CN1258765A - Rare-earth compound pulp and surface sculpture method for diamond thick-film - Google Patents
Rare-earth compound pulp and surface sculpture method for diamond thick-film Download PDFInfo
- Publication number
- CN1258765A CN1258765A CN 99124562 CN99124562A CN1258765A CN 1258765 A CN1258765 A CN 1258765A CN 99124562 CN99124562 CN 99124562 CN 99124562 A CN99124562 A CN 99124562A CN 1258765 A CN1258765 A CN 1258765A
- Authority
- CN
- China
- Prior art keywords
- diamond thick
- rare
- film
- pulp
- earth compound
- 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
Pulp of rare earth compound, such as cerium oxide and lanthanum nitrate, is first printed onto the growth surface of diamond thick film, then sintered at 400-600 deg.c for 2-5 hr and finally cleaned with concentrated sulfuric acid. The pulp is compounded through mixing and grinding material and solvent and adding blender. The present invention uses cheap material, simple etching process and simple equipment to result in good etching effect, needs shorter mechanical polishing period and the pulp may be printed in certain pattern. All these are favorable to the application of diamond thick film in electronic package field.
Description
The invention belongs to the method for CVD diamond thick-film surface being carried out etching.
Diamond thick-film has excellent physical properties, especially unrivaled high heat conductance, high resistivity, and advantages such as low-dielectric loss, low thermal coefficient of expansion are the ideal materials of the radiating insulating substrate in the preparation Electronic Packaging neck city.The application of CVD diamond thick-film in electronics must solve the precision sizing problem of diamond thick-film, and the planeness that makes the surface is greater than 0.03 μ m, and the Rockwell hardness of diamond thick-film is about 10, its surface finish become limit a difficult problem of its application.
The prior art close with the present invention is the rare earth metal etching method of the diamond thick-film surface being carried out etching.The detailed process summary is: with rare earth metal, such as the thin slice of lanthanum, be pressed on the aufwuchsplate of diamond thick-film, place high-temperature vacuum furnace, make rare earth metal fusing under the melting temperature of rare earth metal and generate metallic carbide being higher than with the diamond thick-film surface, from the hardness of face reduction CVD diamond surface, so that further carry out mechanical polishing.This lithographic method: the first, must at high temperature carry out, for the oxidation of avoiding diamond thick-film under the high temperature again must be at molten rare earth metal under the vacuum condition.This not only makes the conditional request of this method very harsh, and needs high-temperature vacuum equipment.Second rare earth metal is very expensive as consumable material.
Purpose of the present invention overcomes the deficiencies in the prior art exactly, by the preparation and the use of rare-earth compound pulp, make the diamond thick-film etching technics reduce required temperature and vacuum condition, reduce equipment requirements, reduce the etching cost, be beneficial to the application of the Electronic Packaging of diamond thick-film.
Lithographic method of the present invention divides pulp preparation-printing-sintering-cleaning several steps.
The slurry that the present invention uses is a rare-earth compound pulp.The composition of slurry comprises that the oxide compound of cerium and lanthanum or salt are raw material, and the mass ratio of cerium, lanthanum compound is 1: (1～0.3), Terpineol 350, citric acid and ethyl cellulose or their mixture are that blender mixes.
The method of diamond thick-film surface etch is that rare-earth compound pulp is printed on the diamond thick-film aufwuchsplate, can adopt the way of silk screen printing; 400～600 ℃ of following sintering 2～5 hours, sintering got final product in air; Use the sintering zone on sulfuric acid cleaned diamond thick-film surface at last.
Wherein sintering time is decided according to the planeness of diamond thick-film.Notice that etch rate of the present invention was approximately about 3 μ m/ hours.Be also noted that sintering temperature can not surpass 600 ℃ to avoid diamond thick-film oxidized in air.
The compound method of aforesaid rare-earth compound pulp is, the oxide compound of raw material cerium and lanthanum or salt pressed mass ratio mix, and adds ethanol or/and ethyl acetate solvent through grinding, adds blender furnishing congee shape again.
