes that in loft drier, the heat-up rate with 10 ℃/min is warmed up to 370～400 ℃ with being placed on the aluminum oxide ceramic chips of print film after drying, and is incubated 3～5h; Described sintering is that in the stove that contains hydrogen reduction atmosphere, the heat-up rate with 2 ℃/min is warmed up to 1500～1700 ℃ with transferring to the aluminum oxide ceramic chips of print film after the binder removal processing, and be incubated 2～3h, wherein nitrogen atmosphere is wet hydrogen atmosphere, when entering, passes through hydrogen the tank in humidifier, bring a certain amount of steam into, just control the size of vapour quantity by water temperature, water temperature is 40～55 ℃;
6) nickel plating
Adopt nickel chemical plating technology, the plating solution of the substrate that sinters being put into sulfur acid nickel keeps, and makes the substrate surface that sinters form one deck nickel dam, namely obtains tungsten-containing alumina ceramic heating substrate.
2. the preparation method of a kind of tungsten-containing alumina ceramic heating substrate as claimed in claim 1, is characterized in that in step 1) in, described pH value is 10～11.
3. the preparation method of a kind of tungsten-containing alumina ceramic heating substrate as claimed in claim 1, is characterized in that in step 2) in, the time of described ball milling is 23～26h; The time of described mix grinding is 0.4～0.6h; The composition of described binding agent is by mass percentage: polyvinyl alcohol 50%～60%, and polyethylene glycol 40%～50%, the add-on of binding agent is 9.7%～11.5% of described alumina powder quality.
4. the preparation method of a kind of tungsten-containing alumina ceramic heating substrate as claimed in claim 1, is characterized in that in step 2) in, described defoamer is the paraffin series emulsion, the add-on of defoamer is 0.4%～1.2% of described alumina powder quality; The vacuum tank of putting under the 4000Pa residual voltage is adopted in described vacuum stripping, stirs 0.5～1h.
5. the preparation method of a kind of tungsten-containing alumina ceramic heating substrate as claimed in claim 1, is characterized in that in step 4), and the print film thickness of described tungsten slurry is 25～40 μ m.
6. the preparation method of a kind of tungsten-containing alumina ceramic heating substrate as claimed in claim 1, is characterized in that in step 5) in, the temperature of described drying is 160～180 ℃, the dry time is 15～20min; Described binder removal processes that in loft drier, the heat-up rate with 10 ℃/min is warmed up to 380～390 ℃ with being placed on the aluminum oxide ceramic chips of print film after drying, and is incubated 3～5h; Described sintering is that in the stove that contains hydrogen reduction atmosphere, the heat-up rate with 2 ℃/min is warmed up to 1550～1600 ℃ with transferring to the aluminum oxide ceramic chips of print film after the binder removal processing, and is incubated 2～3h.
7. the preparation method of a kind of tungsten-containing alumina ceramic heating substrate as claimed in claim 1, is characterized in that in step 6), and the temperature of the plating solution of described sulfur acid nickel is 75～85 ℃.
8. the preparation method of a kind of tungsten-containing alumina ceramic heating substrate as claimed in claim 7, the temperature that it is characterized in that the plating solution of described sulfur acid nickel is 78～83 ℃.
9. the preparation method of a kind of tungsten-containing alumina ceramic heating substrate as claimed in claim 1, is characterized in that in step 6), and the thickness of described nickel dam is 2～5 μ m.
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| CN101328068A (en) * | 2008-07-28 | 2008-12-24 | 浙江大学 | Preparation of boric microwave dielectric ceramic aqueous tape casting diaphragm |
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| CN101913869A (en) * | 2010-08-12 | 2010-12-15 | 哈尔滨工业大学 | Oxide thermoelectric material capable of being sintered at low temperature and preparation method thereof |
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