CN111303773A - Inorganic high-temperature patch adhesive material and preparation method thereof - Google Patents
Inorganic high-temperature patch adhesive material and preparation method thereof Download PDFInfo
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- CN111303773A CN111303773A CN201911258512.7A CN201911258512A CN111303773A CN 111303773 A CN111303773 A CN 111303773A CN 201911258512 A CN201911258512 A CN 201911258512A CN 111303773 A CN111303773 A CN 111303773A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J1/00—Adhesives based on inorganic constituents
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
- G01B7/18—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge using change in resistance
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- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Materials For Medical Uses (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses an inorganic high-temperature patch adhesive material and a preparation method thereof, wherein the raw material components comprise, by mass, 40-72 parts of phosphate, 2-6 parts of curing agent, 9-26 parts of acid inhibitor and 4-20 parts of water. Mixing the raw materials in parts by weight to form jelly. The adhesive tape can not influence the precision of a high-temperature resistance strain gauge in the environment with the high temperature of 900 ℃.
Description
Technical Field
The invention belongs to the field of adhesives, and relates to an inorganic high-temperature surface-mounted adhesive material and a preparation method thereof.
Background
The high-temperature resistance strain gauge is made by using a resistance-strain effect, and can convert the mechanical deformation of a tested piece into a sensitive element with resistance change, namely a sensitive chip which senses stress strain by the change of the resistance value of the high-temperature resistance strain gauge adhered on the tested piece caused by the deformation of the tested piece. The inorganic high-temperature adhesive glue is a strain transmission layer for bearing the high-temperature resistance strain gauge and the tested piece.
In recent years, health detection in a high-temperature environment is forcibly required, the demand of high-temperature stress-strain measurement at the temperature of over 900 ℃ is increased in military and civil industries, the domestic high-temperature stress-strain measurement is limited by inorganic high-temperature patch glue at present, only 750 ℃ high-temperature test can be carried out, and the successful development of the 900 ℃ inorganic high-temperature patch glue has great significance for the high-temperature test of aerospace engines in China.
For the strain test in the high-temperature environment, the high-temperature environment mainly affects the following properties of the high-temperature adhesive:
1. with the rapid change of the temperature, the high-temperature heat output is increased, generally to about +/-2000 mu epsilon, and the measurement precision is influenced.
2. Under a high-temperature field, the relative sensitivity coefficient and creep of the strain gauge generate step change, so that the discreteness of the measurement result is increased.
3. At high temperature, the insulation strength of the inorganic high-temperature adhesive is reduced, so that the measurement signal of the strain gauge is unstable.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an inorganic high-temperature adhesive tape material and a preparation method thereof, wherein the adhesive tape material does not influence the precision of a high-temperature resistance strain gauge in a high-temperature environment of 900 ℃.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
an inorganic high-temperature adhesive plaster material comprises, by mass, 40-72 parts of phosphate, 2-6 parts of a curing agent, 9-26 parts of an acid inhibitor and 4-20 parts of water.
Preferably, the phosphate is magnesium dihydrogen phosphate, aluminum dihydrogen phosphate or sodium dihydrogen phosphate.
Preferably, the curing agent is magnesium oxide and/or zinc oxide.
Preferably, the acid inhibitor is any one or more of chromium oxide, chromium trioxide, and a mixture of silicon dioxide and zirconium dioxide.
According to the preparation method of any one of the inorganic high-temperature adhesive plaster materials, 40-72 parts by weight of phosphate, 2-6 parts by weight of curing agent, 9-26 parts by weight of acid inhibitor and 4-20 parts by weight of water are mixed to form a jelly.
Preferably, the phosphate is dehydrated to form a polymeric phosphate containing multiple phosphorus atoms prior to mixing; and carrying out polycondensation reaction on the obtained polymeric phosphate to obtain chain-shaped polymetaphosphoric acid.
Preferably, the acidic inhibitor is subjected to a high temperature treatment of 400 to 700 ℃ until it is dehydrated before mixing.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, phosphate gel is selected, phosphate ions are contained in phosphate, and the phosphate ions exist in a tetrahedral structure form, the structure endows phosphate with very stable chemical property and high temperature resistance after solidification, chain-shaped polymetaphosphoric acid with higher polymerization degree improves the high temperature resistance of the patch adhesive material, and in a high temperature environment, the high temperature heat output of the patch adhesive material cannot be increased too much, the insulation strength cannot be reduced, and various performances in the high temperature environment are improved.
Drawings
FIG. 1 is a reaction equation of phosphate;
FIG. 2 shows the molecular formula of a chain polymetaphosphate;
FIG. 3 is a plot of GH975 alloy test versus K for samples;
FIG. 4 is a graph of the heat output of the sample at GH975 alloy.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings:
the invention relates to an inorganic high-temperature patch adhesive material and a preparation method thereof; the raw material components of the high-temperature paster adhesive are packaged according to parts by massComprises 40 to 72 parts of phosphate, 1 to 6 parts of curing agent, 3 to 20 parts of acid inhibitor and 4 to 20 parts of water, wherein the phosphate [ X (H)2PO4)n]Belongs to a gelled material, can be used together with a plurality of inorganic oxides, and selects phosphate [ X (H) according to the invention2PO4)n]In particular magnesium dihydrogen phosphate [ Mg (H)2PO4)2]Aluminum dihydrogen phosphate [ Al (H) ]2PO4)3]Or sodium dihydrogen phosphate [ NaH ]2PO4](ii) a The selected curing agent must have a certain reactivity with phosphate, but the reactivity cannot be too high, the curing agent is preferably amphoteric or alkalescent oxide generally, and the strong alkaline oxidation requires high-temperature calcination treatment]And/or zinc oxide [ ZnO ]](ii) a The invention selects the acid inhibitor as chromium oxide [ Cr ]2O3]Chromium trioxide [ CrO ]3]Silicon dioxide [ SiO ]2]And zirconium dioxide [ ZrO ]2]Any one or more of the above materials.
The reaction mechanism is described as follows:
selection of phosphate [ X (H)2PO4)n]It can be used together with many inorganic oxides, and after high-temp. treatment, it can be converted into gelled substance with high hardness and good adhesion. The phosphate solution loses free water molecules through high-temperature heating, becomes a viscous substance with high dilution rate, and generates a white hard ceramic-like substance which has no hygroscopicity and is insoluble in water after high-temperature curing. The reaction mechanism is as follows:
the phosphate contains three phosphate ions: PO (PO)4 3-、HPO4 2-、H2PO4 -Phosphate ions all exist in a tetrahedral structure, and the structure endows phosphate with very stable chemical property and high temperature resistance after being cured. As shown in fig. 1 and 2, the phosphate is dehydrated at a high temperature to generate a polymeric phosphate containing a plurality of phosphorus atoms, and at a high temperature, a cyclic trimetaphosphate is generated, and the temperature is further increased to finally be condensed into a chain-like polymetaphosphate having a higher degree of polymerization.
As a result of the above reaction, an inorganic polyphosphate polymer compound is formed.
Phosphate is an acid salt, and an aqueous solution is acidic and has a corrosive effect on metals. The high-temperature strain gauge is slightly corrosive to sensitive grids, and in order to further reduce the corrosion, a proper amount of an acid inhibitor is required to be added, wherein the acid inhibitor is selected from any one or a mixture of more of chromium sesquioxide, chromium trioxide, silicon dioxide and zirconium dioxide.
Example 1
Preparing inorganic high-temp adhesive from zirconium dioxide (ZrO)2]And chromium trioxide [ CrO ]3]Carrying out high-temperature treatment at 550 ℃ until the moisture is removed; then, 65 parts by mass of magnesium dihydrogen phosphate [ Mg (H) ]2PO4)2]6 parts of zinc oxide [ ZnO ]]11.5 parts of zirconium dioxide [ ZrO ]2]1 part of chromium trioxide [ CrO ]3]And 17.5 parts water to form a gum.
Example 2
Preparing inorganic high-temp adhesive from zirconium dioxide (ZrO)2]And chromium trioxide [ CrO ]3]Carrying out high-temperature treatment at 400 ℃ until the moisture is removed; 70 parts of magnesium dihydrogen phosphate [ Mg (H) ] by mass2PO4)2]4.5 parts of zinc oxide [ ZnO ]]15 parts of zirconium dioxide [ ZrO ]2]1.5 parts of chromium trioxide CrO3]And 15 parts water to form a gum.
Example 3
Preparing inorganic high-temp adhesive from zirconium dioxide (ZrO)2]And chromium trioxide [ CrO ]3]High-temperature treatment at 700 ℃ is carried out until the moisture is removed; then 60 parts of magnesium dihydrogen phosphate [ Mg (H) ] is added according to the mass part2PO4)2]3 parts of zinc oxide [ ZnO ]]8 parts of zirconium dioxide [ ZrO ]2]2 parts of chromium trioxide CrO3]And 20 parts water to form a gum.
Example 4
Preparing inorganic high-temperature adhesive, and mixing chromium oxide (Cr)2O3]Chromium trioxide [ CrO ]3]And silica [ SiO ]2]High-temperature treatment at 700 ℃ is carried out until the moisture is removed; then 72 parts of aluminium dihydrogen phosphate [ Al (H) ] is added according to the mass part2PO4)3]3 parts of magnesium oxide [ MgO]3 portions of chromium sesquioxide [ Cr ]2O3]1 part of chromium trioxide [ CrO ]3]15 parts of silicon dioxide SiO2]And 11.5 parts water to form a gum.
Example 5
Preparing inorganic high-temperature adhesive, and mixing chromium oxide (Cr)2O3]Chromium trioxide [ CrO ]3]And silica [ SiO ]2]Carrying out high-temperature treatment at 550 ℃ until the moisture is removed; 50 parts of aluminum dihydrogen phosphate [ Al (H) ] by mass2PO4)3]4 parts of magnesium oxide [ MgO]1 part of chromium sesquioxide [ Cr ]2O3]0.6 part of chromium trioxide CrO3]20 parts of silicon dioxide SiO2]And 15 parts water to form a gum.
Example 6
Preparing inorganic high-temperature adhesive, and mixing chromium oxide (Cr)2O3]Chromium trioxide [ CrO ]3]And silica [ SiO ]2]Carrying out high-temperature treatment at 400 ℃ until the moisture is removed; then 61 parts of aluminium dihydrogen phosphate [ Al (H) ] by mass part2PO4)3]2 parts of magnesium oxide [ MgO]5 portions of chromium sesquioxide [ Cr ]2O3]0.2 part of chromium trioxide CrO3]3.8 parts of silicon dioxide SiO2]And 8 parts water to form a gum.
Example 7
Preparing inorganic high-temperature adhesive, and mixing chromium oxide (Cr)2O3]Silicon dioxide [ SiO ]2]And zirconium dioxide [ ZrO ]2]Carrying out high-temperature treatment at 400 ℃ until the moisture is removed; then 40 parts of sodium dihydrogen phosphate [ NaH ] are added according to the mass part2PO4]2 parts of magnesium oxide [ MgO]2 parts of zinc oxide (ZnO)]8 portions of chromium sesquioxide [ Cr ]2O3]9 parts of silicon dioxide SiO2]9 parts of zirconium dioxide [ ZrO ]2]And 8 parts water to form a gum.
Example 8
Preparing inorganic high-temperature adhesive, and mixing chromium oxide (Cr)2O3]Silicon dioxide [ SiO ]2]And zirconium dioxide [ ZrO ]2]Carrying out high-temperature treatment at 550 ℃ until the moisture is removed; then 65 parts of sodium dihydrogen phosphate [ NaH ] are added according to the mass part2PO4]1 part of magnesium oxide [ MgO]1 part of zinc oxide (ZnO)]3 portions of chromium sesquioxide [ Cr ]2O3]7 parts of silicon dioxide SiO2]7 parts of zirconium dioxide [ ZrO ]2]And 6 parts water to form a gum.
Example 9
Preparing inorganic high-temperature adhesive, and mixing chromium oxide (Cr)2O3]Silicon dioxide [ SiO ]2]And zirconium dioxide [ ZrO ]2]High-temperature treatment at 700 ℃ is carried out until the moisture is removed; then 52.5 parts of sodium dihydrogen phosphate [ NaH ] are added according to the mass part2PO4]3 parts of magnesium oxide [ MgO]1.5 parts of zinc oxide (ZnO)]5.5 parts of chromium sesquioxide [ Cr ]2O3]5 parts of silicon dioxide SiO2]3 parts of zirconium dioxide [ ZrO ]2]And 4 parts water to form a gum.
The product samples from examples 1-4 were tested for load stability at various temperatures, as shown in Table 1 and FIG. 3, for sample alloy testing versus the K test, with a 1000 + -50 μ ε load on a GH975 standard test beam.
TABLE 1
In table 1, each sample is divided into an upper column and a lower column at each temperature, the upper column is a strain value of the sample calibrated by loading a K value at each temperature, the lower column is a relative ratio K of the strain value of the sample at each temperature and the strain value of the sample at 200 ℃, as can be seen from table 1, the K value of the sample at 900 ℃ is more than 80%, the change degree of the strain is small, and the strain of the product cannot be too large when the product meets the condition of 900 ℃.
Product heat output repeatability tests were performed at various temperatures on product samples from examples 1-4, as shown in table 2 and fig. 4, for samples tested on GH975 alloy heat output, and on GH975 standard heat output test beam surfaces tested at 900 ℃ heat output dispersion of 49.7 μ ∈.
TABLE 2
| Temperature of | 20℃ | 200℃ | 300℃ | 400℃ | 600℃ | 800℃ | 900℃ |
| Sample 1 | -1 | -463 | 1341 | 3107 | 9045 | 15938 | 17931 |
| Sample 2 | 0 | -500 | 1400 | 3300 | 8905 | 14887 | 17893 |
| Sample 3 | -3 | -488 | 1544 | 3122 | 9021 | 15673 | 18001 |
| Sample 4 | 2 | -502 | 1345 | 2989 | 9213 | 16022 | 17985 |
As can be seen from Table 2, the thermal output strain value of each sample at the same temperature is the strain value of the sample at each temperature, the error is small, the thermal output strain value is kept in a certain interval, and the sensitivity coefficient and the creep deformation cannot be changed too much.
The product samples obtained in example 1 were subjected to insulation strength tests at various temperatures as shown in table 3.
TABLE 3
As can be seen from Table 3, the adhesive layer formed by curing the surface mount adhesive at high temperature has an insulation strength of 80M omega after heat preservation for 1 hour at 900 ℃, which is much higher than 2M omega of common inorganic high-temperature adhesive, and ensures the stability of high-temperature test data at 900 ℃.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (7)
1. The inorganic high-temperature adhesive plaster material is characterized by comprising, by mass, 40-72 parts of phosphate, 2-6 parts of a curing agent, 9-26 parts of an acid inhibitor and 4-20 parts of water.
2. The inorganic high-temperature patch adhesive material as claimed in claim 1, wherein the phosphate is magnesium dihydrogen phosphate, aluminum dihydrogen phosphate or sodium dihydrogen phosphate.
3. The inorganic high-temperature patch adhesive material as claimed in claim 1, wherein the curing agent is magnesium oxide and/or zinc oxide.
4. The inorganic high-temperature patch gel material as claimed in claim 1, wherein the acidic inhibitor is a mixture of one or more of chromium oxide, chromium trioxide, silicon dioxide and zirconium dioxide.
5. The method for preparing an inorganic high-temperature patch material according to any one of claims 1 to 4, wherein 40 to 72 parts by mass of phosphate, 2 to 6 parts by mass of curing agent, 9 to 26 parts by mass of acid inhibitor and 4 to 20 parts by mass of water are mixed to form a gel.
6. The method for preparing an inorganic high-temperature patch adhesive material according to claim 5, wherein the phosphate is dehydrated to generate a polymeric phosphate containing multiple phosphorus atoms before mixing; and carrying out polycondensation reaction on the obtained polymeric phosphate to obtain chain-shaped polymetaphosphoric acid.
7. The method for preparing an inorganic high-temperature patch adhesive material according to claim 5, wherein the acidic inhibitor is subjected to a high temperature treatment of 400 to 700 ℃ until it is dehydrated before mixing.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85100057A (en) * | 1985-04-01 | 1986-07-23 | 清华大学 | High-temperature strain sustainable adhesive |
| CN103134417A (en) * | 2011-11-24 | 2013-06-05 | 中国航空工业集团公司沈阳发动机设计研究所 | High-temperature dynamic strain meter |
| CN103615967A (en) * | 2013-11-30 | 2014-03-05 | 中航电测仪器股份有限公司 | High-temperature foil strain gauge and method for manufacturing high-temperature foil strain gauge |
-
2019
- 2019-12-10 CN CN201911258512.7A patent/CN111303773A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85100057A (en) * | 1985-04-01 | 1986-07-23 | 清华大学 | High-temperature strain sustainable adhesive |
| CN103134417A (en) * | 2011-11-24 | 2013-06-05 | 中国航空工业集团公司沈阳发动机设计研究所 | High-temperature dynamic strain meter |
| CN103615967A (en) * | 2013-11-30 | 2014-03-05 | 中航电测仪器股份有限公司 | High-temperature foil strain gauge and method for manufacturing high-temperature foil strain gauge |
Non-Patent Citations (1)
| Title |
|---|
| 李红强 主编: "《胶粘原理、技术及应用》", 31 January 2014, 华南理工大学出版社 * |
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