The effect that adds solvent is to help grinding.Final these solvents will vapor away in air, so have only rare earth compound and blender in the composition of slurry.The effect of blender is the viscosity of regulating slurry, to being fit to printing.
The sulfuric acid (being the vitriol oil) of 98% concentration is preferably used in said cleaning.Mainly be that rare earth compound to the sintering zone cleans, be beneficial to next step mechanical polishing.
The preparation of embodiment 1, rare-earth compound pulp.
Get commercially pure CeO
2And La (NO
3)
3.6H
2Each 10 gram of O, an amount of dehydrated alcohol is a solvent, mixed grinding 5～6 hours.The most of volatilization of solvent back adds the dim acid of 2 gram lemons, ten several Terpineol 350s and 1 gram ethyl cellulose, is in harmonious proportion the back to become rare-earth compound pulp.
The preparation of embodiment 2, rare-earth compound pulp.
Get CeO
2, La (NO
3)
3.6H
2O is respectively 10 grams and 4 grams, and adequate amount of ethanol and ethyl acetate are solvent, mixed grinding 6～7 hours.The most of volatilization of solvent back adds 1.8 gram citric acids, ten several Terpineol 350s, 0.5 gram ethyl cellulose, is in harmonious proportion the back to become the rare earth oxide slurry.
The surface sculpture method of embodiment 3, diamond thick-film.
Select the rare-earth compound pulp of embodiment 1 for use, be coated in silk screen printing on the aufwuchsplate of diamond thick-film, the about 10 μ m of thickness are heated to 460 ℃ ± 10 ℃ insulations 3 hours in box High Temperature Furnaces Heating Apparatus, after the vitriol oil cleans, examine under a microscope the equal etching of crystal grain of CVD diamond thick-film aufwuchsplate, it is smooth that crystal grain becomes, and whole attenuate is about 6 μ m.
Embodiment 4, the surface sculpture method of diamond thick-film.
Select the rare-earth compound pulp of embodiment 1 for use, etching process is also with embodiment 3, and just the temperature of heating is 550 ± 10 ℃, and the time is 4 hours.After the vitriol oil cleans, examine under a microscope that crystal grain etching on the CVD diamond thick-film aufwuchsplate is heavier, thick film surface is smooth.The about 9 μ m of integral body degree of subtracting.
Embodiment 5, the surface sculpture method of diamond thick-film.
Use the rare earth oxide slurry of embodiment 2, with embodiment 3 identical sintering conditions under effect also identical.
Embodiment 6, the surface etch of diamond thick-film.
Etching process is with embodiment 3, and 550 ± 10 ℃ of Heating temperatures are incubated 18 hours.The result is that the diamond thick-film surface etch is serious, and the relatively poor position of local grain is etching all.
Adopt rare-earth compound pulp of the present invention and to the lithographic method of diamond thick-film, the slurry preparation easily, the few raw material of consumption is cheap; Etching technics is simple, and it is low that sintering condition requires, and economized vacuum high-temperature equipment, and etching effect is good, and cost is low, and easy cleaning can reduce time of mechanical polishing.Silk screen printing can also be carried out graphical etching.These all help the application of CVD diamond thick-film in Electronic Packaging neck city.
Claims (4)
1. rare-earth compound pulp that is used for the diamond thick-film surface etch, it is characterized in that, its composition comprises that the oxide compound of cerium and lanthanum or the mass ratio of the compound that salt is raw material, cerium, lanthanum are 1: (1-0.3), Terpineol 350, citric acid and ethyl cellulose or their mixture are that blender mixes.
2. according to the described rare-earth compound pulp of claim 1, it is characterized in that the oxide compound of said cerium, lanthanum or salt are CeO
2And La (NO3)
3.6H
2O.
3. the method for a diamond thick-film surface etch is characterized in that, rare-earth compound pulp is printed on the diamond thick-film aufwuchsplate; 400～600 ℃ of following sintering 2～5 hours; Use the sintering zone on sulfuric acid cleaned diamond thick-film surface at last.
4. according to the method for the described diamond thick-film surface etch of claim 3, it is characterized in that said rare-earth compound pulp, be that oxide compound or salt with raw material cerium and lanthanum mixes by mass ratio, add ethanol or/and ethyl acetate solvent through grinding, adds blender furnishing congee shape again; Said sulfuric acid cleaned is to use the sulfuric acid cleaned of concentration 98%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99124562A CN1087040C (en) | 1999-12-10 | 1999-12-10 | Rare-earth compound pulp and surface sculpture method for diamond thick-film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99124562A CN1087040C (en) | 1999-12-10 | 1999-12-10 | Rare-earth compound pulp and surface sculpture method for diamond thick-film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1258765A true CN1258765A (en) | 2000-07-05 |
| CN1087040C CN1087040C (en) | 2002-07-03 |
Family
ID=5283476
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99124562A Expired - Fee Related CN1087040C (en) | 1999-12-10 | 1999-12-10 | Rare-earth compound pulp and surface sculpture method for diamond thick-film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1087040C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109652977A (en) * | 2018-12-07 | 2019-04-19 | 苏州大学 | A kind of resistance to ultraviolet aramid fiber of flame retardant type |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5328550A (en) * | 1992-10-02 | 1994-07-12 | At&T Bell Laboratories | Thinning a diamond body by means of molten rare-earth-containing alloys |
-
1999
- 1999-12-10 CN CN99124562A patent/CN1087040C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109652977A (en) * | 2018-12-07 | 2019-04-19 | 苏州大学 | A kind of resistance to ultraviolet aramid fiber of flame retardant type |
| CN109652977B (en) * | 2018-12-07 | 2021-05-25 | 苏州大学 | Flame-retardant ultraviolet-resistant aramid fiber |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1087040C (en) | 2002-07-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Toyoda et al. | Synthesis and characterization of Bi4Ti3O12 thin films by sol-gel processing | |
| CN1208495C (en) | Sputtering target and its preparing method | |
| JPH07233469A (en) | Target, its production and production of high-refractive-index film | |
| FR2585015A1 (en) | CERAMIC POWDER OF FRITTABLE CORDIERITY TYPE AT LOW TEMPERATURE, PROCESS FOR PREPARATION AND CERAMIC COMPOSITION OBTAINED BY FRITTING THE POWDER | |
| CA2216457C (en) | Nickel powder and process for preparing the same | |
| CN1087040C (en) | Rare-earth compound pulp and surface sculpture method for diamond thick-film | |
| JPH09249967A (en) | High purity barium-strontium titanate sputtering target material and its production | |
| US4162921A (en) | Glass-crystalline material and method of producing same | |
| JP2008057045A (en) | Oxide sintered compact sputtering target | |
| JPH11135234A (en) | Aluminum nitride heater | |
| JP2585595B2 (en) | Manufacturing method of ceramic sintered body | |
| JP2590255B2 (en) | Copper material with good bondability with ceramics | |
| CN1042698A (en) | Low-temp ceramics over-glaze pigment and preparation method thereof | |
| JP3697277B2 (en) | Ceramic substrate and manufacturing method thereof | |
| KR100200409B1 (en) | Indium-tin-oxide component and process for its production | |
| JP3279450B2 (en) | Grain-oriented electrical steel sheet with insulating coating formed on the surface | |
| KR20200055513A (en) | Cordirerite containing low temperature induction dielectric ceramics and the manufacturing method theref | |
| CN108341661A (en) | Low-friction coefficient coffee color alumina ceramic material | |
| JPS63239150A (en) | Production of superconductive ceramic thin film | |
| JPH03146471A (en) | Production of aluminum nitride sintered body | |
| JPH05330919A (en) | Silicon nitride-based sintered compact and its production | |
| JPH01317164A (en) | Ceramic composition | |
| JPH04280694A (en) | Ceramic board and manufacture thereof | |
| JPH09124382A (en) | Production of ceramic substrate | |
| CN117105672A (en) | Preparation method of molybdenum disilicide target |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |